The Laboratory Quality Assurance System: A Manual of Quality Procedures and Forms

THE LABOATORY

QUALITY' ASSURANCE SYSTEM Third Edition

THE LABOMTORY QUALITY ASSURANCE SYSTEM Third Edition

A Manual of Quality Procedures and Forms Thomas A. Ratliff

WILEYINTERSCI ENCE A JOHN WILEY & SONS PUBLICATION

Copyright 0 2003 by John Wiley & Sons, Inc. All rights reserved. Published by John Wiley & Sons, Inc., Hoboken, New Jersey. Published simultaneously in Canada. No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning, or otherwise, except as permitted under Section 107 or 108 of the 1976 United States Copyright Act, without either the prior written permission of the Publisher, or authorization through payment of the appropriate per-copy fee to the Copyright Clearance Center, Inc., 222 Resewood Drive, Danvers, MA 01923,978-750-8400, fax 978-750-4470, or on the web at www.copyright.com. Requests to the Publisher for permission should be addressed to the Permissions Department, John Wiley & Sons, Inc., 111 River Street, Hoboken, NJ 07030, (201) 748-601 1, fax (201) 748-6008, e-mail: [email protected]. Limit of Liability/Disclaimer of Warranty: While the publisher and author have used their best efforts in preparing this book, they make no representations or warranties with respect to the accuracy or completeness of the contents of this book and specifically disclaim any implied warranties of merchantability or fitness for a particular purpose. No warranty may be created or extended by sales representatives or written sales materials. The advice and strategies contained herein may not be suitable for your situation. You should consult with a professional where appropriate. Neither the publisher nor author shall be liable for any loss of profit or any other commercial damages, including but not limited to special, incidental, consequential, or other damages.

For general information on our other products and services please contact our Customer Care Department within the U.S. at 877-762-2974, outside the U.S. at 317-572-3993 or fax 317-572-4002. Wiley also publishes its books in a variety of electronics formats. Some content that appears in print, however, may not be available in electronic format.

Library of Congress Cataloging-in-Publication Data: Ratliff, Thomas A. The laboratory quality assurance system : a manual of quality procedures and forms /Thomas A. Ratliff.-3rd ed. p. cm. Includes bibliographical references and index. ISBN 0-471-26918-2 (cloth) 1. Testing laboratories-Quality control-Handbooks, manuals, etc. I. Title. TA416 .R37 2003 602.8’74~21 2002070206 Printed in the United States of America. 10 9 8 7 6 5 4 3 2

1

Contents Preface / vii

Section 27 Measurement, Analysis, and Improvement of the Quality System / 20 Section 28 Statistical Methods / 21 Section 29 Subcontracting Services and Supplies / 24 Section 30 Quality Audits / 24 Section 3 1 Nonconformity / 25 Section 32 Customer Satisfaction and Complaints / 26 Section 33 Corrective and Preventive Action / 27 Section 34 Method Validation / 28 Section 35 Reliability / 28 Section 36 Quality Cost Reporting / 3 1

PART 1: LABORATORY QUALITY SYSTEM ELEMENTS / 1 Section Section Section Section Section Section Section

1 2 3 4 5 6 7

Section 8 Section 9 Section 10 Section 11 Section 12 Section 13 Section 14 Section 15 Section 16 Section 17 Section 18 Section 19 Section 20 Section 21 Section 22 Section 23 Section 24 Section 25 Section 26

Introduction / 1 Title Page / 1 Letter of Promulgation / 1 Quality Policies / 1 Quality Objectives / 2 Management of the Quality Manual / 2 Control of Quality Documentation and Records / 2 Customer Focus / 4 Quality System Planning / 4 Organization for Quality / 5 Communications / 6 Management Review / 6 Human Resources / 6 Laboratory Infrastructure / 8 Work Environment / 8 Quality in Procurement / 8 Sample Handling, Identification, Storage, and Shipping / 9 Chain-of-Custody Procedures / 10 Laboratory Testing and Control: Intraand Interlaboratory Proficiency Testing / 11 Design and Development (Excluded) / 14 Customer Property (Excluded) / 14 Control of Measuring and Test Equipment / 14 Preventive Maintenance / 17 Estimate of Uncertainty of Measurement / 18 Reference Standards and Standard Reference Materials / 18 Data Validation / 19

PART 2: HOW TO WRITE A LABORATORY QUALITY ASSURANCE MANUAL / 33 Section 37 Introduction / 33 Section 38 Organizing for Preparation of the Manual / 33 Section 39 Establishing Objectives and Priorities / 33 Section 40 Collection and Review of Existing Procedures / 34 Section 41 Preparation of a Flowchart / 34 Section 42 Identification of Program Requirements / 36 Section 43 Identification of Shortfalls and the Assignment of Priorities / 36 Section 44 Writing the Manual / 36

PART 3: XYZ LABORATORY QUALITY ASSURANCE MANUAL / 37 PART 4: SAMPLE QUALITY ASSURANCE FORMS / 181 Index / 235

V

Preface The purpose of this book is to provide the user with the means to create a quality assurance manual which will satisfy the needs of his or her particular laboratory while meeting the requirements of any regulatory or accrediting body with which the organization may be associated. This third edition has been prepared to assist laboratories seeking accreditation in the preparation of the quality assurance/control manual as required by American National Standard ANSI/ISO/ASQ 49001-2000, Quality management Systems-Requirements, and/or American National Standard ANSUISO 170251999, General requirementsfor the competence of testing and calibration laboratories. New material has been added to cover increased requirements for expanding customer relationships, continual improvement, and other areas as set forth in ANSI/ISO/ASQ 9000-2000. Procedures are suggested to meet these requirements, and blank forms are provided to be used to record results of these activities. The book seeks to achieve the goal of providing an easy-to-use, step-by-step explanation of the preparation of a manual by discussing in detail the elements of laboratory quality systems required by the standards referenced above, describing the mechanics of creating a manual, providing an example of a laboratory quality manual complete with sample forms and instructions for their use, and, finally, providing blank copies of all forms referenced in Part 3. These blank forms may be reproduced, copied, or edited to meet the needs of a particular laboratory. Although many of the examples and references included herein relate to industrial hygiene laboratories, the principles set forth herein are applicable to any testing, analytical, or other laboratory, excluding those dedicated purely to research and development.

vii

Laboratory Quality Assurance System, 3rd Edition. Thomas A. Ratliff Copyright 02003 John Wiley & Sons, Tnc. 4SBN: 0-471-26918-2

Part 1

LABORATORY QUALITY SYSTEM ELEMENTS SECTION 1 INTRODUCTION

to, and support for the laboratory’s quality program. It should also stress the importance of individual responsibility for conduct which enhances and does not endanger the quality of laboratory performance. Lastly, it should emphasize the fact that the policies and procedures published in the manual are binding on each individual and are the authority as well as the requirement for the conduct of the laboratory’s work.

The laboratory may wish to include an Introduction to its quality manual to explain its purpose and how and to whom it is to be distributed. The Introduction may also be used to explain the background authority or standard on which the document is based and how the manual may differ from such a reference if there is any significant deviation from the authority or standard.

SECTION 4 QUALITY POLICIES

SECTION 2 TITLE PAGE

Quality policies are established by management to provide guidance to the organization on the pathway to continuous improvement of its quality performance, meet regulatory or accreditation requirements, or, in the case of larger organizations, to agree with previously established policies mandated by a higher authority within the company. Quality policies may cover such matters as:

The title page of the manual should contain the following information:

@

The name and address of the issuing organization. If the laboratory is a subordinate part of a larger company or organization, the parent body should be identified, together with its address. The name and title of the responsible Quality Control Coordinator or Manager of the laboratory. The name and title of the Laboratory Director, Chief Executive Officer, President of the Corporation, or other individual bearing the ultimate responsibility for the quality of the laboratory output. The date of issue. If the distribution of the quality manual is controlled, the copy number of the manual should be indicated on the title page.

Quality training. Publication, distribution, and retention of current or obsolete documents such as methods, specifications, calibration procedures, instrument operating instructions, and so on. Provide for the assurance of good quality, fresh reagents and chemicals, and appropriate calibrated glassware. Participation in interlaboratory quality evaluationprograms. Determination to reduce the costs of correction and evaluation by increasing preventive measures.

SECTION 3 LETTER OF PROMULGATION If the laboratory desiresto issue the quality manual under the cover of a Letter of Promulgation, this letter should be written by and signed by the same person who signed off on the title page (i.e., the Laboratory Director, Chief Executive Officer, or Corporate President). The Letter of Promulgation serves to demonstrate and emphasize management’s interest in, commitment

These are but a few examples of the kinds of policies that may be established by management in response to requirements generated by the considerations put forth above. Quality policies should be issued by the highest authority available within the laboratory. They should attest to management’s concern about and commitment

1

satisfaction, or performance of internal audits, among others.

to the maintenance of a high level of quality in the laboratory’s work.

SECTION 5 QUALITY OBJECTIVES

References

It is the responsibility of the laboratory’s management to identify and state, in writing, what the quality goals of the laboratory are to be. The primary objective of a laboratory’s quality system is to improve and maintain at a high level the precision and accuracy of the laboratory’s “product.” Here, the laboratory’s product can be defined as “the report issued as the result of analytical, measurement, or testing activity conducted on a sample or samples received from some source.” Management, administrative, statistical, investigative, preventive, and corrective techniques are among those which may be used to maximize the quality of the reported data. Secondary objectives which may be established to reach primary goals might be:

July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and

Health. Juran, J. M. 1988.Juran’s Quality Control Handbook. 4th Ed. New York: McGraw-Hill Book Company.

SECTION 6 MANAGEMENT OF THE QUALITY MANUAL Although the laboratory’s description of its quality system may be contained in more than one document, the usual format, and the one required by Paragraph 4.2.2 of ANSI/ISO/ASQ Q9001-2000, is the quality manual. The principle use of the manual is to present, in one document, the laboratory’s policies and procedures which relate to the control of the quality of the laboratory’s output. The manual should:

To establish the level of the laboratory’s routine performance. To make any changes in the routine methodology found necessary to make it supportive of the management policy regarding reduction of costs associated with corrective action and evaluation. To set forth objectives associated with achieving management’s mandate to assure continuous improvement of quality performance. To establish program goals for the laboratory’s quality and technology training efforts.

Include a Table of Contents. Assign the responsibility for publishing and distributing the manual and keeping its contents current and upto-date and describe the procedures for recommending and making changes. Prescribe the format for paragraphing and maintain the same format throughout the document. Include copies of any reports, forms, tags, or labels to be used by the procedures described in the text of the manual.

Quality objectives should be quantified insofar as possible by establishing target dates for completion or by raising or lowering a numerical value to a higher or lower level established as a goal. Quality objectives should be attainable. If they are not, they lose effect as a management tool since they will lead to frustration and a resulting lack of cooperation and enthusiasm among those charged with the responsibility for reaching established goals. Quality objectives should be clearly defined and so stated that all concerned understand management’s exact intentions with regard to the goals to be reached. Vaguely defined programs, or those not completely understood, are doomed to failure, especially if they are not vigorously supported by management and backed up by adequate follow-up and supervision. Above all, quality objectives must support established policies. The examples of objectives given above are by no means a complete list of quality objectives that might be selected by an individual laboratory. Quality objectives should be based on the particular laboratory’s policies, priorities, and field of interest, results of audits, or requirements of regulatory or accrediting bodies. Other subjects appropriate for selection as quality goals might have to do with quality costs, dealing with customer

If the distribution of the manual is controlled, then each copy should be numbered and a distribution list maintained showing to whom each numbered document has been issued. Unnumbered copies may be distributed on an uncontrolled basis to potential customers, auditors, trainees, and the like.

SECTION 7 CONTROL OF QUALITY DOCUMENTATION AND RECORDS The laboratory quality assurance system program will include provisions for maintaining necessary records and reports and for updating and controlling the issuance of technical documents and operating procedures.

DOCUMENT CONTROL The important elements of the quality assurance system to which document control should be applied include: 1. Sampling procedures 2. Calibration procedures

2

3. 4. 5. 6.

Analytical and test methods Data collection and reporting procedures Auditing procedures and checklists Sample shipping, packaging, receiving, and storage procedures 7. Computation and data validation procedures 8. Quality assurance manuals 9. Quality plans 10. Sampling data sheets 11. Specifications

responsible for their preparation, distribution, and maintenance; the format in which they are published and maintained; the distribution list; and the retention period. Such records include: Test and analytical results Reports on the results of data validation Internal and external quality audits Instrument and gauge record cards Quality cost reports Laboratory notebooks Chain-of-custody records for samples

Each laboratory must maintain full control over the distribution and possession of such documents. A file control should be established showing the following minimum information:

While being stored for specified or required retention periods, documents should be protected from damage, tampering, loss, or degradation due to atmospheric conditions.

Document number Title Source of the document Latest issue date Change number List of addressees

LABORATORY NOTEBOOKS The laboratory notebook is the primary source for documentation of the individual analyst’s, test engineer’s, or technician’s activities. Laboratory notebooks are used for recording all experimental, testing, and analytical notes and data. The issue of notebooks should be controlled by assignment of a serial number for each book. Notebooks are issued to individuals and the serial number entered in a serial number issue log. The serial number is placed on the cover of each notebook together with the recipient’s name and the date issued. Upon completion, the notebook is returned for filing and the completion date noted on the cover. Notebooks are hardcovered and bound. Notebooks with removable pages (e.g., looseleaf notebooks) are not considered by many to be acceptable for use in the laboratory. All entries should be made in ink. The pages should be numbered and dated, and any entries made by an individual other than the person to whom the book was issued should be noted. These notebooks are considered to be the property of the laboratory and are retained as a part of the laboratory’s files. The notebook should contain all the information gathered by the analyst or test technician pertaining to the sample, including method response (raw data) for each sample. Where appropriate, the laboratory number, field number, sequence number, or other identifying numbers should be noted. The specific analysis or test requested, identification of the method, if known, modifications to the method, and the sample source should also be included. A description of the sample, in as much detail as possible, should also be included. Data such as blank values, recovery studies, or duplicate determinations should also be included. Formulas and equations used to calculate results and all calculations should be shown. The minimum data and description entered in the notebook should be sufficient to enable another test

Whenever a change is made, the responsible organization should issue the new, changed document together with the change notice (see Fig. 12-1, Part 4). Whenever practicable, recipients of new or changed documents should acknowledge receipt by signature. Obsolete documents should be removed from points of use and destroyed immediately unless a copy is retained for record purposes. In such cases, record copies must be clearly marked as obsolete. Requests for technical document changes, such as changes to methods, sampling data sheets, calibration procedures, and the like, can be initiated by anyone within the organization, the request being made in writing on the technical document change notice (Fig. 12-1). It should go through established approval procedures before publication and distribution. Changes may be promulgated by (I) the issuance of entire new documents, (2) the issuance of replacement pages, or, in the case of minor changes, correction of errata and so forth, by (3) pen and ink posting on the original document, with this action noted on the change notice. The Quality Control Coordinator should be designated as the individual responsible for ensuring that up-to-date documents are being used and that obsolete documents are removed from use. This includes materials from sources outside the laboratory such as standards, applicable regulations, specification sheets, and so on.

QUALITY RECORDS Records of other laboratory activities should be maintained in addition to those generated by use of the forms and reports listed above. Such records should be controlled by specifying the individual or organization

3

completed when the newly developed system is in place and running. The second phase is a long-term, continuing process and involves constant appraisal, review, and planning to update, improve, or correct deficiencies in the system. In order for the planner to communicate his plan to the person or persons expected to execute it, he must write it out in the form of procedures, together with the necessary criteria, flowcharts, diagrams, tables, forms, and so on. Planning in the field of quality assurance or quality control for the laboratory must fundamentally be geared to the delivery of precise and accurate reports which meet customer requirements at a reasonable quality cost. This objective is realized only by carefully planning and developing the many individual elements of the quality system, which relate properly to each other and are in consonance with the laboratory’s established quality objectives. These elements, taken together, are those discussed in other sections of Part 1 . The steps involved in initial quality planning are discussed in detail in Part 2 of this book. The final result of initial quality planning should be a written document which includes the most important information that the planner (normally the Quality Control Coordinator) feels should be communicated to the users of the document. The resulting overall quality plan then becomes, after management approval, the quality manual. The quality assurance plan, now called the quality assurance manual, has other important functions in addition to the primary purpose already discussed:

engineer, technician, or analyst to derive the same results as the original worker, with no other source of unpublished information. In addition to these minimum data, any other facts pertinent and appropriate to the sample test or analysis should be entered. Deletion of mistakes should be made by drawing a single line through the error. The line drawn should not render the deletion illegible. A notation stating the reason for the deletion should be added and initialed by the person who made the deletion. The recording of data on loose sheets is poor procedure, and, because of the possibility of transcription errors, should be avoided. An analyst’s or test technician’s notebook is always subject to inspection by his colleagues, supervisors, or site visitors, assessors, surveyors, or auditors from outside the laboratory. Therefore, it is imperative that the notebook be maintained in a professional manner and contain all the pertinent information that may be required by other parties, regardless of the importance of that information to the analyst or technician. Furthermore, the notebook must be maintained in such a manner that it can withstand challenges as to the validity, accuracy, or legibility of its contents. Entries should be timely and not accumulated for more than one day. References 1975. Quality Assurance Handbook f o r Air Pollution Measurement Systems. Research Triangle Park, NC: U.S. Environmental Protection Agency. July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health. January, 1987. Qualty Assurance and Laboratory Operations Manual. Cincinnati: National Institute for Occupational Safety and Health.

It is the culmination of a planning effort to design into a program or specific project provisions and policies necessary to assure accurate, precise, and complete quality data. It is an historical record which documents the program or project plans in terms of measurement methods used, calibration standards, auditing planned, data validation requirements, and so forth. It provides management with a document which can be used as an audit checklist to assess whether or not the quality assurance and control procedures called out in the manual are being implemented. It may be used as a textbook for the training of new employees or for refresher training. It may be used as a sales tool. The existence and demonstrated use of a Laboratory Quality Assurance Manual is a powerful sales statement. It may be used to demonstrate compliance with the requirements of regulatory or accreditation bodies.

SECTION 8 CUSTOMER FOCUS The laboratory’s management must, at all times, keep in mind that a primary requisite for the production of the highest quality of laboratory services is to ensure that all concerned are aware of the customers’ needs and expectations and make every effort to satisfy and heighten customer satisfaction.

SECTION 9 QUALITY SYSTEM PLANNING The act of planning is the thinking out, in advance, of the sequence of actions necessary to accomplish a proposed course of action to achieve certain quality objectives which support established quality policies. For the quality professional, the task of planning generally presents itself in two phases, discussed below. The initial phase is encountered when an organization must develop a quality system “from scratch.” It is

The continuing phase of quality planning is kept simmering on the back burner at all times. There should be constant review, appraisal, and surveillance of the quality system to seek out and identify departures from

4

The job description for a Quality Control Coordinator should, as a minimum, include the responsibilities shown below.

procedures specified in the quality manual, omissions of expected conduct, neglect to cany out such procedures, or the introduction of new, unauthorized procedures into the system. This oversight activity should be carried out in addition to the formal, internal audits periodically carried out by management.

JOB

DESCRIPTION

Title: Quality Control Coordinator Reference

1. Basic function: The Quality Control Coordinatoris responsible for the conduct of the laboratory quality control program and for taking or recommending measures to ensure the fulfillment of the quality objectives of management and the carrying out of established quality control policies in the most efficient and economical manner commensurate with ensuring the continuing accuracy and precision of analytical or test data produced. 2. Responsibilities and authority: 2.1. Develops and carries out quality control programs, including the use of statisticalprocedures and techniques, which will help the laboratory to meet required or authorized quality standards at minimum cost and advises and assists management in the installation,staffing, and supervision of such programs. 2.2. Monitors quality control activities of the laboratory to determine conformance with established policies, customer and regulatory or accreditation requirements, and with good laboratory practice. He or she makes recommendations for appropriate corrective action and follow-up as necessary. 2.3. Keeps abreast of and evaluates new ideas and current developmentsin the field of quality technology and recommends courses of action for their adoption or application wherever they fit into the laboratory’s area of expertise or policy requirements. 2.4. Advises the purchasing section regarding the quality of purchased supplies, materials, instruments, reagents, and chemicals. 2.5. Supervises the laboratory’s interlaboratory proficiency testing program. 2.6. Monitors the shipping, delivery, packaging, and handling of samples and makes recommendations for corrective action when conditions are found that lead to damaged, contaminated, or mishandled samples received. 2.7. Makes periodic reports to the Director of the laboratory as to the quality of the laboratory’s output performance and makes recommendations as to the necessary steps to be taken to ensure improvement. 2.8. Continually seeks to make sure that customer expectations are being met, including promoting awareness throughout the laboratory as to what

July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health.

SECTION 10 ORGANIZATION FOR QUALITY The establishment of a quality assumnce system in the laboratory,as described here in Part 1, will require the designation of a Quality Control Coordinator within the laboratory to carry out the monitoring, record-keeping, statistical, calibration, and other functions required in such a program. Other titles, such as “Manager, Quality Assurance,” “Director, Quality Assurance,” “Quality Control Supervisor,” and others, may be used, but the title “Quality Coordinator” seems particularly appropriate in small organizations, such as laboratories are apt to be. Regardless of the title, it is necessary to place on some individual the responsibilities for carrying out the quality policies prescribed by management. This person may have these duties as his or her sole responsibility in a large organization, and may have a staff or clerical or technical assistance, but in a small organization may “wear” this position as another “hat.” The Quality Control Coordinator should be placed in the organization at a position where he reports to the highest level at which he can be effective, unbiased, and objective in serving the needs of the laboratory. In no case, however, should the quality control coordinating function be subordinate to an individual responsible for the direct conduct of the testing or analytical work. An example of a typical organization chart for a small analytical laboratory appears as Figure 5-1 in Part 3, XYZ Laboratories, Inc. Quality Assurance Manual. Note that the Quality Control Coordinator reports to the Laboratory Director. The placement of names in position blocks in the organization charts is optional but often requires unnecessary paperwork due to frequent personnel changes. In larger organizations, where the Quality Control Coordinator may have supporting staff, it is desirable to furnish an additional organization chart for the quality assurance section alone. The Quality Manual should include a copy of the Quality Control Coordinator’sjob description, although this document may be prepared outside the Quality Control Department. Other position descriptions may be included if required by an accrediting organization.

5

and customer-generated requests for changes and corrections. Analytical and testing performance quality. Follow-up on management orders resulting from previous annual quality system reports and recommendations for improvement. Summary Quality Cost Report for the period since the last annual report.

must be done to ensure that these requirements are being met. 2.9. Performs related duties as may be assigned from time to time. References Bennett, C. L. 1958. Defining the Manager’s Job. New York: American Management Association, Inc. July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: The National Institute for Occupational Safety and Health. January, 1987. Quality Assurance and Laboratory Operations Manual. Cincinnati: The National Institute for Occupational Safety and Health.

After reviewing the annual report, management should, based on any decisions based on its contents, prepare Corrective Action Requests, which are orders related to improving the structure and output of the laboratory quality management system and its procedures. Orders affecting how customer satisfaction is being attained and what changes are to be made to meet these requirements are included. If any recommendations have been made related to new equipment acquisition, the necessary arrangements are made to evaluate and determine the validity of such requests.

SECTION 11 COMMUNICATIONS Effective laboratory management is characterized by an efficient communication system that works both up and down within the organization. Management makes sure that all concerned are aware of quality policies, objectives, plans, and procedures, while seeking out and encouraging timely reports on work progress, improvement, and problems. Methods for carrying out such communication activities include:

SECTION 13 HUMAN RESOURCES All personnel involved in any function affecting data quality (sample collection, analysis, testing, data reduction, calibration of instruments, and other quality assurance activities) must have sufficient training in their appointed job to enable them to generate and report accurate, precise, and complete data. The Quality Control Coordinator has the responsibility for seeing that the required training is available for these personnel and for taking appropriate remedial action when it is not. Quality control training programs should have the objective of seeking solutions to laboratory quality problems. This training objective should be concerned with the development, for all laboratory personnel in any aspect or function affecting quality, of those attitudes, that knowledge, and those skills which will enable each person to contribute to the production of high-quality data continuously and effectively. A number of training methods are available for laboratory personnel dealing with quality control:

In-house educational programs related to quality system management. Management visits in work areas. Planned, periodic section meetings to discuss mutual problems, achievements, customer concerns, and the like. Periodic publication of an in-house newsletter which includes articles related to laboratory performance. Use of timely and appropriate notices and posters on the laboratory bulletin board. Conduct of periodic employee opinion polls to elicit suggestions for improvement, bring to light problems that might otherwise go unnoticed, uncover areas of customer dissatisfaction, and so forth.

SECTION 12 MANAGEMENT REVIEW

1. Experience training or “On-the-job” (OJT) training is the process of learning to cope with problems using prior experience. 2. Guidance training is OJT with outside help from supervisors or co-workers. The advice may be solicited or provided informally, or on a planned, structured basis. Employees involved in an effective program employing OJT techniques will: (a) Observe experienced technicians or operators perform the necessary steps in a test or analytical method.

The Quality Control Coordinator should prepare for management a “state of the laboratory quality assurance system report” at least annually, or at such other intervals as the needs of the organization may dictate. This document should include subordinate reports on such activities and topics as: The results of both internal audits and those conducted by others at the laboratory. Customer complaints and feedback. Initiation and completion of corrective and preventive actions required as a result of audit recommendations

6

Perform the various operations in the method under the supervision of an experienced technician or operator. Perform operations independently but be monitored by a high level of quality control checks utilizing the proficiency evaluation methods discussed in Section 19. engaged in independent study involving atten3. dance at night school classes, outside reading, attendance at seminars, or taking correspondence courses on a voluntary basis. 4. Attend in-house training or classroom study taken during working hours, presented on a formal basis. Such classes may be presented as short courses, lasting from two or three days to two weeks, on general or specialized subjects. Numerous universities and technical schools offer long-term, quarter, and semester-length academic courses in statistics, computer science, and other subjects of interest to the quality technologist.

Even though many individuals and smaller elements of a laboratory organization may be involved in quality control activities, the ultimate responsibility for driving the quality effort rests on the shoulders of top management. The best way for a laboratory director or supervisor to demonstrate a desire to achieve high-quality results is to show continuous, conscientious, participatory interest in quality activities, especially in the areas of demonstration of quality improvement efforts and meeting customer requirements. In addition to the communication programs noted in Section 11, some other methods of encouraging attention to management desires are listed below. Motivation by Communication

1. Quality bulletins. 2. Quality propaganda posters. These are available from a number of commercial sources. 3. “Horror story” displays of major quality accidents, taking care to keep the participants anonymous and unidentifiable. 4. Public award ceremonies for good work. 5. Open house programs to demonstrate to employees, customers, employees’ families, and the public how the laboratory operates, stressing quality efforts.

QUALIFICATION RECORDS Certain complex testing or analytical techniques or instruments may require specialized training and the formal qualification of technicians or operators in the performance of such specialties. Once individuals are qualified, records must be kept and requalification undertaken periodically, as necessary. The Quality Control Coordinator should be made responsible for the maintenance of such records and for seeing that requalification is accomplished in a timely manner.

Formal motivational campaigns are effective only if they are:

I . Well-planned and organized. 2. Have a specific objective. 3. Are finite; that is, they must have a well-defined starting point, a planned, well-thought-out path of activity, and an identifiable termination point.

TRAINING EVALUATION Evaluation of the effectiveness of training is accomplished by the conduct of periodic intralaboratory proficiency testing of laboratory personnel involved in the conduct of testing or analytical activity. This evaluation should lead to the determination of the level of knowledge and skill achieved by the technician from the training experiences and the appraisal of the overall training effort, including the discovery of any training areas that show the need for improvement.

Examples of motivational campaigns which have had varying degrees of success are the Zero Defects programs, the Soviet Saratov System, and the Quality Circle Movement, which was introduced in Japan by Deming and Juran and has been used extensively and successfully in that country. For more information on these programs and others, and for reference material on them, see Juran’s Quality Assurance Handbook, 4th Edition, Chapter 10.

MOTIVATION The incentive to produce results with consistently high quality and continuing quality improvement which satisfies customer expectations must be provided from the top of the laboratory organization. As established management policies, the concepts of “Total Quality Control,” “Continuous Quality Improvement,” and “Customer Satisfaction” must be embraced by all employees as the fiats which control how they conduct the business of monitoring and controlling the quality of their product. Thus, these stated policies must not be considered to be mere slogans but as the organization’s way of life.

References Adams, M., Bounds, G., Ranney, G., and Yorks, L. 1994. Beyond Total Quality Managenzent. New York: McGrawHill, Inc. Feigenbaum, A. V. 1961. Total Quality Control. New York: The McGraw-Hill Book Company. Feigenbaum, A. V. 1954. “Company Education in the Quality Problem.” Industrial Quality Control. X (6):24-29. Juran, J. M. 1962. Quality Control Handbook. 2nd Ed. New York: McGraw-Hill Book Company.

7

performance will be enhanced in a work environment where people feel comfortable and are untroubled by unpleasant surroundings. Every consideration must be given to such matters as:

Juran, J. M. 1988.Juran’s Quality Control Handbook. 4th Ed. New York: McGraw-Hill Book Company. Reynolds, E. A. 1954. “Industrial Training of Quality Engineers and Supervisors.” Industrial Quality Control. X (6): 13-20. Reynolds, E. A. 1970. “Training QC Engineers and Managers.” Quality Progress. I11 (4):20-21. 1967.Industrial Quality Control. XXIII ( 1 2). All articles deal with quality education and training. 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health.

Work station ergonomics. Safety rules and practices, including the provision of personal safety equipment. Provision of adequate “people amenities” such as lunchrooms or eating areas and restrooms. Provision of adequate heating, air conditioning, ventilation, and lighting in all areas. Provision for personal health and fitness facilities as required. Meticulous housekeeping standards.

SECTION 14 LABORATORY INFRASTRUCTURE The laboratory infrastructure may be defined here as the work space, building, or buildings in which the laboratory conducts its business, together with the necessary testing and analytical equipment and supplies, plus its administrative support such as clerical, financial, and purchasing activities. Aside from the required control of environmental conditions for calibration activity discussed in detail below, it may often be necessary for the laboratory to control, in a similar manner, the atmospheric and other working conditions for all laboratory operations to the extent necessary to ensure the precision and accuracy of laboratory results. Where the test or method spells out special ambient conditions for the conduct of the test or analysis, the measures taken to control environmental conditions should be described and the resulting data defining working conditions recorded. Such activities include not only elements such as those discussed below but also such things as restricted access provisions, clean room operations (including Standing Operating Procedures), and special housekeeping and safety practices which go beyond the housekeeping and safety activities carried out on a routine, daily basis. Measuring and test equipment and calibration standards should always be calibrated in an area that provides for control of environmental conditions to the degree necessary to assure the required precision and accuracy of results. See section 22.

SECTION 16 QUALITY IN PROCUREMENT The laboratory should establish sufficient control over purchased equipment, supplies, chemical reagents, and testing materials to ensure that laboratory operations are not adversely affected by the inadvertent use of substandard equipment or supplies.

PURCHASE ORDERS A vendor of testing supplies and materials furnished to laboratories is regarded as a resource to, and an extension of, the laboratory organization. Therefore, the standards for quality required for suppliers are the same as those self-imposed on the laboratory. The purchase order instructs vendors to mark containers of test or analytical materials and instruments with the following information, as applicable: Identification of contents Vendor’s name and address Vendor’s lot number Quantity Material specification number and date of publication Material certification documentation This assures that the material is properly identified and that the supplier is using the latest specifications. The enclosed packing slip should contain the same information. Purchase orders should clearly identify the material being ordered and should include the price, expected delivery terms, specifications to be followed, certifications required, delivery method, and payment terms. In addition, when appropriate, the laboratory may:

Reference July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health.

SECTION 15 WORK ENVIRONMENT Laboratory Management must consider the need to take whatever steps are necessary to ensure that the laboratory environment provides a satisfactory atmosphere in which to work. People will be motivated by a positive impression of their surroundings, and

0

0

8

Request permission to conduct a quality audit prior to delivery of the order. Require on-site inspection of the purchased goods prior to delivery.

inventory is kept against which replacement orders can be placed by the Stores Clerk to prevent “stock-outs.’’ Each receiving report is referenced by log number to the applicable purchase order, certification, or report of analytical or test results and is retained in the quality assurance file. Logged disposition notes may be reviewed to establish trends in vendor performance and to ensure a continuing high quality of materials and supplies purchased and accepted. When the Stores Clerk issues materials and supplies to users, checks are made to be sure that the material is properly identified, shows the log number, and has a current shelf-lifeexpiration date. In the case where more than one container of a material is stocked, the oldest is used first, a first-in-first-out (FIFO) regimen. When the quality, strength, concentration, or composition of reagents, chemicals, solutions or solvents, or other materials are always checked against standards or otherwise as a part of the method or procedure, there is no need for any check on these materials before placing them in stores other than to validate the identity, shelflife, or certification, as covered in the paragraphs above. On occasion, it may be necessary to audit a vendor’s quality program to ensure his ability to produce goods to specification. In these cases, a check list such as the Quality System Survey Evaluation Check list (Fig. 8-4, Part 3 ) may be used to evaluate the effectiveness of the vendor’s quality system. The outline above is furnished as a guide to users of this text. It may be changed, added to, simplified, or embroidered upon as the user sees fit. However, it will be the basis for the Laboratory Quality Control Manual example given in Part 3.

Request a copy of the vendor’s quality assurance manual to establish adequacy of the vendor’s quality management system. Copies of all purchase orders for testing equipment and materials, chemicals, and reagents should be sent to the laboratory Quality Control Coordinator,who reviews such orders to ensure that the latest requirements are correctly specified. Purchase orders, receiving documents, and accompanying certifications are used as a part of the receiving control procedure and show information necessary to identify the material received. The Laboratory Stores Clerk or another designated person is responsible for checking lots of material received for the correct quantities, for certification, if required, and for checking the packing slip against the purchase order. Lots of testing items which may be received in large quantities, such as gas detector tubes, may be subjected to incoming inspection procedures to determine whether they meet dimensional and performance specifications. If a discrepancy is found that could affect the quality of laboratory output, the material may be rejected, set aside, and held for disposition. Rejected lots may be returned to the vendor for replacement, discarded, or, in rare cases, used as is under a permissive waiver. In any case, all lots received are posted on a log sheet. Accepted lots are logged in and placed in stores, noting: Identification of the material Vendor identification Date received Purchase order number Assigned log number The container label is stamped with the log number and shelf-life expiration date, if available. No reagents, chemicals, standard solutions, or other time-sensitive materials should be used after the expiration of the shelflife date. When, in the judgment of the Quality Control Coordinator, it is desirable to check the validity of a certification of a purchased material, such a check should be made using the laboratory’s own expertise and equipment or by sending the material to an outside laboratory for a third opinion. Such checks should be made at random intervals or when circumstances dictate the need for a cross-check. In the event of a rejection, the vendor is notified by the Purchasing Department, the material is discarded, and its condition is noted in inventory records. Procedures should be established which require the Stores Clerk to survey the inventory once monthly to identify material approaching a shelf-life expiration date within 30 days so that fresh replacement stocks may be ordered. As supplies are used or requisitioned, the amounts are posted against the log number and thus a running

SECTION 17 SAMPLE HANDLING, IDENTIFICATION, STORAGE, AND SHIPPING Because some samples or their containers are fragile, are sensitive to environmental changes when shipped from collection points to the laboratory, or are held in storage, special precautions must be taken for handling, storage, packaging, and shipping to protect the integrity of samples and to minimize damage, loss, deterioration, degradations, or loss of identification of the samples. Physical damage to the sample’s shipping container may be the fault of the carrier due to mishandling, or it may be the fault of the sender due to defective or poorly designed packaging. Sample integrity refers to the cumulative end result of those factors which detract from the overall validity of a field sample. Such factors are: Physical damage, as discussed above. Loss of the sample due to leakage, breakage of seals, or other causes.

9

Contamination by foreign materials. Improper shipping methods for samples requiring special temperature or atmospheric conditions. Lack of maintenance of valid sample identification.

characteristics of criminal law, particularly when monetary or jail penalties are involved. The legal principles governing chain-of-custody must be adhered to in all three types of litigation. In any litigation, adherence to chain-of-custody principles has two main goals: (1 ) to ensure that the sample which is taken or collected is the same sample that is analyzed; and (2) to ensure that the sample is not altered, changed, substituted, or tampered with between the collection or acquisition and the analysis or testing. If the party attempting to introduce analytical or test results as evidence is challenged by the opposing party, he or she may be obliged to demonstrate an adequate chain-of-custody. This brings up the important question of what constitutes an “adequate” chain-of-custody. In the Gullego case cited above, the court stated that all that is necessary is that a “reasonable probability that the article has not been changed in important respects” be established. In United States v. Robinson, 447 F. 2d 1215 (1971), the court stated that the “probability of misidentification and adulteration must be eliminated not absolutely, but as a matter of reasonable certainty.” It seems clear that absolute security is not necessary for an acceptable chain-of-custody. We will cite one case in which an adequate chain-of-custody was held to be established, and another in which it was not, in order to present to the reader a frame of reference. In Ohio v. Conley, 288N. E. 2d 296 (197 l), the defendant contested the admission of certain orange pills as evidence, claiming that an adequate chain-of-custody had not been established by the state. The pills had been confiscated from the defendant by a police officer, transferred to another officer, and finally transferred to the laboratory. It is at this point that the defendant claimed that the chainof-custody was violated. The second officer testified that he gave the container of pills to a man in the laboratory, who then assigned it a log number. The next testimony was from the chemist who removed the sample from a file drawer and analyzed it. The individual who accepted the sample at the laboratory was not identified, nor did he testify. The exact procedure by which the container found its way into the file cabinet is unknown. The court held that even though direct testimony regarding the period in question was not available, an adequate chain-of-custody was established by inference. The container obtained by the analyst was the same as that supplied by the police, and it contained the same number of orange pills. The inference is strong that it was the same container and pills. In Erickson v. North Dakota Workmen’s Compensation Bureau, 123N. W. 2d 292 (1963), a coroner removed a blood sample from a deceased individual, placed it in an unsealed container, and transported it to a hospital, where it was given to an unidentified emergency room attendant with instructions that it be placed in a refrigerator. The record disclosed that sometime before noon on the following day, a laboratory supervisor found the

References July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health. January, 1987. QualityAssurance and Laboratory Operations Manual. Cincinnati: National Institute for Occupational Safety and Health.

SECTION 18 CHAIN-OF-CUSTODY PROCEDURES Chain-of-custody is a term that refers to the maintenance of an unbroken record of possession of a sample from the time of its collection through some analytical or testing procedure and possibly up to and through a court proceeding. For some laboratories, especially those dealing with forensic, pathological, and environmental samples, the establishment of chain-of-custody procedures is of paramount importance, as the results of testing or analysis might eventually be held as evidence in a trial or hearing. Such organizations should design their samplehandling documentation systems so that, during each step of sample collection, delivery, receipt, storage, analysis, disposition, or other handling, some one individual is responsible for the custody and the identification of the sample and its accompanying documentation. The law that governs the chain-of-custody principles was clearly stated by the court in Gallego v. United States, 276 F. 2d 9 14: “Before a physical object connected with the commission of a crime may properly be admitted in evidence, there must be a showing that such an object is in substantially the same condition as when a crime was committed. Factors to be considered in making this determination include the nature of the article, the circumstances surrounding the preservation and custody of it, and the likelihood of intermeddlers tampering with it. If, upon the consideration of such factors, the trial judge is satisfied that in a reasonable probability, the article has not been changed in important respects, he may permit its introduction in evidence.”

The statement of the court above refers to chain-ofcustody in criminal cases. The principles are essentially the same in civil cases or in administrative law hearings. A laboratory and its personnel may be involved in any one of the three. Litigation under the Occupational Safety and Health Act of 1970, for instance, and the various environmental acts, is basically civil in nature, but it does have the 10

out-of-control points on standard quality-control charts. Careful selection of the variables to be charted, an understanding of the method’s limitations, comparison of results against previously used, independent methods, and active participation in available proficiency testing programs or an exchange of samples between laboratories become important additions to normally used control charts for the scientist, technician, or test engineer. In manufacturing processes, calibration is not usually a significant source of error, whereas in the laboratory, calibration errors may be the largest producers of error. In some instances, these erroneous results may be hidden and related to: (1) limitations in knowledge and agreement over what constitutes the best calibration standard available, (2) errors (both systematic and random) in primary calibration standards, and (3) errors (both systematic and random) inherent in the preparation of working standards. Silica calibration is an example of the first limitation. It used to be the case that universal agreement on the most appropriate calibration to use for “respirable dust” silica determinations was not available. This was made important since silica determinations by all three common methods of analysis (i.e., colorimetric, infrared, and X-ray diffraction) have been reported to have a particle-size dependence. Presently, however, NIST SRMs (standard reference materials) 1878A for quartz and 1879A for cristabolite are available for comparisons. The occurrence of certified, calibration-grade gas cylinders having out-of-specification contents is an example of the second limitation. The U.S. Environmental Protection Agency has reported on the existence of such cylinders, which are commercially available, and the National Institute of Science and Technology (NIST) has reported problems with the reliability of the low-ppm cylinders initially tested in the NIST Standard Reference Material Program. Calibrations involving gases at normal ambient temperature and pressure, such as vinyl chloride, are an example of the third limitation. Because it is difficult to measure the volume of a gas and prevent its loss during the preparation of secondary and working standards, large inaccuracies can occur. When calibration procedures must deviate from accepted practices as taught in college chemistry courses-that is, to rely on gas-versus-liquid-versus-solid measurementsand these procedures fail to use a consecutive dilution of standards to the working range, sizable calibration errors are probable. Precautions including the use of NIST standard reference materials, even though expensive, the verification of commercial standards by a comparison with NIST standards, proper identification and cross-referencing of the standards used in calibration, the expiration dating of all standards, participation in proficiency testing of calibration procedures, and the adherence to proper, written calibration procedures are especially important when one considers that many calibration errors are hidden and can affect laboratory results over a long time period.

tube in a refrigerator and had it analyzed for alcohol content. No one testified as to the time the sample was placed in the refrigerator. The refrigerator was not secured, nor was it in a secure area, and it was in a location accessible to the entire hospital. The court held that the chain-of-custody was defective because the character of the sample could have changed if it was not refrigerated promptly and could have been tampered with while in the uncontrolled refrigerator.

SECTION 19 LABORATORY TESTING AND CONTROL: INTRA- AND INTERLABORATORY PROFICIENCY TESTING INTERLABORATORY PROFICIENCY TESTING All laboratories must establish some means to ensure that testing and analytical procedures are operating within reasonable control. To do this, laboratories engage in intra- and interlaboratory testing programs, making sure that they use rugged, published, approved methods (where available) and that these are employed under controlled conditions. Furthermore, adequate, complete records of testing and analytical results obtained as the output of such testing programs must be documented and retained. In addition, there are many statistical techniques and control procedures discussed in quality control textbooks. However, most of these techniques and procedures are found to be useful in manufacturing operations. Unfortunately, laboratories must contend with a variety of obstacles which are rarely encountered in manufacturing. For example, X-R charts used in recording and controlling manufacturing operations are usually based on a large volume of data generated over a relatively short period of time. However, a laboratory, especially one that performs nonroutine analysis or testing, may take years to develop an adequate database. In this instance, one of two approaches may be taken: (1) a short-term study is conducted to evaluate the variability of data generated using statistical tests which are more useful on a one-time basis, such as t-tests, F-tests, or analysis of variance (ANOVA), or (2) trial statistical control limits are calculated using variability estimates based on prior or published results for similar analytical or test methods or calculations that use the error estimated for each testing or analytical step. Most manufacturing processes involve infrequent process changes, whereas the analytical chemist or test engineer must frequently deal with samples which differ from specified standard products or, in the case of samples to be analyzed, have different concentration levels and interferences, requiring test or method modification. These method modifications can affect the precision and accuracy of results and produce what appear to be

11

Another obstacle is the limited information that may be available to the test engineer, technician, or analyst about the nature of the samples presented for analysis or testing. In the case of analytical samples, without information on what concentration levels or interferences to expect, gross analytical and calculation errors, such as a failure to compensate for interferences, errors in dilution, or misplaced decimal points, may occur. These may go undetected when analytical results on field samples are produced and used. In the case of product samples submitted for physical testing, a lack of pertinent information about the nature of the sample, its source, its intended use, or (perhaps) its history may lead to the selection of the wrong test method, resulting in the production of useless test data. Even when errors are suspected, repetition of tests on, or analyses of, the sample submitted is not possible. This makes careful checking of the procedure, independent verification of calculations, and the use of testers or analysts who are familiar with the product or process being investigated all-important. Perhaps the largest advantage that manufacturing quality control efforts have over laboratory quality control procedures is that management has perceived that improved quality leads to reduced costs and higher profitability. Laboratories, as a rule, have been slow to adopt quality cost reporting as a routine management tool. Conversely,in the manufacturing community, it is a relatively common practice to report on and relate the cost of the control of quality to the savings resulting from these efforts. Indeed, quality cost reporting was a requirement imposed in the United States Standard MIL-Q-9858A, Quality Program Requirements, which for many years was one of the most widely used quality standards in the United States. It is curious to note that a discussion of quality financial measurements appears in Paragraph 8.2 of American National Standard ANSI/ISO/ASQ Q90042000, which is a guideline document and thus imposes no requirements on users. By reporting to top management, on a regular basis, the status of financial measurements, the costs incurred in the conduct of the quality control program will be seen as acceptable since they will be deemed to be a cost-saving measure. A major obstacle to improving customer satisfaction with the quality of the laboratory’s service is the gap in the communication chain between the producer of the sample and the laboratory. Improvements in measurement reliability, precision, and accuracy go unnoticed in the field. This imperfect communication between the laboratory and the producer of the sample to be tested or analyzed results in field personnel being unaware of the limitations of the data. In order to improve communication, laboratory personnel should report limits of detection and confidence limits and make qualifying statements, when necessary or appropriate, to make sure that laboratory results are not misinterpreted or misused. Users, on the other hand, should take a skeptical look at laboratory results. Submission of blind, split, spiked, and reference

samples should be routine when it is possible to provide such test samples. From this we can infer that user requirements that laboratories providing analytical and physical testing services participate in proficiency testing and laboratory accreditation programs and present information on their quality control procedures will provide some assurance that minimum performance standards can be met by the laboratory. As can be seen from the discussion above, participation in interlaboratory testing programs is a vital part of the laboratory quality program. Furthermore, such participation is a requirement of most accreditation programs. Although there are more than 150bodies offering accreditation status for laboratories, not all have a requirement that the laboratory have a quality program in place. Some that do are the American Industrial Hygiene Association (AIHA), 2700 Prosperity Ave., Suite 250, Fairfax, VA 2203 1; The Joint Commission on Accreditation of Health Care Organizations, 875 North Michigan Ave., Chicago, IL 6061 1; and the American Association for Laboratory Accreditation, 5301 Buckeystown Pike, Suite 350, Frederick, MD 21704-8307. Although there are numerous proficiency testing programs established in both the public and private sectors, some that may be of interest to readers follow: 1. The Occupational Safety and Health Administration (OSHA) lead (Pb) standard, 29CFR1910.1025Cj)(2) (iii), requires blood lead analyses to be performed by an approved laboratory participating in the Centers for Disease Control blood lead proficiency testing program. For information concerning this program, as well as other proficiency testing programs in microbiology, immunology, immunohematology, and chemistry, one should contact: Proficiency Testing Branch, Centers for Disease Control, Bldg. 6, Room 315, Atlanta, GA 30333. 2. The U.S. Environmental Protection Agency has programs in microbiology, radiochemistry, water pollution and supply, and interlaboratory audits for air sources, ambient air analyses, and bulk asbestos identification. Information may be obtained by contacting: U.S. EPA Environmental Monitoring and Support Laboratory, Research Triangle Park, NC 277 11. 3. The American Industrial Hygiene Association, 2700 Prosperity Ave., Suite 250, Fairfax, VA 22031, through its several proficiency testing programs (PAT, ELPAT, EMPAT, and Bulk Asbestos) provides reference samples to public and private industrial hygiene laboratories. It is appropriate to mention here that ISO/IEC Guide 431- 1997, Projiciency Testing by Interlaboratory Cnmparisons, and ASTM E 1301-1995, Standard Guide for the Development and Operation of Laboratory Projiciency Testing Programs, offer guidance on how to set up and participate in these necessary activities. 12

In order to illustrate how a typical interlaboratory industrial hygiene testing program operates, we will discuss the AIHA PAT Program in detail. In 1972, the PAT Program was started as a proficiency testing program for laboratories providing analytical services to The National Institute for Occupational Safety and Health (NIOSH) and OSHA to ensure agreement of results from the several laboratories reporting data in the Target Health Hazard Program (THHP). Initially, PAT provided reference samples of lead, silica, and asbestos, three of the five substances included in the Target Health Hazard Program, to participating laboratories every two weeks for each analyst in each laboratory doing THHP analyses. The program was almost immediately expanded to allow other government and university laboratories to participate. Within a year, it became evident that guidelines establishing minimum standards for personnel, facilities, equipment, record-keeping, and internal quality control were necessary to improve analytical performance. Validation of previously volunteerdeveloped criteria by two American Industrial Hygiene Association (AIHA) ad hoc committees and the subsequent formal AIHA Laboratory Accreditation Committee was supported by NIOSH contract. Later in 1972, NIOSH provided the funding for the development of validation criteria by AIHA, and the AIHA Laboratory Accreditation Program became operational in 1974, with NIOSH providing the PAT Program, in which participation was required for laboratories seeking accreditation. Now the AIHA handles the arrangements for the provision of a single sample kit each quarter to each of the participating public and private laboratories. Because the frequency of testing has been reduced from once every two weeks to once every quarter, and from evaluating every analyst performing a particular type of analysis each time to rotating sample kits among all analysts performing similar analyses, the PAT Program is designed to complement, not replace, the laboratory’s internal quality control system. AIHA now has responsibility for the preparation of reference Samples, which presently include the following materials: lead, silica, asbestos, cadmium, zinc, and one of the following organic solvents: methyl acetate, benzene, chloroform, 1,2-dichlorethane, ethyl acetate, 2-propanol, 1,1,1-trichlorethane, methyl ethyl ketone, methanol, tetrachlorethylene, and trichlorethylene, as well as diffusion samples for benzene, toluene, and xylene. Sample generation, data processing, and preliminary data evaluations are performed by a contractor to AIHA specifications. The use of no specific method is required; however, procedures must be furnished to AIHA by participating laboratories. Samples are submitted at four concentration levels plus a blank. These levels are selected as representative of concentrations that would be collected under actual field conditions for normal sampling intervals. They are

designed to span the threshold limit values for the particular materials. Not all laboratories in the program analyze all sample sets, nor are they required to do so. Laboratories are asked to analyze the samples within 30 working days after receipt and submit the results to AIHA via the World Wide Web. AIHA then evaluates these results in more detail, screens laboratories for those with questionable performance, and provides each laboratory with a comprehensive report on its status. Proficiency is determined on the basis of a laboratory’s performance compared with that of peer laboratories. 2 scores, a common statistical measurement of performance over time, for each laboratory for each material are maintained. Prior to any material being included in the PAT Program, it must have undergone preliminary testing to ensure that uniform samples can be prepared, that satisfactory analytical procedures are available, and that samples have a satisfactory shelf life and ruggedness for the program. Although accuracy is not aprerequisite for proficiency, it is a parameter that is not overlooked. As stated above, proficiency test data are evaluated by comparing an individual laboratory’s results with the results of the entire group performing that analysis. For most analysts, comparison is only with an accredited laboratory’s results due to the unusual nature of the data distribution. Similarly, laboratory-to-laboratory variation is provided by comparison of a specific laboratory’s mean results for each of the four filters or charcoal tubes with the results of all laboratories or, in some cases, with the mean of accredited laboratory results.

INTRALABORATORY PROFICIENCY TESTING PROGRAMS

With regard to intralaboratory testing programs, the purpose of such activity is to identify the sources of measurement method error and to estimate their bias (accuracy) and variability (repeatability and replicability). For manual measurement methods, in the case where sample collection is followed by laboratory analysis or tests, bias and variability are determined separately for sample collection and analysis and then combined for total method bias and variability. Where continuous data recording is involved, total method bias and variability are determined directly. Some of the error sources are the operator, the analyst or test technician, the equipment, the calibration, and the operating conditions. The results may be analyzed by making comparisons against each other or against reference standards. Operator or analyst proficiency is an additional consideration for intralaboratory testing. Although many of the techniques employed in the conduct of an interlaboratory testing program are applicable in a modified form to intralaboratory testing, there are additional problems related to in-house proficiency testing of operators, testers, or analysts. The major problems associated with designing a

13

Table 19-1. PROBLEMS IN ASSESSING ANALYST PROFICIENCY Problem

Solutions and decision criteria

Kinds of samples

I . Replicate samples of unknowns or reference standards. 2. Consider cost of samples. 3. Samples must be exposed by the analyst to the same preparatory steps as normal unknown samples.

Introducing the sample

1. Samples should have same labels and appearance as unknowns. 2. Because checking periods should not be obvious, supervisors and analysts should overlap the process of logging in samples. 3. Supervisor can place knowns or replicates into the system occasionally. 4. Save an aliquot from one day for analysis by another analyst. This technique can be used to detect bias.

Frequency of checking performance

assurance program requires accuracy levels of the standards that are consistent with the test or analytical method. Calibration procedures apply to all instruments and gauges used for analyses and tests, the results of which are recorded for purposes of decision-making. The standards used in the calibration of instruments and gauges are also included in the calibration system. Instruments not included are those used as indicators only. An example might be a panel voltmeter which indicates when a switch is moved to the “on” position and whose reading (1I 8 volts, for instance) is not recorded. Indicating instruments should be tagged as such.

CALIBRATION PLAN A detailed plan should be provided for controlling the accuracy of measuring and test equipment, software, and calibration standards used in doing calibration work. The plan should include:

I . Consider degree of automation. 2. Consider total method precision. 3. Consider analyst’s training, attitude, and Derformance record.

1. A listing of all required calibration standards with proper nomenclature and identification numbers assigned. 2. The environmental conditions (temperature, relative humidity, barometric pressure, and so forth) to be maintained by the calibration activity under which the calibration standards will be used and the calibrations performed. 3 . Established, realistic calibration intervals for measuring and test equipment, and for each calibration standard, designation of calibration sources. 4. Written calibration procedures for measuring and test equipment and calibration standards, including document control numbers for reference purposes. 5. A description of the mechanism used to establish traceability of calibration standards to standards available at the National Institute of Science and Technology, or other recognized fundamental standards. 6. A description of the laboratory calibration system showing how gauges and instruments are recalled in a timely manner for scheduled calibration and including samples of labels, decals, record cards, and so forth used in the calibration record system.

program to audit the analyst’s or tester’s proficiency are the following: 1. What kinds of samples to use. 2. How to prepare and introduce the samples into the run without the recipient’s knowledge. 3 . How often to check the analyst’s or tester’s proficiency.

These problems and suggested solutions or criteria for decision-making are found in Table 19-I.

SECTION 20 DESIGN AND DEVELOPMENT (EXCLUDED) SECTION 21 CUSTOMER PROPERTY (EXCLUDED) SECTION 22 CONTROL OF MEASURING AND TEST EQUIPMENT GENERAL

CALIBRATION STANDARDS QUALITY

Calibration procedures require the application of primary or secondary standards. The standards used, whether they are physical or reagent standards, should be certified as being traceable to standards of the National Institute of Science and Technology (NIST) or some other recognizable fundamental standard. This kind of traceability is necessary even when the standards are generated in the laboratory. Regardless of the type of calibration equipment or material, an effective quality

Transfer standards should have four to ten times the accuracy of field and laboratory instruments and gauges. For example, if a thermometer used in the laboratory to determine a solution temperature has a specified accuracy of 2~2’F, it should be calibrated against a standard thermometer with an accuracy of f 0 . 2 ” F. The calibration standards used in the measurement system should, in turn, be calibrated against higher-level, primary standards having unquestionable and higher accuracy. These

14

primary standards, in turn, should be certified by NIST or another recognized organization or derived from accepted values of physical or chemical constants. Calibration gases purchased from commercial vendors normally are accompanied by a certificate of analysis, Whenever a certified gas is available from the National Institute of Science and Technology, commercial gas sources should be asked to establish traceability of the certificate of analysis for the certified gas. Inaccurate concentrations in certified gases may result in serious errors in reported measurements of concentrations undergoing analysis or test.

the absence of a published, established calibration interval based on a manufacturer's recommendation, authorized government specifications, or other source for a particular item, an initial servicing interval should be assigned by the laboratory or calibration service. The calibration intervals should be specified in terms of time or, in the case of certain types of test and measuring equipment, period of use or number of times cycled. The establishment of prescribed intervals should be based on the inherent stability or sensitivity of the equipment, its purpose or use, and the conditions or severity of use. The intervals may be shortened or lengthened by evaluating the results of the previous and present calibrations and adjusting the schedule to reflect the findings. These evaluations and resulting adjustments must provide positive assurance that changes to the calibration intervals will not adversely affect the accuracy of the system. The laboratory should maintain proper usage data and historical records for all test and measuring equipment to ascertain whether an adjustment of the calibration interval is warranted. Adherence to the calibration frequency schedule is mandatory. Prior to the date when the item is due for scheduled calibration, it is recalled and removed from service. The recall system may be a simple tickler file, with Instrument/Gage Calibration Records (Fig. 22-2) being filed by month, in laboratories having a small gauge and instrument inventory. In this case, the cards for items due for calibration in a given month are pulled on the first of that month, and the gauges or instruments involved are recalled for calibration. In the case of organizations having large inventories, it is common to computerize the recall system and publish computer printouts, which are distributed to all affected areas, to initiate the scheduled recalls. On occasion, it may be necessary to calibrate between normal scheduled calibration due dates if there is evidence of damage due to mishandling or suspected or apparent inaccuracy in the equipment.

ENVIRONMENTAL CONDITIONS Measuring and test equipment and calibration standards should be calibrated in an area that provides for control of environmental conditions to the degree necessary to assure the required accuracy of test or analytical results. Therefore, the calibration area should be reasonably free of dust, vapor, vibration, and radio frequency interferences; and it should not be located close to equipment that produces noise, vibration, or chemical emissions or close to areas in which there is chemical production or the use of microwave or radar transmissions. The laboratory calibration area should have adequate temperature and humidity control. A temperature of 68" F-73" F and a relative humidity of 35-50% normally provide a suitable environment. A filtered air supply is desirable in the calibration area. Dust particles are more than just a nuisance; they can be abrasive, conductive, and damaging to instruments. Other environmental conditions that should be considered are: 1 Electric power. Recommended requirements for electrical power for laboratory use should include voltage regulation to within at least 10%(preferably 5%) of nominal, and minimum line transients, as may be caused by interaction with other users on the main line to the laboratory. Separate input power should be provided, if possible. A suitable grounding system should be established to assure equal potentials to ground throughout the laboratory. 2. Lighting. Adequate lighting at suggested values of 80 to 100 foot candles at bench levels should be provided. Fluorescent lights should be shielded properly to reduce electrical noise.

CALIBRATION PROCEDURES Written step-by-step procedures for the calibration of measuring and test equipment and calibration standards must be used by the laboratory to eliminate possible measurement inaccuracies due to differences in techniques, environmental conditions, choice of higher-level standards, and other causes. These calibration procedures may be prepared by the laboratory, or the laboratory may use published standard practices or written instructions proGided by the manufacturer of the equipment. These procedures should include the following information:

CALIBRATION INTERVALS All newly acquired gauges and instruments, as well as those which have been repaired, rebuilt, or reconditioned, should be calibrated prior to being put into service. After initial calibration, all calibration standards and measuring and test equipment should be assigned an established interval for calibration (Fig. 22-1, Part 3). In

1. The identification of the type of equipment for which the procedure is applicable, to include: nomenclature, model number or numbers, and type.

15

in an advisory capacity to the Program Manager. The GIDEP Administration Office implements the functions of GIDEP and the technical operation of the program as directed by the Program Manager. The operation of the Metrology Data Bank is straightforward and simple. Gauge and instrumentation equipment procedures and metrology-related documents submitted by participants in the program are submitted by the organization’s in-house Program Representative to the GIDEP Administration Office for processing. The Administration Office reviews submitted material and enters it into the Metrology Computer Data Base when accepted. Participation in the GIDEP Metrology Data Interchange Program is voluntary and involves no fee payments of an; kind. AlthoughGIDEP was originally &ablished for the use of government agencies, with the FAA, DOE, NASA, and others also co-sponsoring, together with their contractors, others outside these bodies may participate, provided they meet the requirements outlined below. To apply for participation, a formal letter of request must be directed to the GIDEP Administration Office and must be signed by an official duly authorized to commit the organization to the obligations associated with participant status. Again, none of the direct costs of the program are assessed against participants. Applications for participation must be submitted on company stationery and directed to the address given below. The basic admission requirements, discussed immediately following, must be addressed point by point in the application letter. The applicant must have a computer capable of Internet access, a Web browser (version 4+), Adobe Acrobat Reader software, and a printer suitable for downloading and printing selected calibration procedures or other documents. The applicant must agree to appoint a responsible person to act as GIDEP Metrology Data Interchange Representative. Suitable physical facilities and clerical assistance must be made available. Participants must submit a short (one-page) annual Utilization Report showing how they have used the GIDEP Metrology Data Bank during the previous twelve-month period. All participants will be provided with a Policies and Procedures Manual. Initial submittal of at least one calibration procedure or metrology-related report reasonably representative of future submittals is required. GIDEP expects participants to share new technical information with other members as it is developed. For applications or other information, you may contact GIDEP at: GIDEP Operations Center, P.O. Box 8000, Corona, CA 92878-8000. Phone 909-273-4677; DSN 933-4677; FAX 909-273-5200. Internet: [email protected]. navy.org http:llwww.gidep.org

2. A brief abstract of the scope, principle, or theory of the calibration method. 3. A list of calibration standards and accessory equipment required to perform the calibration described. 4. A complete, detailed procedure for calibration arranged in a step-by-step manner, clearly and concisely written. 5. Calibration procedures should provide specific instructions for obtaining and recording data and should include copies of any special forms necessary for recording data obtained during the calibration procedure. 6. Specification of requirements for statistical analysis of results if necessary.

GOVERNMENT-INDUSTRY DATAEXCHANGE PROGRAM (GIDEP) Instrument and gauge calibration procedures are often difficult to obtain; therefore, since the GIDEP Metrology Data Exchange function is a source for over 40,000 written calibrations, it will be brought to the attention of readers at this point. GIDEP is a government-sponsored program designed to facilitate the exchange of data among government activities and any organization supplying goods or services to any branch of the U.S. or Canadian governments. GIDEP, since its inception in 1960, has amply demonstrated a mutual benefit for participants, having reported cost avoidances of over $1 billion. This means that by using calibration procedures from GIDEP, participants have achieved truly significant savings over the life of the program. The Metrology Data Exchange function became part of GIDEP in 1968. This data bank contains over 40,000 calibration procedures and metrologyrelated documents. Government facilities, prime contractors, subcontractors, manufacturers, and business firms, including laboratories involved in the use of, and calibration of, test instrumentation, are currently participating in the Metrology Data Interchange. Information contained within the Metrology Data Bank includes calibration procedures, maintenance and repair manuals, specifications and standards, instrument rework procedures, measurement techniques, and other technical information related to the fabrication, application, and calibration of test and analytical instrumentation and gauging. The Metrology Data Interchange was established to reduce duplication of effort and costs expended by both the government and the private sector for the preparation of gauge and instrument calibration procedures and related metrology information. GIDEP operates under an agreement of the Joint Commanders of the Army Materiel Command (AMC), Naval Materiel Command (NMC), and Air Force Logistics Command (AFLC). A charter established the Program Manager Office within the NMC. A Government Advisory Group and an Industry Advisory Group act

16

CALIBRATION SOURCE

equipment. Geneva, Switzerland: International Organization for Standardization. 15 September 1997. ISO10012-2. International Standard. Quality Assurance for measuring equipment, Part 2: Guidelinesfor control of measurement processes. Geneva, Switzerland: International Organization for Standardization. November 2000. ANSUISO 17025-1999. American National Standard-General requirements for the competence of testing and calibration laboratories. Milwaukee, WI: The American Society for Quality. 13 December 2000. ANSI/ISO/ASQ 49001-2000. American National Standard-Quality management systemsRequirements. Milwaukee, WI: The American Society for Quality. 13 December 2000. ANSI/ISO/ASQ 49004-2000. American National Standard-Quality management systemsGuidelines for Pe$ormance Improvements. Milwaukee, WI: The American Society for Quality.

All calibrations performed by or for the laboratory must be traceable back through an unbroken chain, supported by reports or data sheets to some ultimate or national reference standards maintained by an organization such as NET. The ultimate reference standard can also be an independently reproducible standard (i.e., a standard that depends on accepted values of natural physical constants). An up-to-date calibration report for each calibration standard used in the calibration system must be maintained. If outside calibration services are performed on a contract basis, copies of reports issued must be kept on file. Copies of all calibration records (Fig. 22-2) must be kept on file and should contain the following information: Description of the equipment Manufacturer of the equipment Model name, model number, and serial number Required calibration frequency Number of the calibration procedure to be used Location of the equipment Current calibration date Calibration measurements obtained and corrected Values, if used Name of the person who performed the calibration

SECTION 23 PREVENTIVE MAINTENANCE As defined here, preventive maintenance is an orderly program of positive actions such as equipment cleaning, lubricating, reconditioning, adjustment, or testing in order to prevent instruments from failing during use. The most important effect of a good preventive maintenance program is to increase measurement system reliability and thus increase data completeness. Conversely, a poor preventive maintenance program will result in increased measurement system downtime (i.e., a decrease in data completeness), increased maintenance costs, and may cause distrust in the validity of the data. Data completeness is one of the criteria used to validate data. See Section 26 for a discussion of data validation. Laboratory managers should prepare and implement a preventive maintenance schedule for measurement systems. The planning required to prepare the preventive maintenance schedule will have the effect of (1) highlighting the equipment (or parts thereof) that is most likely to fail without proper preventive maintenance; and (2) defining a spare parts inventory, which should be maintained to replace worn-out parts with a minimum of downtime. The laboratory preventive maintenance schedule should relate to the purpose of the analyses or tests, environmental influences, the physical location of the equipment, and operator skills. Checklists are commonly used to list required maintenance tasks and the frequency or time interval between scheduled maintenance operations. When sampling includes several instruments, it becomes important to integrate checklists into the preventive maintenance schedule. Since instrument calibration is sometimes the responsibility of the operator, in addition to preventive maintenance, and since calibration tasks may be difficult to separate from preventive

LABELING All equipment in the calibration system must have, affixed to it in plain sight, a tag or label bearing the following information (Fig. 22-3): The date last calibrated Calibrated by whom Next calibration due date If the equipment size or its intended use limits or prohibits the use of a tag or label, an identifying code should be used. Equipment past due for calibration should be removed from service or, if this is impractical, should be impounded by tagging (Fig. 22-4) or other means. The use of out-of-calibration equipment must be prohibited (Fig. 22-5). References July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health. 15 January 1992. IS0 10012-1. International Standard. Quality assurance requirementsfor measuring equipment, Part 1: Metrological conjinnation system for measuring

17

maintenance tasks, a combined preventive maintenancecalibration schedule may be appropriate. A record of all preventive maintenance and daily service checks should be kept (see Fig. 23-1). Normally, it is convenient to file the daily service checklists with any measurement data. An acceptable practice to follow for recording task completion is to maintain a preventive maintenance-calibration multiple-copy maintenance record logbook. After tasks have been completed and entered in the logbook, a copy for each task is removed and sent to the supervisor for review and filing. At the minimum, instrument logs will contain a record of the routine performance checks results and the maintenance done i n the instrument as well as a record ofthe day-to-day use of the instrument. The instrument log-

The subject of estimating the uncertainty of measurements, together with the discussions of calibration and preventive maintenance in the two preceding sections, make up a quality control subsystem known as “metrological confirmation.”Taken together, these three activities serve to help ensure that the measuring equipment and gauges used in a specific test method have the precision and accuracy needed for that specific task. Inter- and intralaboratory proficiency bolster the assurance given by other metrological confirmations. References Juran, J. M. 1988. Juran’s Quality Control Handbook, 4th Ed. New York McGraw-Hill Book Company. 15January 1992.International StandardISO 10012-1. Quality assurance requirementsfor measuring equipment, Part I : Metrological conjirmation system for measuring equipment. Geneva, Switzerland: International Organization for Standardization.

book be marked to show the instrument identification and should be kept near the instrument. When not in use, gauges and measuring instruments should be placed in storage in a manner that will protect them from deterioration or damage from handling while out of service. Whenever possible, following calibration or maintenance, they should be sealed or otherwise protected from tampering or unauthorized adjustments.

SECTION 25 REFERENCE STANDARDS AND STANDARD REFERENCE MATERIALS Since we have stated that all measurements should be based on calibration against reference standards or standard reference materials, it is incumbent upon laboratories to obtain reliable reference standards for calibration work. Such standards should be periodically checked against standards of higher accuracy, or against standard reference materials (see Section 14). This phase of internal quality control is critical for laboratories doing trace analytical work. For each method, the analyst must estimate the approximate number and range of standards that will be necessary, using information gained from past experience, or that given by the method. The source of the standard should be determined. Standard Reference Materials (SRMs) from the National Institute for Science and Technology should be used whenever possible. All standard materials should be assayed to assure that they are of sufficient purity for the analysis being performed. The methods for performing this assay will vary, depending on the technique being used. Over 1000 SRMs are available from the National Institute for Scienceand Technology. For price lists, ordering instructions, or for NIST Special Publication 260, NIST Standard Reference Material Catalog, contact: Office of Standard Reference Materials, Room B3 11, Chemistry Building, National Institute for Science and Technology, Washington, D.C. 20234; Telephone: 30 192 1-2045. Also see: NIST Special Publication 250, Calibration and Related Measurement Services of the National Institute for Science and Technology, Available from Superintendent of Documents, U.S. Government Printing Office, Washington, D.C.

References July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health. 13 December 2000. American National Standard-Quality management systems-Requirements. Milwaukee, WI: The American Society for Quality.

SECTION 24 ESTIMATE OF UNCERTAINTY OF MEASUREMENT It has long been recognized that a significant degree of variability may be associated with almost any measurement system. In the laboratory, there may be several sources causing these departures from expected values, such as differences in testing personnel, temperature or humidity variation, differences in samples tested, and differences in the accuracy or precision of the measurement equipment which may be used at different times. Any one or all of these may contribute to the uncertainty of acceptance of the data generated by the test method being used. Laboratory workers using measuring equipment or gauges should be made aware of the possibility of encountering suspicious data. They must be instructed to report such suspicions immediately and request checking and recalibration of the equipment in question. A detailed discussion of how to identify and estimate the magnitude of the degree of variability in suspect results, along with an explanation of how to identify the source or sources of error, may be found in Chapter 18 of Juran’s Quality Control Handbook, Fourth Edition.

18

References

considered to be normal, would be flagged as abnormal if the same concentration appeared at 2:OO A.M. Another indication of spurious data that could be flagged for attention is a large difference in values reported for two successive time intervals. The difference in concentration values which might be considered excessive may vary from one sampling location to another for the same contaminant. Ideally, this difference in concentration is determined through a statistical analysis of historical data. For example, it may be determined that a difference of 0.05 ppm in an SO2 concentration for successive hourly averages occurs rarely (less than 5 % of the time). But at the same location, the hourly average CO concentration may change by as much as 10 ppm. The criteria for what constitutes an excessive change may also be linked to the time of day and contaminant relationships (e.g., high concentrations of SO2 and 0 3 cannot coexist), and data in which this occurs should be considered suspect. Although the examples above deal with industrial hygiene data, the principles illustrated are valid for application in many laboratory situations outside the field of industrial hygiene. The validation criteria for any dataset should ultimately be determined by the objectives for collecting the data. The extent of the decision elements to be used in data validation cannot be defined for the general case. Rather, the validation criteria should be tailored along the lines suggested earlier for varying types of contaminant determinations. There are several statistical tools that can be used in the validation of data generated by continuous monitoring strip charts displaying an analog trace. Usually, strip charts are cut at weekly intervals and are turned over to data-handling staff for interpretation. The technician may estimate by inspection the hourly average contaminant concentrations and convert the analog percent of scale to other units such as parts per million (ppm). Reading strip charts is a tedious job subject to varying degrees of error. A procedure for maintaining a desirable quality for data manually reduced from strip charts is important. One procedure for checking the validity of the data reduced by one technician is to have another technician or supervisor check the data. Because the Values have been taken from the chart by visual inspection, some difference in the values derived by two different individuals can be expected. When the difference exceeds a specified amount and the initial reading has been determined to be incorrect, an error should be noted. If the number of errors exceeds a predetermined number, all data from that strip are rejected and the chart is read again by an individual other than the one who originally read the chart. The question of how many values to check can be answered by applying acceptance sampling techniques such as the use of ANSUASQC Standard Z- 1.4, Sampling Procedures and Tablesfor Inspection by

July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati, OH: National Institute for Occupational Safety and Health. January, 1987. QualityAssurance and Laboratory Operations Manual. Cincinnati, OH: National Institute for Occupational Safety and Health.

SECTION 26 DATA VALIDATION Data validation is the process during which data are checked and accepted or rejected based on an established set of criteria. This requires the critical review of a body of data to locate and identify spurious results. It may involve only a cursory scan to detect extreme values or to spot outliers, or a detailed evaluation requiring the use of a computer. In either case, when a suspect value is located, it is not immediately rejected. Each questionable value must be checked for validity. Records of values that are judged to be invalid, or are otherwise suspicious, should be kept. These records are, among other things, useful sources of information for judging data quality. There are two methods of data Validation: manual inspection and the use of computerized techniques. When employing manual validation, both the analyst or test technician and the laboratory supervisor should inspect integrated daily or weekly results for questionable values. This type of validation is most sensitive to extreme values (i.e., those which are higher or lower than expected values or appear to be outside control chart limits). These latter values are called “outlying observations” or simply “outliers.” The criteria for determining an extreme value are derived from prior data obtained from results of similar methods or, when necessary, by applying the appropriate statistical test to determine how to deal with the outlying observation. The time spent checking data that have been manually reduced by technicians depends on the time available and the demonstrated abilities of the personnel involved. The U.S. Environmental Protection Agency has suggested an audit level of 7% (i.e., checking 7 out of every 100 values). This audit level is somewhat arbitrary, and it should be subject to change when more experience with the method is gained. Computerized techniques can be used both to retrieve and to validate data. The basic system for checking extreme values by manual techniques also applies here. However, the criteria for identifying extreme values may be refined in a number of ways to pinpoint suspect data as affected by various outside conditions. For instance, the program could be made to be specific for individual hours during a period of continuous monitoring. In this way, as an example, an hourly average concentration of carbon monoxide in an air sample taken at 8:OO A.M.,

Attributes.

19

enhance its capability to meet imposed requirements. Historically, prior to World War 11, efforts toward controlling the quality of goods or services were directed chiefly toward the manufacturing sector and consisted chiefly of inspecting 100% of goods produced. Bell Telephone Laboratories had introduced the use of sampling tables in the 1920s, and Walter Shewhart, of the same organization, published his forerunner textbook, Economic Control of Quality of Manufactured Products, which described how to construct, use, and interpret statistically based control charts. These radical departures from current practice never caught on and were little used outside the fields of biometrics and social sciences. The severe manpower shortages in manufacturing during World War 11, however, made the use of 100% inspection nearly impossible, and industry needed help. Colonel Leslie E. Simon of the U.S. Army Ordnance Department published a textbook on statistical sampling methods which was the forerunner of the MIL-STD- 105 series of tables for use in attribute sampling. In 1941, a group of statisticians led by W. E. Deming traveled around the U.S. putting on courses on the use of control charts and sampling plans. These courses met with great success, and it was their “graduates” who later became the nucleus for the foundation of the American Society for Quality Control. From these early efforts, in the postwar years additional elements of quality management responsibility and more systematic approaches have evolved. These range from specific techniques to comprehensive programs. Some of those programs that were introduced, beginning in the 1950s, are:

Acceptance sampling can be applied to data validation to determine the number of data items (individual values on a strip chart) that need to be checked to determine, with a given confidence level, that all data items are acceptable. Management wants to know, without the necessity of checking every data point, whether a defined error level has been exceeded. From each strip chart with N data values, the supervising checker can randomly inspect n data values. If the number of erroneous values is less than or equal to c, the rejection criterion, the values for the strip chart are accepted. If the number of errors is greater than c, the values for the strip chart are rejected and another individual is asked to read the chart. An explanation of how to determine sample sizes and acceptance and rejection values appears in ANSUASQC Standard Z- 1.4. Another useful technique for determining the validity of data is the use of statistical tests for the significance of difference in data. In this approach, the collection of data from a sample of fixed size is required. A statistic is then computed and compared with critical values given in appropriate tables for the test selected. Examples are the t-test, x 2 (chi-square) test, F-test, and so forth. Discussions of the proper applications of these and similar tests for the significance of difference in data can be found in standard statistics texts. When using such a procedure, it is necessary to collect the specified sample observation regardless of the results that may be obtained from the first few observations. A procedure called sequential analysis requires that a decision be made after each observation or group of observations. This procedure has the advantage that, on the average, a decision as to the acceptability of the data can be reached with fewer observations. For a discussion on the use of sequential sampling plans, see Duncan’s

Zero Defects Total Quality Control Total Quality Management Quality Circles Quality is Free

Quality Control and Industrial Statistics.

References

These programs have enjoyed varying degrees of success, and the reasons that some did not survive are many, such as:

Burr, I. W. 1953. Engineering Statistics and Quality Control. New York: McGraw-Hill Book Company. Duncan, A. J. 1959. Quality Control and Industrial Statistics, Revised Ed. Homewood, IL: Richard D. Irwin, Inc. 1967. MIL-STD-78 1B. Reliability Tests, Exponential Distribution. Washington, DC: U.S. Department of Defense. July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health. 1993. ANSWASQC 21.4-1983. Sampling Procedures and Tables for Inspection by Attributes. Milwaukee, WI: The American Society for Quality Control.

Feeble management support. Union objections. No planned, complete, detailed method of attack. They were viewed as just more work-more paper with no visible benefit. They were not presented as achievable goals. Therefore, as new programs were introduced, they were greeted with: “Here we go again!” Thus, the question facing the laboratory manager is: “How do we make the concept of Continual Quality Improvement work in my organization?’ First of all, the laboratory manager and all his or her subordinates must adjust to the fact that attaining continual improvement in laboratory operations changes

SECTION 27 MEASUREMENT, ANALYSIS, AND IMPROVEMENT OF THE QUALITY SYSTEM Definition: Continual improvement is the continuing and unrelenting effort throughout the organization to

20

of performance by putting into place incremental small improvements.” The Quality Improvement Board should therefore endeavor to combine the two principles in order to get the best results from both points of view.

the way that the laboratory goes about its business. It must fold continuous improvement into its routines just as it does its chain-of-custody protocol, data validation, or laboratory proficiency testing activities. Having overcome that important hurdle, the next step is to appoint a Quality Improvement Board. The makeup of this body will vary depending on the size of the organization. However, a representative slate for a mediumsized operation might be:

PERFORMANCE EVALUATION AND MONITORING Having established a program of continuous improvement as required by ANSI/ISO/ASQ Q9001-2000, it is then important to provide means to assess the effectiveness of management’s continuous improvement efforts. In contrast to other organizations involved in quality performance evaluation, laboratories should have in place, as a part of their quality control systems, adequate information-producing activities that will satisfy this need. Typically, these are:

Laboratory Director (Manager, Supervisor, Chief Scientist, or other person) Quality Control Coordinator Laboratory section chiefs (Organic Chemistry, Inorganic Chemistry, Physical Testing, Service, and others) Typical tasks for the Board, when constituted, are:

Inter- and intralaboratory Proficiency Testing (Section 19) Data Validation (Section 26) Quality Audits (Section 30) Customer Satisfaction Reports (Section 32) Method Validation (Section 34) Quality Cost Reports (Section 36)

1. Define and establish Quality Policies and Quality Objectives (Sections 4 and 5 ) , advising the writer of the Laboratory Quality Manual on these matters. 2. Decide on how priorities and projects will be selected. 3. Establish a protocol for developing project candidates; describe how projects will be selected; appoint a Project Team Manager and decide on the composition of the Project Team. 4. Identify the need for specialized training related to Continuous Improvement (Section 13). 5. Provide necessary support-meeting facilities, clerical staff, budget allotment, and so forth. 6. Establish schedules for Board meetings, progress reports, expected completion dates, and other items. 7. Revise measurement activities such as internal audits, quality cost reports, failed test reports, customer complaint analyses, data validation results, and proficiency testing results to reflect quality improvement progression rates. 8. See that job descriptions are revised to reflect responsibility for continuous quality improvement activity. 9. Plan and budget for achievement recognition related to the Continuous Quality Improvement Program. Consider awarding certificates, Merit Awards, bonuses, or other awards. 10. Arrange for publicity for achievement related to the Continuous Quality Improvement Program. Consider bulletin board notices, newsletter articles. newspaper notices, and other forms of recognition.

Data from these sources may be supplemented by other information as deemed necessary by the Quality Improvement Board. Progress in continuous improvement efforts is monitored by analysis of audit checklist results (Part 3, Section 30) and by top management review (Section 12). References July, 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health. 13 December 2000. American National Standard. ANSI/ ISO/ASQ 49001 -2000. Quality munagement system.yRequirements. Milwaukee, WI: The American Society for Quality.

SECTION 28 STATISTICAL METHODS There are a number of statistical tools available to the laboratory practitioner which can be used to obtain more information about the data produced from analytical or test results. The purpose of this discussion is to provide a brief description of statistical techniques that are most used and are most useful in the laboratory, without presenting mathematical details. For further study, the reader is invited to consult the reference material given at the end of this section or any of the standard textbooks on statistics. The control chart is perhaps the most useful and most commonly used statistical tool available to the

Continuous Quality Improvement by “Breakthrough Improvements” vs. “Kaizen” Breakthrough Improvements are defined as: “Innovations that result in significant, one-time strides forward in laboratory performance quality.” Kaizen is defined by M. Imai as:“A gradual, step-bystep series of accomplishments which enhance the level

21

3. Identify the outliers which occur due to unusual or changing conditions of measurement; for example, a carbon monoxide (CO) concentration which is abnormally large due to a local change in environmental conditions during the time of sample collection. Such observations would not be indicative of the average concentration of CO and may be eliminated depending on the use of the data. Ideally, these unusual conditions should be recorded on the field data report.

laboratory. The use of control charts on a routine basis is also requirement of many accreditation programs. The control chart provides a method for distinguishing the pattern of indeterminate (random) error or variation from the determinate (assignable cause) error or variation. This technique displays the test or analytical data from the test or analysis in a form which graphically compares the variability of all test results with the average or expected variability of small groups of data-in effect, a graphic analysis of variance, which is a comparison of the “within groups” variability versus the “between groups” variability. The test or analytical data are plotted on a chart in units of the test result on the vertical scale against time or the sequence of tests on the horizontal scale. After a number of data points have been plotted, preferably not less than 20, the average, or mean value, is calculated and plotted on the chart. The data performance can then be compared to the mean of the data group. There are many forms of control charts, but the type most commonly used in laboratories is the X - R chart. In this type of chart, the average of a group or sample of tests is plotted on an chart and compared with the grand mean or X “average of averages” of the data. Additionally, the upper and lower control limits are calculated and plotted at three standard deviations above and below the grand mean. At the same time, the sample ranges are plotted on a companion R chart, and the average range R and the upper and lower control limits on the range are calculated and plotted in a similar manner (Fig. 22-1). Data points which fall outside the upper and lower control limits indicate a possible out-of-control condition. The laboratory should decide which control charts it intends to use, where they are to be used, and who is responsible for establishing and maintaining the charts. Once these decisions are made, procedures should be put in place to formalize the use of control charts as a part of the laboratory’s routine work. An unusually large or small value or measurement in a set of observations is referred to as an “outlier” in the statistical literature. Outliers are particularly interesting to the laboratory technician because they may appear as data points lying outside the upper or lower control limits in a control chart. The question of testing whether or not the appearance of the anomaly is of any significance then becomes important. The purpose of such tests would be to:

In the laboratory, the need often arises to determine whether or not the differences in sets of data are statistically significant. There are a number of tests available to enable the user to decide on the significance of such differences when they occur. The selection of the proper statistical test depends on the amount and kind of information that is available concerning the results in question. Three tests in common use for determining the significance of differences are: the t-test, the F-test, and the chi-square (x2)test. All of these are based on different patterns of probabilities of distribution. The tables and equations related to these distributions may be found in available textbooks. The t-test may be used for the determination of the significance of a difference between the mean or average value of a sample compared with the mean of the population when the population standard deviation is known and when the population standard deviation is unknown but can be estimated from the sample standard deviation. The t-test is also used for the determination of the significance of differences between the average or mean values of two different samples drawn from the same population when the population standard deviation is known or when the population standard deviation is unknown and is believed to be the same for both samples. The chi-square test is used to determine the significance of differences between the sample standard deviation and the population standard deviation when the population standard deviation is known. The F-test is used to determine the significance of a difference between two different sample standard deviations when the population standard deviation is unknown. The laboratory may need to use sampling techniques in the conduct of data validation, as we have seen in Section 17. In addition, certain larger organizations, which buy laboratory supplies in large quantities, may find it necessary to verify the quality of incoming lots of such material in order to ensure that it meets specified standards. In such cases, the use of sampling plans during incoming inspection is advisable as an economic alternative to 100%inspection of the materials. For simple, nondestructive inspection procedures, the use of acceptance sampling by attributes is customary. This involves determining whether a lot of items should be accepted on the basis of given specifications. A defective or nonconforming item that has a physical attribute

x

1 . Screen data for outliers and identify the need for closer control of the data-generating process. 2. Eliminate outliers prior to analysis of the data. For example, in the development of the control chart, the presence of outliers would lead to limits which are too wide and would make the interpretation and use of the control chart invalid. Incorrect conclusions are likely to result if the outliers are not eliminated prior to analysis of the data.

22

Laboratory Oual i t y Control

Operat ion

-X-R

Date

Hg! Blank Determination

chart

AUG-DDEC

99.7 99.5

x UWL x UCL

99.0

-

X . )

eo

;

*

X

98.5

LWL LCL

98.0 97.7 1

2

4

3

5

6

8

7

9

E E

10

1.4 1.2

UCL A

1.0

g m d=

UWL A

.8

.6

-

.4

R

2 0

1

2

3

4

5

O i rections: value 1. Draw R lina 0.34 2. Draw UCL, l i n e 1-11 3. Draw U K , l i n e 0.86 4. P l o t 5. oram

1 ’ s as f line

6

7

8

Samp I e Number

9

10

line

99.32

8. Draw LWL? I i n e

9825

6. Draw UCL;

7. Draw UIL; line

99.1 1

9. Draw LCL? l i n e 98.04 10. P l o t i ’ s as generated

generated

98.68

Figure 28-1

that falls outside specified limits is considered to be a “reject.” Thus, the sampling is by attributes; for instance, an item is identified as either a defect or a good item. This is often referred to as go-no-go inspection, where this refers to whether the item meets the specification when checked by a gauge or other measuring device or is inspected visually. A tabulation of sampling plans, with a complete discussion of the employment of such plans, appears in ANSUASQC STD Z1.4-1993, listed in the references below. Where inspection or testing is destructive, timeconsuming, or expensive, a considerable savings in sampling may be achieved if the decisions concerning the acceptance of a lot or dataset can be made on the basis of the actual measurements (a continuous value) rather than whether the measurements are outside specified limits. The decision on acceptance of a lot is made by variables; that is, on the basis of the comparison of the mean and standard deviation of the sample on n measurements

and given constants taken from tables provided. Variable sampling plans are described, and the related tables are furnished, in ANSUASQC STD 21.9-198 1 referenced below. References 1975. Quality Assurance Handbook for Air Pollution Measurement Systems, Vol. I. Principles. Research Triangle Park, NC: U S . Environmental Protection Agency. 1983. Industrial Hygiene Laboratory Quality Control Cincinnati: National Institute for Occupational Safety and Health. 1993. American National Standard-Sampling Procedures and Tables for Inspection by Variables for Percent Nonconforming. ANSUASQC Z1.9-1993. Milwaukee, WI: American Society for Quality Control. 1993. American National Standard-Sampling Procedures and Tables for Impection by Attributes-ANSV ASQC Z1.4-1993. Milwaukee, WI: American Society for Quality Control.

23

SECTION 29 SUBCONTRACTING SERVICES AND SUPPLIES

1. The selection of qualified outside laboratories. 2. The transmission of applicable technical and/or method requirements. 3. The evaluation of the test and analytical reports received before providing them to the customer. 4. Providing effective provisions for early information feedback and correction of nonconformances.

It sometimes occurs that a laboratory may not have the expertise or the equipment necessary to conduct a certain test when it is one of a battery of tests or analyses that the company is asked to perform. In such cases, the laboratory may elect to have the work done by an outside laboratory which is competent to perform the task required. In spite of the fact that work will be done by others, the laboratory purchasing or contracting for the work bears the ultimate responsibility for the quality of the work produced and is also responsible for assuring that all services procured from an outside source conform to requirements of the original customer. A possible exception to this may occur when the customer selects the subcontracting laboratory to be used. In this case, the responsibility of the laboratory is abdicated and devolves back to the customer. The selection of a subcontracting laboratory and the nature and extent of surveillance or control should be dependent on the nature of the test or analysis to be performed (that is, how difficult or sensitive it is), the subcontractor’s demonstrated ability to perform as witnessed by being accredited or by records of past performance, and the quality evidence made available. To assure adequate and economical control of the quality of results, the contracting laboratory should use, to the fullest extent possible, objective evidence of quality furnished by the subcontractor, such as data validation results, calibration curves, and results of routine quality checks such as blank determinations and results of duplicate or replicate tests or analyses. Once a subcontractor has been selected, the customer should be notified in writing about the laboratory’s intent to use the services of an outside laboratory for a particular test or analysis, and the customer’s written approval should be requested. It may be necessary to determine the continuing effectiveness and integrity of the control of performance quality by an outside laboratory by assessment and review at intervals consistent with the complexity and degree of usage of the service required. When conducting such assessments or audits, by tests or analytical means, all available objective evidence related to the source’s control of quality should be used in conducting the audit of the subcontracting laboratory (Section 30). Once selected, a subcontracting laboratory’s qualification record, together with particulars regarding areas of expertise and specialized equipment availability, should be entered into a Qualified Outside Laboratory Source List, which the laboratory should maintain as an up-to-date reference. The laboratory’s responsibility for control of purchased services includes the establishment of procedures for:

In summary, when a laboratory contracts work to other, outside laboratories, it must endeavor to ensure that the work meets the quality standards required by its own customer and must take steps accordingly. References 24 October 1960. Handbook H50. Evaluation pf a Contructor’s Quality Program. Washington, DC: U.S. Department of Defense. November, 2000. American National Standard. ANSVISO 17025-1999. General requirements ,for the competence o j testing and calibration luboratories. Milwaukee, WI: The American Society for Quality.

SECTION 30 QUALITY AUDITS Quality audits* conducted within the laboratory fall into two general categories: performance audits and quality system audits. Performance audits refer to independent checks made by a supervisor or auditor* to evaluate the quality of data produced by the sampling and testing or analytical system. Performance audits generally may be categorized as follows:

1. Sampling audits. 2. Analysis or test audits. 3. Data processing audits. These audits are independent of, and in addition to, the normal quality control checks made by the operator, test technician, or analyst. Independence can be achieved by having the audit conducted by a different operator/technician/analyst than the one conducting the routine measurements, or, in the case of sampling or analysis, by the introduction of audit control standards into the sampling, testing, or analytical system and the subsequent plotting of results on control charts by the supervisor. The use of audit control standards should be applied without the knowledge of the operator/technician/analyst, if possible, to ensure that the recorded results reflect normal operating conditions. Examples of performance auditing procedures are listed below. * Some accrediting organizations may use the terms sunvy, asse.wnenf, or sire visit and suweyol; assessol;or site visitor instead of audit and auditor. For the sake of clarity, we will use audit and cruditor in this work.

24

Sampling audit. As an example, the auditor uses a separate set of calibrated flowmeters and reference standards to check the sample collection system using: a. Flow rate devices b. Instrument calibration c. Instrument calibration gases, when applicable Analysis or test audits. The auditor is commonly provided with a set of duplicate samples or a split portion or aliquot of several routine samples for check analysis or test. Data processing audits. Data reporting commonly involves a spot check on calculations, and data also may be checked by inserting in the data processing system a dummy set of raw data followed by a review of the validated data.

For detailed information with regard to the conduct of an audit, see American National Standard ANSVISO/ASQC Q 10011- 1994, Guidelines for Auditing Quality Systems. References 1980. Nuclear Quality Systems Auditor Training Handbook. Milwaukee, WI: American Society for Quality Control. 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health. 1994. ANSVISO/ASQC QlOOl1-1994. Guidelines for Auditing Quality Systems. Milwaukee, WI: The American Society for Quality Control.

SECTION 31 NONCONFORMITY

A major challenge in audit planning is determining the audit frequency and, when dealing with data packages and reports in large numbers, the lot size, in order to determine the number of samples required to estimate population quality with a specified confidence level. A system audit is an on-site inspection and review of the quality assurance system. Since most quality systems are described by the organization’s quality manual, the audit becomes a check to see whether or not the laboratory is following all the policies and procedures prescribed by its own manual, including those requirements imposed by any applicable quality standard under which the laboratory is operating. This audit not only involves areview of all parts of the quality manual which describe how the laboratory’s operating procedures ensure compliance with applicable sections of any national quality standard as cited above but also a physical inspection of records such as Document Change Notices, Minutes of the Quality Improvement Board, Customer Satisfaction Surveys, training records, calibration records, and so on. System audits must be conducted by someone from outside the laboratory quality assurance activity, such as a supervisor from another laboratory, an outside consultant, an auditor from an accrediting body, or, in some cases, an individual from the accounting component of the organization who is familiar with the overall operation of the laboratory. Internal quality system audits should be conducted at least annually, and more often if conditions warrant. Corrective action (Section 33) should be initiated promptly as soon as findings of any operational deficiencies appear, and provision should be made for follow-up audits to ensure that action has been taken to correct any shortcomings. Audit checklists should be prepared and used to minimize the possibility of overlooking any detail during the course of the audit. These checklists will provide a means of grading each of the various areas or quality elements checked during the audit in order to pinpoint areas where a need for improvement is found.

American National Standard ANSVASQC Z 1.4- 1993 defines “nonconformity” as: A departure of a quality characteristic from its intended level or state that occurs with a severity sufficient to cause an associated product or sewice not to meet a specification requirement. (Underline by the author.)

The question to be resolved is: What action should the laboratory take when, as a result of test or analytical procedures, customer feedback, management audits, or data validation, nonconforming results are encountered? The laboratory should establish a set of procedures to be followed when nonconforming results appear, whether obvious or suspected. Such procedures should incorporate, but are not limited to: 1. Reporting and recording the occurrence of a nonconforming event. 2. Suspension of work, and commencement of an investigation. 3. Report to the customer, if necessary. 4. Make sure that the suspect data are not included in any final report to the customer. 5. Repetition of the test or analysis. 6. If work has been suspended and final reports and any required certification of results have been withheld pending completion of corrective action, the authorization to complete the test or analytical work under advisement must be established. 7. Initiate corrective action to prevent reoccurrence of the nonconformance. Reference 1993. American National Standard. ANSVASQC Z1.4-1993. Sampling Procedures and Tables for Inspection by Attributes. Milwaukee, WI: The American Society for Quality Control.

25

consumer surveys or analyzing other indicators of customer attitudes toward the quality of the laboratory’s work output. To satisfy contractual, regulatory, or other requirements imposed by outside agencies that the laboratory demonstrate that it has aggressively sought out and monitored information to establish how well it is achieving customer satisfaction, the laboratory may need to turn to outside help for the conduct of customer surveys, telephone market research programs, collection and analyses of consumer reports in trade journals, news media, and other sources. The laboratory may turn to outside professional market research consultants or organizations or, if it is a subsidiary part of a large corporation, use the services of the marketing component of the parent company. From the results of the efforts to establish how its customers regard the quality of its work, the laboratory must be prepared to demonstrate:

SECTION 32 CUSTOMER SATISFACTION AND COMPLAINTS To satisfy requirements that a laboratory obtain and monitor information related to the customer’s satisfaction with the quality of the laboratory’s work, the organization must go to both its own and outside sources to obtain this knowledge. Internal Sources: 1. Routine personal contacts between laboratory personnel and the customer. These exchanges of information may be written or verbal. 2. Customer complaints may be made in writing or verbally. 3. Requests from the customer for retesting or repeat analyses.

These personal contacts may be informal and conducted by telephone, FAX, or E-mail. However, telephone calls should be logged and a record made of the caller’s identity, the time and date, and a short summary of the subject of the call. E-mail printouts and FAX copies should be retained on file. Formal communications such as purchase orders, contracts, and reports containing specifications, test methods, data, or test results should be filed for reference purposes. The laboratory should have a formal, established procedure for handling technical questions and complaints, whether they originate with customers or regulatory or accrediting bodies. One individual should be assigned the responsibility for handling any inquiries or complaints. The duties of this individual include, in addition to answering the inquiry or compliant:

1. The nature and content of any survey or surveys completed. 2. The frequency of surveys conducted. 3. The identity and capabilities of those conducting the survey or surveys. 4. How the results of surveys were reported and analyzed. 5. The results of any corrective action or actions taken as a result of the information garnered from the survey work. 6. Completion of the follow-up conducted to determine whether corrective action has been accomplished. The aim of these efforts to determine customers’ opinions of the quality of the laboratory’s service should be focused on how well the customer is pleased with the laboratory’s performance with regard to:

Circulating information as to the nature of the complaint to all interested personnel within the laboratory. Conducting a preliminary investigation to determine the nature and validity of the complaint. Initiating a request for corrective action (Section 3 3 ) if necessary. Advising top management if the nature of the complaint is serious or might lead to legal action. Preparing periodic reports to management with regard to the frequency and status of inquiries and complaints.

1. Promptness of service (i.e., the time elapsed from receipt of the sample or samples until the completed report of the test or analysis is received by the customer). 2. The consistency of service. Are the tests or analyses ordered by the customer always conducted by the same methods, using the same instrumentation and/or reagents ‘? 3. Precision and accuracy. Are test or analytical results within the confidence limits of the customer’s expectations? If not, how are the unexpected observations treated?

Customer requests to repeat tests or analyses should be considered to be a reflection of customer dissatisfaction. The causes for such requests must be analyzed and be considered for any necessary corrective action. With regard to the use of external sources for measuring customer satisfaction, most laboratories do not have professional staff for the purpose of conducting

The important matter of concern here is to make sure that the laboratory’s top management gives attention to satisfying the customer’s expectations and monitors continuously how well it succeeds in doing so.

26

References

to implement a corrective action program that achieves the desired results. These steps form the closed-loop system that is necessary for corrective action success, to wit:

Juran, J. M. 1988.Juran’s Quality Control Handbook, 4th Ed. New York: McGraw-Hill Book Company. Vavra, T. G .2002. I S 0 9001:2000 And Customer Satisfaction. Quality Progress 35(5):69-75.

1. The method specifies the required quality. 2. The quality report compares actual results with expected specified results and reports a nonconformity. (Note: This would be a method, analytical, or test result nonconformity-not a nonconformance to a sample specification.) 3. The Corrective Action Analyst, who has been given responsibility for the task, initiates an investigation, including a root-cause analysis, if necessary, and including engineering, research, or testing investigators, if needed. This inquiry should result in recommended changes to correct the nonconformity and make sure that it does not occur again. 4. The Corrective Action Analyst reports on corrective action measures taken. 5. The Quality Control Coordinator follows up to see that the corrective action measures have indeed been completed. He checks results and analyzes quality to ensure that the corrective action “fix” is appropriate and has succeeded in achieving the desired results.

SECTION 33 CORRECTIVE AND PREVENTIVE ACTION In a quality assurance program, one of the most effective means of preventing trouble is to respond immediately to reports of suspicious data or equipment malfunctions from the test or analytical operator. The application of proper corrective action at this point can reduce or prevent the production of poor-quality data. Established procedures for corrective action are often included in the method for the operator’s use when performance limits are found to be exceeded either through direct observation of the parameter in question or through review of control charts. Specific control procedures, calibration, presampling, or preanalysis operational checks, and so forth, are designed to detect instances in which corrective action is necessary. A checklist for logical alternatives for tracing the source of a sampling or analytical error is provided to the operator. Troubleshooting guides for operators, field technicians, or laboratory test or analytical technicians are generally found in instrument manufacturers’ manuals. On-the-spot corrective actions routinely made by technicians should be documented as normal operating procedures, and no specific documentation other than notations in the laboratory workbook need be made. Long-term corrective action is taken to identify and permanently eliminate causes of repetitive nonconformance. To improve the quality of test results to an acceptable level and to maintain the quality at that level, it is necessary that the quality assurance system be sensitive and timely in detecting out-of-control or unsatisfactory conditions. It is equally important that, once the conditions of unacceptable results are indicated, a systematic and timely mechanism be established to assure that the condition is reported to those who can correct it and that a positive loop mechanism is established to assure that appropriate corrective action has been taken in a timely manner. For major problems, it is desirable that a formal system of reporting and recording of corrective actions be established. Experience has shown that most problems will not disappear until positive action has been taken by management. The significant characteristic of any good management system is the step that closes the loop-the initiation of a change if the system demands it. Effective corrective action occurs when several individuals and departments cooperate in a planned program. There are several essential steps that must be taken

Corrective actions should be a continual part of the laboratory system for quality, and they should be formally documented. Corrective action is not complete until it is demonstrated that the action has effectively and permanently corrected the problem. Diligent follow-up is probably the most important element of a successful corrective action system. The document usually employed in a corrective action system is the Corrective Action Request (Fig. 32-1, Part 4), or CAR. The CAR may be initiated by any individual in the laboratory encountering a major problem. However, it should be limited to a single problem. If more than one problem is involved, each should be documented on a separate Corrective Action Request form. Corrective action can be informal if the organization is small or the problems few. When this is not the case and the problems are severe or numerous, corrective action status records may be needed. In addition to the CAR, the system is supplemented by the use of a Corrective Action Master Log (Fig. 32-2, Part 4). Each CAR is assigned a sequential number and logged in with the appropriate information. Even if a problem is reported by letter, memo, customer complaint, or by other means, a CAR should be completed and logged in for action and follow-up. A side benefit of corrective action is that it may be the source of information which offers the opportunity to identify probable causes of potential nonconformances so that they can be averted before they occur.

27

The laboratory should therefore put in place a system designed to identify all sources of available information which would act as indicators that a nonconformance might occur. In a manner similar to corrective action, a system should be developed which will actively seek out potential trouble sources, assign responsibility for investigation, and devise and implement actions needed to eliminate root causes for probable nonconformances. These actions should be documented in a manner similar to that employed in a corrective action procedure, using similar forms and records. There are many sources of indicators of potential nonconformance in the laboratory, such as:

Bush and Taylor (1981). OSHA has developed protocols for both organic and inorganic methods suited to their special logistical and legally imposed needs. ASTM (American Society for Testing and Materials) uses ruggedness testing and then collaborative testing to validate methods. Method validation is, of course, a part of the broad scheme of laboratory quality control and quality assurance systems. Quality control technology, including the use of method validation, has been well-described in numerous articles and books. There is at least one expert system, computer-based, designed to support quality control by providing rapid advice to furnish data for method validation objectives. References

Management review (Section 12) Results of proficiency testing (Section 19) Instrument calibration results (Section 22) Preventive maintenance (Section 23) Data validation (Section 26) The measurement, analysis, and improvement of quality system activities (Section 27) Customer complaints (Section 32) Method validation (Section 34)

Gunderson, E. C. and Anderson, C. C. 1980. Development and Validation of Methods for Sampling and Analysis of Workplace Toxic Substances. Research Report - Contract # 21 10-76-0123. Cincinnati: National Institute for Occupational Safety and Health. Bush, K. A. and Taylor, D. G. 1981. Statistical protocol for the NIOSH validation tests. In Chemical Hazards in the Workplace-Measurement and Control, ed. G . Choudery, ACS Symposium Series No. 149. Washington, DC: American Chemical Society. Dux, J. P. 1986. Handbook of Quality Assurance for the Analytical Chemistry Laboratory. New York: Van Nostrand Reinhold. Garfield, F. M. 1984. Quality Assurance Principles for Analytical Laboratories. Arlington, VA: Association of Official Analytical Chemists.

Preventive action then is both a complement and a supplement to corrective action. Reference 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health.

SECTION 35 RELIABILITY Some laboratories engaged in work where readings generated by remote recording instruments provide the data with which the laboratory must work are vitally interested in the reliabililty of such instrumentation. This section, then, is provided to offer the Quality Control Coordinator basic information about how to deal with concerns about instrument reliability. The reliability of a measurement system is defined as the probability that the system will perform its intended function for a prescribed period of time under the operating conditions specified. Conversely, unreliability is the probability of a device failing to perform as specified. The consideration of reliability is becoming increasingly important because of the increase in complexity and sophistication of sampling, analysis, automatic recording, and telemetering systems. Furthermore, data interpretation depends on data completeness (no breaks in the dataset) for trend analysis. Generally, as equipment becomes more complicated, its probability of failure increases. The subject of reliability is complex. It is a discipline related to, but separate from, quality control. Therefore, reliability really deserves a separate, more detailed treatment. However, because of the relationship

SECTION 34 METHOD VALIDATION The National Institute for Occupational Safety and Health (NIOSH) and the Occupational Safety and Health Administration (OSHA) have for a number of years conducted method validation procedures as described in the references below. Presently, because of operational, regulatory, and liability considerations, it is virtually impossible to operate a laboratory without using validated methods. Wernimont says: The most important single attribute of a measurement process is whether it can be made to run in a state of “statistical control.” Although repetition of measurement is subject to variability, the achievement of statistical control implies that the statistical properties of this variability are uniform over time, so that it becomes meaningful to use measurements [taken] over a limited time span to predict limits of variation for both those and future measurements and to assign the level of confidence to be associated with the limits.

NIOSH Method Validation procedures are described in publications by Gunderson and Anderson (1980) and

28

by the manufacturer. This specification should consist

between reliability and quality control, a brief treatment of reliability elements is given here for the benefit of those laboratories for which unattended instrument performance is a matter of concern. Quality assurance may be thought of as the activity monitoring product or service quality up to or at a given point in time, whereas reliability assurance is that activity concerned with satisfactory product or service performance over a specified or expected period of time. To assure high reliability (i.e., completeness of data), several factors will need to be considered.

Of

1. The product reliability definition, which includes: (a) all functional requirements of the device; (b) safety requirements; and (3) resistance to environmental effects. 2. Allowable failure probabailities expressed as minimum mean time between failures (MTBF) or mean time to failure (MTTF).

EQUIPMENT FAILURERATEMTBF OR MTTF CAN BE PREDICTED FROM PERFORMANCE HISTORY

EXTERNALFACTORSINFLUENCE RELIABILITY ASSURANCE

1. Reliability predictions are made through the summation of known or estimated failure rates of individual components that make up the system. 2. Estimates of component failure rates are obtainable in military standards and from the GIDEP Data Bank (see Section 14). 3. Estimates of the chance of failure-free operation for a specified time period are calculated, assuming the failure rate is constant, by: ps -- R = e - t / m = e-th

Reliability assurance systems are applied to a wide range of instruments, gauges, and measuring systems. Differences are in complexity, kind of use, and the number of pieces of equipment involved. Factors that affect reliability or effectiveness, and should be taken into consideration in planning programs, are: 1. The severity of the reliability requirement. 2. Criticality of the device to the achievement of the desired results. 3. Type of equipment (continuous duty, intermittent duty, one-shot, and so forth). 4. Ambient working conditions. 5 . Established design or state-of-the art equipment to be used. 6. Training, experience, and capability of the operating personnel.

where: P, = R = probability of failure-free opertion for a time period 2 t e = 2.7 18 (the natural log) t = a specified time of failure-free operation m = MTBF h = failure rate (reciprocal of m ) 4. Mean time-to-failure rates will be estimated by the same formula except that here m now refers to MTTF. 5. Uptime will be the running-time data on which the MTBF and MTTF records are based. Downtime will be the time span caused by failure between stop and start records or uptime subtracted from total elapsed running time. 6. Excessive downtime should be analysed and corrective action taken, changing availability factors as necessary to improve operations. Such factors are: a. Redundancy. b. Factors associated with spares. c. Operational and maintenance factors. d. Logistics support factors. e. Detection capabilities. 7. Failure rate estimates should be made as data become available and should be maintained in a current condition for each item and/or class of equipment. These estimates are made in order to: a. Estimate spares requirements. b. Estimate end item replacement requirements. c. Estimate end item backup requirements. d. Estimate maintenance requirements. e. Establish reliability goals. f. Compare realized MTBF values with estimates. g. Establish focal points for corrective action.

RELIABILITY PROGRAMS MUSTBE PLANNED IN ADVANCE Reliability assurance programs, having been designed in consideration of the factors above, should be planned prior to implementation to include the following tasks: 1. Specifications development. 2. Environmental requirements review. 3. Statistical test planning and test data reduction. 4. Failure data system planning. 5. Data analysis planning and programming. 6. Failed parts analysis. 7. Life tests to failure. 8. Quality control coordination. 9. Field tests. 10. Reliability prediction data collection. 1 1. Development of an organization responsible for the reliability function.

EQUIPMENT RELIABILITY REQUIREMENTS MUST BE SPECIFIED IN CONTRACTS Equipmentrelilabililty requirements must be included as a specificationin procurement contracts and must be met

29

INCOMING EQUIPMENT SHOULD BE TESTED AND INSPECTED FOR QUALIFICATION AND ADHERENCE TO CONTRACT SPECIFICATION FOR RELIABILITY

training can be accomplished by the use of lectures, demonstrations, films, posters, and reliability information bulletins. At the supervisory level, in addition to the above, training should be given in the analysis of reported data, program planning, testing, and demonstration procedures. The reliability of the measurement system depends, to a large extent, on the training of the opertor. The completeness of the data, as measured by the proportion of valid data reported, is a function of both the reliability and maintainability of the

1. Quality control acceptance tests should be conducted to determine whether the product in question meets performance and design specifications at the time of testing. 2. Reliability tests should be conducted to determine whether there is a high probability that the product will continue to meet the specified performance requirements, with the specified reliability, for its speck e d service life. 3. Qualificationtests should be coducted on a sample or samples if feasible, testing to failure, to: a. Verify adherence to specified reliability standards. b. Generate data for product improvement. c. Provide an estimate of product service life and reliability.

PROVIDE

PREVENTIVE MAINTENANCE

To prevent or minimize the occurrence of wearout failure, the components of the system subject to wearout must be identified and a preventive maintenance schedule implemented for them. This activity aids in improving the completeness of the data. This maintenance can be performed during nonoperational periods for noncontinuous monitoring equipment, resulting in no downtime. Replacement units should be employed in continuous monitoring systems in order to perform the maintenance while the system is performing its function. Scheduled downtime may also be employed.

Burn-in tests should be conducted for specified times where there is an indication of early failures.

CONTROLTHE OPERATING CONDITIONS Environmental factors affecting performance or reliabililty may be natural, induced, or a combination of both.

CONSIDER MAINTAINABILITY AT THE TIMEOF PURCHASE

1. Natural environmental factors are: a. Barometric pressure changes. b. Temperture. c. Particulate matter, such as sand, dust, insects, fungus, and other particles. d. Moisture, such as icing, salt spray, high humidity, and other sources. 2. Induced factors are: a. Temperature,either self-generated or generated by adjacent or ancillary equipment. b. Dynamic stresses, such as shock and vibration. c. Gaseous and particulate contamination, such as exhaust or combustion emissions. 3. Combined natural and induced conditions. Frequently, the stresses affecting an item result from a combination of one or more factors from both classes. Such combinations may intensify the stress, or the combined factors may cancel each other out.

Maintainability is the probability that the system will be returned to its operational state within a specified time after failure, For continuous monitoring instruments, maintainability is an important consideration during procurement and in some cases may be desirable to include in the purchase contract. Maintainability items to consider for inclusion at the time of procurement are: 1. Design factors: a. The number of moving parts. b. The number of highly stressed parts. c. The number of heat-producing parts. 2. Ease of repair after failure has occurred. 3. Maintainability costs: a. Inventory of spare parts required. b. Amount of technician training required for repair. c. Factory service required. d. Service repair contract required. e. Estimated preventive maintenance required.

PROVIDE FOR THE ADEQUATE TRAINING OFPERSONNEL

PROVIDE RECORDS OF FAILURE AND MAINTENANCE; ANALYZE AND USE TO INITIATE

The implementation of a reliability assurance program requires a training program at both the operational and supervisory levels. At the operator level, instruction shbuld be given in the colleckon of failure and maintenance data, in the maintenance function (both preventive and unscheduled maintenance or repair of equipment), and in the control of operating conditions. This

Field reliability data should be collected to: 1. Provide information on which to base reliability rate predictions.

30

2. Provide specific failure data for equipment improvement efforts. 3 . Provide part of the information needed for corrective action recommendations.

Category of Cost

External Failure Cost

I I I I

References Bazovsky, I. 1961. Reliability Theory and Practice. Englewood Cliffs, NJ: Prentice-Hall. Enrick, N. L. 1972. Qualilty Control and Reliability, 6th Ed. New York The Industrial Press. Haviland, R. P. 1964. Engineering Reliability and Long Life Design. Princeton, NJ: D. Van Nostrand Co. Inc. Juran, J. M. 1974. Quality Control Handbook, 3rd Ed. New York: McGraw-Hill Book Company. Muench, J. 0. 25-27 January 1972. “A Complete Reliability Program.” Paper read at Annual Reliability and Maintainability Symposium, Institute of Electrical and Electronic Engineers. San Francisco, CA. 1967. MIL-STD 7 18B. Reliability Tests, Exponential Distribution. Washington, DC: U.S. Department of Defense. 1975. Quality Assurance Handbook for Air Pollution Measurement. Research Triangle Park, NC: U.S. Environmental Protection Agency. 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati, OH: National Institute for Occupational Safety and Health.

1

1987

SECTION 36 QUALITY COST REPORTING

2

3

4

Internal Failure Cost

I

I

Appraisal Cost Prevention Cost

I I 1

Calendar Quarter

2

3

4

1988

Figure 36-1

As a management tool, quality assurance costs should be identified and recorded primarily to identify elements of quality assurance programs whose costs may be disproportionate to the benefits derived. An additional purpose is to detect cost trends for budget forecasting. Before identifying and setting up a quality cost system in the laboratory, the costs of the quality function are probably widely scattered within the cost accounting system of the organization. It is important then to define those elements and subelements which make up the total quality cost package and adjust the cost accounting system to be able to accumulate and present an accurate quality cost picture to management. The American Society for Quality lists four principal categories for quality costs, as follows:

that fail to meet quality requirements and thus result in manufacturing losses. 4. External-failure costs generated as a result of defective products having been shipped to customers. An examination of these categories, which do not fit very well into the laboratory environment, will, however, give a frame of reference around which a new set of categories, attuned to laboratory operations, may be developed. Since, obviously, the quality assurance activities in laboratories will be different from those in manufacturing, it is more practical to categorize cost areas as follows:

1. Prevention costs associated with personnel engaged in designing, implementing, and maintaining the quality system. (Maintaining the quality system includes auditing the system.) 2. Appraisal costs associated with the measuring, evaluating, or auditing of products, components, and purchased materials to assure conformance with quality standards and performance requirements. 3. Internal-failure costs associated with the manufacture of defective products, components, and materials

1. Prevention costs associated with keeping unacceptable data from being generated in the first place. Included here are such things as quality, planning, and quality control training, for example. 2. Appraisal costs associated with efforts to maintain measurement system performance quality levels by formal audits of performance quality levels and interlaboratory and intralaboratory testing programs, for example.

31

c. Cost of replacing samples and rerunning tests or analyses.

3 . Internal-failure costs caused by the occurrence of determinations or test results that do not meet acceptance standards. These include voided data, spoiled test or analytical samples, and repeated or duplicated tests. 4. External-failure costs caused by unacceptable test or analytical results that have already left the laboratory. This involves effort spent in corrective action, investigations, and repeated tests or analyses required in order to gain customer satisfaction.

After quality cost elements have been listed, it is necessary to allocate to them cost figures available from the accounting system. If actual cost figures are not available, then the accounting component should provide estimates that are as nearly exact as possible. It will usually be found that the costs are not uniformly distributed over the range of elements, a disproportionate percentage generally appearing in appraisal and internal- and external-failure costs. It has been found that a relatively small increase in prevention expenditures will yield large reductions in appraisal and failure costs. Therefore, the laboratory management should consider adoption of preventive measures to reduce total quality control costs. The quality control cost report should be presented periodically to management, showing the costs allocated to each of the four major quality cost categories and the relationships of the individual category costs to total quality costs. It may also be useful to provide further detail showing quality costs for each subelement within the major cost categories. Graphic presentations should be made where appropriate (Fig. 36-1).

Within each major cost category appear a number of subelements, as follows: 1. Prevention costs

a. Quality planning. b. Document control and revision, including measurement method writeups. c. Quality training. d. Quality assurance plans for projects and programs. e. The quality assurance manual. f. Preventive maintenance. 2. Appraisal costs a. Quality assurance activities associated with pretest preparation, sample collection, sample analysis, and data reporting. b. Data validation. c. Procurement quality control. d. Statistical analysis of data. e. Calibration. f. Interlaboratory and intralaboratory testing. g. System audits. h. Quality reports to management, including quality cost reports. 3. InternalTfailure costs a. Scrapping of defective materials. b. Cost of rerunning tests or repeating analyses. c. Costs of corrective action efforts. d. Investigation or research efforts. 4. External-failure costs a. Investigation of complaints from outside sources. b. Cost of corrective action efforts.

References Feigenbaum, A. V. 1961. Total Quality Control. New York. McGraw-Hill Book Company. Juran, J. M. 1974. Quulity Control Handbook. New York: McGraw-Hill Book Company. Juran, J. M. and Gryna, F. M. 1970. Quuliv Planning and Analysis. New York: McGraw-Hill Book Company. Masser, W. J. 1957. “The Quality Manager and Quality Costs.” Industrial Quality Control XIV (4):5-8. Rhodes, R. C. 1972. “Implementing a Quality Costs System.” Quality Progress 5 (2):16-19. 1986. Principles o j Quality Costs. Milwaukee; WI: The American Society for Quality Control. 1983. Industrial Hygiene Laboratory Quality Control. Cincinnati: National Institute for Occupational Safety and Health.

32

Laboratory Quality Assurance System, 3rd Edition. Thomas A. Ratliff Copyright 02003 John Wiley & Sons, Tnc. 4SBN: 0-471-26918-2

Part 2

HOW TO WRITE A LABORATORY QUALITY ASSURANCE MANUAL SECTION 37 INTRODUCTION

which will affect the quality of the laboratory “product,” remembering that the precision and accuracy of analytical or test results are the measures of the laboratory’s performance quality. The Quality Control Coordinator is normally the individual assigned the task of producing the quality manual. Others may be assigned to assist him or her in gathering information and drafting portions of the manual. Additionally, other managers must be made aware of the program and their responsibility to provide procedures, forms, and information affecting laboratory quality. The organizational steps necessary for producing the laboratory quality manual are:

All laboratories employ some sort of quality program or system, but some are more structured and identifiable than others. When a laboratory, driven by regulatory, accreditation, or marketing pressures, decides that it must have a formal, written quality program described in a manual, the question of cost is immediately raised. As we have seen in the discussion of quality costs in Section 36, laboratory quality cost benefits are often not available or identifiable due to the structure of the organization’s accounting system. On the other hand, the efforts made to set up a new laboratory system involving new forms, the introduction of new procedures or changes to existing procedures, added techniques, and so forth are highly visible as expenses. The purpose of Part 2 of this book is thus to disclose to quality practitioners in the laboratory a technique that will lead to the efficient development of a quality manual that describes a system that is not too cumbersome for the laboratory it supports and is not counterproductive because of excessive demands for paperwork and reports.

Establishment of quality policies and objectives (Sections 4 and 5). Collection and review of existing applicable procedures. Preparation of a flowchart. Identification of quality system requirements to be selected. Fitting of existing procedures to requirements. Identification of shortfalls. Establishment of priorities. Writing the manual. Reviewing and making necessary changes.

SECTION 38 ORGANIZING FOR PREPARATION OF THE MANUAL Before dealing specifically with how to go about writing a laboratory quality manual, it would be wise here to firmly establish the purpose or purposes of the document. This is done in order to be able to keep constantly in mind, during the production of the manual, the reason for writing the documents, so that the contents will enable the organization to satisfy the requirements for which the manual is produced. Basically, the quality manual is a document setting forth the laboratory’s policies and operating procedures

SECTION 39 ESTABLISHING OBJECTIVES AND PRIORITIES Since the quality program should be developed to meet the requirements of accrediting bodies, government regulations, higher management, or marketing pressures, it is important that, in planning the laboratory quality program, the considerations above are incorporated into the

33

actually being followed. It is up to the investigator to ferret those out and bring them to the attention of higher management to decide whether any have merit and should be brought into the formal system, or, conversely, if such unauthorized procedures are working to the detriment of the organization, take measures to eliminate their use. The end result of this activity should be a compilation of documents and forms that the Quality Control Coordinator will incorporate as a part of the final quality document. It should be pointed out that a useful tool for keeping track of and filing the various documents that have been collected during the investigation is an “everyday file” fast sorter. After making up a tentative table of contents, the sorter can be used to file the collected documents in numerical order.

system. It is essential at this stage that quality objectives and policies be established and clearly described. These descriptions must be in writing and should be endorsed by the signatures of top laboratory management (see Sections 4 and 5). One way of obtaining the endorsement and support of management is for the Quality Control Coordinator to draft sets of recommended objectives and policies for submission to management for review. After discussion and revision, agreement is reached establishing the course of the laboratory’s programmed activity, and management returns the endorsed objectives and policies to the Quality Control Coordinator. Once the tenor of the laboratory’s quality program has been established, planning can commence. Through either the formal publication of quality objectives and policies or by a letter of promulgation, it should be made clear to all personnel in the organization that the quality manual is an expression of management’s intent that its provisions be binding on all individuals and departments, sections, or branches of the laboratory and is not a document meant just for the quality department. It is thus desirable that as many individuals as possible within the laboratory participate in the preparation and drafting of the document.

SECTION 41 PREPARATION OF A FLOWCHART The next step in the preparation of the laboratory quality manual should be to draw up a detailed analytical or testing operations flowchart. As an illustration, the operations of an industrial hygiene analytical laboratory will be used, showing two parallel flow paths that demonstrate what happens when a sample arrives at a laboratory and moves through the laboratory to final disposition (Fig. 41-1). We have then:

SECTION 40 COLLECTION AND REVIEW OF EXISTING PROCEDURES Whether or not they consider present practices to be a part of a formal quality control system, all laboratories have existing procedures, formal and informal, written or unwritten, that guide their activities and affect the quality of laboratory output. Having established the quality objectives and policies for the laboratory, the next step is to establish an inventory of existing procedures that affect quality and govern the work, either formally or informally, within the organization or in its relationships with other organizations. Procedures are considered to be such things as instructions on the use and distribution of forms and reports, standing operating procedures, detailed explanations of policy statements, protocols for the conduct of interlaboratory testing programs, or any other instruction, rule, or document that governs the conduct of laboratory operations and affects the quality of laboratory output. In small laboratories, the Quality Control Coordinator may have most of the desired information at his fingertips. In larger organizations, it may be necessary to conduct interviews with other department heads and their subordinates, circulate questionnaires, hold meetings with outside agencies, and spend a great deal of time and energy on preliminary investigation. In larger organizations where written policies and procedures have been in existence for some time, there very often exists a subculture of unwritten procedures which are those

1. A flowchart of the path of the sample from receipt through the analytical or test cycle until the report of results is rendered and disposition of the sample is made. 2. A flowchart of the documentation accompanying the sample as well as that generated through the analytical or test cycle. The chart begins with the sample test request and follows through the analytical or test cycle, preparation of the report, and on to distribution of the copies. Preparing the flowchart also provides the opportunity to scrutinize and identify the details of laboratory operations that affect the quality of laboratory output and provide the ground work for the next step in the preparation of the manual, identification of the quality system elements to be selected. In the smaller laboratory, the person designated to prepare the manual may have enough familiarity with the detailed operations of the organization that he or she can prepare the flowchart without having to seek assistance from outside sources. In larger laboratories, assistance in the preparation of the flowchart may be needed from each different department, section, or branch involved, after which the results are combined to establish the flow of work through the laboratory. Given this

34

FIELD INDUSTRIAL HYGIENIST I

Q Bonded Stores

A ( Al iquots

Sample Analysis Request

CLERK Test Sample ASSIGNS Location LAB=

RECEIVING CLERK

TECHNICIAN

-

I

I

1

#

Analyst Work Sheet

-h

--

SUPERVISION ASSIGNS WORK

Analyst

ANALYSIS 2

ANALYSIS 2

LABORATORY NOTEBOOK ENTRI ES

Formal Report

Figure 41-1

the writer to decide on the merit of such unprogrammed activity and take action to adopt or to eliminate it. The next step is to critically review the flowchart to make sure first that it is a fair representation of the procedural system in the laboratory and then, if it is, determine

information, the Quality Control Coordinator or other person preparing the manual should be able to identify those activities that relate to the quality control function. It is during this period that laboratory procedural subcultures may be discovered. It then behooves

35

SECTION 44 WRITING THE MANUAL

whether there is any need for improvement to increase efficiency by eliminating or combining steps to streamline operations.

Presented here are tips and suggestions made to assist the writer in preparing a more acceptable document that will meet the requirements of most regulatory and accrediting organizations. 1. Start with a title page (Section 2), followed by a table of contents. A Letter of Promulgation signed by the highest available authority is not essential but is a definite asset if the laboratory management will actively and demonstrably pursue its commitment to quality. If the letter of promulgation is merely lip service to a requirement grudgingly accepted, then the letter is worse than useless and should be omitted. 2. There is no particular order in which the table of contents should be listed or in the order of appearance of the various elements described in the manual. It seems logical, however, that the goals, policies, and organization sections of the manual should appear early and in that order. 3. The pages of each section of the manual should be numbered sequentially, beginning with “1” with each new section. This makes it easy to insert new pages, should it become necessary at a later date, without having to renumber all subsequent pages of the document. 4. The paragraph numbering system should be uniform throughout the manual. The system may be numeric or alphanumeric but should be the same in each section of the document. 5. The format of each section, onceestablished, should be kept consistent throughout the document. 6 . Blank copies of all forms, tags, labels, stickers, reports, and so on, whenever mentioned in the text of the manual, should be included, either directly following the page on which they are referenced or, in order, at the end of each section. For easy reference, this is preferable to incorporating all forms at the end of the entire document. The latter is not unacceptable, but in the case of a large organization having many formalized procedures, this practice becomes inconvenient. Each form should be numbered and referenced back to the point where it is mentioned in the text.

SECTION 42 IDENTIFICATION OF PROGRAM REQUIREMENTS By this time, the outline of the content of the manual should be taking shape in the mind of the person preparing the manual, and he or she should be in a position to prepare a tentative table of contents. Using the information derived from taking an inventory of existing procedures, taking into consideration requirements generated by the establishment of quality goals and policies and reviewing the requirements of regulatory or accrediting bodies, a list of elements that will comprise the laboratory’s quality system can be prepared.

SECTION 43 IDENTIFICATION OF SHORTFALLS AND THE ASSIGNMENT OF PRIORITIES Once the list of elements is prepared and all are in agreement that this is acceptable as the way for the laboratory to conduct its quality business, the next step is to identify the procedures that are already in place within the organization and then, further, to identify those that are not in existence and must be developed. It is here that the everyday file becomes useful since it can be used to accumulate the various written procedures and forms applicable to each element and file them by subject matter. The elements that need to be developed will have blank pockets and thus be easily identified. Having established what new procedures need to be developed to complete the manual in the manner desired, it will be necessary to establish a priority for accomplishing these tasks. Obviously, not all new procedures can be developed and put into place simultaneously, so the person preparing the manual must decide the sequence in which the new material is to be developed. Once these new procedures have been developed, the writer is ready for the final step.

36

Laboratory Quality Assurance System, 3rd Edition. Thomas A. Ratliff Copyright 02003 John Wiley & Sons, Tnc. 4SBN: 0-471-26918-2

Part 3

XYZ LABORATORY QUALITY ASSURANCE MANUAL INTRODUCTION This part contains a representative example of a Laboratory Quality Assurance Manual. It is intended to be used as a model to be copied, amended, supplemented or extracted from in order to tailor a document that will accurately describe a particular laboratory's operations. It may also be used as a model against which a laboratory's existing manual may be compared to determine how the latter document compares with current doctrine. The sample manual incorporated 27 elements if a typical quality system. The elements are those prescribed by American National Standards ANSVISO/ASQ 49001-2000 and/or ANSUISO 17025- 1999. However, many laboratories will find that they do not use nor will they choose to incorporate all of the elements described. Selection of the individual organization's components for its particular way of conducting laboratory operations depend on regulatory or accrediting requirements, management decisions, and marketing pressures. This part should be used in conjunction with the descriptive material in Part I . The organizational structures, job descriptions, procedural details, and forms, should, of course, be amended and designed to reflect the user's operations.

37

QUALITY ASSURANCE MANUAL

XYZ LABORATORIES,INC. 11 1 Main Street Anytown, MA 45222

Prepared by:

Name & Title: Approved:

Name & Title: Date: Copy No.:

38

Eflecllve Date

Sectlon No.

Subject

TABLE OF CONTENTS

BY Approved

QUALITY ASSURANCE MANUAL

Page Revised

TITLE 1 .o

INTRODUCTION

2.0

LETTER OF PROMULGATION

3.0

MANAGEMENT OF THE QUALITY MANUAL

4.0

QUALITY POLICIES

5.0

QUALITY GOALS AND OBJECTIVES

5.0

THE QUALITY ORGANIZATION

7.0

QUALITY PLANNING

8 .o

QUALITY IN PROCUREMENT

9.0

SAMPLE HANDLING, STORAGE AND SHIPPING

10.0

CHAIN-OF-CUSTODY PROCEDURES

11.0

LABORATORY TESTING AND ANALYSIS CONTROL

12.0

QUALITY DOCUMENTATION AND RECORDS CONTROL

13.0

CONTROL OF MEASURING AND TEST EQUIPMENT

14.0

PREVENTIVE MAINTENANCE

15.0

REFERENCE STANDARDS

16.0

DATA VALIDATION

17.0

ENVIRONMENTAL CONTROLS

18.0

CUSTOMER SATISFACTION AND COMPLAINTS

19.0

SUBCONTRACTING

20.0

PERSONNEL TRAINING, QUALIFICATION AND MOTIVATION

21.0

STATISTICAL METHODS

22.0

NONCONFORMITY

39

Of

2

I

Effectlve Date

I

Sublect

BY

Approved

23.0

TABLE OF CONTENTS

QUALITY ASSURANCE MANUAL

CORRECTIVE ACTION

24.0

QUALITY COST REPORTING

25 .O

QUALITY AUDITS

26.0

RELIABILITY

Z7.0

METHOD VALIDATION

Z8.0

QUALITY MANUAL FORMAT SHEET

40

I

Section No.

Pwe

Revired

Of

2

Effecllve Date

Subject

INTRODUCTION

Section No.

1.0

Pwe

BY

lot

Revised

Approved

T h i s m a n u a l is i s s u e d t o d e s c r i b e t h e q u a l i t y a s s u r a n c e system e m p l o y e d a t XYZLaboratories, I n c . i n c o m p l i a n c e w i t h t h e i n t e n t o f t h e g e n e r a l q u a l i t y system requirements o f t h e c o g n i z a n t a c c r e d i t i n g o r g a n i z a t i o n . T h e p o l i c y o f X Y Z i a b o r a t o r i e s , I n c . is t o a p p l y t h e system t o alltestingandanalyticalactivitiesundertakenonbehalfofthe customers or a n a c c r e d i t i n g o r g a n i z a t i o n . The manual p r o v i d e s personnel and customers of XYZLaboratories,

I n c . w i t h a d e s c r i p t i o n of company p o l i c y f o r m a i n t a i n i n g a n e f f e c t i v e and economical q u a l i t y a s s u r a n c e system planned and developed i n c o n j u n c t i o n w i t h o t h e r management p l a n n i n g f u n c t i o n s . Written procedures f o r implementingthe p o l i c i e s described herein

are a m p l i f i e d b y t h e s e v e r a l s e c t i o n s c o m p r i s i n g t h i s manual. These p r o c e d u r e s are b i n d i n g on a l l p e r s o n n e l of t h e l a b o r a t o r y and s h a l l be adheredtoimplicitly.

41

1

Effective Date

t

2.0

Page

BY Approved

' Section No.

Subjecl

LETTER OF PROMULGATION

t

1'01

1

Revised

I

The Q u a l i t y Assurance Program d e s c r i b e d i n t h i s Q u a l i t y Assurance

Manual h a s t h e a b s o l u t e a n d u n q u a l i f i e d s u p p o r t o f X Y Z L a b o r a t o r i e s , I n c . Management. Our e s t a b l i s h e d g o a l - d e l i v e r a n c e of h i g h e s t q u a l i t y s e r v i c e a t a f a i r p r i c e i s t h e same t o d a y as when t h e l a b o r a t o r y was founded i n 1932.

Our t e s t i n g and a n a l y t i c a l s e r v i c e s - t h e i r p r e c i s i o n and a c c u r a c y , t h e carewithwhichtheyareconducted, and theircustomeracceptance-are themeansbywhichXYZLaboratories, Inc. has gainedanenviable

reputationandhasbecome a l e a d e r i n t h e i n d u s t r y . Q u a l i t y l e a d e r s h i p i s o u r number one p r i o r i t y and e v e r y member ofthelaboratorystaffshares t h e r e s p o n s i b i l i t y of m a i n t a i n i n g o u r p r e s e n t s t a t u s . A t XYZLaboratories, I n c . , q u a l i t y i s t h e r e s p o n s i b i l i t y o f e v e r y

employee. Meeting t h i s commitment w i l l r e s u l t i n t h e c o n t i n u e d s a t i s f a c t i o n o f o u r c u s t o m e r s andanimprovedqualityoflife for o u r employees. The p r o v i s i o n s o f t h i s m a n u a l , describingtheXYZLaboratories, I n c .

Q u a l i t y System, are b i n d i n g on t h o s e i n d i v i d u a l s given t h e responsibilities outlined herein. I w i l l expect everyone c o n c e r n e d t o u s e t h i s manual as a g u i d e t o t h e

c o n t i n u e d m a i n t e n a n c e and improvement o f t h e q u a l i t y of o u r l a b o r a t o r y services. Sincerely,

42

Effective Date

BY Approved

3.1

-

Subject

Section No.

MANAGEMENTOFTHEQUALITY MANUAL

P.ge

3 .O

Revised

1

0'

Purpose The purpose o f t h i s s e c t i o n is t o d e f i n e t h e tasks and

responsibilities relating t o the preparation, distribution, review, andmaintenance o f t h e Q u a l i t y M a n u a 1 . 3.2 ScoDe

T h i s sectiondealsprimarilywiththosemanualswhichareissued

under c o n t r o l l e d c o n d i t i o n s . 3.3 I s s u e , D i s t r i b u t i o n , andMaintenance o f t h e Manual

The Q u a l i t y Control Coordinator bears t h e primary r e s p o n s i b i l i t y f o r t h e p r e p a r a t i o n , i s s u e , review, andupkeepoftheLaboratory Q u a l i t y Manual. After t h e p r e p a r a t i o n o f t h e m a n u a l , t h e Q u a l i t y C o n t r o l C o o r d i n a t o r is r e s p o n s i b l e f o r t h e i n i t i a l d i s t r i b u t i o n o f c o n t r o l l e d c o p i e s o f t h e manual. C o n t r o l l e d c o p i e s are s e r i a l l y numbered, a n d a d i s t r i b u t i o n l i s t i s k e p t s h o w i n g t o w h o m e a c h copy hasbeen issued. The purpose o f t h i s c o n t r o l is tomake s u r e t h a t changes are

d i s t r i b u t e d t o r e c i p i e n t s o f t h e manual when n e c e s s a r y and t h a t c o p i e s are retrievedwhenpersonnelchanges r e q u i r e t h a t t h e manual n o l o n g e r b e i n t h e hands o f t h e a f f e c t e d i n d i v i d u a l . Uncontrolled c o p i e s o f t h e manual maybe d i s t r i b u t e d , f r o m t i m e to-time to i n d i v i d u a l s or o r g a n i z a t i o n s o u t s i d e t h e l a b o r a t o r y .

These c o p i e s w i l l n o t b e numberedorloggedandwillnot r e c e i v e changes as they occur. Uncontrolled c o p i e s w i l l b e so marked.

43

2

Effective Date

MANAGEMENT OF THE QUALITY MANUAL

Approved

Section No.

Revised

The Q u a l i t y Control Coordinator is r e s p o n s i b l e f o r t h e t i m e l y ,

p e r i o d i c review o f t h e c o n t e n t of t h e manual t o e n s u r e t h a t its requirements r e f l e c t c u r r e n t o p e r a t i n g c o n d i t i o n s a n d m e e t w i t h needs. T h i s w i l l normally be done immediately f o l l o w i n g i n t e r n a l q u a l i t y s y s t e m a u d i t s o r a u d i t s , assessments, or s i t e v i s i t s b y an o u t s i d e accreditingorganization.

T h i s manual is a numbered, c o n t r o l l e d d o c u m e n t , u n l e s s o t h e r w i s e

marked. R e v i s i o n s , a d d i t i o n s , or d e l e t i o n s o c c u r r i n g a s a r e s u l t o f

p e r i o d i c review or o t h e r a u t h o r i z e d changes w i l l be c o n t r o l l e d through t h e i s s u e ofrevisionstoindividualsorlaboratory

c o m p o n e n t s l i s t e d o n t h e master d i s t r i b u t i o n l i s t . 3.4

Preparation 3.4.1

The Q u a l i t y A s s u r a n c e M a n u a l w i l l b e p u b l i s h e d u s i n g t h e

s t a n d a r d format onwhich t h i s S e c t i o n a p p e a r s . For d e t a i l s on t h e u s e of t h i s format, see S e c t i o n 33.0

3.4.2 Thismanualwillusethealpha-numericsystemofparagraphing

as i l l u s t r a t e d by Par. 11.2.2 f f . and example: 1.1

1.2 1.2.1 1.2.2

a.

44

Effectlve Date

BY

Subject

Section No.

QUALITY POLICIES

Pwe

Approved

4.0 Of

2

Revlsed

4.1 Purpose

This section lists policies to be implemented by the laboratory in order to provide guidance toward the goal of achieving continuous improvementinthe qualrty of laboratory p

w

e and in the

fbrtherance of the laboratory’s overall quality control program. 4.2 Scope

This seCtiansetsfarthody the ~Utlinesof management’s policies with regard to Quality Assurance. Details for carrying out these

paliciesappear inlater sectionsof thismanual 4.3 Laboratory quality policies include:. 43.3 Quality activities shall emphasize theprevention of quality

problems rather than detection and correction of problems

afterthey occur. 4.3.2 Quality Cost figures shall be computed quarterly and

r e p a t d t n management. 4.3.3 All Employees engaged in making decisions affecting the

~yoflabmakq~shaU&g.otrainingpragrams designed to be commensurate with their positions, duties and responsWies. 4.3.4 The laboratory shall use published analytical and test

methods whenever available.

45

Elfectlve Date

SubJecl

BY L

QUALITY POLICIES

Approved

Sectlon No. pwe

4 .O

2

0'

Revlnd

4.3.5The laboratory shall control the issue, distribution, and

retentionafalitestand.d~~t.e&jical documents; and will see that all obsolete documents are

re~avedfromnnintaafuse. 4.3-6Thelaboratory shall. hawa compn&ensivecalibration

p r o g r a m i n v o l v i n g a l l i n s t r u m e n t a t i o n u s e d for making d e t e r m i n a t i o n s , t h e results o f which are r e p o r t e d .

4 . 3 . 7 The l a b o r a t o r y s h a l l use a p p r o p r i a t e , fresh r e a g e n t s and

chemicals, c e r t i f i e d w h e n necessary, and a p p r o p r i a t e calibrated g l a s s w a r e . 4 . 3 . 8 The l a b o r a t o r y shallestablishandmaintainatotal

i n t r a l a b o r a t o r y q u a l i t y c o n t r o l system t o a s s u r e continued p r e c i s i o n and accuracy of l a b o r a t o r y r e s u l t s . 4 . 3 . 9 T h e l a b o r a t o r y s h a l l p a r t i c i p a t e i n an i n t e r l a b o r a t o r y

t e s t i n g p r o g r a m a s p r e s c r i b e d b y t h e cognizant a c c r e d i t i n g organization.

46

2

I

Effccllve Date

I

Sublect

QUALITY GOALS AND OBJECTIVE

I Secllon No. Revleed

5.1 Purpose

The purpose af this document is to delineate the Quality Qbjectives of

X Y Z Laboratories, Inc.

5.2 Scope The primary objective of the Laboratory Quality Assurance Program is to improve and maintain the accuracy and precision as well as the reliability of the laboratory “product”. Our product is the repart issued as a result of the testing or analysis of the customer’s sample. Management, administrative, statistical, investigative, preventive, and corrective actions will be employed to maximize reliability of the data.

5.3 Specific objectives are: 5.3.1 To develop and put into service rugged methods capable of meeting the user’s need for precision, accuracy, sensitivity, and specificity.

5.3.2To ensure that all staff members receive training in basic quality technology, in sufficient depth to enable them to carry out the provisions of this manual. In addition, the Quality Control Coordinator shall receive sufficient additional training to enable him

47

I I

Effecllve Dale

Sectbn No.

SubJect

QUALITY GOALS AND OBJECTIVES Psst

H BV

2

of2

Revbed

Approved

I

5.0

I

I

to receive American Society for Quality certification within the prescribed period. 5.3.3 To establish the level of quality of the laboratory’s routine

p e r f a ~ as~ a~baseline ~ ~ e against which to measure the effectiveness of continuous quality improvement efforts.

5.3,4To makeanychangesinroutine methaddcgy found necessary to make it compatible with performance needs as established in Par. 5.3.1 above.

5.3-5To monitor the rautine operational perfarmame of the laboratory through participation in appropriate interlaboratory proficiency testing pagrams and to provide for corrective actions as necessary

1 2 . 1 Purpose T h i s s e c t i o n d e s c r i b e s howthelaboratorywillcontroltheissue

and r e t r i e v a l of a l l documents r e l a t i n g t o t h e a n a l y t i c a l and

testingactivitiesofthelaboratory, t o t h e c o n t r o l o f q u a l i t y o f these a c t i v i t i e s a n d t o t h e s t o r a g e a n d s e c u r i t y o f t h e t e c h n i c a l

documentation g e n e r a t e d b y t h e s e a c t i v i t i e s . 1 2 . 2 Scope The c o n t r o l s d e s c r i b e d i n t h i s s e c t i o n a r e l i m i t e d t o t h e d o c u m e n t s

and r e p o r t s l i s t e d b e l o w , and do n o t a f f e c t documentation r e l a t e d

t o o t h e r l a b o r a t o r y management a c t i v i t i e s . Such document c o n t r o l procedures are d e s c r i b e d i n o t h e r l a b o r a t o r y s t a n d a r d o p e r a t i n g procedures. 1 2 . 3 Themost important e l e m e n t s o f t h e q u a l i t y a s s u r a n c e program t o w h i c h document c o n t r o l is a p p l i e d i n c l u d e :

Samplingprocedures Calibration procedures A n a l y t i c a l and t e s t p r o c e d u r e s

Data c o l l e c t i o n and r e p o r t i n g p r o c e d u r e s Auditingprocedures

Computationalanddatavalidationprocedures *TheQualityAssuranceYanual

A n a l y t i c a l and t e s t i n g r e p o r t s Laboratory notebooks

89

Effective Date

Section No.

Subject

BY Approved

QUALITY DOCUMENTATION AND RECORDS CONTROL

12 . 0

Page

2

0'

5

Revised

Validation reports Vendor and i n t e r n a l a u d i t r e p o r t s C a l i b r a t i o n and p r e v e n t i v e maintenance r e c o r d s C h a i n - o f - c u s t o d y documentation Technical document change r e q u e s t s Corrective ActionRequests 1 2 . 4 The q u a l i t y r e c o r d s l i s t e d a b o v e whichare o r i g i n a t e d a n d maintained a s hard c o p i e s w i l l b e r e t a i n e d for a period o f f i v e years i n laboratory f i l e s . After a period of f i v e years, they w i l l be reviewed f o r d i s p o s i t i o n . Those n o t d i s c a r d e d w i l l b e t r a n s f e r r e d t o m i c r o f i c h e and r e t a i n e d i n d e f i n i t e l y . Records g e n e r a t e d b y c o m p u t e r w i l l be r e t a i n e d i n t h a t format i n d e f i n i t e l y , with due c a r e t o k e e p i n g t h e m i n s a f e , h a z a r d - f r e e s t o r a g e . 1 2 . 5 The Q u a l i t y Control Coordinator w i l l m a i n t a i n f u l l c o n t r o l over thedistributionofdocumentslistedinPar.

12.3,above. A f i l e

c o n t r o l w i l l be m a i n t a i n e d s h o w i n g t h e f o l l o w i n g i n f o r m a t i o n : Document number

Distribution

Title

Format

O r i g i n a t o r of t h e document

F i l e location

Latest i s s u e d a t e

Lengthof r e t e n t i o n Change number

Signatureofthepersons receivingthedocument.

90

Effective Date

Section No.

Subject

12 0

QUALITYDOCUMENTATION AND

RECORDS CONTROL t

Whenevera changeismadetoacontrolleddocument, t h e Q u a l i t y Control C o o r d i n a t o r w i l l i s s u e t h e new document t o g e t h e r w i t h t h e Technical Document Change Notice ( F i g u r e 1 2 - 1 ) . The T e c h n i c a l Document ChangeNotice i s t o b e f i l l e d o u t a s f o l l o w s : ( 1 )The d a t e of p r e p a r a t i o n o f t h e C h a n g e N o t i c e . ( 2 ) The T e c h n i c a l Document ChangeNoticenumber. T h i s n u m b e r s h o u l d a l s o b e e n t e r e d o n t h e documentbeingchanged. ( 3 ) T h e e f f e c t i v i t y p o i n t s h o u l d b e c l e a r l y e s t a b l i s h e d , a d v i s i n g t h e r e c i p i e n t o f t h e cut-off pointwhenthe

olddocument becomes o b s o l e t e and t h e change becomes e f f e c t i v e . The e f f e c t i v i t y p o i n t c a n be described i n terms of a date, t h e r e c e i p t of a new c o n t r a c t , t h e d e p l e t i o n o f a supply o f t e s t samples, e t c . ( 4 ) Indicatethetypeofdocumentbeingchanged. ( 5 )

E n t e r t h e document t i t l e . ( 6 ) I d e n t i f y t h e i n d i v i d u a l i n i t i a t i n g t h e Change N o t i c e . ( 7 ) D e s c r i b e t h e c o n d i t i o n or i n f o r m a t i o n t h a t

is t o be changed. ( 8 ) D e s c r i b e , i n d e t a i l , t h e n a t u r e o f t h e change

t o b e m a d e . ( 9 ) Give i n d e t a i l , t h e r e a s o n s f o r making t h e change. ( 1 0 ) L i s t t h e i n d i v i d u a l s o r l a b o r a t o r ys e c t i o n s o r d e p a r t m e n t s t o

whomthe c h a n g e d d o c u m e n t i s t o b e d i s t r i b u t e d . ( 1 1 ) W h e n t h e c h a n g e d d o c u m e n t i s d i s t r i b u t e d , o b t a i n t h e s i g n a t u r e of each r e c i p i e n t . ( 1 2 ) L i s t t h e c o s t s , i f any, i n v o l v e d i n a c c o m p l i s h i n g t h e change d e s c r i b e d b g t h e N o t i c e . G i v e d e t a i l s o n t h e r e v e r s e

s i d e o f t h e C h a n g e N o t i c e . (13) I n d i c a t e h e r e a l l n e c e s s a r y a p p r o v a l s o b t a i n e d i n o r d e r t o r a t i f y t h e ChangeNotice.

91

f

Effective Dale

QUALITY DOCUMENTATION AND RECORDS CONTROL

BY

t

Section No.

Subject

Approved

I

-

12. O

page

4

0'

5

Revised

I

The Q u a l i t y Control Co o r dinator is r e s p o n s i b l e f o r s e e i n g t h a t

copiesofobsoletedocuments are removed f r o m p o i n t s o f u s e a n d a r e

d e s t r o y e d . He i s a l s o r e s p o n s i b l e f o r m o n i t o r i n g a c t i v i t y t o ensurethatapprovedchangesareincorporatedintoth;

laboratory's routineworkactivity. 1 2 . 5 Document Chanves 1 2 . 5 . 1 ARequest f o r c h a n g e s t o m e t h o d s , s a m p l i n g d a t a s h e e t s , or

calibrationinstructionsmaybemadebyanyone, the r e q u e s t

beingmade i n w r i t i n g o n t h e T e c h n i c a 1 Document Change Notice, s i n c e t h i s form acts as a r e q u e s t when being i n i t i a t e d , itmustbeapprovedbytheLaboratoryDirector b e f o r e t h e changeispublishedanddistributed. 1 2 . 5 . 2 Changesmaybe p r o m u l g a t e d b y t h e i s s u e of e n t i r e new

documents, o f replacement page s t h e r e t o , or, i n t h e case of c o r r e c t i o n s o f errata, e t c . , b y p e n a n d i n k p o s t i n g o n t h e o r i g i n a l document w i t h t h i s a c t i o n n o t e d o n t h e Change Notice. 1 2 . 6 The Q u a l i t y Co n t r o l Co o r d inator is r e s p o n s i b l e f o r d i s t r i b u t i o n and r e t r i e v a l ofdocument s a n d f o r o b t a i n i n g a l l r e q u i r e d signatures. 1 2 . 7 A l l f i l e s , when n o t i n u s e w i l l be kept i n locked f i l e c a b i n e t s . Computer data s e c u r i t y w i l l . b e m aintained i n accordance w i t h d a t a p r o c e s s i n g s t a n d a r d o p e r a t i n g p r o c e d u r e s for r e s t r i c t i n g e n t r a n c e t o computer data i n f o r m a t i o n .

92

Q u a l i t yD o c u m t a t i o n and Records Control

BY ApPr-

5

p.00 'Revised

XYZ LABORATORIES, INC. TECHNICAL DOCUMENT CHANGE NOTICE

DATE

(l)

TDCN No.

{-

-METHOD

(4) TYPE

(2)

EFFECTIVE (3)

SAMPLING DATA SHEET.

CALIBRATION INSTRUCTION

-OTHER (DESCRIBE)

DOCUMENT TITLE

(5)

REOUESTED B Y

(6)

CHANGE FROM:

17)

CHANGE TO:

(8)

REASON FOR CHANGE ( 9 )

DISTRISUTIONS

(10)

SIGNATURES

(11)

-

*COSTS

(12)

NEW LOUIP. NEW Y A r L SCRAPPED OR 011s. EQUIP.

0115. MATL PERSONNEL OTHER

93

*

APPROVALS

(13)

0'

5

1 Effective Date

1 Subject

t

I

CONTROLOFMEASURINGANDTEST EQUIPMENT

Section No.

13 .0

I

13.1 Pu n o s e T h i s s e c t i o n i s w r i t t e n t o a s s u r e t h a t o n l y gages and i n s t r u m e n t s

whichareproperlyandcurrently c a l i b r a t e d a r e u s e d i n m a k i n g

d e t e r m i n a t i o n s , t h e r e s u l t s o f w h i c h a r e recordedandreportedupon. 1 3 . 2 Scope The c a l i b r a t i o n of l a b o r a t o r y i n s t r u m e n t s f a l l s i n t o two c a t e g o r i e s : calibrationwhichisconductedonaroutinebasisprior t o each u s e ; and p e r i o d i c , s c h e d u l e d c a l i b r a t i o n o f i n s t r u m e n t s and gages a g a i n s t known s t a n d a r d s , traceable t o t h e N a t i o n a l I n s t i t u t e ofScienceandTechnology ( N I S T ) toensure t h e continuing p r e c i s i o n and accuracy of such i n s t r u m e n t s . The c a l i b r a t i o n p o l i c i e s and procedures s e t f o r t h i n t h i s s e c t i o n a p p l y t o a l l instrumentsin the latter category, including: a . Sampling equipment a t remote sampling s t a t i o n s b . A n a l y t i c a l and t e s t equipmen t i n t he l a b o r a t o r y

c . F l o w r a t e ( e . g . . r o t a m e t e r s ) , volume ( e . g . , d r y g a s

meters), p r e s s u r e , vacuum a n d t e m p e r a t u r e measurement equipment, b a l a n c e s , h a r d n e s s testers, t e n s i l e t e s t e r s , ph meters, e l e c t r i c a l meters, e t c .

13.3 C a l i b r a t i o n S t a n d a r d s Q u a l i t y

T r a n s f e r s t a n d a r d s w i l l have 4 t o 10 times t h e a c c u r a c y of f i e l d and

laboratoryinstrumentsand gages. For example, a t h e r m o m e t e r u s e d

94

I EIte~tfvcDaC BY Appro4

'

ISection No.

I Subject CONTROL OF MEASURING AND TEST EQUIPMENT

---

13 0

Page Reviaed

2

Of

i n t h e f i e l d t o d e t e r m i n e a i r temperature, h a v i n g a s p e c i f i e d a c c u r a c y o f f 2 ' F . w i l l be calibratedagainstalaboratory thermometerwithanaccuracyof~0.5'F.The S t a n d a r d s u s e d i n t h e

l a b o r a t o r y measurement s y s t e m w i l l be calibrated a g a i n s t h i g h e r - l e v e l , primary s t a n d a r d s h a v i n g u n q u e s t i o n a b l e and higher accuracy. These higher-level standardswillbe c e r t i f i e d b y N I S T or o t h e r recognizedstandardizationbodies.

C a l i b r a t i o n g a s e s purchased from commercial vendors w i l l be r e q u i r e d t o have a c e r t i f i c a t e o f a n a l y s i s . Whenever a c e r t i f i e d , c a l i b r a t i o n gas is available from NIST, commercial g a s vendors

w i l l be r e q u i r e d t o establishtraceabilityofthe c e r t i f i c a t e of

a n a l y s i s t o t h e c e r t i f i e d g a s . S i n c e i n a c c u r a t e c o n c e n t r a t i o n s of c e r t i f i e d g a s e s may r e s u l t i n s e r i o u s measurement e r r o r s , t h e Q u a l i t y Control Coordinator w i l l s p o t - c h e c k t h e a c c u r a c y a n d v a l i d i t y o f c e r t i f i c a t i o n of calibration g a s e s a s a p a r t o f t h e Receiving I n s p e c t i o n process. (See S e c t i o n 8 . 0 . ) 13.4 Environmental C o n d i t i o n s

Measuring and test equipmentand c a l i b r a t i o n s t a n d a r d s w i l l be c a l i b r a t e d i n a n a r e a t h a t p r o v i d e s c o n t r o l o f environmental conditionstotheextentnecessarytoassure r e q u i r e d a c c u r a c y a n d p r e c i s i o n . The c a l i b r a t i o n areawill be kept reasonably free of d u s t , vapor, v i b r a t i o n and r a d i o frequency i n t e r f e r e n c e s ; and i t w i l l be remote f r o m o r s h i e l d e d fromequipmentproducingnoise.

95

12

Elfcctlve O a k

BY

Subject '

Approved

CONTROL OF MEASURING AND TEST EQUIPMENT

Section No.

13,0

Page

3

0'

12

Revlsed

v i b r a t i o n , chemical or micro-wave em issions, e t c . T h e l a b o r a t o r y c a l i b r a t i o n area w i l l have t e m p e r a t u r e a n d h u m i d i t y c o n t r o l s , maintainingatemperature of68OFto73'Fanda r e l a t i v e humidityof 3 5 z t o 50%.A f i l t e r e d a i r s u p p l y w i l l b e p r o v i d e d , a n d h o o d s w i l l be checked f o r p r o p e r o p e r a t i o n b e f o r e e a c h u s e .

13.4.1 E l e c t r i c Power. The power f o r t h e l a b o r a t o r y w i l l b e

r e g u l a t e d t o p r o v i d e a continuous v o l t a g e o f +5$; c o n t r o l of harmonic d i s t o r t i o n ; c o n t r o l o f l i n e t r a n s i e n t s caused byinteractionofotherusers; a n d a s u i t a b l e grounding

system t o a s s u r e e q u a l p o t e n t i a l s throughout t h e laboratory. 1 3 . 4 . 2 L i g h t i n g . Adequate l i g h t i n g a t l e v e l s o f 80 t o 100 f o o t c a n d l e s a t w o r k b e n c h a r e a s . F l u o r e s c e n t l i g h t s w i l l be shielded t o reduce e l e c t r i c a l n o i s e .

13.5 C a l i b r a t i o n I n t e r v a l s . A l l c a l i b r a t i o n s t a n d a r d s a n d i n s t r u m e n t s and gages w i l l be

a s s i g n e d a n e s t a b l i s h e d c a l i b r a t i o n i n t e r v a l . The form f o r l i s t i n g gage and i n s t r u me n t i n t e r v a l s i s F i g u r e 1 3 - l w h i c h i s f i l l e d o u t a s f o l l ow s : ( 1 ) L i s t a l l i n s t r u m e n t s and gageswhich are i n c l u d e d i n t h e l a b o r a t o r y c a l i b r a t i o n system, by i n s t r u m e n t type or fam ily,

I n s tr u me n t s s h o u l d notbelistedindividually. ( 2 ) E n t e r t h e

c a l i b r a t i o n i n t e r v a l f o r each i n s t r u m e n t i n terms o f e l a p s e d t i m e ornumberofcompletedcycles o f u s e . ( 3 ) E n t e r t h e C a l i b r a t i o n

Procedure ormethodnumberwhichpertainstotheinstrumentgroup.

1

Eflectlve Date

BY Approved

Subject

CONTROL OF MEASURING AND TEST EQUIPMENT

Section No.

13.0

Page

4 of

12

_I

Revised

I n t h e a b s e n c e ofanestablishedintervalbasedontheequipment m a n u f a c t u r e r ' s recommendations, a n i n i t i a l c a l i b r a t i o n p e r i o d w i l l be a s s i g n e d b y t h e Q u a l i t y C o n t r o l Coordinator. The

c a l i b r a t i o n i n t e r v a l s w i l l be a d j u s t e d f r o m t i m e t o time, b a s e d o n e x p e r i e n c e gainedthroughuseoveraperiodoftime, a s e v i d e n c e d by data from gage c a l i b r a t i o n r e c o r d s . The c a l i b r a t i o n i n t e r v a l s w i l l be s p e c i f i e d i n terms o f time o r , i n t h e c a s e of c e r t a i n t y p e s

ofmeasuringandtestequipment. usage c y c l e s , o r u s a g e p e r i o d s . The c h o i c e of s i g n i f i c a n t i n t e r v a l s w i l l b e b a s e d o n t h e i n h e r e n t

stabilityandsensitivityoftheinstrument, its purpose or u s e ,

a c c u r a c y , c o n d i t i o n s o f u s e , and frequencyoramountofusage. The i n t e r v a l s w i l l be shortenedorlengthenedafterevaluatingthe

resultsofpresentandpastcalibrationsandadjustingthe s c h e d u l e

t o r e f l e c t t h e f i n d i n g s . These evaluationsmustprovidepositive

a s s u r a n c e thatcalibrationintervaladjustmentswillnotadversely

e f f e c t t h e a c c u r a c y of t h e system. Adherence t o t h e C a l i b r a t i o n Frequency Schedule i s m a n d a t o r y . Compliance i s a s s u r e d b y t h e f o l l o w i n g p r o c e d u r e : For each gage or i n s t r u m e n t i n t h e c a l i b r a t i o n system, a Gage C a l i b r a t i o n Record

card is p r e p a r e d as f o l l o w s : (1)E n t e r t h e gage or i n s t r u m e n t a s s i g n e d c a l i b r a t i o n number. I n t h i s l a b o r a t o r y , t h e c a l i b r a t i o n number i s t h e same as t h e P r o p e r t y InventoryNumber. ( 2 ) E n t e r t h e

97

.

Effective Date

BY Approved

Section No.

Subject

.

CONTROLOFMEASURINGANDTEST EQUIPMENT

13.0

page

5

0'

Revised

12

d e s c r i p t i o n o f t h e gage or i n s t r u m e n t . (3)Give t h e m a n u f a c t u r e r ' s name. ( 4 ) E n t e r t h e e q u i p m e n t s e r i a l n u m b e r . ( 5 ) E n t e r t h e I U o d e l

Number. ( 6 ) I n d i c a t e t h e l o c a t i o n o f t h e equipm entor t h e department or s e c t i o n w h e r e u s e d . ('7) Enter t h e c a l i b r a t i o n frequency from t h e C a l i b r a t i o n Frequency Schedule ( F i g u r e 13-1 ) . ( 8 ) E n t e r t h e a p p l i c a b l e C a l i b r a t i o n Procedure number. For each

scheduledcalibrationoperation e n t e r : ( 9 ) t h e date t h a t t h e

c a l i b r a t i o n i s p e r f o r m e d ; ( 1 O ) t h e name o f t h e i n d i v i d u a l p e r f o r m i n g t h e c a l i b r a t i o n ; (11) t h e s e c t i o n or department u s i n g

t h e i n s t r u m e n t or gage a t t h e time o f c a l i b r a t i o n ; ( 1 2 ) The r e s u l t s

o f t h e calibration. The Gage C a l i b r a t i o n Record Cards w i l l be s o r t e d and f i l e d by

month, s o t h a t t h e cardswhichareinaparticularmonth g r o u p w i l l i d e n t i f y w h i c h i n s t r u m e n t s are t o be r e c a l l e d f o r c a l i b r a t i o n d u r i n g t h a t m o n t h . N o t i c e o f recall w i l l be g i v e n p r i o r t o t h e d u e d a t e . It maybe n e c e s s a r y t o c a l i b r a t e b e t w e e n n o r m a l c a l i b r a t i o n d a t e s i f t h e r e is e v i d e n c e of i n a c c u r a c y or damage. C a l i b r a t i o n of

a m e a s u r e me n t d e v i c e c a n b e r e q u e s t e d a t a n y t i m e , r e g a r d l e s s o f t h e c a l i b r a t i o n d u e d a t e f o r t h a t item, f o l l o w i n g t h e occurrence o f

any e v e n t t h a t places t h e d e v i c e ' s a c c u r a c y i n d o u b t . The Q u a l i t y C o n t r o l Co o rdinator w i l l m aintain s u r v e i l l a n c e by

p e r i o d i c a l l y a n d randomly a u d i t i n g f o r compliance w i t h t h e c a l i b r a t i o n c o n t r o l and r e c a l l system.

98

Efftctlve Date

Section No.

Subjtct

13.0

CONTROLOFMEASURINGANDTEST EQUIPMENT

13.6 C a l i b r a t i o n Procedures

W r i t t e n step-by-step procedures f o r calibrationofmeasuringand t e s t equipment, and f o r t h e u s e o f c a l i b r a t i o n s t a n d a r d s w i l l be

used i n o r d e r t o e l i m i n a t e p o s s i b l e measurement i n a c c u r a c i e s due t o d i f f e r e n c e s i n t e c h n i q u e s , environmentalconditions, c h o i c e of h i g h e r - l e v e l s t a n d a r d s , personnel changes, e t c . These c a l i b r a t i o n p r o c e d u r e s m a y b e preparedbythelaboratory, maybe published s t a n d a r d practices or w r i t t e n i n s t r u c t i o n s t h a t accompany

purchasedequipment, or maybe o b t a i n e d fromtheGovernmentI n d u s t r y DataExchange ProgramMetrology DataBank (GIDEP). These p r o c e d u r e s w i l l c o n t a i n t h e following information: 13.6.1 The s p e c i f i c equipmentor group o f e q u i p m e n t t o w h i c h t h e

procedure is applicable. Like equipment orequipments o f t h e same type, having compatible c a l i b r a t i o n p o i n t s ,

environmental c o n d i t i o n s , andaccuracy requirements, may b e s e r v i c e d b y t h e s a m e c a l i b r a t i o n procedure. 1 3 . 6 . 2 A b r i e f d e s c r i p t i o n , or abstract, o f t h e scope, p r i n c i p l e , a n d / o r t h e o r y o f t h e calibrationmethod. 13.6.3 Fundamental c a l i b r a t i o n s p e c i f i c a t i o n s , such as

c a l i b r a t i o n p o i n t s , environmental c o n d i t i o n s , and accuracy requirements.

99

I Elfectlve Date

1 Subject

Section No.

CONTROL OF MEASURING AND TEST EQUIPMENT

BY Approved

Page

13 0

7

of

12

Reviaed

13.6.4 A l i s t o f c a l i b r a t i o n s t a n d a r d s a n d a c c e s s o r y equipment

r e q u i r e d t o perform t h e c a l i b r a t i o n s t e p s . The manufacturer'sname, model number, and r e q u i r e d i n s t r u m e n t accuracywillbe furnishedas applicable. 13.6.5 The complete procedure f o r p e r f o r m i n g t h e c a l i b r a t i o n ,

arrangedinastep-by-stepmanner,c l e a r l y a n d c o n c i s e l y

written. 13.6.6 The c a l i b r a t i o n p r o c e d u r e s w i l l provide s p e c i f i c

i n s t r u c t i o n s for obtainingand recording t h e calibration data, a n d w i l l i n c l u d e , where applicable, c o p i e s o f

c a l i b r a t i o n d a t a r e c o r d i n g forms. Note: Many c a l i b r a t i o n procedures r e q u i r e s t a t i s t i c a l analysis of results. 13.7 C a l i b r a t i o n S o u r c e s

Allcalibrationsperformedbythelaboratorywillbetracedthrough

anunbroken c h a i n , s u p p o r t e d b y reportsordatasheetstoultimate or national reference standardsmaintainedbya national

organization suchasTheNationa1 I n s t i t u t e o f S c i e n c e a n d Technology ( N I S T ) . Thelaboratorymayalsouse, a t i t s d i s c r e t i o n , as an u l t i m a t e r e f e r e n c e s t a n d a r d , a n independent, r e p r o d u c i b l e

s t a n d a r d , such asastandardthatdependsonacceptedvalues o f a n a t u r a l p h y s i c a l c o n s t a n t . A n u p - t o - d a t e c a l i b r a t i o n report f o r

I00

Eftectlw Date

BY

t

Approved

Section No.

Subject

a

CONTROLOFMEASURINGANDTEST EQUIPMENT

I

13.o

page

t

8

Of

Revised

12

eachstandardusedinthelaboratorywillbe r e t a i n e d i n t h e

l a b o r a t o r y ' s f i l e s . When calibrationservicesareprovidedbyan

outsidernetrologylaboratory, o n a c o n t r a c t b a s i s , c o p i e s o f t h e

c a l i b r a t i o n r e p o r t s furnishedbythemwillalsobekepton f i l e .

A l l s t a n d a r d s c a l i b r a t i o n r e p o r t s w i l l contain t h e following

information: a. Report number. b . I d e n t i f i c a t i o n number of t h e c a l i b r a t i o n s t a n d a r d t o which t h e

reportpertains. c . Environmental c o n d i t i o n s under which t h e c a l i b r a t i o n w a s

performed, d. R e q u i r e d a c c u r a c y o f t h e c a l i b r a t i o n s t a n d a r d .

e . D e v i a t i o n or c o r r e c t i o n s .

f. C o r r e c t i o n s t h a t must be applied i f standard c o n d i t i o n s o f

temperature, e t c , are not met or d i f f e r fromthose a t t h e place

and time o f c a l i b r a t i o n . C o n t r a c t s l e t for c a l i b r a t i o n s e r v i c e s w i l l r e q u i r e t h e m e t r o l o g y l a b o r a t o r y t o f u r n i s h r e c o r d s onthetraceabilityoftheir calibration standards. 13.8 Labeling

A l l e q u i p m e n t t o b e calibratedwillhaveaffixedtoitinplain

s i g h t , on t h e instrument i t s e l f , or i t s c o n t a i n e r , a t a g o r l a b e l

( F i g u r e 13-3). T h i s label is t o be f i l l e d o u t i n t h e following

Elfective Date BY Approved

Section No.

Subject

CONTROLOFMEASURINGANDTEST

EQUIPMENT

13.0

page Revkcd

9

Of

12

service. (2)Enterthedatethecalibrationwasperformed. (3) Enter t h e d a t e t h a t t h e n e x t c a l i b r a t i o n s e r v i c e i s d u e . b a s e d o n information fromtheGage CalibrationRecordCard (Figure 13-2) and t h e C a l i b r a t i o n Frequency Schedule ( F i g u r e 13-1).Equipment

past due f o r c a l i b r a t i o n w i l l be s e q u e s t e r e d , or i f t h i s is

impractical, willbeimpoundedbytaggingwiththeOutof Service label ( F i g u r e 13-4)which w i l l be f i l l e d o u t as f o l l o w s : (1)E n t e r

t h e s i g n a t u r e o f t h e Q u a l i t y Control C o o r d i n a t o r . ( 2 ) E n t e r t h e dateimpoundedorotherwisetakenoutofservice. C e r t a i n instrumentsin the laboratoryareused onlyasindicators, andthe r e a d i n g s f r o m t h e m a r e n o t r e c o r d e d o r r e p o r t e d . These i n s t r u m e n t s w i l l be l a b e l e d w i t h t h e N o t C a l i b r a t e d l a b e 1 ( F i g u r e 13-5).

I02

I

Eflecllve Dale

Subjecl

Section No.

CONTROL OF MEASURING AND TEST EQUIPMENT

BY

Approved

Page

Revised

13.0

10

CALIBRATION FREQUENCY SCHEDULE

Minimum Frequency

103

instruction Number or Calibration Method

0'

12

Eltectlve Date

Section

Subject

CONTROLOFMEASURINGANDTEST EQUIPMENT

I

No.

13.0

t

I

INSTRUMENT / GAUGE CALIBRATION RECORD

FIGURE 22-2

104

Sadon No.

mwm

E f l ~ ~ tD lw .1.

COtTLXOL OF MEASURING AND TEST EQUIPMEm

BY

P.0.

RWbd

APP-

BY (1) DATE (21 NEXT CAL. DUE (31

c

-.I

FIGURE 22-3

OUT OF SERVICE MUST BE REPAIRED AND/OR CALIBRATED BEFORE USE NAME

DATE

FIGURE 22-4

NOT TO BE USED FOR OFFICIAL MEASUREMENT PURPOSES 1

FIGURE 22-5

105

2

13.0 12 of 12

Eflectlve Date

BY Approved

1

I

Subject

PREVENTIVE MAINTENANCE

I

Section No.

14 0

page

Revised

1

0'

3

14.1 Purpose

This s e c t i o n d e s c r i b e s t h e Q u a l i t y Control Coordinator's r e s p o n s i b i l i t i e s f o r c a r r y i n g o u t a comprehensive p r e v e n t i v e ma i n t e na nc e program f o r g a g e s , i n s t r u m e n t s , and t e s t equipment u s e d i n i t s analyticalandtestingactivities. 14.2 Scope

T h i s s e c t i o n a p p l i e s t o a l l g a g e s , meas u rin g eq u ip men t, an d t e s t i n s t r u m e n t s i n c l u d e d i n t h e l a b o r a t o r y c a l i b r a t i o n program; i . e . , any e q u i p m e n t u s e d formakingdeterminations, t h e r e s u l t s o f w h i c h

are r e c o r d e d a n d r e p o r t e d u p o n . 14.3 P r e v e n t i v e M a i n t e n a n c e

Thelaboratorywillconductanorderly p ro g ramo f p o s i t i v e a c t i o n s (e qu i pm e nt c l e a n i n g , l u b r i c a t i n g , r e c o n d i t i o n i n g , a d j u s t i n g , a n d / o r t e s t i n g ) t o p r e v e n t i n s t r u m e n t s or equipment from f a i l u r e d u r i n g u s e . The p u r p o s e o f t h i s p r e v e n t i v e maintenance program is t o i n c r e a s e measurement s y s t e m r e l i a b i l i t y and t h u s i n c r e a s e d a t a c o m p l e t e n e s s . C o n v e r s e l y , i f t h e p r e v e n t i v e maintenance program i s n o t p r o p e r l y carried o u t t h e r e s u l t s w i l l b e : i n c r e a s e d measurement s y s t e m downtime w i t h a d e c r e a s e i n data c o m p l e t e n e s s ; i n c r e a s e d m a i n t e n a n c e costsandadistrustinthevalidityofthe d a t a . Datacompletenessisacriterionusedtovalidatedata.

Eflectlve Dale

Section No.

Subject

PREVENTIVEMAINTENANCE

BY Approved

14. 0

Page Revised

2

Of

3

14.3.1 Preventive Maintenance Schedule The Q u a l i t y Control

Coordinator w i l l prepare a n d i m p l e m e n t a p r e v e n t i v e maintenance schedule forlaboratorymeasurement systems. The planning r e q u i r e d t o p r e p a r e t h e schedule w i l l take i n t o c o n s i deration: a . Highlightingthatequipmentorpartsthereofwhichare

most l i k e l y t o f a i l without proper p r e v e n t i v e maintenance. b.

Definingasparepartsinventorywhich s h o u l d b e

m a i n t a i n e d t o r e p l a c e worn-out parts w i t h aminimum of downtime . The p r e v e n t i v e maintenance s c h e d u l e s h o u l d relate to the

purpose of a n a l y s i s o r t e s t i n g , environmental i n f l u e n c e s , physicallocationofequipment, and t h e l e v e l of o p e r a t o r s k i l l s . C h e c k l i s t s w i l l be u s e d t o s p e c i f y maintenance

tasks, as recommendedbymanufacturers o f t h e equipment.

F r e q u e n c i e s o r t i m e intervalsbetweenmaintenance s e r v i c e

w i l l a l s o b e specifiedinaccordancewith recommended

practices.

S i n c e i n s t r u me n t c a l i b r a t i o n is commonly t h e responsibility o f t h e operator i n addition t o preventive m a i n t e n a n c e t a s k s , a combined p r e v e n t i v e maintenancec a l i b r a t i o n s c h e d u l e w i l l b e u s e d i n t h o s e cases.

107

Etteellve Date BY

Subject

PREVENTIVE MAINTENANCE

Sectlon No.

14. 0

P.ge

Revised

3

1 4 . 3 . 2 PreventiveMaintenanceRecord (SeeSection26.0andFigure26-1)Arecordofall preventive maintenance anddailyservice checks w i l l be maintainedby the Quality Control Coordinator. Daily

Maintenance/ServiceReports (Figure 26-1) w i l l be f i l e d w i t h themeasurement data.

108

O'

3

EflecUw Date

%lion No.

Subject

REFERENCE STANDARDS

BY

15.0

p.ge Revised

Approwd

1 0' 3

15.1 PurDose T h i s s e c t i o n d i s c u s s e s t h e u s e of S t a n d a r d R e f e r e n c e materials

a v a i l a b l e f r o m t h e National I n s t i t u t e of S c i e n c e andTechnology (NIST ) .

15.2 Scope T h i s sectiondealswiththeStandardsReferenceMaterialsusedin

a n a l y s e s a n d t e s t s . It d o e s not c o n c e r n i t s e l f w i t h themeasurement standardsdiscussedinSection13.0, " C o n t r o l o f M e a s u r i n g a n d

Test Equipment." 15.3 A v a i l a b i l i t y o f Standard Reference M a t e r i a l s

The Q u a l i t y Control Coordinator w i l l keep on f i l e a c u r r e n t c o p y o f NISTSpecial P u b l i c a t i o n 260, 'lNISTStandardReferenceMaterial Catalog"

fortheinformationofallconcerned. Asanexample, a

c o p y o f t h e N I S T ( f o r m e r l y NBS) Certificate o f A n a l y s i s N o . 2676. (Figure15-1) isshownhere. T h i s c o n s i s t s o f t h r e e concentrations of l e a d , cadmium, z i n c , andmanganese onmembrane f i l t e r s . T h i s i l l u s t r a t e s a t y p i c a l SRMavailable fromNIST. 15.4 Use o f SRM's

T h i s l a b o r a t o r y w i l l u s e S t a n d a r d R e f e r e n c e Materials as a v a i l a b l e fromNIST for calibrationofinstruments, p r e p a r a t i o n of lower

t i e r s t a n d a r d s o r a s r e f e r e n c e standardsagainstsamplestobe

analyzedortestedasapplicable.

109

PREPRINT

Standard Reference Material 2676 Metals on Filter Media This Standard Reference Material is intended p r i m a r i l y f o r w e as an a n a l y t i c a l s t a n d a r d for the d e t e r m i n a t i o n of cadmium, lead, manganese, and z i n c i n the i n d u s t r i a l atmosphere. The SRM c o n s i s t s of a set of membrane f i l t e r s on which have been deposited t h e i n d i c a t e d q u a n t i t i e s of s a l t s of the p a r t i c u l a r metals. Filter

A 1

A 2

A3

Metal Content , ug/f ilter Pb Mn

Cd 0.50 2 - 0 4

2.48 10.1

2 f

.I4 .4

6 . 8 i 1.1

29. 102.

f 2

2.6 6

1.93 2 -29 10.3 f 1.5 20.6 2 1.0

Zn 1.02 t 5.10 f

10.1

f

-06 .26 1.1

The f i l t e r s were prepared by d e p o s i t i n g on them known and c a r e f u l l y reproduced volumes of s o l u t i o n s of pure s a l t s , using t h e technique d e s c r i b e d i n NBS r e p o r t NBSIR 73-256.

The c e r t i f i e d v a l u e s are based upon determination of the m e t a l conte:lt by atanic a b s o r p t i o n spectrometry and by polarographic measurement'. I n these a n a l y s e s , e n t i r e f i l t e r s were mineralized by d i g e s t i o n i n acid prior t o measurement. The c e r t i f i e d values are t h e means of those found by the two techniques while the uncertainties represent t h e 95 percent tolerance l i m i t s based on measurement error and v a r i a b i l i t y between samples*.

The f i l t e r s are i d e n t i f i e d by t h e numbers A l , A2, A3 p r i n t e d on t h e i r edge. The metal c o n t e n t o f t h e inked i d e n t i f i c a t i o n is n e g l i g i b l e so it need n o t be removed. An e n t i r e f i l t e r m u s t be used f o r each measurenrent s i n c e the metale are not uniformly d i s t r i b u t e d .

See page 1 4 , The Role of Standard Reference Materials in Measurement System, NBS Monograph 148, 1975. The Concept of t o l e r a n c e l i m i t is also d i s c u s s e d i n Chapter 2, Experimental Statistics, NDS Handbook 91, 1966.

I n b r i e f , i f measurements w e r e made on a l l the units, almost a l l ( a t least 95 percent) of t h e s e measured values woL.ld be expected t o f a l l w i t h i n the i n d i c a t e d tolerance l i m i t s with a confidence c o e f f i c i e n t of 95 p e r c e n t ( O r p r d m b i l i t y = .95). (over) FIGURE 15-1

The filters were prepared by R. Mavrodineanu and J. R. Baldwin. A t o m i c a b a o r b t i o n a n a l y s e s w e r e made by them and also by T o C . Rain.. E. J. Maienthal performed the polarographic analyrea

.

The overall d i r e c t i o n and c o o r d i n a t i o n of the technical

measurements l e a d i n g to c e r t i f i c a t i o n were under the chairnun8hip of J. K. Taylor. The t e c h n i c a l and s u p p o r t aspects involved i n c e r t i f i c a t i o n and iaauanco of this Standard Reference Material w a s c o o r d i n a t e d t h r o u g h the O f f i c e of Standard Reference Materials by W. P. Reed.

Waahington, D ,C June 30, 1 9 7 5

.

20234

J . Paul C a l i , C h i e f O f f i c e of Standard Reference Materials

Etfectlve Dale

Subject

Section No.

DATA VALIDATION

BY Approved

16. 0

Paw

1

Of

Revised

16.1 Purpose T h i s s e c t i o n e x p l a i n s t h e need f o r d a t a v a l i d a t i o n a n d t h e methods

of d a t a v a l i d a t i o n w h i c h w i l l be employedbythislaboratory.

1 6 . 2 Scope D a t a v a l i d a t i o n can be a c c om plishedby s e v e r a l m e t h o d s . T h e v a l i d a t i o n p r o c e s s c a n b e manual or computerized. 1 6 . 2 . 1 D a t a v a l i d a t i o n is t h e p r o c e s s i n w h i c h d a t a a r e checked a n d a c c e p t e d o r rejectedbasedonasetofcriteria. Validation is performedto i s o l a t e spurious values since suchvaluesarenotautomatically rejected. R ecordsof

i n v a l i d data found w i l l be r e t a i n e d i n accordance w i t h established r e c o r d s r e t e n t i o n p o l i c i e s .

16.2.2 V a l i d a t i o n method s w i l l i n c l u d e reviewby s u p e r v i s o r s as well a s c o m p a r i s o n w i t h c r i t e r i a b y c o m p u t e r . Criteria w i l l dependon t h e t y p e s o f d a t a a n d o n the p u r p o s e o f t h e

measurement. measurement. 16.2.3 Various s t a t i s t i c a l t e c h n i q u e s are u s e f u l . P e r i o d i c

c h e c k i n g o f m a n u a l l y reduceddataisimperative. The

statistical technique t h a t ismostcommonlyusedis a c c e p t a n c e sampling.

I12

6

Etlectlvc Date

Section No.

Subject

BY

16. 0

DATAVALIDATION Revlrd

Approved

2

O C 6

1 6 . 3 DataValidation-General Datavalidation i s the process inwhichdataare checkedand acceptedor rejectedbasedonasetofestablishedcriteria. This

involvesacriticalreviewofabodyofdatainordertoidentify

spuriousvalues o r outlyingobservations. The reviewmaybeonlya

quickscantodetectextremevaluesoradetailedevaluation requiringtheuse ofacomputer. I n e i t h e r situation, whena spuriousvalue i s l o c a t e d , i t i s n o t immediately rejected. Each questionablevalueoranomalymustbechecked f o r v a l i d i t y . Records ofvaluesthatarejudgedtobeinvalidorare otherwisedoubtful

w i l l be retained. These recordsbecome ausefulresource of

iinformation n f o r m a t i o n for udgingdataquality. for jjudgingdataquality. 16.4 Manual D a t a V a l i d a t i o n

Both t h e t e c h n i c i a n and t h e l a b o r a t o r y s u p e r v i s o r s w i l l i n s p e c t i n t e g r a t e d d a i l y andweekly r e s u l t s for q u e s t i o n a b l e v a l u e s . T h i s

k i n d o f i n s p e c t i o n is most u s e f u l for t h e d e t e c t i o n of extreme

v a l u e s or o u t l i e r s appearingasunusuallyhigh o r l o w d a t a p o i n t s . The c r i t e r i a f o r determining extreme v a l u e s a r e d e r i v e d from p r i o r

i

d a t a o b t a i n e d fromsimilartestsoranalyticalwork.T h e d a t a u s e d t o d e t e r m i n e extremesmaybetheminimumandmaximumdatapoints

I13

Eflectlve Date

BY

1

F=l

k Section No.

Subject

DATAVALIDATION

Approved

16.0

Revised

f o r a l l p r i o r data f r o m s i m i l a r t e s t s o r a n a l y s e s . The time s p e n t o n checkingdatathathavebeenmanually r e d u c e d b y t e c h n i c i a n s

depends on t h e t i n e a v a i l a b l e and i n t h e d e m o n s t r a t e d a b i l i t i e s of thetechnicians. 16.5 ComputerizedTechniaues As n e c e s s a r y , t h e c o m p u t e r w i l l b e u s e d n o t o n l y t o s t o r e and

r e t r i e v e d a t a b u t a l s o t o v a l i d a t e d a t a . T h e u s e o f t h e computer a l l o w s t h e f i n e - t u n i n g o f t h e c r i t e r i a f o r extreme v a l u e s s o a s t o be s p e c i f i c f o r i n d i v i d u a l h o u r s d u r i n g t h e day, i f d e s i r a b l e . For

i n s t a n c e , w i t h t h i s r e f i n e m e n t , a n h o u r l y average c o n c e n t r a t i o n of carbonmonoxideof15ppmmightnotbe c o n s i d e r e d a n e x t r e m e v a l u e

at8:00AM, b u t w o u l d b e e v a l u a t e d a s q u e s t i o n a b l e i f i t a p p e a r e d a t

2:oo AM.

Anotherindicationofspuriousdataisalarge d i f f e r e n c e i n

c o n c e n t r a t i o n s r e p o r t e d i n two s u c c e s s i v e time p e r i o d s . The d i f f e r e n c e i n c o n c e n t r a t i o n s , which might be c o n s i d e r e d e x c e s s i v e , mayvary fromone contaminant t o a n o t h e r a n d q u i t e p o s s i b l y m a y vary fromone sample s o u r c e t o a n o t h e r f o r t h e same contaminant. T h i s d i f f e r e n c e w i l l be t e s t e d for s i g n i f i c a n c e through

s t a t i s t i c a l a n a l y s i s , u s i n g an a p p r o p r i a t e t e s t f o r s i g n i f i c a n c e o f d i f f e r e n c e s . dependingonthekindofinformationavailablein

I14

Effectlve Date

Section No.

Subject

DATAVALIDATION

BY Approved

16.

Page

4

Of

6

Revised

t h e d a t a package i n q u e s t i o n . The c r i t e r i a f o r what c o n s t i t u t e s a n

e x c e s s i v e change may a l s o b e l i n k e d t o t h e t i m e of day and contaminant r e l a t i o n s h i p s . For i n s t a n c e , high c o n c e n t r a t i o n s o f SOp and O5 cannot c o - e x i s t , and s u c h d a t a s h o u l d b e s u s p e c t e d .

16.6 T o o l s U s e d i n D a t a V a l i d a t i o n 16.6.1 S t r i p C h a r t Data

Whenacontinuousmonitoringdeviceisused, t h e o u t p u t i s a n a n a l o g t r a c e o n a s t r i p c h a r t . S t r i p c h a r t s w i l l be c u t

atweeklyintervalsandwillbe s e n t t o t h e l a b o r a t o r y s u p e r v i s o r f o r i n t e r p r e t a t i o n . Reading s t r i p charts is a t e d i o u s task, s u b j e c t t o v a r y i n g d e g r e e s of e r r o r , t h e r e f o r e a procedure f o r m a i n t a i n i n g d e s i r e d q u a l i t y for d a t a m a n u a l l y reduced f r o m s t r i p c h a r t s w i l l be followed.Theproceduretobeused f o r c h e c k i n g t h e v a l i d i t y

o f t h e d a t a reduced by a t e c h n i c i a n is t o have a n o t h e r t e c h n i c i a n o r s u p e r v i s o r c h e c k t h e d a t a . Because t h e v a l u e s w i l l have been t a k e n f r o m t h e s t r i p chart by v i s u a l

i n s p e c t i o n , some differencesinthevaluesderivedbytwo d i f f e r e n t i n d i d i v u a l s c a n b e expected. When t h e d i f f e r e n c e exceeds a s p e c i f i e d amount, and t h e i n i t i a l r e a d i n g h a s beendetermined t o b e i n c o r r e c t , a n e r r o r w i l l be noted. I f t h e number oferrorsexceedsapredeterminednumber, a l l

1 IS

Elfectlve Dale

Section No.

Subjecl

DATA VALIDATION

BY Approved

16. 0

P W

5

Of

6

Revised

data f r o m t h e s t r i p c h a r t are r e j e c t e d , and t h e chart is

readagainby another individual. Thequestionof determininghowmanyvalueswillbe c h e c k e d c a n b e a n s w e r e d by u s i n g a c c e p t a n c e s a m p l i n g t e c h n i q u e s . 1 6 . 6 . 2 ADDlication o f Acceptance SamDlinaTechniaues Acceptance s a m p l i n g w i l l be u s e d i n d a t a v a l i d a t i o n t o d e t e r m i n e thenumber o f d a t a items ( i n d i v i d u a l v a l u e s on a s t r i p c h a r t ) t h a t must be c h e c k e d t o d e t e r m i n e w i t h a given c o n f i d e n c e l e v e l t h a t a l l d a t a items are a c c e p t a b l e . The s u p e r v i s o r n e e d s t o k n o w , w i t h a h i g h d e g r e e of a s s u r a n c e , w i t h o u t c h e c k i n g e v e r y d a t a v a l u e , whether a d e f i n e d e r r o r levelhasbeenexceeded. FromeachstripchartwithNdata v a l u e s ( t h e p o p u l a t i o n ) t h e s u p e r v i s o r can randomly i n s p e c t a s a m p l e o f n d a t a v a l u e s . I f thenumber o f erroneousvaluesisequal t o o r l e s s t h a n c , the rejection

criteria, thevalues f o r t h e s t r i p c h a r t areaccepted. I f thenumberoferrorsisgreaterthanc, t h e v a l u e s o n t h e

s t r i p chart are rejectedandanotherindividual is a s k e d t o

Eflcciive Date

Subject

Section No.

DATAVALIDATION

BY

Pwe

16 0 60'6

Revlsed

Approved

sample s i z e s a n d f o r t h e u s e o f r e j e c t i o n a n d a c c e p t a n c e

criteriaappearsinANSI/ASQCZ1.4-1981, "Sampling Procedures andTables f o r I n s p e c t i o n B y A t t r i b u t e s . "

117

Eflectlve Date

BY

Section No.

Subject

ENVIRONMENTAL CONTROLS

Approved

17. O

Page

1 0' 1

Revised

17.1 Purpose T h i s s e c t i o n w i l l d e s c r i b e t h e environmental c o n t r o l s r e q u i r e d f o r

laboratory operations. 1 7 . 2 Scope T h i s s e c t i o n w i l l d e a l w i t h t h e c o n t r o l of environmental c o n d i t i o n s

inlaboratoryworkingareas. Environmental c o n t r o l s f o r t h e

c a l i b r a t i o n area are covered i n S e c t i o n 1 3 . 0 , P a r . 13.4. 17 3 Environmental C o n t r o l s i n Workinp: Areas

The environment i n t h e working areas o f t h e l a b o r a t o r y w i l l b e

c o n t r o l l e d o n l y t o t h e e x t e n t a f f o r d e d by normal, commonly used h e a t i n g , v e n t i l a t i n g , and a i r - c o n d i t i o n i n g equipment which w i l l

maintainaworkingtemperature o f 6 8 ' t o 7 6 " F a n d a r e l a t i v e humidity a t a b o u t 5 0 z . T h i s l a b o r a t o r y h a s n o requirement f o r clean-room f a c i l i t i e s , nor are t h e r e any s p e c i a l requirements beyond normal goodhousekeepingpractices. 17.4 Hoods

H o o d s w i l l be checked f o r p r o p e r o p e r a t i o n p r i o r t o e a c h u s e .

118

Effective Dnte

Subject

D Approved

3.1

CUSTOMER SATISFACTION AND COMPLAINT

I

Sectlon No.

Revised

1

18.0 Of

3

Purpose This section sets forth the procedures and responsibilities for handling customer complaints and negative audit results. It also describes the requirements for seeking and improving customer satisfaction, and for periodically measuring and appraising the degree of customer appreciation of laboratory quality performance achieved.

3.2

Scooe This section applies to all efforts made by the laboratoryto achieve, improve, and

maintain customer satisfiction, and to monitor continuously customer attitudes toward the quality of service provided by the laboratory. It also sets forth how all customer complaints are to be handled, regardless of the source. 3.3

Communications Since an easy and unrestricted flow of information between the laboratory and its customers is fundamental to the establishment of satisfactory relationships between them, it is necessary to ensure that all laboratory personnel who routinely communicate with customers pass on any customer concerns not, immediately resolved to their superiors or others having the expertise to handle the matter at hand.

To make sure that all customer contacts, f o q l or informal, are promptly acted upon, all laboratory personnel having contact

a customer, will log the occurrence on the

Customer Contact Log Sheet. (Figure 18-1) These forms will be forwarded daily to the Quahty Control Coordinator who will review themto determine whether any additional action is necessary, such as the initiation of a Corrective Action Request. 8.4

Customer Contact Log Sheet Form (1) Laboratory employee’s name

119

Effective Date

Subject

CUSTOMER SATISFACTION AM) COMPLAINTS

Section No.

(2) Enter the name of the laboratory department or section to which the writer is assigned. (3) Enter the time and date that the communication was received. (4) Enter the means of communication, i.e.: telephone, visit, FAX, e-mail, letter, etc. ( 5 ) Enter the names of the customer and his or her company or organization.

(6) Describe briefly the subject discussed i.5

Complaints All complaints and negative comments or suggestions fiom customers, government agencies or other sources outside the laboratory will be turned over to the Quality Control Coordinator for review, handling, and reply. In each case, he will advise the individuals concerned as to the nature of the complaint. Additionally, he will initiate corrective action measures when necessary. Upon completion of the corrective action and the finding of a solution to the problem, the Qua& Control Coordinator will advise the customer accordingly. In the case of corrective action taken to satisfy the comments or suggestions of outside auditors fiom accrediting organizations, detailed explanationswill be given of measures taken to prevent reoccurrence of the problems causing the negative comments.

1.6

Customer Satisfixtion

It is the responsibility of the Quality Control Coordinatorto review and measure annually our customers’ appreciation of the quality of the laboratory’s performance. Accordingly, he will, at the end of each fiscal year, arrange with a qualified marketing analysis agency

to conduct whatever surveys are necessary in order to appraise the effectiveness of the laboratory’s continuous improvement of customer satisfaction efforts. He will make recommendations to management based on the results of these surveys.

I 20

1-1

Subject

Effective Date

Approved

I

CUSTOMER SATISFACTION AND COMPLAINTS

I

L

Sectlon No.

‘we

3

18aO

0‘

Revled

XYZ LABORATORIES, INC. CUSTOMER CONTACT LOG SHEET NAME

DATE (ql

DEPT/SECTION

(1)

I

CONTACT TYPE

1

CUSTOMER NAME

t r

Figure 18-1

121

(5)

I

(2)

SUBJECT DISCUSSED (6)

3

Eflectlve Date

BY

Subject

SUBCONTRACTING

Approved

Seclion No.

19. 0

Page

1

0'

2

Revised

19.1 Purpose

T h i s s e c t i o n d e s c r i b e s t h e requirements f o r t h e c o n t r o l o f t h e q u a l i t y o f work imposed upon o u t s i d e l a b o r a t o r i e s doing a n a l y t i c a l ortestingtaskswhicharebeyondthe c a p a b i l i t i e s o f t h i s

laboratory, 1 9 . 2 Scope T h i s s e c t i o n a p p l i e s notonlytooutsidelaboratoriesdoing

analyticalortestingworkonacontractbasis, b u t a l s o t o metrology l a b o r a t o r i e s p r o v i d i n g c a l i b r a t i o n s e r v i c e s i n accordancewith Section13.0. 19.3 Q u a l i t y Assurance i n C o n t r a c t L a b o r a t o r i e s

Each c o n t r a c t l a b o r a t o r y , which t h i s l a b o r a t o r y employs f o r

p r o v i d i n g t e s t i n g s e r v i c e s , chemical a n a l y s e s , or c a l i b r a t i o n s e r v i c e s , w i l l m a i n t a i n its own i n t e r n a l q u a l i t y a s s u r a n c e system. The c a p a b i l i t y o f t h e contractortomaintainahighlevelof

quality ofworkwill betaken into considerationasapart o f t h e contractevaluationprocessandwillbeweighedheavilyinthat

process. The Q u a l i t y C o n t r o l Coordinator w i l l f u r n i s h each new c o n t r a c t

122

1 Effectlve Date

W

SUBCONTRACTING

19 0

Revised

Approved

I

t-ISection No.

I Subject

I

l a b o r a t o r y , p r i o r t o t h e completion o f t h e c o n t r a c t agreement, ' L a u d i t " s a m p l e s t o h e l p i n gaininganunderstandingofthe

qualityofdataproducedbythe c o n t r a c t l a b o r a t o r y . The data from these s a m p l e s w i l l s e r v e a n u m b e r o f p u r p o s e s . F i r s t , t h e d a t a m a y

b e u s e d t o h e l p m a k i n g d e c i s i o n s as t o t h e a b i l i t y o f a n o u t s i d e l a b o r a t o r y t o p e r f o r m t o d e s i r e d s t a n d a r d s . Secondly, t h e d a t a m a y beusedtopointoutproblemareasinmethodssuchasambiguityof

language, sample i n s t a b i l i t y , or c r i t i c a l a n a l y t i c a l or t e s t i n g steps.

I n f u r t h e r a n c e o f t h i s , whenanewmethodcomesintoquestion, t h e

Q u a l i t y Co n t r o l C o o r d i n a t o r w i l l f u r n i s h t h e c o n t r a c t o r w i t h a s e t o f " u s e r check" spiked s a m p l e s t o a n a l y z e b y them ethod i n q u e s t i o n . T h i s s e r v e s t h e d u a l purpose o f t e s t i n g t h e c o n t r a c t o r ' s proficiencyinperformingthemethodandalsotestingtheclarity

and t e c h n i c a l p r o f i c i e n c y o f t h e method language.

I23

I

Effedlve Date

I

I Section No.

Subject

PERSONNELTRAINING,

QUALIFICATION AND MOTIVATION

20.0

Page

1 Of 6

Revised

2 0 . 1 Purpose To s e t f o r t h t h e t r a i n i n g m e t h o d s , e v a l u a t i o n and q u a l i f i c a t i o n procedures, and r e s p o n s i b i l i t i e s f o r m o t i v a t i o n a l programs i n t h e laboratory. 20.2 Scope A l l pe r s o n n e l involved i n any function e f f e c t i n g data q u a l i t y

(sample c o l l e c t i o n , a n a l y s i s , t e s t i n g , data r e d u c t i o n , and q u a l i t y

c o n t r o l and a s s u r a n c e ) , w i l l have s u f f i c i e n t t r a i n i n g i n t h e i r appointedpositionsto contribute t o t h e reportingofcomplete, high q u a l i t y data. The Q u a l i t y Control Coordinator is r e s p o n s i b l e for s e e i n g t h a t t h e r e q u i r e d t r a i n i n g i s m a d e a v a i l a b l e t o these

personnelandthatrecordsaremaintainedoneachperson r e f l e c t i n g s a t i s f a c t o r y completion o f t r a i n i n g programs or q u a l i f i c a t i o n tests.

20.3

Oualitv Training Objectives Quality control training programs will have objectivesthat: 1) Seek solutions to laboratory quality problems. 2) Instill in all laboratory personnel recognition of the need to continually improve

customers’ satisfactionwith the qmhy ofthe laboratory’s performance. 3) Provide all laboratorypersonnel with the knowledge required in order to carry out

management’s determination to continually improve its quality performance. These training objectives will help to develop for all laboratory personnel involved in any aspect or function affectingquality, those attitudes, that knowledge, and those skills which will enable each one to contributeto the production ofhigh quality data continuously and effectively.

I24

I EIlccllvc Date

I

I Section No. 20. 0

Subject

PERSONNEL TRAINING, QUALIFICATION ANDMOTIVATION 20.4 Available T r a i n i n g Methods 2 0 . 4 . 1 experience training-this ison-the-job training (OJT), l e a r n i n g t o c o p e w i t h p r o b l e m s u s i n g p r i o r experience or

knowledge as t h e basis f o r a c t i o n . 20.4.2

guidance training-ThisisOJTwithoutsidehelp from

s u p e r v i s o r s o r co-workers. The advice maybe s o l i c i t e d , provided on a n informal basis, or on a planned, scheduled b a s i s . On-the-job trainingwillbe c o n d u c t e d a s follows: a. Observe an experienced o p e r a t o r perform t h e d i f f e r e n t t a s k s i n t h e measurement process. b. P e r f o r m t h e o p e r a t i o n u n d e r t h e d i r e c t s u p e r v i s i o n o f an

experienced o p e r a t o r . c. Perform t h e operationsindependentlybutwithahigh l e v e l of q u a l i t y c o n t r o l c h e c k s u s i n g t h e t e c h n i q u e s described i n P a r . 20.5 below, which d e a l s with o p e r a t o r p r o f i c i e n c y e v a l u a t i o n procedures. 20.4.3

Independent study-Thismagbenightschoolclasses, o u t s i d e r e a d i n g , a t t e n d a n c e a t seminars, or

p r o f e s s i o n a l s o c i e t y meetings, e t c . on a v o l u n t a r y basis. (See PersonnelDepartmentPo1icyNo.--- f o r

information on t u i t i o n and f e e payments by t h e laboratory.)

125

Effectlw Date

PERSONNELTRAINING,

BY

QUALIFICATION

Approved

20.4.4

Section No.

Subjecl

ANDMOTIVATION

20.0

Page

3

0'

6

Revised

In-house t r a i n i n g - T h i s is class room s t u d y , h e l d d u r i n g workinghours, p r e s e n t e d o n a formal basis. Coursesmaybe g i v e n b y qualifiedlaboratorypersonnel or o u t s i d e instructors.

20.4.5

outside part-timecourses-it isthepolicyofthe

l a b o r a t o r y t o encourage c o n t i n u e d e d u c a t i o n i n a l l j o b r e l a t e d a r e a s . There aremanysourcesofqualitycontrol t r a i n i n g a v a i l a b l e . The Q u a l i t y C o n t r o l Coordinator w i l l seekoutandmaintainlistsofschools, p r o f e s s i o n a l

s o c i e t i e s , andother organizations o f f e r i n g courses related t o laboratory quality control a c t i v i t i e s . He w i l l be a v a i l a b l e for c o n s u l t a t i o n w i t h t h o s e s e e k i n g

continuing education o p p o r t u n i t i e s i n t h e f i e l d of q u a l i t y control.

20 5 Traininv Evaluation

T r a i n i n g w i l l be e v a l u a t e d i n terms o f : ( 1 ) l e v e l o f k n o w l e d g eand s k i l l achieved by t h e o p e r a t o r from t h e t r a i n i n g , and (2)t h e

o v e r a l l e f f e c t i v e n e s s o f t h e trainingincludingdetermination of t h e t r a i n i n g a r e a s w h i c h n e e d improvement. When a q u a n t i t a t i v e

performance ratingismadeontheoperatorduringthetraining period, intermsofskillandknowledge achieved, t h i s r a t i n g w i l l

I26

Effectlw Data

Subject

PERSONNEL T R A I N I N G , QUALIFICATION AND MOTIVATION

BY Approved

Section No.

20. 0

pw*

4

0'

6

Revlsed

r

a l s o provide anassessment o f t h e o v e r a l l e f f e c t i v e n e s s o f t h e trainingprogram. S e v e r a l t e c h n i q u e s are a v a i l a b l e t o e v a l u a t e t h e o p e r a t o r and t h e effectivenessofthetrainingprogram. One o r m o r e o f t h e s e

techniqueswillbeusedduringthe e v a l u a t i o n . Themost common

t y p e s o f e v a l u a t i o n t e c h n i q u e s applicable t o ameasurement system

t r a i n i n g program are t h e f o llowing: 2 0 . 5 . 1 T e s t i n g - A w r i t t e n t e s t following t r a i n i n g w i l l be given i n o r d e r t o assess t h e e f f e c t i v e n e s s o f t h e t r a i n i n g e f f o r t . The i n s t r u c t o r m a y . because o f c i r c u m s t a n c e s , g i v e a p r e -

t r a i n i n g t e s t i n o r d e r t o d e t e r m i n e t h e l e v e l o f knowledge prevailingprior t o t h e s t a r t o f t h e trainingcourse. Postt r a i n i n g tests a l s o provide t h e i n s t r u c t o r w i t h i n f o r m a t i o n on t r a i n i n g areas which need improvement. 2 0 . 5 .2

P r o f i c i e n c y c h e c k s - I n o r d e r t o measure s k i l l improvement i n b o t h OJT and s h o r t course t r a i n i n g , t r a i n e e s w i l l be a s s i g n e d work t a s k s related t o t r a i n i n g s u b j e c t matter. Accuracyandcompletenesswillbeusedasindicatorsto s c o r e t h e t r a i n e e s ' p r o f i c i e n c y . The work t a s k s w i l l b e i n t h e f o l l o w i n g form:

a. Sample collection-Traineewillbeaskedtolistall s t e p s involved i n s a m p l e c o l l e c t i o n f o r a h y p o t h e t i c a l

127

Effective Date

Section No.

Subject

PERSONNELTRAINING,

BY

QUALIFICATION

Approved

ANDMOTIVATION

20.0

Page

5

0'

6

Revised

c a s e . I n a d d i t i o n , t h e traineewillbeaskedtoperform selected calculations. b. T e s t i n g o r a n a l y s i s - T r a i n e e w i l l be providedunknown

samplestowhichaprescribedmethodistobeapplied. A s

u s e d h e r e , anunknown i s a s a m p l e w h o s e c o m p o s i t i o n o r i d e n t i t y isknownto the supervisor (OJT) o r instructor ( o f a c o u r s e ) b u t u n k n o w n t o t h e t r a i n e e .P r o f i c i e n c y i s

judgedintermsofaccuracy.

c . Data reduction-Trainees r e s p o n s i b l e f o r data reduction w i l l be given data s e t s t o v a l i d a t e . P r o f i c i e n c y w i l l be

judgedintermsofcompletenessandaccuracy.

Whenproficiencychecksareconductedonarecurringbasis,

a c o n t r o l c h a r t w i l l be u s e d t o show p r o g r e s s o f t h e t r a i n i n g e f f o r t . The resultsofallcompletedtraining c o u r s e s w i l l be p o s t e d t o t h e i n d i v i d u a l s ' personnel j a c k e t . Note w i l l bemade o f t h e e x p i r a t i o n d a t e s of q u a l i f i c a t i o n c e r t i f i c a t e s , so t h a t a follow-up can be made t o eensure n s u r e ttiim enewal. meel y rrenewal. 20.5.3 I n t e r v i e w s

A s necessary, o r a l interviewswillbeusedtodetermine

whethertrainingeffortswere e f f e c t i v e . I n t e r v i e w s m a y b e conducted by t h e immediate s u p e r v i s o r or t h e Q u a l i t y

Control Coordinator, as appropriate t o t h e s i t u a t i o n .

128

I Effecthe Date

I Subject

PERSONNEL TRAINING.

E= ISection No. 20.0 Revised

20.6 Q u a l i t y Motivation

The Quality Control Coordinator is responsible f o r conducting, f r o m t i m e t o t i m e , suchmotivationalcampaignsasdeemednecessary.

H e w i l l alsomake recommendationstomanagementwith regard to e f f o r t s t o i n c r e a s e employee awareness o f e a c h i n d i v i d u a l ' s r e s p o n s i b i l i t y f o r t h e q u a l i t y of laboratory output.

129

Elfectlve Date

BY Approved

Subject

STATISTICAL METHODS

-

Section No.

21.0

1

Page Revired

O'

5

2 1 . 1 Purpose

T h i s s e c t i o n l i s t s a n u m b e r of statistical t o o l s a n d techniques availabletothelaboratoryworker. Thesetoolsandtechniquesare u s e d t o gainmoreinformationaboutdataproducedbytestingand a n a l y t i c a l p r o c e d u r e s . Thisinformationwillbeusedtomake

p r e d i c t i o n s o r c o m e t o c o n c l u s i o n s a b o u t t h e n a t u r e o f t h e data. 2 1 . 2 Scope

The list given h e r e i s p r o v i d e d t o f a m i l i a r i z e t h e u s e r w i t h t h e k i n d o f s t a t i s t i c a l t o o l s t h a t maybe r e q u i r e d f o r u s e b y r e g u l a t o r y o r a c c r e d i t i n g b o d i e s , or maybe o t h e r w i s e u s e f u l t o t h e l a b o r a t o r y . T h i s s e c t i o n w i l l not p r o v i d e d e t a i l e d i n s t r u c t i o n s f o r t h e u s e o f such t o o l s o r t e c h n i q u e s . 21.3 S t a t i s t i c a l Tools andTechniaues

a . Summary s t a t i s t i c s - S u m m a r y s t a t i s t i c s s u c h as t h e mean s t a n d a r d d e v i a t i o n ( a ) a n d t h e v a r i a n c e (a2)are u s e d t o

(x),t h e

s i m p l i f y t h e p r e s e n t a t i o n o f data and a t t h e same time summarize e s s e n t i a l characteristics. b. Frequencydistributions-Frequencydistributions s u c h a s normal

are u s e d t o p r e s e n t r e l a t i v e l y l a r g e d a t a s e t s . T h e i r u n d e r s t a n d i n g a n d u s e is i m p o r t a n t because t h e u s e f u l n e s s ofcontrolchartsisbasedonthe

assumption t h a t t h e rawdataisnormallydistributed. For data t h a t is log-normallydistributed; s u c h a s t h e d a i l y

I30

EWcctlve Date

Section No.

Subfeet

BY

STATISTICALMETHODS

2 1 .o

Page

Approved

Revised

2

0'

t

c o n c e n t r a t i o n s ofsuspendedparticulatesin ambient a i r , t r a n s f o r m a t i o n p r o v i d e s t h e normal d i s t r i b u t i o n u s ed i n m a k i n g decisions concerningthe results.

c . Testsofhypotheses-Ahypothesisisabeliefheldoran a s s e r t i o n m a d e about t h e n a t u r e o f n u m e r i c a l v a l u e s o f s o m e p a r a m e t e r o f a p o p u l a t i o n . Inmakingahypothesisthereisthe opportunityofmakingoneoftwokindsoferrors:

(1) Type I e r r o r , which is r e j e c t i o n o f t h e h y p o t h e s i s w h e n i t is

true. ( 2 ) Type I I e r r o r , which i s a c c e p t a n c e o f t h e h y p o t h e s i s w h e n i t is f a l s e . d . Outliers-outlying observations are u n u s u a l l y l a r g e o r small

v a l u e s which appear as anomalies i n a data s e t . A number o f s t a t i s t i c a l tests are a v a i l a b l e fordeterminingthepresence o f

o u t l y i n g data. e . Control Charts-Control c h a r t s are, perhaps, t h e most u s e f u l

s t a t i s t i c a l toolavailabletothelaboratory. They w i l l be used inthislaboratoryasprescribedbymethodsandasdirectedby t h e Q u a l i t y Control Coordinator ( F i g u r e s 2 1 - 1 a n d 2 1 - 2 ) . f . Sampling-Thislaboratorywilluse s a m p l i n g p l a n s fromASQCZ

1.4*,

1993

llSamplingProceduresandTables f o r InspectionBy

Attributes"

f o r incoming i n s p e c t i o n o f t e s t i n g a n d a n a l y t i c a l

s u p p l i e s and materials as directed by t h e Q u a l i t y Control Coordinator. and for t h e s e l e c t i o n o f sample data for data validation.

131

5

Effective Date

Subject

STATISTICALMETHODS Approved

1

Revised

g. T e s t s f o r s i g n i f i c a n c e of d i f f e r e n c e - D i f f e r e n c e s o f t e n

a p p e a r i n g b e t w e e n t w o s e t s o f data g i v e rise t o t h e q u e s t i o n of whetherthedifferencehasanyimportanceorsignificance. or

occursmerelyduetochance cause. I n these cases, t e s t s u s i n g t h e F, t , or C h i - s q u a r e d i s t r i b u t i o n s a r e u s e f u l i n m a k i n g a decisionabout the datasets inquestion. h . R e l i a b i l i t y and m a i n t a i n a b i l i t y - A s measurement s y s t e m s grow

more complex, system r e l i a b i l i t y b e c o m e s an i n c r e a s i n g l y i m p o r t a n t c o n c e r n i n d e t e r m i n i n g t h e c o m p l e t e n e s s a n d accuracy of r e s u l t s . Thisisespeciallytruewhendealingwith remote recording instruments.

I32

99.7 99.5 UCL-

X UWLX

99.0 X

i

t f

e

X

98.5 LWLX LCLX

98.0

97.7

1 1 1 1 1

1

2

3

4

5

s

7-

8'

A

i i i i i i i i i i J 0

1.4 1.2

a

1.0

f m

.I

5

a

UCLR UWL-

R

.s

-

A

R

2 0

1

2

3

4

5

DirectioEs: value 1. Drar A l i n e 034 2. Drar UCL, l i n e 1-11 3. Draw UIL, l i n e 0.86 4. P l o t 1's as generated 5. Drar 1 l i n e 96.68

6 7 8 9 Samp I e Number

6. 7. 8. 9. ID.

FlGUAE21-1

Draw Draw Draw Draw Plot

10

UCLi l i n e 99.32 UIL? l i n e 99.11 L I L i line 9825 LMi l i n e 98.04 i t s as generated

En-

~atr

STATISTICAL METHODS

BY

-~-

L

Revbod

Approwd

l a b o r a t o r y Qua1 i t y Control Operation

-

X-R Chart

Date

H

m

U

a

L-

m

L

-c

Y)

m U

c a

m

Sample Number O i rections: 1. Draw R l i n e

value

2. Draw UCL, l i n e 3. Draw UIL, l i n e 4. P l o t 5. Draw

1's as ii l i n e

generated

6. Draw UCLi l i n e 7. Draw UIL: l i n e 8. Draw L I L i l i n e 9. Draw LCLi l i n e 10. P l o t i ' s as generated

FIGURE 21-2

134

21.0 5

of

5

Effectlvc Date

Section No.

Subject

NONCONFORMITY

BY

22. 0

Page

1 O' 4

Revised

Approved

2 2 . 1 Pu ruo s e The purpose o f t h i s s e c t i o n is t o p r e s c r i b e a c t i o n s t o b e takenwhen

t h e r e is s u s p i c i o n o f nonconforming r e s u l t s o c c u r r i n g d u r i n g t e s t i n g o r a n a l y t i c a l o p e r a t i o n s , or when such nonconformities occur as a r e s u l t o f d a t a v a l i d a t i o n , i n independent a u d i t r e p o r t s , i n customer complaints, or asaresultofequipmentmalfunction. 22.2 Scope The s u b j e c t m a t e r i a l i n t h i s s e c t i o n is related t o t h a t of t h e

followingSection23.0-11CorrectiveAction.11 However, C o r r e c t i v e

Action is t h e m o s t important one o f t h e s e v e r a l s t e p s t h a t s h o u l d b e takenwhenanonconformityisdiscovered. t h e r e f o r e , i t is treated

separately. 22.3 Actions 2 2 . 3 . 1 Whenanonconforming result is d i s c o v e r e d o r s u s p e c t e d , t h e occurrence w i l l b e reportedimmediatelyandthe d e t a i l s of t h e event noted i n t h e l a b o r a t o r y notebook. 22.3.2

The Q u a l i t y Control Coordinator w i l l be r e s p o n s i b l e for

reviewing t h e circumstances of a l l i n s t a n c e s o f o c c u r r e n c e o f n o n c o n f o r m i t i e s , t o d e t e r m i n e whether c o r r e c t i v e actionshouldbetaken, ifnewsamplesare required, i f the customershouldbenotified, i f r e t e s t i n g o r r e a n a l y s i s i s

necessary, o r w h e t h e r t h e resultsshouldbeconfirmedby

independentthirdpartytestingoranalysis. The r e s u l t s o f

1

I

Elicctlve Detc

Approved

I

Section No.

Subject

NONCONFORMITY

I

22 0

P.ge

Revired

t h i s reviewby t h e Q u a l i t y Control Coordinator w i l l be

recorded on t h e Nonconformance Event ReviewReport ( F i g u r e 22-1) inwhich t h e f i r s t 6 e n t r i e s w i l l b e f i l l e d o u t b y t h e a n a l y s t or t e s t t e c h n i c i a n a s f o l l o w s : ( 1 ) E n t e r t h e S a m p l e I d e n t i f i c a t i o n N u m b e r . ( 2 ) E n t e r t h e date t h e Report is o r i g i n a t e d . (3)Describe t h e sample i n as much detail as p o s s i b l e . ( 4 ) E n t e r t h e number andname o f t h e m e t h o d b e i n g used a t t h e time of t h e occurrence o f t h e nonconformity. ( 5 ) Describe t h e nonconforming e v e n t s u s p e c t e d . ( 6 )

Describe t h e expected r e s u l t . ( 7 ) T h i s a n d t h e rest o f t h e

e n t r i e s w i l l b e m a d e b y t h e Q u a l i t y Control Coordinator. Enter here ( 7 ) t h e name o f t h e i n d i v i d u a l r e c e i v i n g t h e Report. ( 8 ) E n t e r t h e name oftheindividualinitiatingthe Report. (9)TheQualityControlCoordinatorwillcheckthe entryinthelaboratorynotebook a n d n o t e i t s p r e s e n c e . ( 1 0 ) The Q u a l i t y Control C o o r d i n a t o r w i l l n o t e t h e

n e c e s s i t y t o i n i t i a t e a C o r r e c t i v e Action Request ( F i g u r e 2 3 - 1 ) a n d a t t a c h a copy i f t h e C A R i s i n i t i a t e d . (11)The need f o r new samples w i l l be i n d i c a t e d . ( 1 2 ) The fact t h a t t h e customerwas notifiedwillbeindicated. (13)I f

r e t e s t i n g o r reanalysisofsamplesonhandisdeemed n e c e s s a r y , i t w i l l b e i n d i c a t e d h e r e , and t h e n a m e o f t h e a n a l y s t or t e s t t e c h n i c i a n towhom t h e w o r k i s a s s i g n e d

136

2

01

4

Eftectlve Dale L

BY

Subject

NONCONFORMITY

Section No.

Pwe

22.0

Revised

Approved

w i l l be e n t e r e d . (14) Ifanoutsidelaboratoryisusedto

c o n f i r m t h e r e s u l t s i n q u e s t i o n , t h e name a n d a d d r e s s o f t h e l a b o r a t o r y w i l l b e e n t e r e d . ( 1 5 ) T h e date t h a t t h e Q u a l i t y Co n t r o l Coordinator completes t h e Review Report w i l l be e n t e r e d . (16) The Review Report w i l l be s i g n e d by t h e Q u a l i t y Co n t r o l Co ordinator.

.

22 3.3 The Q u a l i t y C o o r d i n a t o r w i l l take a l l s t e p s n e c e s s a r y t o

p r e v e n t r e p e t i t i o n of nonconformances i n c l u d i n g t h e i n i t i a t i o n o f a C o r r e c t i v e Action Request ( F i g u r e 23-1). q . v .

137

3

Ot

4

Effectlve Date

Section NO.

Subject

NONCONFORMITY

BY Approved

prpe

22.0 4

Of

Reviwd

NONCONFORMANCE EVENT REVIEW REPORT SAMPLE IDENT. NO. (1) SAMPLE DESCRIPTION

DATE

(3)

SUSPECTED NONCONFORMANCF

EXPECTED RESULT

(6)

1. REPORTED T O

C7)

2 REPORTED BY:

(*)

13)

(’)

2 EVENT LOGGED IN LABORATORY NOTEBOOK: YES( ) NO( ) ( 9 )

3. CORRECTIVE ACTION REOUEST INITIATED YES( ) NO( ) (10) 4. NEW SAMPLES REQUESTED: YES( ) NO( )

5.CUSTOMERNOTIFIED

YES( ) NO( )

(ATTACH COPY)

(1 1)

(12)

6. RETEST OR REANALYSIS NECESSARY YES( ) NO( ) (13) IF YES. TO WHOM ASSIGNED

7. THIRD PARTY LABORATORY CONFIRMATION NECESSARY: YES( ) NO( ) IF YES. NAME OF UBORATORY (14)

(16)

OUALllY CONTROL COORDINATOR

FIGURE 22-1

138

4

Effecllve Dale

Scclion No.

Subjeel

CORRECTIVE ACTION

BY Approved

23 .0

Page

1 Of 8

Revised

23.1 Purpose T h i s s e c t i o n describesthe procedures f o r c o r r e c t i n g a d e p a r t u r e

fromstandardofanysort, fixing responsibility f o r t h e action t o be t a k e n , documentingthe s t e p s t a k e n , a n d s e c u r i n g a r e p o r t on t h e

r e s o l u t i o n o f t h e problem. 23.2 Scope T h i s s e c t i o n deals w i t h b o t h - s h o r t -term o r immediate c o r r e c t i v e

a c t i o n and long-term c o r r e c t i v e a c t i o n t a k e n t o a v o i d r e c u r r e n c e o f t h e problem. 23.3 K i n d s o f C o r r e c t i v e Action

T h e r e a r e two t y p e s o f c o r r e c t i v e a c t i o n a v a i l a b l e t o t h e l a b o r a t o r y : on-the-spot orimmediate, t o c o r r e c t o r r e p a i r n o n c o n f o r m i n g d a t a or equipment. C o r r e c t i v e action-long term, t o e l i m i n a t e c a u s e s o f n o n - c o n f o r m a n c e and t a k e m e a s u r e s t o see t h a t t h e y d o n o t r e c u r . Stepscornprisingaclosed-loopcorrectiveaction system are: a . Define t h e problem. b. Assign r e s p o n s i b i l i t y f o r i n v e s t i n g t h e problem.

c . Determineacorrectiveactionto e l i m i n a t e t h e problem. d . Assign and a c c e p t r e s p o n s i b i l i t y f o r i m p l e m e n t i n g t h e

corrective action. e . E s t a b l i s h t h e e f f e c t i v e n e s s o f t h e c o r r e c t i v e a c t i o n and implement t h e c o r r e c t i o n . f . Verify t h a t t h e corrective a c t i o n h a s eliminatedthe

problem.

Etfectlve Date

Section No.

Subjec:

CORRECTIVE ACTION

BY Approved

23 .0

Page

20' 8

Revised

C o r r e c t i v e a c t i o n p r o c e d u r e s recognize t h e need f o r a d e s i g n a t e d individual t o t e s t continually t h e effectiveness o f t h e systemand the corrective actions.

23.3.1

On-the-spot or

Immediate C o r r e c t i v e Action-this isthe

p r o c e s s o f c o r r e c t i n g malfunctioning equipment. The o p e r a t o r h a s t h e r e s p o n s i b i l i t y f o r c o n d u c t i n g

immediate c o r r e c t i v e a c t i o n when a p r o b l e m arises.

A p p r o p r i a t e p r o c e d u r e s are: a . Found i n t h e m e t h o d b e i n g u s e d , o r -

b . Providedbythelaboratoryasatrouble-shooting

c h e c k l i s t , or -

c . Providedbyequipmentmanufacturersastrouble-shooting g u i d e s , or -

d . I n t h e e v e n t t h a t t h e s o l u t i o n t o t h e problem i s n o t

found i n t h e s o u r c e s a b o v e , o r i s b e y o n d t h e c a p a b i l i t i e s o f t h e operator, hewill report h i s f i n d i n g s t o higher authority. 2 3 . 3 . 2 L o n g - t e r m c o r r e c t i v e Action t a k e n f o r r e c u r r i n g p r o b l e m s , w i l l be i n i t i a t e d b y t h e u s e o f t h e C o r r e c t i v e A c t i o n

Request form ( F i g u r e 2 3 - 1 ) w h i c h w i l l be c o m p l e t e d a s f o l l o w s : (1)E n t e r t h e C o r r e c t i v e Action Request ( C A R )

Effecllve Date

ScctionNo.

Subject

CORRECTIVE ACTION

BY

-

Approved

23 0

P8Qe

3

Of

8

Revised

number. ( 2 ) Enter t h e suspense date. T h i s is t h e date by whichasolutionisexpected. ( 3 ) E n t e r t h e n a m e a n d a d d r e s s

o f t h e o r i g i n a t o r o f t h e CAR. ( 4 ) E n t e r t h e d a t e t h a t t h e C A R i s o r i g i n a t e d . ( 5 ) Enter t h e name o f t h e i n d i v i d u a l t o

whomthe r e s p o n s i b i l i t y i s given f o r a r r i v i n g a t a s o l u t i o n t o t h e problem. ( 6 ) E n t e r t h e name o f t h e o r g a n i z a t i o n o f t h e p e r s o n a s s i g n e d t h e r e s p o n s i b i l i t y i n ( 5 ) . (?)Describe t h e n a t u r e oftheprobleminasmuchdetailas n e c e s s a r y f o r

aclearunderstandingoftheproblem. ( 8 ) Ifknown,

d e s c r i b e t h e u n d e r l y i n g cause o f t h e problem. ( 9 ) E n t e r t h e s i g n a t u r e of t h e person b r i g i n a t i n g t h e CAR. ( 1 0 ) Describe t h e phase o f t h e operationormethodduringwhichthe

problem was discovered. (11)E n t e r t h e name and address o f t h e person t o whom t h e s o l u t i o n t o t h e p r o b l e m i s t o b e

reported, and t h e date by which t h e r e p o r t is t o be completedand r e t u r n e d . (12)L i s t t h e n a m e s a n d a d d r e s s e s o f o t h e r i n d i v i d u a l s t o whom c o p i e s of t h e r e p o r t are t o be s e n t . (Reverse side-13) Repeat t h e CAR number a t t h e t o p o f t h e reverse s i d e . (14) Enter t h e d e t a i l s o f t h e recommended

c o r r e c t i v e a c t i o n . (15) I n d i c a t e whether or n o t t h i s i s a temporary f i x . (16) Indicateifthisisapermanent

s o l u t i o n . (17) T o b e s i g n e d b y t h e p e r s o n towhom t h e

141

Eftectlve Date

Subjecl

Section

CORRECTIVE ACTION

BY Approved

No.

23 0

pwe

4

01

Revised

r e s p o n s i b i l i t y f o r completion o f t h e c o r r e c t i v e a c t i o n w a s a s s i g n e d . (18) E n t e r t h e d a t e o f t h e completed c o r r e c t i v e action. (19)Listthenameoftheindividualstowhomcopies ofthecompletedCARaretobe routed. ( 2 0 ) E n t e r t h e

i n i t i a l s o f t h e a u t h o r i t y approving t h e C A R . ( 2 1 ) E n t e r t h e d a t e i n i t i a l e d . ( 2 2 ) E n t e r t h es u s p e n s e d a t e t h a t a f o l l o w up i s t o b e m a d e t o e n s u r e t h a t t h e recommendedaction h a s taken place. ( 2 3 ) Enter t h e i n i t i a l s o f t h e a u t h o r i t y approving t h e c o r r e c t i v e a c t i o n measures recommended. When s e v e r a l CAR'S are simultaneouslybeingprocessed, i t w i l l b e n e c e s s a r y t o r e c o r d t h e m o n t h e C o r r e c t i v e Action

Master Log, ( F i g u r e 2 3 - 2 ) which w i l l be f i l l e d o u t as f o l l o w s : ( 1 )E n t e r t h e a s s i g n e d CAR No. from t h e f i r s t heading on t h e CAR. (CARnumberswillbe c a r r i e d a c r o s s t h e t o p o f t h i s form. I n t h i s example there is room f o r f i v e s i m u l t a n e o u s e n t r i e s . ) ( 2 ) Enter t h e date s u b m i t t e d from Entry ( 4 ) o f t h e CAR. ( 3 ) E n t e r t h e d a t e l o g g e d i n . ( 4 ) E n t e r t h e name o f t h e o r i g i n a t o r o f t h e CAR f r o m E n t r y ( 3 ) o f t h e CAR. ( 5 ) E n t e r a b r i e f d e s c r i p t i o n o f t h e p r o b l e m p r e s e n t e d . ( 6 ) F u r n i s h a b r i e f d e s c r i p t i o n o f t h e c a u s e of t h e problem, i f k n o w n . ( 7 ) E n t e r t h e name o f t h e i n d i v i d u a l

towhom t h e p r o b l e m w a s a s s i g n e d f o r s o l u t i o n . ( 8 ) I n d i c a t e t h e s u s p e n s e d a t e . ( 9 ) Describe t h e n a t u r e or k i n d o f

i n v e s t i g a t i o n u n d e r t a k e n , ifknown. ( 1 0 ) I n d i c a t e t h e c a u s e o f t h e problem, whendiscovered. ( 1 1 ) D e s c r i b e t h e

a

Etfccllve Dale

Subject

CORRECTIVE ACTION

BY Approved

J

Section No.

23.0

Page

5

Of

Revised

c o r r e c t i v e a c t i o n recommended. ( 1 2 ) I n d i c a t e who is t o b e r e s p o n s i b l e f o r t a k i n g t h e recommended c o r r e c t i v e a c t i o n . (13) I n d i c a t e how t h e o r i g i n a t o r o f t h e C A R i s t o b e

n o t i f i e d o r was n o t i f i e d o f t h e outcome o f t h e i n v e s t i g a t i o n . (14) I n d i c a t e t h e r e s u l t s o f a n y f o l l o w - u p i n v e s t i g a t i o n conductedto determine whether t h e recommendedactionwastakenandifitwas e f f e c t i v e i n c o r r e c t i n g t h e p r o b l e m . (15) T h e Q u a l i t y C o n t r o l Coordinator w i l l i n i t i a l t o i n d i c a t e t h a t t h e C A R w a s s a t i s f a c t o r i l y closed out. R e g a r d l e s s o f w h o i n i t i a t es t h e CAR, The Q u a l i t y C o n t r o l Coordinator is r e s p o n s i b l e f o r t h e maintenance o f t h e C o r r e c t i v e A c t i o n R e q u e s t Master Log and f o r p r e p a r a t i o n o f a n y p e r i o d i c CARstatus reportrequiredbymanagement.

I43

0

-

f

Eweuw oar

suqut

CORRECTTVE ACTION

CORRECTIVE ACTION REQUEST

FIGURE 32-1

144

Ellrtlw Dato

Subfrcl

CORRECTIVE ACTION

BY

Section No.

W e

7

71.1)

Of

8

NOTE: Pbaw nturn lhls lorm Lo (h.Originator w i ~ hUU correctiw actam plannod on or blare camnutmonI~ I O If. you dabnnh (h.1 in. action required Is beyond Ihe #cope 01 your position. please indicate below r h o La responsible.

C A

oc A T

R I L O C N

T I

V

E

CAR FINAL DISTRIBUTION OngUW: &WNIOr

ACCEPTANCE OF CA

145

THIS SPACE n EseavEo Fon FOLLOW-UP

f

Ettoetlvo Dab

~tlon-No.

SUWl

CORRECTIVE ACTION

BY

23.0 O'

CORRECTIVE ACTION REQUEST MASTER LOG Corrective Action Request Form No.

(1)

Dale Submilled

(2)

Dale Received

(3)

Submillod BY

(4)

General ProbI em De8criptio.n

Arsigned

To

I

(7)

Answer Due

(8)

caure 01 Problm

(10)

Correctlve Action

(w

I

I

Corrective Action Rorponribilily

FIGURE 32-2

L

I46

I

8

Ellectlve Date

Section No.

Subject

QUALITY COSTREPORTING

BY Approved

24.1

24.0

Page

1

Of

5

Revised

Purpose T h i s s e c t i o n d e s c r i b e s how o p e r a t i n g c o s t s w i l l be a l l o c a t e d

a c c o r d i n g t o q u a l i t y a s s u r a n c e e l e m e n t s and groupedby c o s t c a t e g o r i e s and s u b - c a t e g o r i e s . Q u a l i t yc o n t r o l c o s t r e p o r t i n g i s also requiredbythis section. 24.2

Scope T h i s s e c t i o n d e a l s o n l y w i t h o p e r a t i n g costs r e l a t e d t o t h e q u a l i t y

c o n t r o l f u n c t i o n a n d d o e s n o t c o n s i d e r o t h e r c o s t s r e l a t e d t o such f u n c t i o n s as a d v e r t i s i n g , marketing, d e p r e c i a t i o n , u t i l i t i e s , taxes, e t c . 24.3

Reasons f o r I d e n t i f s i n v Q u a l i t y C o s t s Q u a l i t y a s s u r a n c e c o s t s s h o u l d be i d e n t i f i e d and recorded p r i m a r i l y t o i d e n t i f y e l e m e n t s whose c o s t s are d i s p r o p o r t i o n a t e t o t h e b e n e f i t s d e r i v e d . A n a d d i t i o n a l purpose is t o d e t e c t cost t r e n d s f o r budget f o r e c a s t i n g . Identificationofcostsisa p r e r e q u i s i t e t o c o s t reduction e f f o r t s .

24.4

D e f i n i t i o n s o f Q u a l i t y Cost C a t e g o r i e s 24.4.1 P r e v e n t i o n c o s t s a r e t h o s e e x p e n s e s i n c u r r e d i n k e e p i n g

u n a c c e p t a b l e data f r o m b e i n g g e n e r a t e d i n t h e f i r s t place. I n c l u d e d i n t h i s categoryare suchthingsasquality planning, q u a l i t y t r a i n i n g , etc.

I47

EnccuW Date

suqect

BY

QUALITY COSTREPORTING

w

24.0

e

2

Of

Rcvird

Approved

24.4.2

Section No.

A p p r a i s a l c o s t s a r e t h o s e causedbythe n e c e s s i t y t o evaluate determinations o r r e s u l t s t h a t do not meet acceptance standards.

24.4.3

Internal f a i l u r e c o s t s a r e t h o s e causedbyinadequate o r spoiled samples, d e f e c t i v e testingmaterials o r reagents, malfunctioning instrumentation, o r operator f a i l u r e s which lead t o t h e productionofunacceptabledata.

24.4.4

External f a i l u r e c o s t s a r e t h o s e a r i s i n g fromincorrector nonconformingdata reported t o customers. Inother words, t h e defective product has already gone outside the

laboratory. 24.5

Sub-categoriesofLaboratoryQualityCosts-Theelementsofquality 24.5.1 P r e v e n t i o n C o s t s

a. Qualityplanning. b. Document c o n t r o l and r e v i s i o n .

c. Q u a l i t y t r a i n i n g . d. Q u a l i t y a s s u r a n c e p l a n s f o r special p r o j e c t s and

programs.

I

e . The Q u a l i t y Assurance Manual. f . P r e v e n t i v e maintenance.

I48

5

1 Eff&llvc Date

section NO.

Subject

QUALITY COSTREPORTING

BY

Pwe

24.0

3

Of

Revised

Approved

2 4 . 5 . 2 Amraisal C o s t s

a. Quality assurance a c t i v i t i e s a s s o c i a t e d w i t h p r e - t e s t p r e p a r a t i o n , sample c o l l e c t i o n , sample a n a l y s i s and

t e s t , and data r e p o r t i n g . b. Data v a l i d a t i o n .

c. Statistical analysis o f d a t a . d . Procurement q u a l i t y c o n t r o l .

e. Calibration. f . I n t e r l a b o r a t o r y andintralaboratorytesting. g . Audit p r o c e d u r e s .

h . Q u a l i t y r e p o r t s t o management. 24.5.3

I n t e r n a l f a i l u r e Costs a . A d d i t i o n a l sample c o l l e c t i o n and a d d i t i o n a l a n a l y s i s or t e s t i n g r e q u i r e d b e c a u s e of i n v a l i d samples. b. R e a n a l y s i s or retestingofcollectedsamplesbecause of equipment f a i l u r e or o p e r a t o r e r r o r .

c. Scrappingofdata, becausedatawasdetermined t o b e invalid. 24.5.4 E x t e r n a l f a i l u r e C o s t s

a . I n v e s t i g a t i o n o f customer complaints. b. C o r r e c t i v e a c t i o n e f f o r t s .

c . No c h a r g e r e p e t i t i o n of t e s t s or a n a l y s i s t o s a t i s f y customer c o m p l a i n t s .

I49

5

Effective Date

Subject

BY

QUALITY COSTREPORTING

Approved

Section No.

24. 0

Psge

4

O f 5

Revised

A f t e r q u a l i t y c o s t element s h a v e b e e n l i s t e d i t w i l l be necessary t o a l l o c a t e tothem cost f i g u r e s a v a i l a b l e fromtheaccounting system. Ifactualcostingfiguresarenotavailable,t h e a c c o u n t i n g component w i l l p r o v i d e estimates as n e a r l y a c c u r a t e a s p o s s i b l e . 24.7 Q u a l i t y Cost R e p o r t s

Q u a l i t y c o n t r o l c o s t f i g u r e s w i l l be r e p o r t e d q u a r t e r l y t o management, showing c o s t figuresallocatedtoeachofthe f o u r major q u a l i t y c o s t c a t e g o r i e s and t h e r e l a t i o n s h i p of c a t e g o r y c o s t s t o t o t a l q u a l i t y costs. The Q u a l i t y Cost Report ( F i g u r e 24-1)w i l l b e p r e p a r e d a s a b a r graph showing :

a . E x p e n d i t u r e by c o s t c a t e g o r y . b. Totalqualitycostexpenditure.

c. Quarterlyquality cost trends.

150

.

Eftectlve bate

Sccllon No.

Subject

QUALITY AUDITS

BY

Approved

25.0

Page

1

0‘

20

Revised

PurDose T h i s s e c t i o n d e s c r i b e s t h e c o n d u c t o f Q u a l i t y S y s t e m A u d l t sA.

check list is appended f & use i n c a r r y i n g out system a u d i t s . A s y s t e m a u d i t i s an o n - s i t e , formal i n s p e c t i o n a n d review o f t h e

1 a b o r a t o r y Q u a l i t y Control System, t a k i n g p l a c e on a p e r i o d i c unannouncedor announcedbasis, t o v e r i f y t h e e f f e c t i v e n e s s o f t h e laboratory’squalityprogram, a s d e s c r i b e d i n t h e s e v e r a l s e c t i o n s

o f t h i s m a n u a l . The Q u a l i t y SystemAudit i s a Q u a l i t y Assurance activity. 2 5 . 2 Scope T h i s procedure a p p l i e s t o t h e f o l l o w i n g i n t e r n a l f u n c t i o n s ;

Receiving, Re c e i v i n g I n s p e c t i o n ( i f a p p l i c a b l e ) , Sample S t o r a g e , Chain-of-Custodyprocedures, C a l i b r a t i o n , Preventive Maintenance, D a t a V a l i d a t i o n , a n d o t h e r a r e a s t h a t a f f e c t t h e q u a l i t y o f l a b o r a t o r y o u t p u t , a s d e s c r i b e d i n t h i s m a n u a l . The qualityauditingofsupplierandsubcontractoractivities i s coveredbySections8.0and19.0. 2 5 . 3 Procedure

25.3.1

The Q u a l i t y Control C oordinator w i l l be r e s p o n s i b l e f o r

a r r a n g i n g for t h e conduct o f Q u a l i t y System Audits. They

w i l l be c a r r i e d o u t b y a n a u d i t o r f r o m a n o u t s i d e a g e n c y , or

by a n a u d i t o r or a u d i t team selected f r o r n o u t s i d e t h e

l a b o r a t o r y Q u a l i ty Control organization. I n t e r n a l a u d i t s w i l l be conducted semiannually, as scheduled.

I

Effective Date

Subject

Section No.

QUAL I T Y A U D I T S

BY Approved

25.3.2

25.0

Page

2

0'

Revised

T h e a u d i t o r , or a u d i t teamwill use t h e Q u a l i t y System

Audit C h e c k L i s t ( F i g u r e 2 5 - 1 ) as a guide when c o n d u c t i n g the audit anduse thismanual t o establish t h e c r i t e r i a f o r

d e t e r m i n i n g t h e d e g r e e of compliance w i t h t h e r e q u i r e m e n t s o f t h i s document. 2 5 . 3 . 3 The s t e p s t o b e f o l l o w e d i n c o n d u c t i n g t h e s y s t e m a u d i t a r e : a. Notification o f t h e d a t e s a n d t i m e s o f t h e plannedaudit t o a l l i n d i v i d u a l s concerned. b . Hold p r e a u d i t conference.

c . Conduct of t h e a u d i t . d . Hold p o s t a u d i t conference, c r i t i q u e , and wrap-up.

e . Follow-up t o d e t e r m i n e i f d e f i c i e n c i e s d i s c o v e r e d duringthe audithavebeencorrected. 2 5 . 3 . 4 The Q u a l i t y C o n t r o l Coordinator w i l l be r e s p o n s i b l e f o r i n i t i a t i n g any C o r r e c t i v e ActionRequest ( s e e S e c t i o n 2 3 . 0 ) made n e c e s s a r y a s a r e s u l t o f t h e a u d i t . 2 5 . 3 . 5 The Q u a l i t y System Audit C h e c k L i s t f o l l o w i n g ( F i g u r e 2 5 - 1 ) w i l l be u s e d t o conduct t h e a u d i t .

The c o v e r page o f t h e Audit C h e c k L i s t w i l l b e f i l l e d o u t as f o l l o w s : (1)E n t e r t h e name and t i t l e o f t h e i n d i v i d u a l making t h e s u r v e y , or t h e name and t i t l e o f t h e head o f t h e

152

20

-

Eftectlvc Date

Section No.

Subjul

QUALITY AUDITS

BY Approved

25 .o

P.ge Revl8ed

3

a u d i t team. ( 2 ) E n t e r t h e survey r e s u l t s fromthe s c o r i n g g r i d on the followingpage showing t h e t o t a l a p p l i c a b l e p o i n t s , the t o t a l survey poi nts and the percentage grade. (3)Enterthedate. a. T h e a u d i t w i l l be g r a d e d u s i n g t h e i n s t r u c t i o n s given on t h e f i r s t page o f t h e c h e c k l i s t . b. A l l personnel whose a c t i v i t i e s have been

a u d i t e d w i l l b e given t h e grading r e s u l t s , however no p a s s / f a i l grade w i l l be established a s t h e primarypurpose o f t h e

a u d i t w i l l be t o i d e n t i f y a r e a s o f weakness a n d n o n c o n f o r m i t y w i t h p o l i c i e s and procedures e s t a b l i s h e d i n t h i s Manual.

Of

20

8ubj.ct

WALITY ALQTTS

I

S.ctbnN0.

QUALITY CONTROL QUALITY SYSTEM AUDIT CHECK LIST INSTRUCTIONS Laboralory compliance with each queslion will be indicated by placinp 0. I . 2. 3. or NA on the ltne opposite each quesllon.

0. Required but no1 being done. I. Below acceplancc standards.

2. Adequate with minor deparlures lrom good pracllces. 3. Adequate in all respects.

NA. INol Applicable1 when i t is obvious Ihal a question would be inapproprtale. due lo type acllvlty. lackolfacllllles.rprcial mclhods or other valid reasons. A l the conclusion ol the survey. each category 01 questions should be analyzed and summarized lor acceptability. Space is provided In Ihe index lor entering these resutls. Remarks or comments by the survey team will be placed on the blank m eopporitc at!qurstlon. The lollowing method shall be used in summarizing each category: Total the survey poinls lor all appltablr queslians. Oivlde thls talal by the lolal applicable questions. Mutliplied by the weighting laclor 013. this compulalion will resull In a percent accepUbillly Irgure.

Tolal paints lor applicable querlions rated Number 01 applicable questions X 3

= Percent Acceptability

Example: Far category 1. we have a tolat 01 10 applicable q m l i o n s and a weighling lactor 01 3 per question 110 I 31 Therelore-

20 10x3

43% (Percent acceplability lor calcgoryl

SURVEY By AND DATE

SURVEY RESULTSLLOF = K

(1)

NAME - TlTLE

- OAT€

(3)

FIGURE 25-1

154

Effoeh Dak

- suqed

-On

QUALITY ALDITS

BY

I

I

Pwe

No*

25.0 5

Of

I

QUALITY SYSTEM AUDIT CHECK LIST

SURVEY RESULTS

OF

CATEGORY 1 2 3 4

5 6

7

a

9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24

Quality Goals and Objectives Quality Policies The Ouality Organization Management of the Ouality Manual Quality Planning Ouality in Procurement Sample Handling, Storage and Shipping Chain-of-custody Procedures Laboratory Testing and Analysis Control Quality Documentation and Records Control Control of Measuring and Test Equipment Preventive Maintainance Reference Standards Data Validation Epironmental Control Customer Complaints Subcontracting Personnel Training. Qualification & Motivation Statistical Methods Nonconformity Corrective Action Ouality Cost Reporting Ouality Audits Reliability

FIGURE 25.1

15s

'la

3n

I

BY

w

QUALITY AUDITS

p.a.

01

R.vird

CATEGORY 1 QUALITY POLICIES 1.

2.

3.

4.

Are the Quality Policiesclearly statad?

7

Are the Quality poficies consistaotwith auyrequirsmeatr of

regulatory or acmdithg bodies?

-

ofthe quality management system?

-

Arethe Qualay Policiesthe basis for estobliraii Quality Objectives?

__

Do the Quality Policii support the need fbr oontinuour improvement

Tatel Appliible Points TdSmyPoiatS psrcentags

-

-

CATEGORY 2

QUAL~GOALSANDOBJEcIlvEs

1.

Are the QualityObjectivesclearlystated?

2.

Are the Quality Objectives quaatifid kuofrr as posnib?

3.

DotheQualityObjactivessupporttheQualityPolicies?

4.

finthe Qualitr O&ctives besllapproved by management?

5.

Do~QualityObjec&miucludathecommitmanttoimpraM

-

-

Total ApplicablepoiPra -

coatinwuolycu&mer ~ m d t z l e ~ o f p c r f b n a a o e t ?

Tds\pveypOintr

p=-w

156

-

-

QUALITY ALQITS

sv

CATEGORY 3 THE QUALITY ORGFINIZRTION 1.

Laboratory management reflects a positive attitude toward Quality Control

2.

Direct responsibility for Quality Control has been formal 1 y establ ished.

3.

The functional relationship betueen Quality Control and other laboratory components has been clear1 y delineated.

4.

The line of authority uithin the Quality Control organization has been clearly delineated.

5.

The job description for the Quality Control Coordinator is up-to-date

and accurately describes

the current duties, responsibilites and authority of that individual.

6. The Quality Control Coordinator is not subordinate t o any individual who is responsible f o r carryins out teeti-

or analytical responsibilities.

Total Rpplicable Points Total Survey Points Percent ape

FIGURE 25-1

25.0 7

*

20

EtluiJvo D8b

I subJ.ct

8.ctkn No.

OUALITY ALDITS

I

CFlTEGQHY 4 M A G E H E N T OF THE QUALITY PIANUAL 1.

The r e s p o n s i b i l i t y f o r m a i n t e n a n c e of t h e Q u a l i t y Nanual is c l e a r l y e s t a b l i s h e d .

2.

The i s s u e o f t h e manual is c o n t r o l l e d .

3.

P r o v i s i o n is made f o r u p d a t i n s t h e manual a n d i s s u i n g r e v i s i o n s t o h o l d e r s of c o n t r o l l e d copies.

4.

P r o v i s i o n is made f o r t h e i s s u e of u n c o n t r o l l e d c o p i e s as n e c e s s a r y . T o t a l Applicable P o i n t s T o t a l Survey P o i n t s Percentage CRTEGQRY 5

Q U A L I T Y PLANNING

1.

The r e s p o n s i b i l i t y f o r t h e q u a l i t y p l a n n i n s f u n c t i o n is c l e a r l y d e f i n e d .

2.

T h e r e is o b j e c t i v e e v i d e n c e t h a t p l a n n i n s is a n o n - s o i n s .

3.

quality

continuous process.

The Q u a l i t y Manual a c c u r a t e l y reflects c u r r e n t q u a l i t y s y s t e m activities i n t h e laboratory. Total Wplicable Points T o t a l Survey P o i n t s Percentase

FIGURE 25-1

IS8

25.0

Eft&

Soctlon No.

M

QUALITY AUDITS

ey rrpprad

I

PWJ Rdnd

t

I CATEGORY 6

QUALITY I N PROCUREPENT 1.

Inspection is performed by Quality Control.

2.

Inspection instructions are available to inspection personnel.

3.

Inspection personnel perform inspection operations i n accordance with current instructions and procedures.

4.

There is a syetem t o maintain inspection i nstructions current.

5.

There is a prosram for Quality Control approval of vendors and subcontractors.

6.

Vendors and subcontractors are required to have a a Bystem for quality control.

7.

Inspection and test results are used to evaluate vendor quality performance.

8.

Purchase orders, specifications. and vendors' cataloss are available to receiving inspection.

9.

Inspection gases and test equiplrrent are adequate to perform required inspection.

10. Sampling inspection (uhen applicable) is perforlaed

t o ANSI/ASQC Z 1.4-1981.

RNSI/MQC 2 1.9-1980.

or other approved samplinn plan. 11. -proved

laboratories are used for special

tests and analyees outside the scope of the

laboratory 's capabi lit ies.

FlGURE25-1

IS9

25.0

9

O'

20

tkction No.

4

QUALITY AUDITS BY

Rwld

12. A l l r e a ~ e n tstock is properly labeled, dated and

marked with shelf-life expiration &en 13.

neceesary.

Chemical/physical analysis. test specifications, or certifications are required when applicable. Total Applicable Points Total Survey Points Percentage CRTTEGORY 7 SWTPLE HANDLING. STORAGE AND SHIPMENT

1.

The Quality Control Coordinator monitors the physical condition of incoming test samplee.

2.

Test and analytical samples are properly identified.

3.

Sample Submittal Forme are completely and accurately filled out. Total Rpplicable Points Total Survey Pointe Percent age CATEGORY 8 CHAIN-OF-CUSTODYPROCEDURES

1.

Is the Chain-of-Custody

DocuDentation Form correctly

and completely filled out? 2.

Doee the Chain-of -Custody Documentation Form establish custody of the sample at all times? Total Applicable Points Total Survey Pointn Percentage

FIGURE 25-1

160

25.0

I

*m

E(kcorrD8t.

er

QUALITY AL'DXTS

Sadon No.

R.rk.d

CFITEGORY 9 LRBOWTORY TESTING AND RNCILYSIS CONTROL 1.

F u n c t i o n checks are r o u t i n e l y p e r f o r a r e d b y t h e operator.

2.

The o p e r a t o r p e r f o r m c o n t r o l checks d u r i n g t h e a n a l y t i c a l or testins p r o c e d u r e s .

3.

T e s t s f o r a i s n i f i c a n c e of d i f f e r e n c e are made u h e n r e s u l t s i n d i c a t e t h e need.

4.

C o n t r o l charts are u s e d r o u t i n e l y f o r suspected or d i f f i c u l t lnethod d e t e r m i n a t i o n s .

5.

T h e Q u a l i t y C o n t r o l C o o r d i n a t o r is r e s p o n s i b l e for deciding u h i c h t e s t i n n o r a n a l y t i c a l operations w i l l be charted.

Total Applicable Points T o t a l Survey Points Percentage CRTEGORY 1 0 QURLITY DOCUPENTATION AND RECORDS CONTROL

1.

The q u a l i t y d o c u m e n t s t o b e c o n t r o l l e d are l i s t e d i n t h e Q u a l i t y Hanual.

2.

D o c u m n t r e t e n t i o n p o l i c i e s are p u b l i s h e d i n i n t h e Q u a l i t y ?lanual

o r eleeuhere i n u r i t i n p .

3.

The Q u a l i t y S y s t e m is adequately documented.

4.

T h e Q u a l i t y C o n t r o l C o o r d i n a t o r issues periodic reports t o n s n a s e r e n t w h i c h reflect q u a l i t y levels.

q u a l i t y c o s t s . customer c o m p l a i n t s . etc.

FIGURE 25-1

161

25.0

fl

ol

0

5. There is adequate control over the issue of new

technical documents and changes. 6.

Obsolete documents are retrieved from vork stations and are not permitted to remain in the hande of

---

ueers. Total M p l i c a b l e Points Total Survey Points Percentage CATEGORY 11 CONTROL OF I'EASURING AND TEST EQUIPMENT 1.

Quality Control procedures insure that instruments, gages. messurins devices and test e q u i p m n t are periodically inspected and recalibrated at estsbl ished i ntervale.

2.

Workins and reference standards of required accuracy that are periodically calibrated t o Primary standards traceable to the NIST are maintained in a suitable environment.

3.

Neu or repaired test e q u i p w n t and measurins devices are calibrated and proved satisfactory by Quality Control before release for

4.

-8.

There are uritten calibration procedures for each type of instrument and aeasurinp device.

5.

Objective evidence includes calibration date and date next calibration must be performed on measuring i nat rumentat ion.

FIGURE 25-1

I62

Ethctln Data

m

subjut

QUALITY AL!ITS

M l o n No.

P.0.

6.

R e c o r d eyetern provides f o r a u t o m a t i c recall of

sasee. i n s t r u m e n t s a n d test e q u i p m e n t due for calibration.

T o t a l Applicable Points T o t a l Survey Points Percentage CfiTEGORY 12 PREVENTIVE HAINTENCINCE 3.

T h e r e is a p l a n n e d , s c h e d u l e d w i t h the calibration system.

program t i e d i n t h a t ensures that

a l l m e a s u r i n s t a n d teat e q u i p m e n t u n d e r g o e s periodic p r e v e n t i v e maintenance. 2.

P r e v e n t i v e m a i n t e n a n c e c h e c k l i s t s are i n use a n d o n file.

3.

Rn adequate spars p a r t s i n v e n t o r y is o n hand. Total Applicable Points T o t a l Survey P o i n t s Percentape

FIGURE 25-1

163

25.0

13

Of

20

Effecllve Ds!e

QUALITY AUDITS

SubJect

BY Approved

Section No. .

,..23.0

14

Psge Revlaed

CATEGORY 1 3

REFERENCE STANDARDS 1.

L a b o r a t o r y p o l i c y r e q u i r e s t h e use of r e f e r e n c e standards.

2.

uhen a v a i l a b l e ,

-

The Q u a l i t y C o n t r o l C o o r d i n a t o r keep8 on f i l e a c o p y of N I S I P u b l i c a t i o n 260 a n d c o p i e s of N I S I C e r t i c a t e s of R n a l m i e .

T o t a l Applicable Points

-

T o t a l Survey P o i n t s

___

Percentase

-

CRTEGORY 1 4 DGTR VALIDRTION

1.

D a t a v a l i d a t i o n is r o u t i n e l y emploved t o d e t e c t o u t l i e r s or s p u r i o u s v a l u e s .

2.

P h n u a l d a t a v a l i d a t i o n t e c h n i q u e s are t h e o n l y m e t h o d s used t o detect o u t l i e r e a n d s p u r i o u e valueo.

3.

-

B o t h manual and c o m p u t e r i z e d t e c h n i q u e s are u s e d f o r data v a l i d a t i o n .

4.

Samplins plans f r o m ANSI/6SspC 21.4,

1981 are used

when selectinn samples f o r d a t a v a l i d a t i o n of l a r n e

-

q u a n t i t i e s of data. Total mplicable Points T o t a l Survey P o i n t s Percentwe

-

CATEGORY 15

ENVIRONI7ENTCU. CONTROLS 1.

The l a b o r a t o r y u o r k i m e n v i r o n m e n t i s c o n t r o l l e d t o the extent Prescribed by t h e h n u a l Total 6xwlicable Points

-

T o t a l Survey P o i n t s Percentane

Figure 25-1 I64

-

O'

20

Effective Date

Subject

QUALITY AUDITS

Section No.

Revised

15

CATEGORY 16 CUSTOMER SATISFACTION AND COMPLAINTS 1.

A record is kept of all customer contacts and the Quality Control coordinator is responsible for reviewing them and taking any necessary action.

2.

One individual is charged with the responsibility for handling all complaints from customers, regulatory agencies, and accrediting

-

organizations. 3.

There is a system for providing feedback to all laboratory personnel

-

concerned. 4.

Ifrequired by contractual, regulatory, or accreditation bodies, the Quality Control Coordinator will arrange with an outside marketing analysis agency to conduct whatever surveys are necessary in order to appraise the effectiveness of the laboratory’s customer satisfaction

-

efforts. 5.

One individual is charged with the responsibility for initiating

Total applicable points

-

Total survey points

-

Percentage

-

corrective action, if this becomes necessary.

Figure 25-1 165

t

-0.c

er

r-+m

&cuon No.

QUALITY AUDITS

R.rtrd

CATEGORY 1 7

SUBCONTRKTING 1.

C o n t r a c t l a b o r a t o r i e s are r e q u i r e d t o have a v i a b l e Q u a l i t y C o n t r o l System i n place.

2.

P r o v i s i o n is made f o r f u r n i s h i n g c o n t r a c t l a b o r a t o r i e s with *audit” samples t o test l a b o r a t o r y proficiency.

3.

When a new method is introduced.

p r o v i s i o n is made

f o r f u r n i s h i n g c o n t r a c t l a b o r a t o r i e s with spiked samples t o test the p r o f i c i e n c y of t h e l a b o r a t o r y i n performing t h e Irethod. T o t a l Elpplicable P o i n t s Total Survey P o i n t s Percentwe CATEGORY 18 PERSONNEL TRAINING. QUALIFICATION M D tlOTIVATION 1. The l a b o r a t o r y p r o v i d e s f o r employee i n d o c t r i n a t i o n

and t r a i n i n g i n Q u a l i t y Control

2.

The l a b o r a t o r y hae a propram t o t e s t the effectiven e s s of t h e t r a i n i n g e f f o r t .

3.

T r a i n i n g r e c o r d s are a v a i l a b l e t o indicate t h e

s t a t u s of i n d i v i d u a l t r a i n i n % . 4.

The l a b o r a t o r y conducts c-ainne,

s u p p o r t e d by

a s w e a e n t , t o promote t h e a c h i e v e a e n t of s u p e r i o r q u a l i t y output. Total WplicabJe Points T o t a l Survey P o i n t s Percentase

FIGURE 25-1

166

25.0

16

of

n

m w

Elhc(trrW

BY

QUALITY AUDITS

(kctkn No.

P.0. Rdwd

'-

CATEGORY IS STRTISTICRL HETHODS 1.

The l a b o r a t o r y employe t h e f o l l o u i n g s t a t i s t i c a l t e c h n i q u e s i n t h e r o u t i n e conduct of a n a l y t i c a l a n d testing work: a.

Tests of h y p o t h e s e s

b.

T r e a t ~ m n tof o u t l i e r s

c.

Control C h a r t s

d.

Sampling P l a n e

8.

Tests f o r s i g n i f i c a n c e o f d i f f e r e n c e s Total Applicable P o i n t s Total Survey P o i n t e Percentage CATEGORY 20 NONCONFORMITY

1.

The Q u a l i t y C o n t r o l Syetem a s s u r e s t h a t p o s i t i v e a c t i o n is t a k e n , uhen a nonconformino e v e n t o c c u r s , t o e n s u r e t h a t a l l r e q u i r e d tasks are performed i n a c c o r d a n c e w i t h p r o v i s i o n s of t h e Q u a l i t y Pbnual.

2.

Adequate records are k e p t of n o n c o n f o r m i t i e e . Total Applicable P o i n t s Total Survey P o i n t s Percentane

-

FIGURE 25-1

167

25.0 1 7 Of J.r

3n L"

L

E f f u t k 0-

Section No.

QUALITY AUDITS

*bJ.ct

Pago

BY

R.rh.d

Apprad

CATEGORY 21 CORRECTIVE ACTION 1.

The laboratory has a method of recurrence control to prevent repetitive discrepancies.

2.

Corrective action requests on nonconforming events are initiated promptly.

3.

Records provide for follow-up on all corrective action requests.

4.

The responaibilty for solvin8

the problem by

taking corrective action is clearly established. 5.

The Suspense Date uhen the corrective action is expected to be completed is clearly established.

6.

The Corrective Action LO8 c o n t r o l s the progress of the corrective action initiated by the Corrective Action Request. Total Applicable Points Total Survey Points Percent age

FIGURE 25-1

168

25.0

18

of

0

CATEGORY 22

QUALITY COST REPORTING 1.

Q u a l i t y c o s t s are accumulated for the f o l l o w i n g categories:

a-

2.

-

Prevention coets

b.

Appraisal c o s t s

c.

Internal failure costs

d.

E x t e r n a l f a i l u r e costs

m e n actual c o s t s f i g u r e e cannot be o b t a i n e d from t h e c o s t accounting c o v o n e n t .

reaeonably

a c c u r a t e e s t i m a t e s are d. 3.

Q u a l i t y Cost r e p o r t s are made t o mnnauerent periodically.

4.

Q u a l i t y cost f i g u r e s are used i n t h e a n n w l

b e e t i n u process.

Total m p l i c a b l e Points T o t a l Survey P o i n t 0 Percentwe

I

FIGURE25-1

-

-

.

E t f u t h 081.

subject

QC'ALITY AUDITS

Section No. p-0

BY

Rwlnd

Ap-

CATEGORY 23

QUALITY AUDITS 1.

Q u a l i t y a u d i t s are p e r f o r m e d o n a n announced. scheduled b a s i s by i n d i v i d u a l s o u t s i d e t h e

qua1 i t y o r g a n i z a t i o n .

2.

All areas of t h e l a b o r a t o r y c o n t r i b u t i n g t o t h e Q u a l i t y o f work o u t p u t are a u d i t e d .

3.

The r e s u l t s o f t h e a u d i t are r e p o r t e d t o manasement i n w r i t i n s .

4.

P r e a u d i t a n d p o s t a u d i t c o n f e r e n c e s are h e l d p r i o r t o and after e a c h a u d i t . Total Applicable Points Total Survey Points P e r c e n t a8e CATEGORY 24

E L I RBI LI TY 1.

R e l i a b i l i t y f o r e c e s t e i n ternm of " W a n Time t o Failure"

(MTTF) are r o u t i n e l y p r o v i d e d b y Q u a l i t y

Control f o r remotely s i t u a t e d r e c o r d i n g

i n a t ruments. Total Rpplicable Points Total Survey Points P e r c e n t age

FlGUAE25-1

I70

25.0

20

Of

20

Efleclive Dale

Seelion No.

Suqecl

BY

RELIABILITY

26. 0

P.92

10'4

Revised

Approved

2 6 . 1 Purpose T h i s s e c t i o n d e s c r i b e s t h e r e s p o n s i b i l i t i e s o f t h e Q u a l i t y Control

Coordinator w i t h regard t o ensuring t h e r e l i a b i l i t y of remote recordinginstrumentsusedbythe l a b o r a t o r y .

2 6 . 2 Scope The a c t i o n s requiredinthissectionapplyonlytomeasurement

equipmentlocatedoff-site, i n remote a r e a s w h e r e t h e r e i s no dayto-day oversighton equipmentoperation. T h i s s e c t i o n is n o t

applicable t o gages, instruments, and equipment used w i t h i n t h e

laboratory. 2 6 . 3 Actions andResponsibilities-Quality Control Coordinator I n o r d e r t o ensure high r e l i a b i l i t y ( c o m p 1 e t e n e s s o f d a t a ) t h e Q u a l i t y Control Coordinator is r e s p o n s i b l e f o r t h e f o l l o w i n g actions: a. He must see t h a t equipment r e l i a b i l i t y is s p e c i f i e d i n purchase contracts. b . Incomingequipmentmustbeinspectedandtested f o r adherence t o

contract specificationsbyburn-in ordemonstratedperformance

acceptance t e s t i n g . c . The o p e r a t i n g environment which i n f l u e n c es t h e r e l i a b i l i t y o f measurements must be c o n t r o l l e d i n s o f a r a s p o s s i b l e . d . P r o v i s o n m u s t b e made for adequate t r a i n i n g o f personnel.

171

Eflecllve Dale

BY

Seclion No.

Subject

RELIABILITY

Approved

Pipe Revised

26 0

2 0'4

e . Ensure t h a t p e r i o d i c p r e v e n t i v e maintenance is carried o u t t o minimize wear-out f a i l u r e s . ( S e c t i o n 1 4 . 0 ) f . Keep r e c o r d s of f a i l u r e s , and a n a l y z e and u s e these data t o

provide t h e b a s i s f o r t h e i n i t i a t i o n o f c o r r e c t i v e a c t i o n s and p r e d i c t r e l i a b i l i t y rates. 26.4 The t e c h n i c i a n o p e r a t i n g t h e e q u i p m e n t h a s t h e f o l l o w i n g

responsibilitiestoensurehighreliability ( c o m p l e t e n e s s o f d a t a ) :

a . When t h e measurement system is o p e r a t i o n a l , r o u t i n e p r e v e n t i v e maintenance w i l l be performed. b . Whenthe system f a i l s t o o p e r a t e as r e q u i r e d , t h e

time of f a i l u r e

w i l l be n o t e d o n t h e e q u i p m e n t s t r i p chart or i n t h e l a b o r a t o r y

notebook, whichever is a p p l i c a b l e . I n a d d i t i o n , t h e t o p p o r t i o n ( b l o c k s l - 1 3 ) o f t h e t d a i n t e n a n c e ServiceReport(Figure26-1) w i l l be f i l l e d o u t a s f o l l o w s : (1)E n t e r t h e name o f t h e

equipment. ( 2 ) E n t e r . t h e i d e n t i f i c a t i o n n u m b e r o f t h e test b e i n g runon the failedequipment. ( 3 ) E n t e r t h e d a t e a n d t i m e t h e t e s t wasbegun. ( 4 ) G i v e t h e n a m e o f t h e equipmentmanufacturer. ( 5 ) E n t e r t h e time t h e f a i l u r e w a s n o t e d . ( 6 ) E n t e r t h e d a t e t h e

f a i l u r e w a s d i s c o v e r e d . ( 7 ) Give t h e model number o f t h e f a i l e d p i e c e o f e q u i p m e n t . (8)Givetheoperator'sname. ( 9 ) I d e n t i f y t h e l o c a t i o n o f t h e equipment. ( 1 0 ) E n t e r t h e i n t e r v a l s i n c e t h e

I72

Efleclive Dale

BY Approved

I I

Seclion No.

Subject

RELIABILITY

26.0

Revised

l a s t r e c o r d e d m a i n t e n a n c e or repair s e r v i c e . (11)Give a g e n e r a l d e s c r i p t i o n o f t h e n a t u r e o f t h e equipment f a i l u r e , and i t s

c a u s e , i f k n o w n , ( 1 2 ) Describe t h e environmental c o n d i t i o n s o b t a i n i n g a t t h e time of f a i l u r e as c l o s e l y a s p o s s i b l e . (13)

Enter t h e time, Md, s p e n t o n d i a g n o s i n g t h e f a i l u r e , and i t s c a u s e . c . After t h e measurement s y s t e m h a s b e e n r e p a i r e d , complete t h e Maintenance S e r v i c e Report as f o l l o w s : ( 1 4 ) D e s c r i b e , i n d e t a i l t h e a c t i o n t a k e n t o r e p a i r t h e equipment. ( 1 5 ) L i s t t h e f a i l e d components replaced. ( 1 6 ) L i s t t h e f a i l e d components r e p a i r e d . ( 1 7 ) N o t e w h e t h e r t a m p e r p r o o f s e a l s w e r e r e q u i r e d . (18) Describe w h a t p r e v e n t i v e maintenance workwas completed. (19) Note w h a t

o p e r a t i o n a l t e s t s w e r e conductedand completed. ( 2 0 ) Record time, Mr for t o t a l repair, preventive maintenance, and o p e r a t i o n a l t e s t i n g . ( 2 1 ) Theindividualcompletingthe Report w i l l s i g n a t t h e bottom where i n d i c a t e d . d. TheoperatorwilldelivertotheQualityControlCoordinatorthe

o r i g i n a l o f t h e M a i n t e n a n c e S e r v i c e R e p o r t for c a l c u l a t i o n o f

Uptime U , Downtime D, and A v a i l a b i l i t y . A = U/(D 4- U)

173

MAINTENANCE / SERVICE REPORT (1)

ITEMNAME

FAILURE CONDITIONS LOCATION

INTERVAL SINCE LAST SEW1

(9)

FfO)

GENERAL DESCRIPTION OF FAiLURE AND CAUSE

(11)

ENVIRONMENTAL CONDITIONS

DIAGNOSTIC TIME SPENT

(12)

(13)

CORRECTIVE ACTION TAKEN

(14)

855

FAILEO COM

N NTS REPLACED

FAILED COMPONENTS REPAIREO

(16)

c

SERVICE REOUIREMENTS TAMPER-PROOF SEALING REOUIRED 0

(1 7)

PREVENTIVE MAINTAINANCE COMPLETED

(18)

OPERATIONAL TEST COMPLETED

NOT REOUIRED 0

(19)

SIGNATURE FIGURE 26-1

174

t

METHODVALJDATION

p.ge

1

O'

2 7 . 1 Purpose T h i s s e c t i o n w i l l s e t f o r t h t h i s l a b o r a t o r y ' s requirements f o r e s t a b l i s h i n g a n d v e r i f y i n g m e t h o d performance s p e c i f i c a t i o n s

(validationoftestmethods) a n d p r e s c r i b e t h e methodof such validation t o b e usedbythislaboratory. 27.2

Scope A l l new p a t i e n t t e s t i n g p r o c e d u r e s i n t r o d u c e d b y t h e l a b o r a t o r y

mustbevalidatedbeforethe reportedresultsmaybeused, i n c l u d i n g : 2 7 . 2 . 1 Newdevices ( i n s t r u m e n t , k i t , or t e s t system) c l e a r e d b y t h e FDAasmeetingcertainCLIA requirements f o r q u a l i t y control 2 7 . 2 . 2 Newmethodsordevicesasspecifiedineither P a r . 4 9 3 . 1 2 0 2 ( a ) o r ( b ) , or P a r . 4 9 3 . 1 2 0 3 ( a ) .

2 7 . 3 MethodValidation Requirements 2 7 . 3 . 1 Foreachnewtestprocedureusingadevice c l e a r e d b y FDAas meeting CLIA requirements f o r q u a l i t y c o n t r o l , t h e

laboratorywilldeterminethatitstest r e s u l t s f o r t h e methodunder c o n s i d e r a t i o n w i l l meet performance s p e c i f i c a t i o n s b y f i n d i n g t e s t v a l u e s comparable t o t h o s e e s t a b l i s h e d b y t h e manufacturerbyusing:

a . The t t e s t f o r s i g n i f i c a n c e of d i f f e r e n c e between t h e two samplemeanstodeterminethedegree of accuracy o f t h e test. b . The F t e s t f o r s i g n i f i c a n c e o f d i f f e r e n c e between t h e two

samplevariancestodeterminedegreeofprecisionofthe test.

c . Determinationofwhether any o u t l y i n g v a l u e s exceed those of t h e manufacturer's r e f e r e n c e range.

175

4

Eftecllve Dale

BY

-Approved

Subjecl

METHOD VALIDATION

Section No.

27.0

Page

2

Of

Revised

2 7 . 3 . 2 Adeterminationwillbemadeto findwhether the

m a n u f a c t u r e r ' s r e f e r e n c e range i s a p p r o p r i a t e f o r v a l u e s alreadyestablishedbythelaboratory'spatientpopulation.

2 7 . 3 . 3 Newmethodsdevelopedinhouse, modified f r o m e x i s t i n g

procedure, o r n o t c l e a r e d b y FDA: Verify or e s t a b l i s h f o r eachnewmethodtheperformance s p e c i f i c a t i o n s f o r t h e

following performance c h a r a c t e r i s t i c s , u s i n g :

a . The t t e s t f o r s i g n i f i c a n c e of d i f f e r e n c e between t h e two samplemeanstodeterminedegree o f a c c u r a c y . b . The F t e s t f o r s i g n i f i c a n c e of d i f f e r e n c e between t h e two

sample v a r i a n c e s t o determine degree of p r e c i s i o n .

c

4

r I

Elfectlve Date

METHODVALIDATION

BY

I

Approved

Section No.

Subject

1

27.

Page Revised

I

3

O'

I

2 7 . 4 Method V a l i d a t i o n Reporting The r e s u l t s o f t h e l a b o r a t o r y ' s v e r i f i c a t i o n or e s t a b l i s h m e n t of performance c h a r a c t e r i s t i c s (Method V a l i d a t i o n ) w i l l be r e p o r t e d ontheMethodValidationApprova1 Report ( F i g u r e 2 7 - 1 ) w h i c h w i l l be

c o m p l e t e d a s follows: ( 1 ) E n t e r t h e d a t e onwhichtheMethod V a l i d a t i o n forthemethodinquestionwascompleted. ( 2 ) D e s c r i b e t h e p a t i e n t t e s t method f o r w h i c h t h e r e p o r t i s b e i n g r e n d e r e d . (3)

I d e n t i f y t h e t e s t specimen (sample) inasmuchdetailasnecessary tomake s u r e t h a t t h e r e i s n o m i s u n d e r s t a n d i n g a s t o t h e n a t u r e of t h e specimen. ( 4 ) G i v e a b r i e f d e s c r i p t i o n o f t h e t e s t method v a l i d a t e d . ( 5 ) Describe t h e m e t h o d v a l i d a t i o n s y s t e m u s e d i n

v e r i f y i n g t h e p e r f o r m a n c e c h a r a c t e r i s t i c s o f t h e method, i . e . , ( a )

comparisonoftestresultswiththose o b t a i n e d froman a l t e r n a t e

method or ( b ) comparison of s p l i t sample r e s u l t s w i t h r e s u l t s obtained frompreviously run, h i s t o r i c a l l y v a l i d t e s t s . ( 6 )

I n d i c a t e by checkmarks t h e r e s u l t s o f v a l i d a t i o n f i n d i n g s . ( 7 ) Provide t h e name o f t h e i n d i v i d u a l d o i n g t h e v a l i d a t i o n t e s t work or calculations. ( 8 )Ifadditional datahavebeen generatedbythe m e t h o d v a l i d a t i o n t e s t s , provide t h o s e r e s u l t s as appendices on a d d i t i o n a l p a g e s . ( 9 ) T h i s s p a c e is provided f o r t h e s i g n a t u r e of the approvingauthority. ( 1 0 ) E n t e r t h e t i t l e o f t h e individual approving t h e m e t h o d v a l i d a t i o n r e s u l t s . ( 1 1 ) E n t e r t h e d a t e of approval.

177

4

Effectlve Date

Section No.

Subject

METHODVALIDATION

BY

Page

27.0 4

Of

4

Revised

Approved

METHOD VALIDATION APPROVAL REPORT DATE: PATIENTTEST METHOD DESCRIPTION:

SPECIMEN DESCRIPTION:

(*)

(3’1

ABSTRACT OF TEST METHOD:

(k)

METHOD VALIDATION TYPYS USED FOR THIS DETERMINATION: ( 5 )

RESULTSOF PERFORMANCE SPECIFICATION VERIFICATION OR ESTABLISHMENTSTUDY ( 6 )

a.

Acarracy

b.

Preasion

c.

Analyticalsensitivity

d.

Analyticalspecifity (Interferences)

8.

Reportable range of patient test results

1.

Reference range@)

g.

Other performance characteristicsas required.

METHOD VALIDATION PERFORMED BY:

17)

-

FOR DATA SEE APPENDIX FOLLOWING. (8) APPROVED B Y DATE:

(9)

TITLE

(11)

Figure 27-1

178

(10)

OK

FAIL

Effective Dale

SUbjtCl

BY

I 28.1

28.2

&)prod

t

QUALITY MANUAL, FORMAT SHEET

-ScctiOnNo. p.ge

,

28.0

1Of 2

Reviaed

I

Purpose Thissectionprovidesinstruction i n h o w t o u s e t h e M a n u a l s t a n d a r d

formatsheet(Figure33-1).

'

Scope These i n s t r u c t i o n s a p p l y t o a l l t h o s e i n d i v i d u a l s r e s p o n s i b l e f o r

28.3

t h e p r e p a r a t i o n o f t h e Q u a l i t y Manual or i t s r e v i s i o n s . Use of t h e Manual Standard Format S h e e t

The Laboratory Q u a l i t y Manual S t a n d a r d F o r m a t S h e e t w i l l be t y p e w r i t t e n or prepared on a word p r o c e s s o r and w i l l be f i l l e d o u t as follows: ( 1 ) T h i s s p a c e m a y b e u s e d t o show t h e l a b o r a t o r y logotype. ( 2 ) Enter t h e d a t e t h a t t h i s pagebecomes e f f e c t i v e and t h e olddocument b e c o m e s o b s o l e t e . ( 3 ) E n t e r t h e name o f t h e a u t h o r

orpersonpreparingthisdocument. ( 4 ) E n t e r t h e name or i n i t i a l s of t h e i n d i v i d u a l approving t h i s document. ( 5 ) E n t e r t h e t i t l e o f t h e

qualityelementbeingaddressed. ( 6 ) I n d i c a t e t h e S e c t i o n N u m b e r o f t h e element, taken f r o m t h e T a b l e 0 f C o n t e n t . s . ( 7 ) E n t e r t h e page number o f t h e d o c u m e n t . P a g e s i n e a c h s e c t i o n w i l l be numbered

consecutivelyandwillbeginwith l a t t h e s t a r t of e a c h n e w s e c t i o n . ( 8 )Inthe

case o f r e v i s e d d o c u m e n t s , e n t e r t h e r e v i s i o n d a t e . ( 9 )

Type t h e t e x t material i n t h e space p r o v i d e d .

I79

BY

Approved

QUALITY MANUAL FORMAT SHEET

I80

Page Revised

2

Of

2

Laboratory Quality Assurance System, 3rd Edition. Thomas A. Ratliff Copyright 02003 John Wiley & Sons, Tnc. 4SBN: 0-471-26918-2

Part 4

SAMPLE QUALITY ASSURANCE FORMS On the following pages are examples of forms used in the laboratory quality system. They are presented full-sized so that they can be reproduced. Of course, they may be changed in any way that makes them applicable to the individual laboratory’s procedures and work methods. The forms are the same as those shown in the body of the sample Laboratory Quality Assurance Manual in Part 3, with the instructional reference numbers removed. The figure numbers are identical.

181

182

CONTENTS FORM NAME

FIGURE NO. Figure 8-1.

Receiving Report

Figure 8-2.

Classification of Defects Inspection Instructions

Figure 8-3.

Testing and Analytical Supplies Receiving and Stores Log

Figure 8-4.

Quality System Survey Evaluation Check List

Figure 9-1.

Sample Submittal Form

Figure 10-1.

Chain-of-Custody Documentation Accountability Record

Figure 12-1.

Technical Document Change Notice

Figure 13-1.

Calibration Frequency Schedule

Figure 13-2.

Instrument/Gage Calibration Record

Figure 13-3.

“CALIBRATED” label

Figure 13-4.

“OUT OF SERVICE” label

Figure 13-5.

“NOT CALIBRATED” label

Figure 15-1.

NBS Standard Reference Material No, 2676

Figure 18-1.

Customer Contact Log Sheet

Figure 21-1.

Control Chart (completed)

Figure 2 1-2.

Control Chart (blank)

Figure 22- 1.

Nonconformance Event Review Report

Figure 23- 1.

Corrective Action Request

Figure 23-2.

Corrective Action Request Master Log

Figure 25-1.

Quality Control System Audit Check List

Figure 26-1.

Maintenance Service Report

Figure 27- 1.

Method Validation Approval Report

Figure 28- 1.

Quality Manual Format Sheet

183

184

XYZ LABORATORIES, INC. RECEIVING REPORT Date Received From

20

-

Shipped From.

SHIPPING CHARGE

QUANTITY

PREPAID

COLLECT

CAR INITIALS AND NO

FREIGHT BILL NO

1 DESCRIPTION OF MATERIALS

I CONDITION

I

I

I

I

I

Remarks:

RECEIVING CLERK FIGURE 8-1

185

I

XYZ LABORATORIES, INC. QUALITY ASSURANCE CLASSIFICATION OF DEFECTS INSPECTION INSTRUCTIONS DESCRIPTION PART NUMBER

LOT SIZE

SAMPLING PROCEDURE: ANSI / ASQC / Z 1.4 Level 11, unless otherwise noted. CRITICAL 100% (no defects allowed) 1.

INSPECTION PROCEDURE

I

I

3. 28

4. 5.

6.

METHOD

I I MAJOR “A” AQL 1.0 %

101. 102. 103. 104. 105. 106.

MAJOR “B” AQL 2.5 Yo

MINOR AQL 4 Yo

Ei______=1

304. 305.

FIGURE 8-2

186

TESTING AND ANALYTICAL SUPPLIES

RECEIVING AND STORES LOG

FIGURE 8-3

187

XYZ LABORATORIES, INC. QUALITY SYSTEM SURVEY EVALUATION CHECK LIST COMPANY ADDRESS

PHONE

GENERAL PRODUCTS

TOTAL NUMBER OF EMPLOYEES

.QC

PERSONNEL CONTACTED AND PRODUCTS CONSIDERED SURVEY BY AND DATE SURVEY RESULTS

NAME-TITLE-DATE FIGURE 8-4

188

OF-

-

-%

INDEX Page 1 Page 2 Page 3 Page 3 &4 Page 4 Page 4

Category 1 Category 2 Category 3 Category 4 Category 5 Category 6

Page 5

Category 7

Page 5 Page 5

Category 8 Category 9

Page 6 Page 6

Category 10 Category 11

Page 7

Category 12

Page 7

Category 13

Quality Control Organization Control of Procured Supplies In-Process Inspection Final Inspection Shipping Inspection Calibration of Mechanical Measuring Equipment Calibration of all other Test Equipment Drawing and Change Control Environmental Testing Facilities (When Applicable) Non-Conforming Material Housekeeping, Storage & Handling Customer Satisfaction and Complaints Continual Improvement Total

189

SURVEY RESULTS of Yo

INSTRUCTIONS An applicant’s compliance to each question shall be indicated by placing 0, 1, 2, 3, or NA on the line opposite each question.

0.

Required but not being done.

1.

Below acceptance standards.

2.

Adequate with minor departures from good practices.

3.

Adequate in all respects.

NA.

(Not Applicable) when it is obvious that a question would be inappropriate, due to type of product, lack of facilities, special processes or other valid reasons.

At the conclusion of the survey, each category of questions should be analyzed and summarized for acceptability. Space is provided in the index for entering these results. Remarks or comments by the survey team will be placed on the blank page opposite the question. The following method shall be used in summarizing each category: Total the survey points for all applicable questions. Divide this total by the total applicable questions. Multiplied by the weighting factor of 3, this computation will result in a percent acceptability figure. Total points for applicable questions rated = PercentAcceptability Number of applicable questionsx 3

Example: For category 1, we have a total of 10 applicable questions and a weighting factor of 3 per 28 question (10 x 3) Therefore -= 93% (Percent acceptability for category) 10x3

CATEGORY 1 QUALITY CONTROL ORGANIZATION

1.

Company management reflects a positive attitude toward Quality Control.

2.

Direct responsibility for Quality Control has been formally established.

190

3.

The functional relationship between Quality Control and other departments has been clearly delineated.

4.

Line of authority within the Quality Control organization has been clearly delineated.

5.

The Quality Control System has been designed to promote defect prevention.

6.

The Quality Control System is adequately documented.

7.

The Quality Control Department issues periodic reports to management which reflect quality levels, rework, scrap, work realization, quality costs, etc.

8.

The documented Quality Control System carries management approval.

9.

The Quality Control Department adequately provides for the use and control of inspection stamps.

10.

The applicant provides for employee indoctrination and training in Quality Control methods.

11.

Quality Control System assures that Engineering drawings and specification requirements, procured materials and manufactured items satisfy all customer contractual requirements. Total Applicable Points Total Survey Points Percentage of Acceptability

191

-

CATEGORY 2

CONTROL OF PROCURED SUPPLIES 1.

OPERATION AND DOCUMENTATION

a.

Inspection is preformed by Quality Control.

b.

Inspection instruction/procedures are available to inspection personnel.

C.

d. 2.

Inspection personnel perform inspection operations in accordance with current instructions and procedures. Applicant has provided a instructiodprocedures current.

system

to

maintain

VENDOR PROGRAM

a.

Applicant’s Quality Control reviews environmental and life requirements and assures that Qualified Products are being procured.

b.

Applicant has an established program for processing drawing changes to his vendors and subcontractors.

C.

Receiving Inspection records reflect quality history of applicant’s vendors and subcontractors.

d.

Vendor quality performance data reports are used by other departments in making procurement decisions.

e.

Applicant has program for Quality Control approval of vendors and subcontractors.

f.

Applicant performs source surveillance at subcontractor’s plant when applicable.

g*

Applicant requires his vendors and subcontractors to have a system for quality control.

h.

Applicant uses inspectiodtest results to contribute to vendors evaluation.

192

INSPECTION CRITERIA

3.

Purchase Orders, Drawings, Engineering Orders, specifications, and vendor’s catalogs are available to Receiving Inspection. INSTRUMENTATION

4. a.

Inspection gages and test equipment are adequate to perform required inspection.

b.

Tools, fixtures, and inspection equipment are identified, stored and issued under controlled conditions. SAMPLING INSPECTION (When Applicable)

5. a.

Sampling Inspection is performed to ASNI-ASQC Z1.4 ANSIASQC Z1.9, or other approved plan.

b.

Inspection personnel are provided with instructions covering Sampling Inspection. CONTRACTED SPECIAL PROCESSES

6. a.

Applicant has established certified and/or approved source for special process services.

b.

Applicant’s Quality Control performs surveillance over special processing.

193

7.

STOCK CONTROL a.

Applicant uses a positive means of identification on all stock.

b.

Applicant requires and receives chemical/physical analysis or test specifications when applicable

c.

Applicant provides adequate control area for customer furnished material when required.

d.

Applicant has an acceptable system for “age control” for items where acceptability is limited by maximum age. Total Applicable Points Total Survey Points Percentage of Acceptability

CATEGORY 3 IN-PROCESS INSPECTION 1.

OPERATION AND DOCUMENTATION a.

In-process inspection is performed by Quality Control.

b.

Inspection instructions/procedures are Inspection personnel.

c.

Inspection personnel perform inspection operations in accordance with current instruction and procedures.

d.

Applicant has provided a system for First Article Inspection and re-inspection after changes in manufacturing process.

e.

Applicant procedures provide for inspection control of inprocess material.

2.

available to

INSPECTION CRITERIA a.

Illegible or obsolete drawings are not in use by inspection.

b.

Current Drawings, Engineering Orders, and specifications are available at Inspection area.

3.

INSTRUMENTATION a.

b.

Adequate in-process inspection facilities are available. Inspection gages and test equipment are adequate to perform required inspection.

194

-

c.

4.

Adequate surveillance and maintenance of inspection equipment when in use, transported or stored is maintained. STATISTICAL Applicable)

QUALITY

CONTROL

(When

a.

Sampling inspection is preformed to ANSI-ASQC 21.4 OR ANSI-ASQC Z1.9, or other approved plan.

b.

Inspection personnel are provided with instructions covering sampling inspection.

c.

Control charts or other in-process statistical quality control methods are used. Total Applicable Points Total Survey Points Percentage of Acceptance

CATEGORY 4 FINAL INSPECTION

1.

2.

OPERATION AND DOCUMENTATION a

Final inspection is performed by Quality Control.

b.

Current Inspection instructiodprocedures available to Inspection personnel.

c.

Inspection personnel perform inspection operations in accordance with current instructions and procedures.

d.

Completed supplies are inspected as necessary to assure that contract requirements have been met.

e.

Environmental and life tests are periodically performed to assure that manufacturing and process degradation has not significantly effected design integrity.

are

INSPECTION CRITERIA Current Drawings, Engineering Orders, specifications and/or customer requirements are available at final inspection.

195

-

INSTRUMENTATION

3.

a.

Inspection gages and test equipment are adequate to perform required inspection.

b.

Tools, fixtures, and inspection equipment are identified, stored, and issued under controlled conditions.

c.

Adequate final inspection facilities are available. STATISTICAL OUALITY CONTROL (When Applicable)

4.

a.

Sampling Inspection is performed to ANSL'ASQC 21.41993, ANSVASQC 21.9-1993, or other approved plan.

b.

Inspection personnel are provided with instructions covering sampling inspection.

c.

Control charts or other statistical quality control methods are used. MATERIAL HANDLING

5.

Provisions are made to prevent unauthorized use of uninspected and/or conforming material. Total Applicable Points Total Survey Points Percentage of Acceptability

-

CATEGORY 5 SHIPPING INSPECTION

1.

OPERATION AND DOCUMENTATION

a.

Shipping Inspection is under the surveillance of Quality Control.

b.

Inspection operations are performed in accordance with current instructions and procedures.

196

2.

INSPECTION CRITERIA a.

Inspectors have packaging requirements.

b.

Packaging tests are performedwitnessed as required by applicable specifications.

c.

Certified packaging materials are used where required. Total Applicable Points Total Survey Points Percentage of Acceptability

CATEGORY 6 CALIBRATION OF MECHANICAL MEASURING EQUIPMENT 1.

Quality Control procedures insure that inspection gages, measuring devices, and test equipment are periodically inspected and recalibrated at established intervals.

2.

Production tooling which is in use as a medium of inspection is periodically inspected by Quality Control at intervals that assure the maintenance of required accuracy.

3.

Applicant has system for modification of inspectiodtest equipment to latest engineering changes.

4.

Applicant does maintain, in a suitable environment, working standards of required accuracy that are periodically calibrated to primary standards traceable to the National Bureau of Standards.

5.

Personally owned tools and gages show evidence of periodic recalibration.

6.

Specialized test equipment used for acceptance purposes is proved satisfactory by Quality Control before release for use.

7.

New or reworked testhspection equipment is inspected and calibrated prior to use.

8.

Applicant has written instmctiodprocedures for “gage and test calibration.’’

9.

Objective evidence includes calibration date and date next calibration must be performed on measuring instrumentation.

10.

Records are maintained for periodic recalibration of inspection gages and test equipment.

197

-

11.

Record system provides for automatic recall of inspection gages and test equipment. Total Applicable Points Total Survey Points Percentage of Acceptability

CATEGORY 7 CALIBRATION OF ALL OTHER TEST EQUIPMENT 1.

Quality Control procedures insure that inspection equipment is periodically inspected and recalibrated at established intervals.

2.

Production tooling which is in use as a medium of inspection is periodically inspected by Quality Control at intervals that assure the maintenance of required accuracy.

3.

Applicant has system for modification of inspection/test equipment to latest engineering changes.

4.

Applicant does maintain, in a suitable environment, working standards of required accuracy that are periodically calibrated to primary standards traceable to the National Bureau of Standards.

5.

Personally owned tools show evidence of periodic recalibration.

6.

Specialized test equipment used for acceptance purposes is “proved” by Quality Control before release for use.

7.

New or reworked test/inspection equipment is inspected and calibrated prior to use.

8.

Applicant has written instructiodprocedures for all Measuring Equipment Calibration.

9.

Objective evidence includes calibration date and date next calibration must be performed on measuring instrument.

10.

Records are maintained for periodic recalibration of all inspection measuring equipment.

11.

Record system provides for automatic recall of all inspection measuring equipment. Total Applicable Points Total Survey Points Percentage of Acceptability

198

-

CATEGORY 8 DRAWING AND CHANGE CONTROL 1.

The direct and specific responsibility to verify that changes are incorporated at effective points is clearly defined and formally established.

2.

Applicant has written procedures describing drawing change control.

3.

A control system exists for the issue and return of each drawing .

4.

Drawing and change control system prevents the use of illegible or obsolete drawings by Inspection. Total Applicable Points Total Survey Points Percentage of Acceptability

CATEGORY 9 ENVIRONMENTAL TEST FACILITIES (When Applicable) 1.

Applicant has suitable environmental test equipment to perform full range of required tests on product under consideration, or uses recognized test laboratories.

2.

Applicant maintains records that show results of tests performed and failure rates.

3.

Applicant has established program of calibration and maintenance of instrumentation used in environmental laboratory. Total Applicable Points Total Survey Points Percentage of Acceptability

199

-

CATEGORY 10 NON-CONFORMING MATERIAL (Materials Review) 1.

Applicant’s procedures reflects control of authority to repair non-conforming supplies.

2.

Applicant has a system for the diversion of nonconforming supplies from normal production flow.

3.

Applicant has method of recurrence control to prevent repetitive discrepancies.

4.

Corrective action requests on non-conforming materials are initiated promptly.

5.

Records provide for follow-up on all corrective action requests.

6.

Disposition of non-conforming material does not establish criteria for like dispositions.

7.

Reports on non-conforming materials are issued to management for action. Total Applicable Points Total Survey Points Percentage of Acceptability

CATEGORY 11 HOUSEKEEPING, STORAGE & HANDLING 1.

Materials, supplies, and work in process are arranged in a neat workmanlike manner.

2.

Work and storage areas are clean and free from dirt, rejected materials, and other materials which could contaminate or damage acceptable materials.

3.

In the case of extended or indefinite storage, equipment is given proper preservative treatment.

200

4.

Facilities for storage of materials or equipment assures prevention of deterioration and contamination.

5.

During storage, material is packaged in a manner to prevent deterioration and damage.

6.

Delicate instruments are handled in a manner that will not jeopardize the reliability of the design characteristics.

7.

Transfer procedures are adequate comingling, contamination, and loss.

8.

Tags and labels are properly used to indicate the identity, condition, and status of the equipment.

9.

Components, assemblies, and materials are handled so as to prevent damage and deterioration.

10.

Provisions are made to prevent unauthorized use of uninspected materials.

to

prevent

Total Applicable Points Total Survey Points Percentage of Acceptability

CATEGORY 12 CUSTOMER SATISFACTION AND COMPLAINTS 1.

Personal contacts with customers, verbal or in writing are recorded and logged.

2.

All formal, written customer communications are filed.

3.

Customer complaint information is throughout the laboratory to all concerned.

4.

Complaints are investigated in a timely manner; Corrective Action Requests are initiated as necessary.

5.

Periodic reports are made to top management regarding frequency and status of of customer complaints.

20 1

circulated

6.

The laboratory periodically engages the services of outside public relations experts to determine its status with regards to public opinions of the quality of the laboratory’s service. Total Applicable Points Total Survey Points Percentage of Acceptability

-

-

CATEGORY 13 CONTINUAL IMPROVEMENT

1.

A Quality Improvement Board has been appointed.

2.

A written protocol for development of improvement projects has been established.

3.

Specialized training for continual improvement is incorporated in the quality improvement program.

4.

Top management visibly Improvement Program.

5.

Quality measurement activities results reflect improvement progress.

6.

Job Descriptions reflect the assignment of responsibility for Continuous Improvement.

7.

Successful Continuous Improvement achievement is publicized.

8.

The effectiveness of the Continuous Improvement effort is monitored by top management.

supports

the

-

Continual

Total Applicable Points Total Survey Points Percentage of Acceptability

202

-

SAMPLE SUBMITTAL FORM Sample Log No.

Date

Originator: Address

Telephone No.

Project No.

Sample Description. Sampling Source. Number of Samples Submitted. Date of Collection Date of Sample Shipment Request for Analysis Sample Field Number

I

Sample Characteristics Manuf.

Lot No.

I

Test or Analyses Requested

Comments Possible Interfering Compounds

FIGURE 9-1 203

Remarks

CHAIN OF CUSTODY DOCUMENTATION SAMPLE #: NAME OF SUBMITTER

TELEPHONE

NUMBER:

ADDRESS: DESCRIPTION OF SAMPLE: SAMPLE SOURCE: DATE AND TIME OF COLLECTION: METHOD OF SHIPMENT:

DATE RECEIVED IN LAB:

RECEIVED BY WHOM:

RECEIPT CONDITION (CONTAINERS, PACKAGING, AND LABELING): INITIAL WEIGHT OF CONTAINER (BULKS): WHERE INITIALLY STORED:

ACCOUNTABILITY RECORD REMOVAL DATE & TIME

BY WHOM

LOCATION

RETURNED DATE AMOUNT TIME (% OF INITIAL)

SAMPLE DISPOSITION: DATE DISPOSED: BY WHOM: HOW DISPOSED: FIGURE 10-1

TO WHOM

LOCATION

XYZ LABORATORIES, INC.

TECHNICAL DOCUMENT CHANGE NOTICE DATE TDCN No. EFFECTIVE DOCUMENT TYPE METHOD SAMPLING DATA SHEET CALIBRATION INSTRUCTION OTHER (DESCRIBE) DOCUMENT TITLE REQUESTED BY:

CHANGE FROM:

CHANGE TO:

REASON FOR CHANGE:

DISTRIBUTIONS

SIGNATURES

COSTS NEW EQUIP. NEW MAT’L SCRAPPED OR OBS. EQUIP. SCRAPPED OR OBS. MAT’L PERSONNEL OTHER

DETAIL ON REVERSE SIDE FIGURE 12-1

205

APPROVALS:

CALIBRATION FREQUENCY SCHEDULE Minimum Frequency

I

Instruction Number or Calibration Method I

FIGURE 13-1

206

INSTRUMENT / GAUGE CALIBRATION RECORD

DATE CALIBRATED

CHECKED BY

DEPT.

RESULTS

I

I

I

I

I

I

I

I

I

FIGURE 13-2

207

BY DATE NEXT CAL. DUE

FIGURE 13-3

OUT OF SERVICE MUST BE REPAIRED AND/OR CALIBRATED BEFORE USE NAME

DATE

FIGURE 13-4

N O T TO BE USED FOR OFFICIAL MEASUREMENT PURPOSES

FIGURE 13-5

208

National Bureau of Standards Certificate of Analysis Standard Reference Material 2676 Metals on Filter Media

(Pb, Zn, Cd, Mn) This Standard Reference Material is intended primarily for use as an analytical standard for the determination of cadmium, lead, manganese, and zinc in the industrial atmosphere. The SRM consists of a set of membrane filters on which have been deposited the indicated quantities of salts of the particular metals. Filter A 1 A 2 A 3

Cd 0.50 f .04 2.48 f .14 10.1 f . 4

Metal Content, pg/ fi1ter Pb Mn Zn 1.93 f .29 1.02 f .06 6.8 f 1.1 10.3 f 1.5 5.10 f .26 29. f 2.6 102. f 6 20.6 f 1.0 10.1 L 1.1

The filters were prepared by depositing on them known and carefully reproduced volumes of solutions of pure salts, using the technique described in NBS report NBSIR 73-256.

The certified values are based upon determination of the metal content by atomic absorption spectrometry and by polarographic measurement. In these analyses, entire filters were mineralized by digestion in acid prior to measurement. The certified values are the means of those found by the two techniques while the uncertainties represent the 95 percent tolerance limits based on measurement error and variability between samples.*

The filters are identified by the numbers Al, A2, A3 printed on their edge. The metal content of the inked identification is negligible so it need not be removed. An entire filter must be used for each measurement since the metals are not uniformly distributed. *See page 14, The Role of Standard Reference Materials in Measurement System, NBS Monograph 148, 1975. The concept of tolerance limit is also discussed in Chapter 2, Experimental Statistics, NBS Handbook 91, 1966.

209

In brief, if measurements were made on all the units, almost all (at least 95 percent) of these measured values would be expected to fall within the indicated tolerance limits with a confidence coefficient of 95 percent (or probability = . 9 5 ) .

The filters were prepared by R. Mavrodineanu and J. R. Baldwin. Atomic absorbtion analyses were made by them and also by T. C. Rains. E. J. Maienthal performed the polarographic analyses.

The overall direction and coordination of the technical measurements leading to certification were under the chairmanship of J. K. Taylor.

The technical and support aspects involved in certification and issuance of this Standard Reference Material was coordinated through the office of Standard Reference Materials by W. P. Reed. J. Paul Cali, Washington, D.C. 20234 Chief Office of Standard Reference Materials June 30, 1975

FIGURE 15-1

210

XYZ LABORATORIES, INC. CUSTOMER CONTACT LOG SHEET NAME

DEPTBECTION

Figure 18-1

21 1

1.4 1.2

a u

0)

OD C

;

UCLR UWLR

1.o .8 .6

-

.4

R

1 1

2

3

4

5

value p i rec t i ons: 1. Draw Si l i n e 0.34 2. DJar UCL, I ne 1.11

3. Draw U K , I ne 4. P l o t 5. Draw

as generated line 58.68

R'S

=X

0.86

6

7

8

9

10

Samp 1 e Numbe r 6. Draw UCL; l i n e 7. Draw Ulki l i n e

99.32

m.11

8. Draw LWLi l i n e 98.25 9. Draw L C L i l i n e 98.04 la. Plot i ' t as generated

FIGURE 2 1- 1

212

Laboratory Qua1 i t y Control Operation

X-R Chart

Date

D i rsctions: Va I us I . Draw l i n e 2. Draw UCL, l i n e 3. Draw UIL, l i n e

ii

4. P l o t 5. Draw

-

R's as generated

i

I ine

$amp I e Numbe r

6. Draw UCL: i n s 7. Draw UWL? ine 8. Draw LUL; l i n e 9. Draw LCLi l i n e 10. P l o t i ' s as generated

FIGURE 2 1-2

213

NONCONFORMANCE EVENT REVIEW REPORT SAMPLE IDENT. NO.

Date

SAMPLE DESCRIPTION

METHOD

SUSPECTED NONCONFORMANCE

EXPECTEDRESULT ACTIONS TAKEN

1. REPORTED TO: 2. REPORTED BY: 3 . EVENT LOGGED IN LABORATORY NOTEBOOK: YES( ) NO( ) 4.

CORRECTIVE ACTION REQUEST INITIATED: YES( ) NO( )

(ATTACH COPY)

5 . NEW SAMPLES REQUESTED: YES( ) NO( )

6. CUSTOMER NOTIFIED: YES( ) NO( )

7. RETEST OR REANALYSIS NECESSARY: YES( ) NO( ) IF YES, TO WHOM ASSIGNED 8. THIRD PARTY LABORATORY CONFIRMATION NECESSARY: YES( ) NO( ) IF YES, NAME OF LABORATORY

REVIEW DATE QUALITY CONTROL COORDINATOR FIGURE 22-1

214

CORRECTIVE ACTION REQUEST 7

Corrective Action Request Form No.

Suspense Date:

Originator

Date

Person responsible for replying

Organization

Nature of problem below: PI

RD

/OE BN LT

EI MF

1

C Cause of problem:

A T I

I 0

I

Signature

I During what phase of operation was the problem identified?

["

To: Name

T

U

Address By: (Date)

Information coplen 10: (Names and addresses)

R

N

FIGURE 23-1

215

CORRECTIVE ACTION REQUEST MASTER LOG Corrective Action Request Form No. Date Submitted

I I

I

Date Received Submitted By General Problem Description Suspected Cause Assigned To Answer Due Nature of Problem Investigation Cause of Problem Corrective Action Corrective Action Responsibility Originator Notified Demonstration of Effectiveness Final Close-Out FIGURE 23-2

I

I

I

QUALITY CONTROL QUALITY SYSTEM AUDIT CHECK LIST INSTRUCTIONS Laboratory compliance with each question will be indicated by placing 0. I . 2. 3. or NA on the line opposite each question.

0.

Required but not being done.

1.

Below acceptance standards.

2.

Adequate with minor departures from good practices.

3.

Adequate in all respects.

NA.

[Not Applicable] when it is obvious that a question would be inappropriate. due to type activity. lack of facilities. special methods or other valid reasons.

At the conclusion of the survey. each category of questions should be analyzed and summarized for acceptability. Space is provided in the index for entering these results. Remarks or comments by the survey team will be placed on the blank page opposite the question. The following method shall be used in summarizing each category: Total the survey points for all applicable questions. Divide this total by the total applicable questions. Multiplied by the weighting factor of 3. this computation will result in a percent acceptability figure. Total points for applicable questions rated = Percent Acceptability Number of applicable questions x 3 Example: For category 1. we have a total of I0 applicable questions and a weighting factor of 3 per 28 question [ 10 x 31 Therefore -93% [Percent acceptability for category] 10x3 SURVEY BY AND DATE SURVEY RESULTS

NAME-TITLE-DATE

FIGURE! 25-1

217

OF-

-

-%

QUALITY SYSTEM AUDIT CHECK LIST INDEX CATEGORY 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24

SUBJECT Quality Goals and Objectives Quality Policies The Quality Organization Management of the Quality Manual Quality Planning Quality in Procurement Sample Handling, Storage and Shipping Chain-of-custody Procedures Laboratory Testing and Analysis Control Quality Documentation and Records Control Control of Measuring and Test Equipment Preventive Maintainance Reference Standards Data Validation Environmental Control Customer Satisfaction and Complaints Subcontracting Personnel Training, Qualification & Motivation Statistical Methods Nonconformity Corrective Action Quality Cost Reporting Quality Audits Reliability

218

SURVEY RESULTS OF %

CATEGORY 1 QUALITY POLICIES

1.

Are the Quality Policies clearly stated?

2.

Are the Quality Policies consistent with any requirements of regulatory or accrediting bodies?

3.

Do the Quality Policies support the need for continuous improvement of the quality management system?

4.

Are the Quality Policies the basis for establishing Quality Objectives? Total Applicable Points Total Survey Points Percentage

CATEGORY 2 QUALITY GOALS AND OBJECTIVES

1.

Are the Quality Objectives clearly stated?

2.

Are the Quality Objectives quantified insofar as possible?

3.

Do the Quality Objectives support the Quality Policies?

4.

Have the Quality Objectives been approved by management?

5.

Do the Quality Objectives include the commitment to improve continuously customer satisfaction and the quality of performance? Total Applicable Points Total Survey Points Percentage

2 19

-

CATEGORY 3 THE QUALITY ORGANIZATION 1.

Laboratory management reflects a positive attitude toward Quality Control.

2.

Direct responsibility for Quality Control has been formally established.

3.

The functional relationship between Quality Control and other laboratory components has been clearly delineated.

4.

The line of authority within the Quality Control organization has been clearly delineated.

5.

The job description for the Quality Control Coordinator is up-to-date and accurately describes the current duties, responsibilites and authority of that individual.

6.

The Quality Control Coordinator is not subordinate to any individual who is responsible for carrying out testing or analytical responsibilities. Total Applicable Points Total Survey Points Percentage

-

CATEGORY 4 MANAGEMENT OF THE QUALITY MANUAL 1.

The responsibility for maintenance of the Quality Manual is clearly established.

2.

The issue of the manual is controlled.

3.

Provision is made for updating the Manual and issuing revisions to holders of controlled copies.

4.

Provision is made for the issue of uncontrolled copies as necessary. Total Applicable Points Total Survey Points Percentage

220

-

-

CATEGORY 5 QUALITY PLANNING 1.

The responsibility for the quality planning function is clearly defined.

2.

There is objective evidence that quality planning is an ongoing, continuous process.

3.

The Quality Manual accurately reflects current quality system activities in the laboratory. Total Applicable Points Total Survey Points Percentage

CATEGORY 6 QUALITY IN PROCUREMENT 1.

Inspection is performed by Quality Control.

2.

Inspection instructions are available to inspection personnel.

3.

Inspection personnel perform inspection operations in accordance with current instructions and procedures.

4.

There is a system to maintain inspection instructions current.

5.

There is a program for Quality Control approval of vendors and subcontractors.

6.

Vendors and subcontractors are required to have a a system for quality control.

7.

Inspection and test results are used to evaluate vendor quality performance.

8.

Purchase orders, specifications, and vendors’ catalogs are available to receiving inspection.

22 1

9.

Inspection gages and test equipment are adequate to perform required inspection.

10.

Sampling inspection (when applicable) is performed to ANSUASQC Z 1. 4-1981, ANSVASQC Z 1. 9-1987, or other approved sampling plan.

11.

Approved laboratories are used for special tests and analyses outside the scope of the laboratory’s capabilities.

12.

All reagent stock is properly labeled, dated and marked with shelf-life expiration when necessary.

13.

Chemical/physical analysis, test specifications, or certifications are required when applicable. Total Applicable Points Total Survey Points Percentage

-

CATEGORY 7 SAMPLE HANDLING, STORAGE AND SHIPMENT 1.

The Quality Control Coordinator monitors the physical condition of incoming test samples.

2.

Test and analytical samples are properly identified.

3.

Sample Submittal Forms are completely and accurately filled out. Total Applicable Points Total Survey Points Percentage

222

-

CATEGORY 8 CHAIN-OF-CUSTODY PROCEDURES 1.

Is the Chain-of-Custody Documentation Form correctly and completely filled out?

2.

Does the Chain-of-Custody Documentation Form establish custody of the sample at all times? Total Applicable Points Total Survey Points Percentage

CATEGORY 9 LABORATORY TESTING AND ANALYSIS CONTROL 1.

Function checks are routinely performed by the operator.

2.

The operator performs control checks during the analytical or testing procedures.

3.

Tests for significance of difference are made when results indicate the need.

4.

Control charts are used routinely for suspected or difficult method determinations,

5.

The Quality Control Coordinator is responsible for deciding which testing or analytical operations will be charted. Total Applicable Points Total Survey Points Percentage

CATEGORY 10 QUALITY DOCUMENTATION AND RECORDS CONTROL 1.

The quality documents to be controlled are listed in the Quality Manual.

2.

Document retention policies are published in in the Quality Manual or elsewhere in writing.

223

-

3.

The Quality System is adequately documented.

4.

The Quality Control Coordinator issues periodic reports to management which reflect quality levels, quality costs, customer complaints, etc.

5.

There is adequate control over the issue of new technical documents and changes.

6.

Obsolete documents are retrieved from work stations and are not permitted to remain in the hands of users. Total Applicable Points Total Survey Points Percentage

-

CATEGORY 11

CONTROL OF MEASURING AND TEST EQUIPMENT 1.

Quality Control procedures insure that instruments, gages, measuring devices and test equipment are periodically inspected and recalibrated at established intervals.

2.

Working and reference standards of required accuracy that are periodically calibrated to primary standards traceable to the NIST are maintained in a suitable environment.

3.

New or repaired test equipment and measuring devices are calibrated and proved satisfactory by Quality Control before release for use.

4. There are written calibration procedures for each type of instrument and measuring device.

5.

Objective evidence includes calibration date and date next calibration must be performed on measuring instrumentation.

6.

Record system provides for automatic recall of gages, instruments and test equipment due for calibration. Total Applicable Points Total Survey Points Percentage

224

-

CATEGORY 12 PREVENTIVE MAINTENANCE 1.

There is a planned, scheduled program tied in with the calibration system, that ensures that all measuring and test equipment undergoes periodic preventive maintenance.

2.

Preventive maintenance checklists are in use and on file.

3.

An adequate spare parts inventory is on hand.

-

Total Applicable Points Total Survey Points Percentage

CATEGORY 13 REFERENCE STANDARDS 1.

Laboratory policy requires the use of reference standards, when available.

2.

The Quality Control Coordinator keeps on file a copy of NIST Publication 260 and copies of NIST Certicates of Analysis. Total Applicable Points Total Survey Points Percentage

CATEGORY 14 DATA VALIDATION 1.

Data validation is routinely employed to detect outliers or spurious values.

2.

Manual data validation techniques are the only methods used to detect outliers and spurious values.

3.

Both manual and computerized techniques are used for data validation.

225

Sampling plans from ANSVASQC 21.4, 1981 are used when selecting samples for data validation of large quantities of data.

4.

Total Applicable Points Total Survey Points Percentage

CATEGORY 15 ENVIRONMENTAL CONTROLS 1.

The laboratory working environment is controlled to the extent prescribed by the Manual Total Applicable Points Total Survey Points Percentage

CATEGORY 16 CUSTOMER SATISFACTION AND COMPLAINTS 1.

A record is kept of all customer contacts and the Quality Control coordinator is responsible for reviewing them and taking any necessary action.

2.

One individual is charged with the responsibility for handling all complaints from customers, regulatory agencies, and accrediting organizations.

3.

There is a system for providing feedback to all laboratory personnel concerned.

4.

If required by contractual, regulatory, or accreditation bodies, the Quality Control Coordinator will arrange with an outside marketing analysis agency to conduct whatever surveys are necessary in order to appraise the effectiveness of the laboratory’s customer satisfaction efforts.

226

5.

One individual is charged with the responsibility for initiating corrective action, if this becomes necessary. Total Applicable Points Total Survey Points Percentage

CATEGORY 17 SUBCONTRACTING

1.

Contract laboratories are required to have a viable Quality Control System in place.

2.

Provision is made for furnishing contract laboratories with “audit” samples to test laboratory proficiency.

3.

When a new method is introduced, provision is made for furnishing contract laboratories with spiked samples to test the proficiency of the laboratory in performing the method. Total Applicable Points Total Survey Points Percentage

CATEGORY 18 PERSONNEL TRAINING, QUALIFICATION AND MOTIVATION

1.

The laboratory provides for employee indoctrination and training in Quality Control.

2.

The laboratory has a program to test the effectiveness of the training effort.

3.

Training records are available to indicate the status of individual training.

4.

The laboratory conducts campaigns, supported by management, to promote the achievement of superior quality output. Total Applicable Points Total Survey Points Percentage

227

-

CATEGORY 19 STATISTICAL METHODS The laboratory employs the following statistical techniques in the routine conduct of analytical and testing work:

1. a.

Tests of hypotheses

b.

Treatment of outliers

c.

Control Charts

6.

Sampling Plans

e.

Tests for significance of differences Total Applicable Points Total Survey Points Percentage

-

CATEGORY 20 NONCONFORMITY 1.

The Quality Control System assures that positive action is taken, when a nonconforming event occurs, to ensure that all required tasks are performed in accordance with provisions of the Quality Manual.

2.

Adequate records are kept of nonconformities.

-

Total Applicable Points Total Survey Points Percentage

228

-

CATEGORY 21 CORRECTIVE ACTION 1.

The laboratory has a method of recurrence control to prevent repetitive discrepancies.

2.

Corrective action requests on nonconforming events are initiated promptly

3.

Records provide for follow-up on all corrective action requests.

4.

The responsibility for solving the problem by taking corrective action is clearly established.

5.

The Suspense Date when the corrective action is expected to be completed is clearly established.

6.

The Corrective Action Log controls the progress of the corrective action initiated by the Corrective Action Request. Total Applicable Points Total Survey Points Percentage

CATEGORY 22 QUALITY COST REPORTING 1.

Quality costs are accumulated for the following categories: a.

Prevention costs

b.

Appraisal costs

C.

Internal failure costs

d.

External failure costs

2.

When actual costs figures cannot be obtained from the cost accounting component, reasonably accurate estimates are used.

3.

Quality Cost reports are made management periodically.

4.

Quality cost figures are used in the annual budgeting process.

to

Total Applicable Points Total Survey Points Percentage

229

CATEGORY 23 QUALITY AUDITS 1.

Quality audits are performed on an announced, scheduled basis by individuals outside the quality organization.

2.

All areas of the laboratory contributing to the quality of work output are audited.

3.

The results of the audit are reported to management in writing.

4.

Pre-audit and post-audit conferences are held prior to and after each audit. Total Applicable Points Total Survey Points Percentage

CATEGORY 24 RELIABILITY 1.

Reliability forecasts in terms of “Mean Time to Failure” (MTTF) are routinely provided by Quality Control for remotely situated recording instruments, Total Applicable Points Total Survey Points Percentage

230

-

MAINTENANCE / SERVICE REPORT ITEM NAME

TEST NO

TIME STARTED

MANUFACTURER

TIME

DATE

MODEL

OPERATOR FAILURE CONDITIONS

I INTERVAL SINCE LAST SERVICE

LOCATION

I

GENERAL DESCRIPTION OF FAILURE AND CAUSE ENVIRONMENTAL CONDITIONS

DIAGNOSTIC TIME SPENT

CORRECTIVE ACTION TAKEN FAILED COMPONENTS REPLACED FAILED COMPONENTS REPAIRED SERVICE REQUIREMENTS

I NOT REQUIRED

TAMPER-PROOF SEALING REQUIRED PREVENTIVE MAINTAINANCE COMPLETED OPERATIONAL TEST COMPLETED

SIGNATURE

FIGURE 26- 1

23 1

METHOD VALIDATION APPROVAL REPORT DATE: PATIENT TEST METHOD DESCRIPTION: SPECIMEN DESCRIPTION:

ABSTRACT OF TEST METHOD:

METHOD VALIDATION TYPE/S USED FOR THIS DETERMINATION:

OF PERFORMANCE RESULTS ESTABLISHMENT STUDY:

SPECIFICATION

a.

Accuracy

b.

Precision

c.

Analytical sensitivity

d.

Analytical specifity (Interferences)

e.

Reportable range of patient test results

f.

Reference range(s)

g.

Other performance characteristics as required.

METHOD VALIDATION PERFORMED BY: FOR DATA - SEE APPENDIX FOLLOWING. APPROVED BY:

TITLE

DATE: Figure 27-1

232

VERIFICATION

OR

OK

FAIL

Effective Date BY Approved

Subject

Figure 28-1

233

Section No. Page of Reviewed

Laboratory Quality Assurance System, 3rd Edition. Thomas A. Ratliff Copyright 02003 John Wiley & Sons, Tnc. 4SBN: 0-471-26918-2

Index Acceptance sampling, 20 Accreditation requirements, 12 Administrative support, 8 AIHA Laboratory Accreditation CommitteeL'rogram, 13 Air conditioning system, 8 Air Force Logistics Command (AFLC), 16 American Association for Laboratory Accreditation, 12 American Industrial Hygiene Association (AIHA), 12-13 American Society for Quality, 31 American Society for Testing and Materials (ASTM), 28 Analysis audits, 24-25 Analysis of variance (ANOVA), 11 Analyst proficiency, 13-14 ANSVASQC Standards: 2- I.4. 19-20 Z- I.4-1993,23,25 Z-1.9-1981,23 ANS [/ISO/ASQ: 49001-2000,2,21 Q9004-2000, 12 Q10011-1994,25 Anuual reports, 6 Appraisal costs, 31-32 ASTM E-1301-1995, 12 Audits, see Quality audits Award program, 21 Bell Telephone Laboratories, 20 Bonus program, 21 Bulk Asbestos, proficiency testing, 12 Calibration procedures/standards: interlaboratory proficiency testing, 11 intervals, 15 plan design, 14 procedures, 15-16 source, 17 standards quality, 14-15 Chaiii-of-custody procedures, 10-1 1 Chief Executive Officer, 1 Chi-square test, 20, 22 Communications: customer complaints, 26 motivational, 7 system guidelines, 6 Complaints: handling procedures, 26 managerial review of, 6 Consumer surveys, 26 Continual improvement, 20 Continuous Quality Improvement policies, 7,21 Control chart. 22

Corrective Action: components of, 27-28 initiation of, 30-3 1 managerial review, 6 quality control cost report, 32 Requests, 6 Corrective Action Analyst, functions of, 27 Corrective Action Request (CAR), 27 Cost reporting, 31-32 Customer complaints, 26 Customer focus, 4-5 Customer Satisfaction: consumer surveys, 26 policies, 7 Reports, 21 Customer service, 26 Daily service checklists, 30 Data processing audits, 24-25 Data validation: components of, 19-21 quality control cost report, 32 statistical testing, 22 SUbCOntrdCting laboratories, 24 Documentation, see Recordkeeping/records: control, 2-3 of quality policy, 1 Eating arreas, 8 Economic Control of Quality of Munufuctured Products (Shewhart), 20 Electric system standards, 15 ELPAT, 12 EMPAT, 12 Employee(s): recognition programs, 2 1 training, 30 Environmental laboratories, 10 Equipment: contracts, 29-30 corrective/preventive action procedures, 27-28 failure rate, 29 maintainability, 30 measurement and test: calibration intervals, 15 calibration plan, 14 calibration procedures, 15-1 6 calibration source, 17 calibration standards quality, 14-15 environmental conditions, 15 Government-Industry Data Exchange Program (GIDEP), 16 labeling, 17 preventive maintenance, 17-1 8 reliability requirements, 29 testing procedures, 30 External-failure costs, 32

235

First-in, first-out (FIFO), 9 Fitness facilities, 8 Flowchart, quality assurance manual, 34-36 Forensic laboratories, I0 Format, for quality manual, 2, 36 F-tests, 11, 20, 22 Government-Industry Data Exchange Program (GIDEP), 16,29 Graphics, quality control cost report, 32 Handling samples, 9-10 Health facilities, 8 Heating system, 8 Housekeeping practices/standards, 8 Human resources, responsibilities of motivation, 7 overview, 6-7 qualification records, 7 training evaluation, 7 Independent study, 7 Information resources, proficiency testing programs, 13 In-house training, 7 Inspection procedures: destructive, 23 equipment, 30 nondestructive, 22-23 quality audits, 25 of supplies, 8-9 Interlaboratory audits, 12 Interlaboratory proficiency: appraisal costs, 31 performance evaluation and, 2 I quality policy, 1 testing for, 11-12 Internal-failure costs, 32 Intralaboratory proficiency testing program, 13-14,21,31 Inventory, first-in, first-out (FIFO), 9 ISO/IEC Guide 43-1-1997, 12 Japanese managerial techniques: Kaizen, 21 types of, 7 Job descriptions, 5-6 Joint Commanders of the Army Materiel Command (AMC), 16 Joint Commission on Accreditation of Health Care Organizations (JCAHO), 12 Kaizen, 21

Laboratory Director: Quality Control Coordinator, relationship with,

5

Quality Improvement Board, 2 I quality manual, recognition of, 1 Laboratory infrastructure, 8 Laboratory notebooks, 3 4 Laboratory Quality Assurance Manual, benefits of, 4 Laboratory Stores Clerk, functions of, 9 Laboratory testing: interlaboratory proficiency, 11-12, 21, 31 intralaboratory proficiency testing programs, 13-14,21,31 Lead, OSHA requirements, 12 Letter of Promulgation, I , 36 Lighting design, 8, 15 Logs: equipment maintenance, 18 of inventory, 9 Lunchrooms, 8 Maintainability factor, 30 Management review, 6 Mean time-to-failure rates, 29 Meawrement uncertainty, estimate of, 18 Merit Awards, 21 Method Validation, 21, 28 MIL-STD-105, 20 Monitoring guidelines, 21 Motivational campaigns, 7 National Institute for Occupational Safety and Health (NIOSH), 13, 28 National Institute of Science and Technology (NIST): calibration standards, 14-15, 17 special publications, listing of, 18 Standard Reference Material Program, 11,18 Naval Materiel Command (NMC), 16 Nonconformity, 25, 28 Objectives, types of, 2 Occupational Safety and Health Act of 1970 (OSHA), 10, 12-13,28 On-the-job (OTJ) training, 6 Operations guidelines, 30 Organization considerations, 5-6 Pathological laboratories, 10 PAT proficiency testing program. 12-1 3 Performance evaluation, 2 1 Planning guidelines, 4-5 President of Corporation, in quality manual, 1 Prevention costs, 3 1-32 Preventive Action: components of, 27-28 managerial review, 6 Preventive maintenance, 17-1 8, 30 Primary objectives, 2 Procurement quality control, 32. See also Purchasing guidelines Program Manager, Government-Industry Data Exchange Program (GIDEP), 16 Project team management, functions of, 21 Purchase orders, 8-9 Purchasing Department, functions of, 8-9 Purchasing guidelines. purchase orders, 8-9

Qualified Outside Laboratory Source List, 24 Quality assurance manual: elements of, overview, 1-2,5 introduction section, 1 Letter of Promulgation, 1, 36 management of, 2 page numbering, 36 quality objectives, 2 quality policies, 1-2 table of contents, 36 title page, 1 writing guidelines: documentation, 36 existing procedure$, 34 flowchart preparation, 34-36 format, 2, 36 new procedures, 36 objectives, 33-34 preparation organization, 33 priorities, 33-34 program requirements, identification of, 36 Quality assurance plan development, 4-5 Quality Assurance Hundhook,4th Edition (Juran), 7, 18 Quality audits: components of. 24-25 importance of. 6, 21 of vendors, 8-9 Quality Circles, 7, 20 Quality Control Coordinator: functions of: corrective action, 27 document control, 3 employee training programs, 6 overview, 1. 5-6 preventive action, 27 purchase orders, 9 qualification records, 7 Quality Improvement Board, 21 reliability procedures, 28-29 state of laboratory quality assurance system report, 6 in system planning, 4 writing quality assurance manual, 33-36 job description, 5-6 Quality Cost Reports, 6, 21 Quality Improvement Board, functions of, 21 Quality is Free program, 20 Quality manual, see Quality assurance manual Quality objectives, 2 Quality policies, 1-2, 21 Quality system: analysis of, 20-21 elements of, overview, 1-2 improvement of, 20-21 monitoring, 21 measurement, 20-2 1 performance evaluation, 2 I Quality System Survey Evaluation Checklist, 9 Receiving report, 9 Recordkeeping/records: chain-of-custody procedures, 10-1 I equipment maintenance, 18, 30 guidelines for, 2-3 quality audit inspections, 25 reliability programs, 30-3 1 X-R charts, I I, 22 Reference materials, standard, 18-19 Reference standards, 18-1 9

236

Reliability programs: employee training, 30 equipment contracts, 29-30 equipment failure rate, 29 equipment tests, 30 influential external factors, 29 maintainability, 30 operations guidelines, 30 planning process, 29 recordkeeping guidelines, 30-3 1 Restrooms. 8 Safety practices/standards, 8 Samples, handling, identification, storage, and shipping, 9-10 Sampling audits, 24-25 Sampling techniques, 22 Secondary objectives, 2 Sequential analysis, 20 Services, subcontracting, 24 Shewhart, Walter, 20 Shipping standards for samples, 9-10 Simon, Colonel Leslie E., 20 Soviet Saratov System, 7 Standard Reference Materials (SRMs), 11. 18 Statistical methods, 21-23 Statistical tests, 20 Storage, of samples, 9-10 Subcontracting labot'dtorieS, 24 Summary Quality Cost Report. 6 Supplies, subcontracting, 24 Target Health Hazard Program (THHP), 13 Test audits, 24-25 Total Quality Control, 20 Total Quality Control policies, 7 Total Quality Management, 20 Training programs: employees, 6-7, 30 evaluation of, 7 quality policie\, 1 types of, 6-7 t-tests, 1 I , 20, 22

U.S. EPA Environmental Monitoring and Support Laboratory, 12 United States Standard MIL-Q-9858A. 12 Vendors: purchase orders, 8-9 quality assurance manual, 9 Ventilation system, 8 Work environment, 8 Work station ergonomics, 8 Writing guidelines for manual: documentation, 36 existing procedures, 34 flowchart preparation, 34-36 format, 2, 36 new procedures, 36 objectives, 33-34 preparation organization, 33 priorities, 33-34 program requirements, identification of, 36 X-R charts. I 1, 22 Zero Defects programs, 7, 20