United States Prevention, Pesticides, EPA 747-R-92-005

Environmental Protection and Toxic Substances May 1993

Agency (TS-798)

Pb-Based Paint

Laboratory Accreditation:

Curricula Recommendations

for Assessor Training Programs

Revision 1.0
(BLANK PAGE)
Pb-Based Paint

Laboratory Accreditation:

Curricula Recommendations

for Assessor Training Programs

Revision 1.0

Technical Programs Branch

Office of Pollution Prevention and Toxics

U. S. Environmental Protection Agency

401 M Street, S.W.

Washington, D.C. 20460

John V. Scalera, Work Assignment Manager

Janet C. Remmers, Project Officer 

May 14, 1993
DISCLAIMER

This document has been reviewed and approved for publication by the

Office of Prevention, Pesticides, and Toxic Substances, U.S. Environmental Protection Agency. The use of trade names or commercial

products does not constitute Agency endorsement or recommendation for

use.
NOTICE

This document provides recommendations for site assessor training curricula for

assessors of laboratories that analyze Pb in paint film or chips, Pb-based paint

contaminated soils, and deposited dust (vacuum dust and wipe samples). These

recommendations will form the basis of the training curricula EPA will establish for

accrediting organizations that seek recognition as participants in the EPA National

Lead Laboratory Accreditation Program (NLLAP). Two training course curricula for

assessors were developed. The Level One Course is an extensive course of 3 to

5 days for the beginning assessor, and the Level Two Course is of 12 hours

duration for the experienced assessor from related fields. Specific lesson plans

should be developed by the accrediting organization, addressing the curricula

recommendations presented in this document.
(BLANK PAGE)
 * In order to avoid confusion in the terms lead (for Pb) and lead (for leader), the

following conventions are used. Pb will be used for the heavy metal and lead will be

used for all other uses. The terms, Auditor, Assessor, and Site Visitor, are used

interchangeably. The term, Assessor, which is the term preferred by the ISO

(International Organization for Standardization), is used in this report. The term, paint,

in this document refers to dried paint film or paint chips and not to liquid, uncured paint. 

v

AUTHORS AND CONTRIBUTORS

Midwest Research Institute (MRI) was requested by the Environmental

Protection Agency (EPA) to develop recommended curricula for the training of on-site

assessors. These on-site assessors will perform on-site assessments of laboratories

seeking accreditation for the analysis of lead (Pb) in paint, soil, and deposited dust,

including vacuumed dust and wipe samples, from EPA-recognized accreditation

organizations as part of the EPA National Lead Laboratory Accreditation Program

(NLLAP).* These curricula were developed with the cooperation of the Technical

Programs Branch, Office of Pollution Prevention and Toxics (OPPT), under EPA

Contract No. 68-DO-0137. A working meeting was held in Gaithersburg, Maryland,

from June 22 to 24, 1992, with a group of metals laboratory accreditation experts to

gather information for the basis of this report. The affiliations of the working group and

the role of each organization are presented below.

MIDWEST RESEARCH INSTITUTE (MRI)

MRI was responsible for the planning and the conduct of the working meeting

held in Gaithersburg, Maryland, from June 22 to 24, 1992. Dr. Larry Lowry, who was

the Work Assignment Leader, had primary responsibility for conducting the meeting and

writing the final reports with input from working group members and Mr. Paul Constant,

Dr. Gary Dewalt, and Mr. Jack Balsinger from MRI.

WORKING GROUP PARTICIPANTS

The following individuals actively participated in the working meeting and in the

review of this document. Their affiliations and the organizations they represent are

listed.

` Ms. Harriotte Hurley, C.I.H. 

Clayton Environmental Consultants

1252 Quarry Lane, P.O. Box 9019

Pleasanton, CA 94566

Chair of the American Industrial Hygiene Association (AIHA)

Environmental Lead Laboratory Accreditation Committee (ELLAC).
vi

` Larry K. Lowry, Ph.D.

Senior Advisor, Exposure Assessment

Midwest Research Institute

425 Volker Boulevard

Kansas City, MO 64110

Work Assignment Leader (WAL) and principal author of this report.

` James Nelson, Ph.D., C.I.H.

Director, Data Chem Laboratories

960 W. LeVoy Drive, Sorenson Research Park

Salt Lake City, UT 84123

An AIHA industrial hygiene laboratory assessor, representing AIHA and Data

Chem Laboratories.

` James Pearson, Ph.D. - Division Director

Division of Consolidated Laboratory Services

One North 14th Street

Richmond, VA 23219

Representing the Association of State and Territorial Public Health 

Laboratory Directors (ASTPHLD) and state laboratory accrediting organizations. 

` Mr. John V. Scalera

Technical Programs Branch, 

Chemical Management Division,

Office of Pollution Prevention and Toxics

U.S. Environmental Protection Agency

401 M Street SW

Washington, DC 20460

Work Assignment Manager (WAM) and principal EPA reviewer.

` James Scott, M.S. 

Georgia Power Company

Environmental Laboratory

5131 Maner Road

Smyrna, GA 30080

A lead assessor for the American Association for Laboratory Accreditation

(A2LA).
vii

` Mr. Peter Unger

Vice President

American Association for Laboratory Accreditation

656 Quince Orchard Road, No. 304

Gaithersburg, MD 20878-1409

Vice President, the American Association for Laboratory Accreditation (A2LA).

` Barbara J. Weaver, C.I.H.

Lancaster Laboratories, Inc.

2425 New Holland Pike

Lancaster, PA 17601

Represents the laboratory director, Dr. Wilson Hershey, the American Council of

Independent Laboratories (ACIL) and the Committee on National Accreditation of

Environmental Laboratories (CNAEL).

EPA, CHEMICAL MANAGEMENT DIVISION, TECHNICAL PROGRAMS BRANCH

(CMD/TPB)

EPA was responsible for oversight in the development of the study plan;

managing and coordinating the conduct of the overall project; and reviewing, editing,

and finalizing this report. Key staff included Mr. John Scalera, Work Assignment

Manager; Janet C. Remmers, Project Officer; and Dr. Joseph J. Breen, former Project

Officer.

EXTERNAL REVIEWERS

The following individuals served as external reviewers to this document. Their

participation in this review is gratefully acknowledged.

Mr. Michael Beard, EPA, Research Triangle Park, NC

Mr. Albert D. Tholen, NIST, Gaithersburg, MD

Ms. Regina Bushong, EPA, Washington, DC

Mr. Fred Grunder, AIHA, Fairfax, VA

Mr. Frederic Siegelman, EPA, Washington, DC

Dr. Al Liabastre, U.S. Army, Fort McPherson, GA

May 14, 1993
viii

(BLANK PAGE)
ix

CONTENTS

Authors and Contributors .............................................. v

External Reviewers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . vii

Executive Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xi

1. Introduction .............................................. 1

1.1 Background ................................... 1

1.2 EPA recognition of laboratories .................... 1

1.3 Purpose . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

1.4 Approach . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

2. Level One Course—The Beginner Course ...................... 5

2.1 Course outline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

2.2 Qualifications of assessor candidates ............... 7

2.3 Qualifications of course instructors . . . . . . . . . . . . . . . . . 8

2.4 Module I. General Overview of the 

Assessment Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

2.5 Module II. Technical Aspects of Pb Sampling

and Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

2.6 Module III. The Assessment Process, or 

How to Conduct an Assessment . . . . . . . . . . . . . . . . . . . 40

2.7 Module IV. Interpersonal Skills . . . . . . . . . . . . . . . . . . . 46

2.8 Module V. Practical Role-playing Exercise . . . . . . . . . . 50

2.9 Module VI. Written Examination . . . . . . . . . . . . . . . . . . 51

2.10 Module VII. On-site Internship . . . . . . . . . . . . . . . . . . . . 52

3. Level Two Course—Update for the Experienced Assessor . . . . . . . . . 53

3.1 Course outline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53

3.2 Qualifications for admission . . . . . . . . . . . . . . . . . . . . . . . 54

3.3 Written examination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54

4. Continuing Education Refresher Course for All Assessors . . . . . . . . . . 55

4.1 Objective . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

4.2 Outline of Continuing education program . . . . . . . . . . . . 55

5. Administrative Issues . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57

5.1 Who offers the courses? . . . . . . . . . . . . . . . . . . . . . . . . . 57

5.2 Hiring, use, and dismissal of assessors . . . . . . . . . . . . . . 57

6. List of References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59

Appendices

A. Acronyms and glossary of terms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1

B. Assessor checklist for laboratories engages in the analysis of Pb 

in paint, soils, and deposited dust . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
x

(BLANK PAGE)
 * The Environmental Lead Proficiency Analytical Testing (ELPAT) Program is a

cooperative effort to improve and evaluate the performance of laboratories involved in the

analysis of Pb in paint, dust, and soil matrices. The National Institute for Occupational Safety

and Health (NIOSH) performs ELPAT data analysis under a Memorandum of Understanding

(MOU No. PW593570-01-0) with the U.S. Environmental Protection Agency (EPA). The

American Industrial Hygiene Association (AIHA) contracts for ELPAT sample production and

administers the ELPAT program as permitted under a Cooperative Research and

Development Agreement (CRADA No. NIOSH-92-1) with NIOSH covering cooperation in

analytical research and proficiency test programs.

xi

EXECUTIVE SUMMARY

The hazards of Pb-based paint have become a leading public health issue of the

1990s, and Pb-paint abatement of homes is a high priority among many different health

and environmental organizations. The Environmental Protection Agency (EPA)

estimates there are several hundred laboratories, not currently performing analysis, that

will be involved in new, extensive Pb-abatement programs.

Following the lead of the Interagency Lead-Based Paint Task Force (U.S. EPA,

1992a), the EPA Office of Pollution Prevention and Toxics (OPPT) is establishing the

National Lead Laboratory Accreditation Program (NLLAP). The NLLAP will provide

federal oversight for state and private sector laboratory accreditation programs involved

in the accreditation of laboratories analyzing paint, soil, and dust samples associated

with the abatement and control of Pb-based paint contaminated housing. The NLLAP

will recognize accrediting organizations that meet EPA minimum requirements through

a Memorandum of Understanding (MOU). Each NLLAP-recognized accrediting

organization will administer its laboratory accreditation program under NLLAP oversight. 

In order to be recognized by the NLLAP, laboratories must meet the following criteria:

` The laboratory must successfully undergo a systems audit inclusive of an

on-site assessment by an analytical laboratory accrediting organization

recognized by EPA through an MOU.

` The laboratory must successfully participate in the Environmental Lead

Proficiency Analytical Testing (ELPAT) program.* 

The purpose of this document is to recommend criteria for site assessor training

curricula for assessors of laboratories that analyze Pb in paint, dust, and soil. These

recommendations will form the basis of the training curricula that EPA will establish for
xii

accrediting organizations which seek EPA recognition through an MOU as a part of the

NLLAP.

These recommendations for site assessor training programs were prepared

following a working meeting of experts in metals analysis from government and from

independent laboratories. Two training course curricula were developed. 

The Level One Course is an extensive course of 3 to 5 days duration for the

beginning assessor. The course consists of seven modules, including a written

examination and an on-site assessment internship. The seven modules cover: (1) a

general overview of the accreditation process; (2) the technical aspects of Pb sampling

and analysis; (3) the assessment process or how to conduct an assessment; (4) the

interpersonal skills needed to conduct an assessment; (5) a practical role-playing

exercise; (6) a written examination; and (7) an on-site assessment internship.

The Level Two Course is a 12-hour course for the experienced assessor from

qualified NLLAP-recognized accrediting organizations. This course covers three

modules, including modules (1) and (2) from the Level One Course. A written

examination is also included. The two courses are designed so that they can be taught

concurrently.

Both courses have minimum education/experience requirements for prospective

students and instructors. The courses make extensive use of a checklist that is based

on the ISO Guide 25, the international standard (ISO/IEC Guide 25, 1990). The

courses should be taught by a team that includes an experienced assessor and an

experienced inorganic chemist familiar with Pb analyses in dust and paint matrices. 

The two courses are generic in scope and require supplemental instruction on

policies and procedures specific for individual NLLAP-recognized accrediting

organizations. 

The NLLAP-recognized accrediting organization will conduct all modules of the

course. The accrediting organization will certify the assessor and have the option of

hiring the graduates of the program. The NLLAP-recognized accrediting organization

will also be responsible for monitoring the assessor's performance following completion

of the training program and for conducting continuing education programs annually.
1

SECTION 1

INTRODUCTION

1.1 BACKGROUND

The hazards of Pb-based paint have become a leading public health issue of the

1990s, and Pb-paint abatement of homes is a high priority among many different health

and environmental organizations. The Environmental Protection Agency (EPA)

estimates there are several hundred laboratories, not currently performing analysis, that

will be involved in new, extensive Pb-abatement programs.

1.2 EPA RECOGNITION OF LABORATORIES

Following the lead of the Interagency Lead-Based Paint Task Force (U.S. EPA,

1992a), the EPA Office of Pollution Prevention and Toxics (OPPT) is establishing the

National Lead Laboratory Accreditation Program (NLLAP). The NLLAP will provide

federal oversight for state and private sector, laboratory accreditation programs

involved in the accreditation of laboratories analyzing paint, soil, and dust samples

associated with the abatement and control of Pb-based paint contaminated housing. 

The NLLAP will recognize accrediting organizations that meet NLLAP minimum requirements through a Memorandum of Understanding (MOU). Each NLLAP-recognized

accrediting organization will administer its laboratory accreditation program under

NLLAP oversight. In order to be recognized by NLLAP, laboratories must meet the

following criteria:

` The laboratory must successfully undergo a systems audit inclusive of an

on-site assessment by an analytical laboratory accrediting organization

recognized by EPA through an MOU.

` The laboratory must successfully participate in the Environmental Lead

Proficiency Analytical Testing (ELPAT) program. (See footnote on page xi.)

The completion of a proficiency testing-based program alone is not sufficient

proof that a laboratory can perform successfully on real world samples. The proficiency

testing sample, even though it is a matrix-based material, will usually receive special

treatment in the laboratory. The systems audit is necessary to ensure that a laboratory

has the required staff, methods, facilities, quality assurance plans, and other essentials

necessary to perform the analysis within a stated level of confidence.
2

1.3 PURPOSE

The purpose of this document is to recommend criteria for site assessor training

curricula for assessors of laboratories that analyze Pb in paint, dust and soil. These

recommendations will form the basis of the training curricula that EPA will establish for

accrediting organizations which seek recognition by NLLAP through an MOU. 

Because of the need to maintain flexibility, this curriculum is intended to be a

working guideline rather than a program outlining specific requirements. At this time,

there are no standard EPA-validated analysis methods for Pb in paint, soil, and

deposited dust (including wipe samples and vacuumed samples). In addition, there are

no standardized wipe-sampling media. As standardized methods are developed, they

will be incorporated into the training program and replace some of the generic sections

in the current program.

1.4 APPROACH

Curricula recommendations for site assessor training programs were prepared

following a working meeting of experts in metals analysis from government and from

independent laboratories. Two training course curricula were developed. 

The Level One Course is an extensive course of 3 to 5 days duration for the

beginning assessor. The minimum qualifications for admission are (1) a B.S. degree in

chemistry or related science, (2) a minimum of 3 years nonacademic analytical

laboratory experience, two of which are in metals analysis, (3) documented experience

with laboratory quality assurance/quality control procedures, and (4) good interpersonal

skills. The course consists of seven modules, including a written examination and an

on-site assessment internship. The seven modules cover: (1) a general overview of

the accreditation process; (2) the technical aspects of Pb sampling and analysis; (3) the

assessment process or how to conduct an assessment; (4) the interpersonal skills

needed to conduct an assessment; (5) a practical role-playing exercise; (6) a written

examination; and (7) an on-site assessment internship.

The Level Two Course is a 12-hour course for the experienced assessor from

qualified NLLAP-recognized accrediting organizations. The qualifications for admission

are (1) the general educational and experience requirements for assessors, as

specified by NLLAP-recognized accrediting organizations, (2) experience in conducting

assessments with a minimum of three assessments per year for the most recent 2-year

period, and (3) a letter of recommendation from the assessor's accrediting organization. 

This course covers three modules, including modules (1) and (2) from the Level One

Course. A written examination is included. The two courses are designed so that they

can be taught concurrently.

Both courses have minimum education/experience requirements for prospective

students and instructors. The courses make extensive use of a checklist based on the

ISO Guide 25, the international standard (ISO/IEC Guide 25, 1990). The checklist will
3

be provided to the laboratory prior to the site visit for a self-assessment and returned to

the designated assessor. The designated assessor will use the same checklist to

perform the on-site assessment. The courses should be taught by a team that includes

an experienced assessor and an experienced inorganic chemist familiar with Pb

analyses in dust, soil, and paint matrices. The two courses, which are generic in scope,

require supplemental instruction on policies and procedures specific for individual

NLLAP-recognized accrediting organizations. 

The NLLAP-recognized accrediting organization will conduct the final phase of

the training: the on-site assessment internship. The accrediting organization will certify

the assessor and have the option of hiring the graduates of the program. The NLLAPrecognized accrediting organization will also be responsible for monitoring the

assessor's performance following completion of the training program and for conducting

continuing education programs annually.

A continuing education course (refresher course) will be required for all

assessors. It would be offered annually and required every two years. It should be

taught by the specific NLLAP-recognized accrediting organization and would include

updates on (1) policies of the NLLAP-recognized accrediting organization, (2)

regulations update, (3) health issues associated with Pb, and (4) new technical aspects

of sampling and analysis. The curriculum would be based on case discussions and

problem resolution.

The remainder of this document contains the Level One Course (Section 2), the

Level Two Course for the experienced assessor (Section 3), and the continuing

education module (Section 4). A discussion of various administrative issues is in

Section 5. Section 6 gives a list of references. Two appendices include (A) a list of

acronyms and glossary of terms, and (B) the site assessor checklist.
4

(BLANK PAGE)
5

SECTION 2

LEVEL ONE COURSE—THE BEGINNER COURSE

2.1 COURSE OUTLINE

This beginner course is open to individuals possessing a minimum set of

qualifications as outlined in a variety of publications, including ASTM standard E-994

(ASTM E-994, 1990), the Registrar Accreditation Board (1992), the Interagency Leadbased Paint Task Force (U.S. EPA, 1992a), and ISO guides (ISO/IEC 58, 1992). It

runs for 3 to 5 days, depending on the type and number of case studies and the

number of hands-on classroom exercises used. Qualifications for assessor candidates

are given in Section 2.2. Qualifications for instructors are given in Section 2.3. The

course is also open to individuals with an interest in the assessment process, but who

have no interest in becoming qualified assessors. Educational/experience requirements for these "observer" students would be waived, as would be the examination and

on-site internship. The major modules of this course are outlined below.

2.1.1 Module I. General Overview of the Accreditation Process

This 2-hour module covers the generic aspects of the accreditation process, the

history of the health effects of Pb, and the current status of Pb paint abatement issues

and legislation. This section should be taught by a current assessor or individual

familiar with laboratory accreditation and Pb analysis. 

An additional 2-hour session is required to acquaint the prospective assessor

with the specific accreditation policies and procedures. This program should be taught

by a representative of the NLLAP-recognized accrediting organization, because the

accreditation process can be expected to be different for each NLLAP-recognized

accrediting organization. 

2.1.2 Module II. Technical Aspects of Pb Sampling and Analysis

This 8-hour module, which covers the technical aspects of Pb sampling and

analysis, is aimed at the laboratory chemist. It covers all aspects of laboratory issues

related to sampling, analysis, and reporting of data for Pb in paint, soil, and deposited

dust matrices. This module should be taught by a chemist with experience in analyses

of these matrices for Pb.
6

Additional information is incorporated in this module by reference. The EPA

report, "Pb-Based Paint Laboratory Operations Guidelines: Analysis of Pb in Paint,

Dust, and Soil," (U.S. EPA, 1992b) describes many of the issues related to sampling

and analysis of paint, soil, and deposited dust for Pb from a laboratory perspective. It

contains specific sections on quality assurance and provides guidance on selection of

digestion and analysis methods. This EPA report should be utilized in the training

curriculum.

2.1.3 Module III. The Assessment Process, or How to Conduct an Assessment

This 8-hour module addresses the assessment process and all steps required to

perform a successful assessment. Included are pre-assessment steps, the conduct of

the on-site assessment, reporting requirements, and assessor performance ratings.

This section should be taught by an experienced assessor. The following items should

be included:

` Pre-assessment review of documents

` Pre-assessment communication with the laboratory

` Preparation for the assessment, including which documents to take

` Conduct of the on-site assessment to include the following:

- Opening conference

- Pre-assessment walk through

- Use of checklist

- Documentation of sample tracking (through use of an audit sample or

tracking of samples)

- Interviews with key personnel

- On-site report writing, as required by the accrediting organization

- Closing conference

` Assessor reporting requirements

` Assessor performance rating from the laboratory and NLLAP-recognized

accrediting organization
7

2.1.4 Module IV. Interpersonal Skills

This 4-hour module includes the important aspects of how to conduct an

assessment and lists of do's and don'ts appropriate for a professional objective

assessor. This component is possibly the most important module because technical

expertise is in vain if the assessor does not have good interpersonal skills. This module

should be taught by an experienced assessor or an individual knowledgeable in and

experienced with interpersonal skills training.

2.1.5 Module V. Practical Role-playing Exercise

This module includes a practical role-playing application of the assessment

process. A variety of approaches can be used, such as mock site visits, case studies

with role-playing by students, or video cases with role-playing. The objective is to apply

skills learned in the lecture portion of the course. The length of this module can vary

from a few hours to a full day, depending on the format of the role-playing exercise. 

This module should be taught by an experienced assessor.

2.1.6 Module VI. Written Examination

A 1-hour written examination must be administered to document the successful

completion of the course. Guidelines for passing the course were established as

described later in this document, along with recommendations for remedial action in the

event of failure. Observer students would not be eligible for the written examination or

assessor status. 

2.1.7 Module VII. On-site Internship with a Certified Assessor

This module covers the practical application of the assessment process in an

actual laboratory. The recommended criteria include a minimum of two on-site visits,

one as an active intern, the second as a primary assessor with the assistance of a

supervising assessor from the specific NLLAP-recognized accrediting organization. 

This module is not part of the generic course and must be administered by an assessor

from an NLLAP-recognized accrediting organization. Successful completion of the onsite internship should result in certification from an NLLAP-recognized accrediting

organization.

2.2 QUALIFICATIONS OF ASSESSOR CANDIDATES

Assessor candidates should meet the following minimum requirements:

` A B.S. degree in chemistry or related science.

` Minimum of 3 years nonacademic analytical laboratory experience, two of

which are in metals analysis.
8

` Documented experience with laboratory quality assurance/quality control

procedures.

` Good interpersonal skills. 

Prospective students who are interested in the assessment process, but do not

wish to become assessors, would be admitted as "observer" students. Such students

would not be eligible for the written examination or any recognized assessor status.

2.3 QUALIFICATIONS OF COURSE INSTRUCTORS

Team teaching of these courses is most effective because many diverse areas

are included in the curriculum. Instructors must meet the requirements for admission to

the Level One course. In addition, they must have experience as current assessors for

environmental metals laboratories (minimum of three assessments per year for the

most recent 2-year period) and familiarity with Pb-analysis techniques and quality

assurance for the specific matrices. Experience with or knowledge of the ISO Guide 25

testing laboratory requirements is essential. Instructors who teach interpersonal skills

may not be required to be assessors or inorganic chemists, provided that they have

knowledge and experience in interpersonal skills training.

The initial cadre of instructors may be drawn from current assessors in related

fields, along with experienced Pb chemists. As the cadre of trained assessors in this

specific field increases, requirements for instructors may be raised to include successful

completion of these courses as a student and demonstrated experience in assessment

with these Pb-based matrices. 

2.4 MODULE I. GENERAL OVERVIEW OF THE ASSESSMENT PROCESS

(4 HOURS)

The course objective is to provide the student with an overview of the

assessment process, including introductions to the health effects of Pb exposure, the

current status of legislation, and issues related to laboratory accreditation.

2.4.1 Generic Overview Module Applicable to All Assessors and Accrediting

Organizations (2 Hours)

The overview module includes generic aspects of Pb laboratory operations

associated with matrices of paint, soil, and deposited dust, and is applicable to all

accrediting organizations. It includes the following topics:

` History of government regulatory processes related to Pb and Pb paint

laboratory issues, including discussion of the HUD Guidelines for Pb

abatement (HUD, 1990).
9

` History of health effects of Pb on children and the need for laboratory

measurements and a laboratory accreditation program. Some discussion of

the Centers for Disease Control (CDC) statement, "Preventing Lead (Pb)

Poisoning in Young Children," should be included (CDC, 1991).

` General requirements for accreditation as an "NLLAP-recognized"

laboratory.

- A systems audit inclusive of an on-site assessment by an accrediting

organization recognized by NLLAP.

- Participation in the ELPAT program (see footnote xi for explanation). 

Note: It is not necessary to be accredited by an NLLAP-recognized

accrediting organization to participate in this program.

` General requirements of accreditation through an NLLAP-recognized

accrediting organization based on the ISO Guide 25 (ISO/IEC Guide 25,

1990) criteria, as well as:

- Application Procedures.

- On-Site Assessment, including frequency.

- Participation in ELPAT program, including frequency.

- Audit of assessor performance as specified by ISO Guide 58 and the

accrediting organization.

- Requirements for "need-based" assessment, such as failed ELPAT

rounds, change in director or management, or failure to respond to

deficiencies.

- Requirements for removal of accreditation, such as repeated failure to

correct deficiencies noted on an audit, repeated failure of ELPAT

rounds, or fraud.

- Ethics of assessors

2.4.2 Accreditation Organization Procedures

This 2-hour module, which is a required supplement to the general module, is

designed to familiarize the student with the policies and procedures of a specific

accrediting organization, since these requirements vary by organization. This module

would be presented by a representative of an NLLAP-recognized accrediting

organization. The lecture would cover the following topics:
10

` Specific organization and policies of the accrediting organization.

` Application process, including fees.

` Review of the application.

` Time schedules and basic information on the process.

` Detailed requirements for staff, facilities, etc. 

` Advertising limitations to specific matrices and Pb.

` Reporting requirements to accrediting organization.

` Responsibility for communicating accreditation requirements to applicant.

` Responsibility at the accrediting organization for answering administrative

and technical questions.

` Addition of other criteria to the program.

` Communication of new changes (new equipment, staff) to the accrediting

organization.

` Specific criteria for "need-based" assessment, such as failed ELPAT results,

change in director or management, or failure to respond to deficiencies.

` Specific criteria for removal of accreditation, such as repeated failure to

correct deficiencies noted on an audit, repeated failure of ELPAT rounds, or

fraud.

2.5 MODULE II. TECHNICAL ASPECTS OF Pb SAMPLING AND ANALYSIS

(8 HOURS)

The objective of this module is to provide the assessor student, who should have

a basic knowledge of operation of a metals laboratory, with a detailed knowledge

necessary to perform a complete and objective site assessment of laboratories

performing analysis of Pb in paint chips, soil, and deposited dust (including dust wipes

and vacuumed dust.)

2.5.1 General Overview

This module covers subsampling of the sample and the analysis and reporting of

data for Pb in paint, soil, and deposited dust matrices. This module should be taught by

a chemist with experience in analyses of these matrices for Pb. Note: This module
11

provides a recommended curriculum, but the actual minimum laboratory requirements

are specified by NLLAP.

Additional information is incorporated in this module by reference. The EPA

report, "Pb-Based Paint Laboratory Operation Guidelines: Analysis of Pb in Paint,

Dust, and Soil" (U.S. EPA, 1992b), describes many of the issues related to sampling

and analysis of paint, soil, and deposited dust for Pb from a laboratory perspective. It

contains specific sections on quality assurance and provides guidance on selection of

digestion and analysis methods. Many of the recommendations in the Laboratory

Operations Guidelines are being incorporated as laboratory quality system

requirements for the NLLAP. This module should highlight those NLLAP requirements. 

When the NLLAP quality system requirements are finalized, a notice of their availability

will be placed in the Federal Register.

2.5.2 Facilities and Personnel Qualifications

2.5.2.1 Facilities—

These laboratory guidelines apply to fixed location, temporary, and mobile

laboratories. 

A laboratory must have the space, equipment, instruments, ventilation, utility

services, storage, safety equipment, and manuals necessary to accomplish Pb

analyses of paint, soil, and deposited dust. The facility should have restricted access

for security reasons and controlled access to sample preparation areas to reduce

contamination. Other recommendations are listed in the TSCA Good Laboratory

Practices Standards (U.S. EPA, 1989). Minimum recommendations for metals

laboratories include: 

` Appropriate area for sample receipt, processing, and storage (secured,

controlled temperature).

` A laboratory hood for digestion of samples that meets the requirements

specified in the Industrial Hygiene Ventilation Manual of the American

Conference of Governmental Industrial Hygienists (ACGIH, 1991).

` An adequate number of grounded electrical circuits that meet local electrical

codes and ensure stable electrical supply to instruments and data systems.

Uninterrupted power supplies may be needed in some areas to protect data

systems.

` Ambient temperature and humidity control adequate to insure reliable

operation of instrumentation and sample/digest stability.

` Cross-contamination control procedures to prevent sample contamination

and contamination of work areas. Controlled access to sample preparation
12

areas and other procedures to minimize sample contamination. Documentation of effectiveness of contamination control by use of surface wipe

samples.

` A glassware-cleaning facility with SOPs and monitoring requirements.

` Procedures for disposal of hazardous waste in compliance with local, state,

and federal regulations.

2.5.2.2 Personnel and Qualifications—

The laboratory management must provide technical and quality managers who

operate the laboratory in conformance with ISO Guide 25 (ISO/IEC Guide 25, 1990)

and the accrediting organization requirements. Following are the personnel and

minimum qualifications that are needed.

Technical Manager, or however named 

This individual must have a B.S. degree in Chemistry, or related field, with a

minimum of 3 years' nonacademic laboratory experience, two of which are in

metals analysis. This individual is responsible for the technical effort and must

be available to the analyst at the laboratory at least 50% of the normal work day. 

The technical manager may also serve as the inorganic chemistry supervisor.

Quality Manager, or however named

This individual must have a B.S. degree in a basic science and have at least

1 year of nonacademic analytical chemistry experience and training in statistics, or

4 years nonacademic analytical chemistry experience and training in statistics. 

Experience or knowledge of ISO Guide 25 is required. The quality manager should be

separated from the analytical chemistry operations. In some small laboratories, the

technical manager may also function as the quality manager, as long as this person is

not involved in the direct supervision of the lead analyst/technician doing the routine

sample analysis.

Inorganic Chemist, Spectroscopist, or however named

This individual must have a B.S. degree in Chemistry, or related field, with a

minimum of 1 year in metals analysis in a nonacademic laboratory. Training in

specific metals methods used in the laboratory must be documented; proficiency

in analysis must also be documented. This category includes the following

persons:
13

` Inductively Coupled Plasma-Emission Spectroscopist

Experience: 1 year minimum recommended (nonacademic)

Training: Satisfactory completion of a short course on Inductively Coupled

Plasma Emission Spectrometry (ICP-AES). An in-house training program is

acceptable.

` Flameless Atomic Absorption Spectroscopist

Experience: 1 year minimum recommended (nonacademic)

Training: Satisfactory completion of a short course on Graphite Furnace

Atomic Absorption Spectrometry (GFAA). An in-house training program is

acceptable.

` Flame Atomic Absorption Spectroscopist

Experience: 1 year minimum recommended (nonacademic)

Training: Satisfactory completion of a short course on Flame Aspiration

Atomic Absorption Spectrometry (FLAA). An in-house training program is

acceptable.

Analyst, Technician, or however named

Two years of technical education at the college level is recommended. This

individual must have documented training in specific metal methods used in the

laboratory and must have documented proficiency in performing assigned tasks. 

This category includes the following persons: 

` Inorganic Sample Preparation Technician

Experience: 3 months minimum recommended (nonacademic)

` Routine Sample Analyst (instrumentation)

Experience: 6 months minimum recommended (nonacademic)

The above staff must have documented training on instruments specific to the

laboratory and have demonstrated proficiency in these techniques. Junior staff, such

as analysts or technicians, must work under the direct supervision of a degreed chemist

in one of the "Chemist/Spectroscopist" categories. Junior staff may also work under the

supervision of the Technical Manager or a sample analyst/technician who has

performed successfully over a period of 3 years in the analysis of metals, using the

same technologies that will be used for the analysis of Pb-containing samples.

2.5.3 Quality Assurance Program

Quality assurance programs are required for laboratories that analyze paint, soil,

and deposited dust for Pb. The ISO Guide 25 (ISO/IEC Guide 25, 1990), the

internationally accepted quality system for testing laboratories should serve as the basis

for the laboratory quality system. There are several good general references for quality

assurance programs listed in the bibliography. The reference by Liabastre (Liabastre,
14

1992) is recommended as it addresses all aspects of quality assurance for

environmental assessment laboratories. The reference by Ratliff (Ratliff, 1990) is also

recommended. Information specific for laboratories that analyze paint, soil, and

deposited dust for Pb is located in the HUD Interim Guidelines (HUD, 1990) and in the

various other referenced publications.

2.5.3.1 The Quality System—

The laboratory must have a quality system documented in a quality manual. The

manual should document the policies and objectives of the quality system. The specific

program requirements are found in individual accrediting organization policies. The

major components of a typical quality system, which are listed below, should be

addressed and documented in a quality manual and in related supporting documents. 

The components are listed according to ISO Guide 25 headings (ISO/IEC Guide 25,

1990).

` QA management should be directed by a full-time employee with power to

oversee the situation, identify problems, and make corrections, while being

independent of the analyses. 

` A quality policy statement, including objectives and commitments by top

management.

` Organization and management structure of the laboratory, its place in any

parent organization, and relevant organizational charts.

` Relationship between management, technical operations, support services,

and the quality program.

` Procedures to control and maintain documentation of the quality manual and

related supporting documents.

` Job descriptions of key staff and reference to other staff.

` The introduction of new employees to the quality manual and the

requirement that all employees periodically review the manual.

` A documented training program for employees that includes site-specific

SOPs.

` Identification of the laboratory sign-off person for reports.

` Traceability of calibration standards to SRMs.

` Scope of the laboratory operation and services offered.
15

` Procedures for review of incoming work to assure adequate facilities and

staff. 

` Reference to the calibration, verification, and test procedures used.

` Procedures for handling calibration and test items.

` SOPs for sample log-in procedures.

` SOPs for sample preparation, including debris removal, substrate removal,

drying, grinding, sieving, and mixing.

` SOPs for sample and subsample identification, including digests and

extracts.

` SOPs for the preparation of working standards and calibration solutions.

` SOPs for digestion procedures, methods of analysis, and calibration

procedures.

 ` SOPs for major equipment calibration, reference standards used, and

maintenance of equipment.

` References to verification practices, including interlaboratory comparisons,

proficiency testing programs, use of reference materials, and internal quality

control schemes.

 

` SOPs for feedback and corrective action whenever testing discrepancies are

detected, or departures from documented policies and procedures occur.

` Arrangements for exemptions permitting departures from documented

policies/procedures as specified in SOPs. 

` References to procedures for dealing with complaints.

` References to procedures for protecting confidentiality of results.

 

` SOPs for data audit and review. 

` Quality system audits must be conducted to ensure that the documented

quality system is implemented as written.

2.5.3.2 Review of the Quality System—

The quality system requires frequent inspection and audits to ensure its

effectiveness. The following are recommendations for quality system audits.
16

` Quality system audits should be conducted at regular intervals by trained

and qualified staff to verify the system is implemented as written. 

Discrepancies found should be corrected, and any client whose reported

data are affected should be notified in writing immediately.

 

` The quality system should be reviewed at least once per year by

management to ensure its continuing suitability and effectiveness and to

introduce any necessary changes or improvements.

 

` All audit and review findings, and any corrective actions that arise from

them, should be brought to the attention of the Quality Manager and

resolved in a timely manner.

 

2.5.3.3 Quality Control—

The quality manual and related supporting documents must contain the following

sections on quality control:

Quality Control System

` QC procedures required by applicable federal or state environmental or

public health agencies should be listed, documented, and followed.

` A sample tracking system should be maintained. 

` Control chart data or equivalent should be maintained for each analytical

technique. See Handbook for SRM Users (Taylor, 1985) for

recommendations on control charting.

` Supervisory personnel should review the data calculations and QC results

(internal data review).

 

` Deviations or deficiencies in QC should be documented and reported to

management immediately.

` A documented corrective action plan should be implemented when analytical

results fail to meet QC criteria. 

` QC data should be retrievable for all analytical results.

Calibration and Quality Checks

` Standard calibration curves should be prepared to adequately cover the

expected concentration ranges of the samples and the expected "action

levels" of Pb (HUD, 1990).
17

` Standard calibration curves should be prepared using at least three

standards and one blank, unless otherwise specified by the method.

 

` New calibration curves should be prepared whenever out-of-control

conditions are indicated and after new reagents are prepared and used.

` Method detection limits should be determined and documented (40 CFR

136, Appendix B).

` The laboratory should ensure the quality of results by implementing and

reviewing quality checks, as appropriate, but not limited to:

` Internal quality control charting based upon statistical techniques. This

is most useful for identifying trends and out-of-control incidents.

` Regular use of standard reference materials and certified reference

materials as primary reference materials. 

` Participation in the ELPAT Pb-proficiency testing program.

` Replicate testings using the same or different methods.

` Retesting of retained items as needed.

SOPs

` The QC procedures (SOPs) should be specific to each test technology and

matrix addressing the following:

` Reagent and method blanks

` Glassware cleaning

` Trip and field blanks

` Sampling and subsampling

` Replicate/duplicate analysis

 

` Spiked and blank sample analysis

` Blind samples 

` Quality control samples

` Control charts
18

` Calibration standards

 

` Reference samples and SRMs

` Internal standards 

2.5.3.4 Quality Control Practices—

The laboratory quality control program should include the continual evaluation of

its performance (system process control) for each matrix, which includes the

determination of accuracy and precision. One possible method used for laboratory

system process control is the use of control charts to monitor the performance of a

specific QC sample. Control charts should specify warning and action limits. In the

absence of a statistically sufficient data base to determine the necessary frequency for

QC samples, the laboratory should default to the use of a set frequency for QC samples

stated in its analytical standard operating procedure.

Quality control practices can be broken down into those processes that are

affected by the instrumentation and those that are related to the sample matrix. The

following recommendations for matrix-based quality control practices applicable to AA

or ICP-AES should be used in the absence of laboratory-based process control data.

Precision and Accuracy Determinations

Accuracy studies are performed to determine how close a measurement comes

to an actual or accepted reference value. Accuracy can be expressed as percent

recovery and evaluated by analysis of matrix spike samples. A matrix spike is an

aliquot of a sample fortified (spiked) with a known quantity of the analyte of interest and

subjected to the entire analytical procedure. The spike must be prepared from a

standard stock, which is different from the calibration standard stock, and should have a

Pb concentration that is within the range of the sample to be run.

Precision is evaluated by the reproducibility of analyses. Precision is commonly

expressed as standard deviation or relative percent difference (RPD) and can be

evaluated by the analysis of replicate samples. Replicate sample analyses are one or

more additional analyses on separate portions of a given sample in order to assist in

the evaluation of method variance. Most commonly, two replicate analyses (defined as

a duplicate analysis) are performed.

In the analysis of soil, dust (vacuum), and paint chips matrices, samples may be

too small and difficult to homogenize and split in order to obtain samples for matrix

spike evaluations or replicate analysis. For these sample matrices, the laboratory

should select alternate QC options, such as the analysis of duplicate laboratory control

samples per batch.
19

Paint Chips, Soil, and Vacuumed Dust Samples.

Accuracy determination. Matrix spiked samples should be analyzed with a

minimum frequency of 5% of the samples for each matrix, per batch of samples

(samples processed at a single time). If there are fewer than 20 samples in a batch, at

least one spiked sample for each matrix per batch should be analyzed.

Precision determination. Replicate (duplicate) samples should be analyzed with

a minimum frequency of 5% of samples for each matrix per batch of samples. If there

are fewer than 20 samples in a batch, at least sample for each matrix per batch should

be analyzed. In the event the analyte is not detected in the sample, replicate matrix

spike samples may be analyzed.

Dust Wipe Samples—Accuracy and Precision Determinations.

When analyzing wipe samples, method spike samples are prepared using blank

collection media and analyzed with a minimum frequency of 5% of samples for each

matrix per batch of samples. If there are fewer than 20 samples per batch, at least 1

method spike/spike duplicate set should be run per batch. The matrix samples are to

be prepared using a Pb-based paint NIST SRM applied directly to the wipe. It is

recommended that the client submit blank wipes representative of the lots to be used in

the field for lead contamination analysis prior to field sampling.

Method Blanks

When using methods requiring sample pretreatment not performed on calibration

standards, a method blank containing all reagents and subject to all preparation steps

shall be processed and analyzed along with the samples. Method blanks should be

analyzed with a minimum frequency of 5% of the samples for each matrix per batch of

samples. If there are fewer than 20 samples in a batch, at least 1 method blank for

each matrix per batch should be analyzed. The use of method blanks provides a

measurement of laboratory and/or reagent contamination. Method blanks are not to be

used to correct sample results.

External Reference or Laboratory Control Sample Analysis 

At least one reference or laboratory control sample (LCS) should be analyzed

with each matrix per batch of samples with a minimum frequency of 5%. If there are

fewer than 20 samples per batch, then at least 1 LCS should be run per batch per

matrix type. The concentration of the LCS should be within the working range of the

method and should not require extensive pretreatment, dilution, or concentration prior

to analysis. Sources of these samples include but are not limited to: NIST Standard

Reference Materials, commercially available certified reference samples, or samples

prepared from different sources of analyte than calibration standards and whose
20

concentrations were determined using definitive methods. If available, all these

reference materials shall be NIST traceable.

Recommended QC Sample Criteria

The following recommendations for analytical instrument quality control practices

should be used in the absence of laboratory-based process control data.

Acceptable performance limits for analytical instrumentation, as well as each

method, should be established based upon the continuing statistical evaluation of the

data generated by the analysis of quality control samples, unless specific minimum

acceptance limits are established by the method. The laboratory's calculation

procedures for statistically derived acceptance limits should be documented. Some

methods have listed acceptance criteria for applicable analytes based upon determinations by a single laboratory, the compilation of data from many laboratories, or

limits that are assumed or expected. These limits may be too broad to define accurate

acceptance criteria for routine use. These limits are best used as guidelines during the

initial phases of method use and are superseded when the laboratory has collected

sufficient self-generated data for proper statistical evaluation.

In the absence of sufficient data for the determination of QC sample frequency

and acceptance criteria, the following minimum QC sample frequencies and

acceptance limits are required (where applicable) for analytical SOPs employing AA or

ICP-AES instrumentation:

QC sample Frequency Acceptance limits

Initial calibration Once per run after Within ±10% of known

verification (ICV) calibration value

Initial calibration blank Once per run at the Absolute value not more

(ICB) beginning of run than 20% of the

regulatory limit or level

of concern

Continuing calibration Before and at the end of a Within ±10% of known

verification (CCV) sample run, as well as value for ICP or FLAA;

every 10 samples within ±20% for GFAA

Interference check sample Beginning and end of each Within 20% of known

(ICS) run or twice every 8 hr value

Continuing calibration After each ICS and CCV Absolute value not more

blank (CCB) than 20% of the

regulatory limit or level

of concern
QC sample Frequency Acceptance limits

21

Laboratory control sample 1 per 20 samples or batch Within ±20% of known

(LCS) (5%) value

Matrix spike 1 per 20 samples or batch Within ±25% of known

(5%) value

Duplicate sample 1 per 20 samples or batch Within ±25% relative

(5%) percent difference

(RPD)

Method blank 1 per 20 samples a batch Absolute value not more

(5%) than 20% of the

regulatory limit or level

of concern

A detailed recommended analysis protocol is listed in Section 2.5.14.

2.5.4 Required Standard Operating Procedures (SOPs)

All methods, including sample collection, subsampling, digestion, and analysis,

must have laboratory-generated Standard Operating Procedures (SOPs). There are no

standard methods from EPA or other organizations/agencies with published validations

for the analysis of Pb in paint and deposited dust matrices. There is a standard method

for digestion of soils (U.S. EPA SW 846 Method 3050). Modifications of methods must

be documented in revised SOPs. Minor modifications (for example, the use of more

acid) should be specified in SOPs and include the reasons to make such adjustments. 

No deviations should be permitted during routine sample analysis beyond those limits

specified in the laboratory SOP, but deviation within stated limits is acceptable. 

Guidelines for the preparation of SOPs have been published by the EPA Office of

Solid Waste (U.S. EPA, 1990c). Elements of SOPs are listed in the companion EPA

report on laboratory practices (U.S. EPA, 1992b).

2.5.5 Field Sampling of Paint Films, Soils, and Dust Wipes, Including Vacuumed

Dust

 Although the laboratory staff is often not involved in field sampling, they need to

understand the process in order to advise the client, if asked, and to better understand

the heterogeneity of samples submitted to the laboratory. The HUD Interim Guidelines

(HUD, 1990) provide a general summary of sampling requirements for Pb from abatement projects. The companion EPA report on laboratory practices also provides a

summary of field sampling recommendations (U.S. EPA, 1992b). The laboratory

should provide guidance only in the form of a written SOP or a copy of specific

sampling guidelines.
 * Use of a riffle box to separate coal and coke is described in ASTM Method (D5).

22

2.5.6 Sample Preparation Steps Prior to Analysis (Subsampling).

This section covers the handling of the sample after it is received from the field

and prior to digestion. Cleanup activities (removal of rocks, substrate, hair, etc.) and

subsampling or aliquoting of the bulk sample into uniform portions suitable for analysis

are also covered. Subsection 2.5.7 gives recommendations for sample tracking and

storage.

2.5.6.1 Solids—General Considerations—

Particle size distribution, debris, and stratification of solid samples is a major

problem. The following general considerations apply to all solid samples. 

` Samples must be examined for debris, such as hair, paper clips, pins, and

insects, prior to subsampling the sample. Debris should be removed with

tweezers or by screening through a course #4-mesh (4 to 7 mm) sieve. 

` Samples of dust or finely ground paint or soil are subject to stratification from

vibration in the laboratory. Therefore, thorough mixing is essential prior to

removing an aliquot for analysis. 

` A representative sample must be obtained. A device such as a "riffle" box,

or equivalent, should be used for separating and allocating fractions of dust

or soil that have been ground to a #10-mesh (1.9 mm) and sieved. A riffle

box randomly aliquots one-half of the sample to one side and one-half of the

sample to the other. Several passes may be necessary to reach usable

sample sizes for digestion.*

` Humidity control is very important in sampling of solids, particularly if results

are expressed on a weight basis. Oven drying at 105` C to a constant

weight is recommended.

2.5.6.2 Wipe Samples—

The handling of wipes in the laboratory must be detailed by an SOP. Wipes are

used to collect deposited dust over a defined surface area. In most cases, the Pb

content in the wipe material is unknown and appears to vary from lot to lot and among

sources. The pickup efficiency (ability to pick up and retain dust on the wipe material)

and the digestibility properties are also unknown. Research on the development of

standardized wipes is in progress. Until such time as some "standardized wipe" is

developed, the laboratory must perform the following tests on each type of wipe

submitted. 
23

` Determine the Pb background level in the "blank" wipe submitted with the

samples. Ideally, Pb background levels of wipe samples should be determined prior to sample collection. If the background level is greater than 5 μg

Pb per wipe, blank correction may be necessary. Blank correction can be

used if the blank is < 20% of the regulatory limit or level of concern. If blank

correction is used, it must be documented on the report. It should be noted

that blank values of 5 μg per wipe are insignificant at HUD clearance

recommendations of 200 μg per wipe collected over a 1 sq ft area.

 

` Perform a recovery study of a spiked wipe (extractable Pb) using the

laboratory standard digestion technique. The digestion technique does not

have to destroy wipe fibers (total Pb), but it should be able to digest Pb from

dust deposited on the wipe (extractable Pb). 

Results should be expressed per wipe or per area sampled. If the area is less

than 1 sq ft, results should be corrected and reported as μg Pb/sq ft.

2.5.6.3 Paint Chips—

Appropriate steps must be taken to ensure uniformity of the sample before

subsampling. The presence of "substrate" compromises the results, particularly if the

results are presented on a weight basis. The handling of paint chips must be covered

by an SOP. Because paint chips containing substrate present special problems, the

following should be addressed: 

` Attempts should be made to remove the paint from substrate. If the paint

cannot be removed from the substrate, the analytical report must include an

annotation that results may be invalid. Substrate contamination of paint

must be noted because large amounts of nonlead containing substrate will

produce low-Pb concentrations and may lead to false negative results.

Paint chips relatively free of substrate should be handled as follows:

` Cut paint chips into small pieces with scissors or a knife.

` Grind up the pieces of paint chips into a powder with a mortar and pestle or

other nonmetal contaminating material to improve digestibility. Paints with a

high latex content may not be suitable for grinding due to their tendency to

form "gummy" residues.

2.5.6.4 Dust-Vacuumed Samples—

There are no defined procedures for preparation of vacuumed dust samples. An

SOP must be developed covering the steps listed below.
24

` Dust samples should be sieved (#10 mesh, 1.9 mm) to remove debris

(metal, glass, hair, pins, etc.) prior to digestion because this debris is not

dust.

` Dust samples must be subjected to humidity control. If dust is moist, it

should be dried in an oven at 105` C to a constant weight. Crosscontamination during drying can be reduced by placing dust samples in

covered drying bottles. 

2.5.6.5 Soils—

The handling of soil samples must be covered by an SOP that addresses:

` Screening to remove debris, including metal, glass, plant material, rocks,

plaster, and bricks. If large paint chips are present in the soil, these should

be removed and digested separately.

` Drying of the soil at 105` C to a constant weight to control for variable

moisture content.

` Grinding to a fine mesh (#10 mesh) to aid digestion.

` Thorough mixing prior to analysis to avoid stratification.

2.5.7 Sample Tracking and Storage

A sample tracking system must be detailed in an SOP and referred to in the QA

manual. A subsampling system of unique numbers must be used for all digests and

dilutions of the original sample so that original sample identification is not lost. If

computer log-in procedures are used, the sample log-in procedure must include hard

copy backup of computer log-in records. Although a legal chain of custody is not

usually required, a client may demand it in some cases that may involve potential

litigation. 

The SOP must detail the specifics for storage of unused samples during the

analysis cycle and after completion of analysis. Digests can be kept for 2 to 4 weeks,

as long as digest volumes are monitored gravimetrically for evaporation loss. Holding

times for matrix samples are not a problem. It is recommended that the laboratory

establish an automatic discard date for digests and samples, such as 90 days after

reporting to the client, unless contacted by the client.

The requirements for storage of samples and digests include:

` Secure storage in a locked or controlled-access area.
25

` Uniform environmental conditions must be maintained, such as a cool, dry

storage area.

` Storage of digests require special conditions. Fluid loss in digests by

evaporation must be monitored gravimetrically. 

2.5.8 Sample Digestion Procedures

At this time, there are no standard EPA-approved digestion methods for paint

and dust matrices. EPA SW-846 Method 3050 is approved for soils, but not necessarily

for analysis of Pb in soils contaminated with paint chips. There are three basic sample

digestion techniques that have been applied, often with some modification, to digest

paint chips, dust (wipes and collected dust), and soil samples. These methods are

outlined below and cited in Section 2.5.10. However, little published information is

available to document the suitability of these digestion methods.

` Dry ashing, followed by wet digestion with HNO or HNO /H O 3 3 22

` Wet digestion using a hot plate with HNO or HNO /H O 3 3 22

` Microwave digestion with HNO , HNO /HCl, or HNO /H O 3 3 3 22

Dry ashing is not recommended because it is difficult to control and has the

possibility of uneven heating and splatter/cross-contamination of samples. Therefore

"wet digestion" techniques are preferable. "Wet digestion" techniques using HNO3

alone are not generally recommended because digestion may be incomplete. Wet

digestion techniques, such as U.S. EPA SW-846 Method 3050, a validated method for

soils, are suggested and may be suitable for digestion of most samples. But this

method has not been validated for other matrices. NIOSH Method 7082 is also suitable

for digestion of dust samples. Perchloric acid has also been used in combination with

nitric acid with acceptable results. However, since the use of perchloric acid requires

special safety precautions (i.e., a perchloric acid hood), it is generally not

recommended.

Research is currently underway to develop a standard digestion procedure that

would work with all matrices using 200-250 mg of sample. The ASTM has prepared

draft wet digestion methods for wipes, dust, soils, and paint chips, which are currently

undergoing review and testing. Digestion acids must be chosen with analytical

instrumentation in mind because of incompatibility of HCl with GFAA instrumentation. 

Whatever digestion technique is used, it is recommended that the digest be filtered or

centrifuged prior to instrumental analysis. The specified digestion procedure must be

documented in an SOP.
26

2.5.9 Instrumentation

There are three general types of instrumentation suitable for analysis of Pb in

paint, soil, and dust matrices. These are listed below and are available from a variety

of vendors in many different configurations. 

2.5.9.1 Atomic Absorption Spectrometry Using Direct Flame Aspiration—

This instrumentation, which is widely available with and without autosamplers,

has adequate sensitivity for most samples, depending on dilution volumes used in the

digestion process. Following are characteristics of Atomic Absorption Spectrometry

Using Direct Flame Aspiration (FLAA):

` Instrument detection limits: Instrument detection limits are adequate for

most samples, but are the highest of the three techniques considered in this

guide. Since direct aspiration is required, a minimum of 5 mL of digest is

needed for aspiration and measurement of a stable signal.

` Principal interference: Light scattering and molecular absorption by matrix

components are common for measurements near detection limit and can

cause a false positive signal. They can best be corrected using methods

such as a continuum source or Zeeman background correction schemes. 

Correction using alternate nonabsorbing Pb lines is possible, but not optimal. 

Matrix enhancement, or suppression of the Pb absorbance signal, is

possible at all concentration levels and can be corrected by using the

method of standard additions.

` Cost: Initial instrument cost is low and consumables, such as acetylene gas,

are inexpensive.

` Sample throughput: Sample throughput is good using either autosamplers

or manual aspiration and can be several samples per minute.

` Maintenance and potential downtime: Routine maintenance is limited to

periodic cleaning of the aspirator, mixing chamber, and burner, as well as

external optics as necessary. Of the three methods, maintenance and

potential downtime is lowest.

` Principal Pb lines: The 283.3-nm line is preferred because of less molecular

absorption and scattering. The 217.0-nm line, however, is more sensitive

and can be used if a continuous source background correction is employed.

` Range of analysis: The linear range of analysis is approximately two orders

of magnitude, from about 0.2 μg Pb/mL to 20 μg Pb/mL, but can be

extended by rotating the burner head.
27

` Potential problem areas: The method detection capabilities are borderline

for wipes below HUD "Clearance" levels. For such samples, the 217.0-nm

line and background correction must be used.

2.5.9.2 Atomic Absorption Spectrometry Using the Graphite Furnace—

This instrumentation is widely available and is the most sensitive technique of

the three techniques. Throughput is good with autosamplers and sample size requirements are very small. The following are characteristics of Atomic Absorption

Spectrometry Using the Graphite Furnace (GFAA):

` Instrument detection limits: Detection limits are the lowest of the three

instrumental techniques. Because only 20 μL of sample is used for analysis,

digest volume requirements are the smallest (10-25 μL). If the laboratory is

also involved with blood Pb determinations, GFAA is the instrumentation of

choice. 

` Principal interference: Light scattering and molecular absorption by matrix

components are common for most measurements and can cause a false

positive signal. They can best be corrected by methods such as a

continuum source (Deuterium Arc) or Zeeman or Smith-Hieftje background

correction schemes. Matrix enhancement or suppression of the Pbabsorbance signal is often significant and can be corrected by using the

method of standard additions. Matrix modifiers, such as magnesium nitrate,

lanthanum nitrate, palladium, or ammonium dihydrogen phosphate, minimize

loss of Pb during the sample charring step and allow higher charring

temperatures. This also minimizes, but does not eliminate, matrix

enhancement or suppression effects. Chloride arising from the use of HCl in

a digestion can cause significant interferences in GFAA.

` Cost: Initial instrument cost is intermediate. Maintenance and consumable

costs are significant, since the graphite furnace tubes must be replaced

approximately every 500 firings and argon gas must constantly flow through

the system to prevent oxidation of the graphite.

` Sample throughput: Autosamplers are required to increase precision and

throughput. Manual sample introduction is tiresome and often irreproducible. Throughput is approximately one sample every 2 to 3 min.

` Maintenance and potential downtime: The primary difference between

maintenance of GFAA and FLAA is the alignment and cleaning of furnace

components of the former. Because of the complexity of some graphite

furnace systems, downtime may be greater than with FLAA.

` Principal Pb lines: The 283.3-nm line is preferred because of less

interference. The 217.0-nm line, however, is more sensitive and may be

used as needed, provided the interference and noise are not severe.
28

` Range of analysis: The linear range of analysis for an intermediate sample

size is from about 0.001 μg Pb/mL to 0.1 μg Pb/mL, but can be varied by

adjusting sample size and dilution.

` Potential problem areas: Matrix interference and contamination.

` Advantages: This instrumentation is widely available and is the most

sensitive technique of the three. Throughput is good with auto-samplers and

sample size requirements are very small. 

2.5.9.3 Inductively Coupled Plasma Emission Spectrometry—

This instrumentation is available in many laboratories and offers the advantage

of simultaneous multielement determinations. Sensitivity for Pb is intermediate, but

adequate for all Pb matrix samples. Sample volume requirements are moderate

because the digest is aspirated into the plasma torch.

` Instrument detection limits: Instrument detection limits, which are similar to

FLAA, are adequate for most samples, but may present analysis difficulties

at the lowest level of wipe samples. Because the direct aspiration rate of

inductively coupled plasma emission spectrometry (ICP-AES) is less than

FLAA, less sample is required. If other elements are desired in

environmental samples, this is the instrumentation of choice.

` Principal interference: Spectral interferences caused by radiation from lines

of other elements present in the sample are most common and can be

corrected by several methods. Background correction can be performed by

selecting wavelengths near the Pb line, or an alternate Pb line can be used. 

It is important to include an interfering element check sample that contains

high levels of suspected elements (aluminum, titanium, chromium, calcium,

or iron).

` Cost: Initial instrument cost is high, but major consumable cost is only argon

gas, unless the instrument is operated incorrectly and the torch is destroyed.

` Sample throughput: Sample throughput is intermediate between FLAA and

GFAA. Samples that are directly aspirated require a longer period for

equilibration and washout. Throughput is typically slightly less than one

sample per minute.

` Maintenance and potential downtime: Maintenance costs are the highest of

all the instruments discussed because of the complicated design of ICP-AES

instruments and the requirements for critical alignment of components.

` Principal Pb lines: Usually the 220.35-nm line is used, although an alternate

line is at 217.0 nm.
29

` Range of analysis: The linear range of analysis for the 220.35-nm line is

from about 0.2 μg Pb/mL to 3,000 μg Pb/mL.

` Potential problem areas: Spectral interferences from high levels of other

metals and insufficient washout of the mixing chamber can occur after the

analysis of a sample of high Pb concentration. 

` Advantages: This instrumentation is available in many laboratories and

offers the advantage of simultaneous multielement determinations. 

Sensitivity for Pb is intermediate, but adequate for all Pb matrix samples. 

Sample volume requirements are moderate because the digest is aspirated

into the plasma torch.

2.5.9.4 Other Instrumentation—

In addition to these instruments, there are others that are not currently

recommended. X-ray fluorescence (XRF) is currently being evaluated for laboratory

use and may be suitable. However, sample preparation steps, including sample loading, can significantly affect precision and bias. On the other hand, the results are not

affected by inclusion of substrate with the sample. Inductively Coupled Plasma-Mass

Spectrometry (ICP-MS), although a powerful and sensitive technique, is not recommended at this time because of a lack of need for this level of instrumentation

sophistication and costs. Anodic stripping voltametry may be suitable, provided that the

method is compatible with digestion techniques. Methods using spectrophotometric

instrumentation for Pb, such as the dithizone method, are not recommended because

of the potential for contamination and interference. The latter method also may not be

compatible with digestion procedures.

2.5.10 Analytical Methods

This section gives a list of published methods and discusses calibration

standards applicable to paint, soils, and deposited dust matrices. References from

agencies of the Federal Government can be obtained from the National Technical

Information Service (NTIS), (703) 487-4650.

2.5.10.1 Lists of Methods—

AOAC 5.009 (1984) - Lead in Paint Using Direct Aspiration Atomic Absorption.

ASTM D-3335-85a - Test Method for Low Concentrations of Lead,

Cadmium, and Cobalt in Paint by Atomic Absorption Spectrometry (direct

aspiration).

ASTM D 3618 - Test Method for the Detection of Lead in Paint/Dried Paint Films.
 * These methods do not include a digestion technique and are for digests of Pb

prepared by one of the digestion techniques listed above.

30

U.S. EPA Reference Method for the Determination of Lead in Suspended

Particulate Matter Collected from Ambient Air (40 CFR Part 50, Appendix G)

NIOSH 7082, Lead in Air Collected on Cellulose Ester Filters. Nitric

acid/hydrogen peroxide hot plate digestion followed by direct aspiration atomic

absorption at 283.3 nm.

NIOSH 7105, Lead in Air Collected on Cellulose Ester Filters, Nitric acid/

Hydrogen Peroxide Hot Plate Digestion Followed by GFAA.

NIOSH 7300, Elements in Air Collected on Cellulose Ester Filters, Nitric/

Perchloric Acid Hot Plate Digestion Followed by ICP-AES at 220.4 nm. 

*U.S. EPA SW-846 Method 7420, Pb - Atomic Absorption, Direct Aspiration

(U.S. EPA, 1990c).

*U.S. EPA SW-846 Method 7421, Pb - Atomic Absorption, Graphite Furnace

(U.S. EPA 1990c).

*U.S. EPA SW-846 Method 6010A, Metals - Inductively Coupled Plasma

Emission Spectroscopy (U.S. EPA 1990c).
 * These methods are general digestion techniques for the matrices listed. The mild

conditions used in SW-846 methods must be evaluated for their efficiency in digesting

these matrices. They must be combined with an analytical method such as the EPA

SW-846 Methods 6010A, 7420, or 7421 for completion of analysis.

31

*U.S. EPA SW-846 Method 3050A - Acid Digestion of Sediments, Sludges and

Soils (Metals) (U.S. EPA 1990c).

*U.S. EPA SW-846 Method 3051 - Microwave Assisted Acid Digestion of

Sediments, Sludges, Soils and Oils (Metals) (U.S. EPA 1990c).

In addition to these cited methods, the ASTM E36 subcommittee is working on

several standard methods for Pb. These include GFAA, FLAA, and ICP-AES. These

draft methods include digestion techniques for paint, dust, wipes, and soil, and use hot

plate wet digestion techniques or microwave digestion methods. These draft methods

are not yet available for distribution.

2.5.11 Calibration

2.5.11.1 Primary Standards—

Primary standards are solutions of standards that are traceable to aqueousbased SRMs from NIST and that must be used for instrument calibration. The preparation of primary standards must be detailed in an SOP. The SOP must detail the

traceability of the primary standard to primary calibrant SRMs from NIST.

The NIST aqueous 10,000 ppm Pb (in 10% HNO ) SRM is suitable for calibrant 3

material and must be used to check laboratory working standards. The SRM is

available as SRM 3128 (50 mL of a 10 mg/mL solution in 10% HNO ). Matrix-based 3

SRMs are not primary standards and are not suitable for instrument calibration.

2.5.11.2 Working Standards—

Stock primary standards must be prepared from material traceable to NIST SRM

3128. These stock standards are stable, but are subject to evaporation and loss of Pb

to the container wall. The possible loss of solvent can be monitored by weighing the

stock solution at regular intervals. The preparation of stock and working standards,

including storage conditions, must be detailed in an SOP. Acids used in standards

must match the acids used in the matrix. Purchased stock standards must include

certifications that standards are traceable to SRM-3128.

Working standards should be prepared from stock primary standard solutions of

1000 to 10,000 ppm Pb. Working standards are used for initial calibration of the

instrument and to verify the calibration at intervals dependent on the instrumental

method. The recommended minimum intervals are at the beginning, midpoint, and at
32

the end of a batch of samples (usually 20 samples) run on any particular day. Results

that are reportable must be in the calibration range.

2.5.11.3 Matrix-Based Quality Control Samples—

A variety of matrix-specific materials (LCS) contain Pb and can be used for

quality control samples. These internal QC samples must be independent of the

instrument calibrant and used only to monitor the performance of the entire process,

including the digestion step.

2.5.11.4 SRMs from NIST—

NIST prepares a variety of SRMs. These reference materials are rigorously

characterized and analyzed by definitive methods. They are expensive and are not

intended to be used for routine quality control. They are intended to be used in the

development and validation of methods and as a real-world tool to evaluate method

performance. Examples of NIST SRMs available for Pb-based matrices are listed in

the table below. Certificates are available from NIST.

SRM Description and date Certified Pb value

1579a Powdered Pb-based paint, Feb. 3, 1992 11.995% ± 0.031

— Powdered Pb-based paint (in pro a gress) 4.0%

— Powdered Pb-based paint (in pro a gress) 0.5%

1648 Urban particulate matter, Nov. 16, 1978 0.655% ± 0.008

2704 Buffalo River sediment, July 9, 1990 161 μg/g ± 17

2709 Baseline agricultural soil, Oct. 16, 1992 18.9 μg/g ± 0.5

2710 Highly contaminated soil, Oct. 16, 1992 5532 μg/g ± 80

2711 Moderately contaminated soil, Oct. 16, 1992 1162 μg/g ± 31

2579 Lead paint film on Mylar sheet, set of 5, July 3.53 mg/cm ± 0.24

7, 1992 1.63 mg/cm ± 0.08

2

2

1.02 mg/cm ± 0.04 2

0.29 mg/cm ± 0.01 2

< 0.0001 mg/cm2

 These NIST SRMs are under development. a
33

2.5.11.5 Other Reference Materials—

Reference materials from other sources are available, but they are not NISTcertified and may be less well-defined and characterized. However, they may be

suitable for use as internal quality control materials. 

There are three CRADA certified materials available. They are labeled: "This

product was verified for accuracy and stability under a cooperative research and

development agreement (CRADA) with the U.S. Environmental Protection Agency." 

They are manufactured by Resource Technology Corporation, Laramie, Wyoming, and

are available from Fisher Scientific. These reference materials have also been certified

by A2LA. These materials are not characterized like SRMs and cannot be used as

substitutes for NIST SRMs. ELPAT samples may be available for use in evaluation of

method performance (call 703-849-8888).

2.5.12 Reports and Record Management

Reporting and record-keeping requirements are outlined in the HUD Interim

Guidelines (HUD, 1990).

"All information relating to field sample analysis and QA/QC sample analysis,

along with information on laboratory facilities, equipment, methods, and

procedures must be documented by the laboratory, so that an analytical event

can be recreated for an audit or investigation."

The HUD Interim Guidelines (HUD, 1990) recommend that the following general

categories of records should be kept.

` Cover page information including methods, dates, instruments, digestions,

and sign-offs by the laboratory director.

` Sample information including identification, blanks, QC samples, sample

weights, dilution factors, and batch identification.

` Results of initial precision and accuracy runs.

` Results of calibration including sources of standards and detection limits.

` Results of blanks including type of blank and any corrections used.

` Results of calibration verification checks.

` Results of tests for accuracy and precision.

` Data reduction and reporting procedures including data calculations, outliers,

and data archiving.
34

More details are given in the HUD Interim Guidelines (HUD, 1990). The client

may have more specific needs, so the laboratory should be prepared to provide that

data.

There are no regulatory requirements for record retention for these matrices. The

HUD Interim Guidelines and NLLAP requirements suggest 10 years. Record-retention

policies must be established with the client, with the realization that there may be future

regulatory requirements.

2.5.13 Proficiency Testing and Data Quality

2.5.13.1 Proficiency testing—

Laboratories must demonstrate proficiency in the Environmental Lead

Proficiency Analytical Testing (ELPAT) Program to be "recognized" by NLLAP. (See

footnote on p. xi.) Laboratories may participate in this program independently without

participating in an NLLAP-recognized accrediting organization program. 

Note: Proficiency testing (PT) matrix materials, including ELPAT samples, are

not to be used for instrument calibration or primary standards. These materials have

not been subjected to rigorous characterization for their target concentrations. PT

materials and SRMs that are fine powders are subject to significant stratifications from

vibration in the laboratory. Therefore, thorough mixing is essential prior to removing an

aliquot for analysis.

2.5.13.2 Rejection Criteria and Corrective Action—

The following guidelines are recommended as minimum rejection criteria that

require corrective action prior to release of data. Data should be thoroughly evaluated,

even if one of these criterion is out of range, and corrective action taken prior to release

of data.

` Within day or intra-day variation of the calibration curve as measured by

CCV is greater than ±10%. 

` Any blank that exceeds 20% of the regulatory limit or minimum limit of

concern.

` Spike recoveries of extractable Pb less than 75% or greater than 125% at

the midrange concentration.

` Matrix-based quality control or check sample (also called control or

laboratory control sample) outside 80-120% of stated value.
 * Calibration requirements are both instrument and method specific. SOPs for

specific analytical methods should be followed.

35

` Unacceptable precision (> ±25% RPD) of duplicate samples (two aliquots of

the same bulk sample carried through the entire procedure.) Precision is

based on the concentration of the sample and the method detection limit.

Corrective actions include reanalysis of QC check samples. If these QC

samples are out of range, then repeat entire analysis, including recalibrations and all

QC samples. 

2.5.14 General Recommendations, Analysis Protocol

The analysis protocol for a digest may be specified in individual method citations. 

Individual laboratory SOPs must provide specifics. The quality control program should

be based on the laboratory's continuous evaluation of its performance (system process

control). In the absence of laboratory generated process controls, the

recommendations in Section 2.5.3.4 should be used regarding frequency of blanks,

calibration, and controls. 

Since Pb is ubiquitous in the environment and in the laboratory, rigorous steps

must be specified in an SOP on how contamination control is to be achieved during

subsampling, digestion, and analysis. Cross-contamination must be documented by

monitoring of surfaces, glassware, and reagents. A protocol to reduce crosscontamination from Pb is described by T. J. Murphy (Murphy, 1976).

The following are general recommendations for an analysis protocol:

` The instrument should be calibrated daily with an aqueous working standard

traceable to an aqueous-based SRM (SRM 3128).

` Stock working standards for Pb (10,000 ppm) are stable. However,

evaporation should be monitored by periodic weighing to document and

correct for evaporative losses. Sealed containers help control evaporation

loss; however, loss to container walls is possible.

` The daily calibration curve should consist of one initial calibration blank and

at least three standards covering the concentration range of the samples.*

` The 3-standard calibration curve should have a correlation coefficient of at

least 0.995.

` The calibration curve should be verified by the periodic use of continuing

calibration blank and continuing calibration verification samples throughout 

the run.
36

` The LCS (matrix-based and near the midpoint of the calibration curve)

should be ±20% of stated value.

` One spiked matrix sample or duplicate matrix sample should be included per

batch of up to 20 samples. A suitable duplicate matrix sample would be split

digest samples because duplicate field samples cannot be collected.

` Instrument drift should be documented and corrected using CCV and CCB

according to the method SOP.

` Interference check samples (ICS-AES) for ICP instrumentation (background

shifts and interelement interference) should be determined prior to performing analyses to correct for potential interferences from components in the

sample matrix. The ability of the instrument to measure lead in the presence

of potential interference should be determined at the beginning, during the

run, and after the sample is run. Correction factors should be applied, if

available, on the specific ICP-AES instrument in use. 

` Background correction for GFAA using simultaneous methods (e.g.,

Zeeman, Smith-Hieftje, Deuterium Arc) should be used at all times. 

` Matrix modifiers, used in GFAA, should be verified to be free of Pb

contamination.

` Matrix-based SRMs at action levels, if available, should be used to verify

working standards and CRMs at monthly intervals.

` All samples exceeding the upper limits of the calibration range should be

diluted to fit within the calibration range. 

` The SOP should provide for a means to control carryover following samples

with high concentrations (memory effect). Reruns of samples following a

high sample is recommended.

` The SOP should provide for possible resampling of the submitted sample if

the result is at or above an "action level" to confirm a "positive" result.

` Sample analysis priorities: Although the following scenario has been

suggested, consideration should also be given to development of an

analysis protocol using randomization of samples and blanks to minimize

bias.

` Assemble all samples, standards, blanks, and background samples.

` Analyze those samples expected to contain Pb first.
` If a significant amount of Pb is found, analyze blanks and background

samples to determine if there is contamination.

` Blank collection media (wipes) should also be analyzed to determine the

background Pb levels.

` QC data should be control charted in order to monitor trends and

QC excursions. The SOP must specify what is done in the event of

unacceptable trends or excursions.

Table 1 shows the recommended process quality control blanks and control

materials to be included in each batch. Table 2 shows the recommended instrumental

QC standards and their specifications.

TABLE 1. QUALITY CONTROL SAMPLES AND PROCESS CONTROL

QC samples Definition Frequency

Method blanks Type 1 water—digest as a 1 per 20 samples, a

sample with addition of all minimum of 1 per batch

reagents. Should reflect the

maximum treatment given any

one sample within the batch.

Spiked samples A portion of a sample is 1 per 20 samples per

fortified with all the target matrix type, a minimum of

analytes before preparation 1 per batch

and analyzed independently.

Spiked sample A portion of a same sample 1 per 20 samples per

duplicates used for the spiked sample is matrix type, a minimum of

fortified with all the target 1 per batch

analytes before preparation.

Reference material A material of known 1 per batch of samples

(standard reference) composition, where analyte

levels are certified by the

manufacturer. These

materials should be traceable

to NIST standards.
38

TABLE 2. RECOMMENDED INSTRUMENTAL QC STANDARDS AND SPECIFICAT

Name Use Specification

ICB—Initial Used for initial calibration Calibration standard that contains no analyte.calibration blank and zeroing instrument

response. Must be measured during calibration and after ca

Measured value to be less than 5 times the instrulimit.

Calibration Used to calibrate Must be matrix matched to acid content present in standards instrument. digestates.

The high standard rerun is Must be measured prior to measuring any sample 

used to check for high

response rollover. Correlation coefficient of ` 0.995, as measured u

regression on instrument response (y) versus con

The highest level calibration standard must be me

calibration. The measured value to fall within ±10

ICV—Initial Used to verify calibration Concentration of analyte to be near midrange of l

calibration standard levels. ICV is made from a stock solution having a differe

verification or manufacturer lot identification than the calibrat

Must be measured after calibration and before me

sample digestates.

Measured value to fall within ±10% of known valu
39

TABLE 2 (CONTINUED)

Name Use Specification

ICS—Interference Used to verify accurate Concentration of analyte to be less than 25% of th

check sample (for analyte response in the calibration standard, concentrations of interferant 

ICP-AES only) presence of possible of Al, Ca, Fe, and Mg.

spectral interferencesfrom other analytes Must be analyzed at least twice, once before and present in samples. sample digestates.

Measured analyte value to fall within ±20% of kno

CCV—Continuing Used to verify freedom Concentration to be near midrange of linear curve

calibration from excessiveverification instrumental drift. Must be analyzed before and after all sample dige

frequency not less than every 10 sample digestat

Measured value to fall within ±10% of known valuFLAA (±20% for GFAA), run 1 every 10 samples.

CCB—Continuing Used to verify blank Calibration standard that contains no analyte.

calibration blank response and freedom

from carryover. Must be analyzed after the CCV and after the ICS

Measured value to be less than 5 times the instrulimit.
40

2.5.15 Safety, Health and Hazardous Waste

An introduction to laboratory safety and health, particularly as it applies to heavy

metals, should be given. Safety and health aspects of laboratory operations are

delineated in the OSHA Laboratory Standard "Occupational Exposures to Hazardous

Chemicals in Laboratories" (29 CFR 1910.1450, Chemical Hygiene Plan). The

assessor should note the existence of such a plan and specify that the evaluation is

only an acknowledgement of the existence of a safety and health plan and not an

evaluation of the effectiveness of such programs. Failure to communicate this to the

laboratory may result in the mistaken assumption that the assessment found that the

laboratory complied with health and safety regulations. A subsequent citation by OSHA

or a laboratory accident could result in liability to the assessor.

Certain Pb materials may be classified as hazardous waste. A solid waste

containing more than 200 ppm of Pb may fail the TCLP (Toxicity Characterization

Leaching Procedure) used to define a hazardous waste (U.S. EPA SW-846

Method 1310 for TCLP, followed by Methods 3050/6010). By failing the TCLP, a waste

is classified as hazardous and, consequently, requires special handling and disposal. 

Therefore, steps must be detailed in an SOP for the handling of potentially hazardous

waste to include compliance with applicable local, state, and federal regulations.

Digests, which are acidic in nature, also contain Pb and perhaps other metals. 

These digests must be disposed of according to local state and federal regulations.

2.6 MODULE III. THE ASSESSMENT PROCESS, OR HOW TO CONDUCT AN

ASSESSMENT (8 HOURS)

The objective of this module is to provide the student with a working knowledge

of how to perform a site assessment, including planning, conducting the assessment,

and preparation of reports.

2.6.1 Instructor Qualifications

This section should be taught by an experienced assessor or a trainer of a

previous assessor training program for an accrediting organization. The practical

experience of the trainer is essential to provide a "real world" rather than a theoretical

perspective to the course.

2.6.2 Pre-Assessment Review

Prior to scheduling an on-site assessment, the assessor will receive a package

of information from the NLLAP-recognized accrediting organization that will include the

documents listed below. These documents need to be reviewed prior to making

arrangements for a site assessment.
41

` Personal responsibilities, qualifications of laboratory staff, key contacts, and

phone numbers.

` Application for accreditation.

` Evaluation of ELPAT data and corrective actions, if available.

` Quality manual and SOPs.

` Previous site assessment reports (if available).

` Previous laboratory in-house audits.

` Laboratory response to previous deficiencies, if applicable.

2.6.3 Pre-Assessment Preparation—How to Pack Your Bags

The assessor should be familiar with the following documents and take copies as

appropriate. The assessor should take all items that may be needed and not assume

that the laboratory will supply needed items.

` Policies and guidelines of the accreditation organization.

` 29 CFR 1910.1450 (OSHA Laboratory Standard).

` Policy for interpretation of proficiency test results as specified by ELPAT and

the accreditation organization.

` Lists of methods and some selected methods.

` QA references, such as ISO Guide 25, as educational guides.

` References to QA programs.

` Accrediting organization forms.

` "Portable office" supplies, including paper clips, notes, pads, tape, binders,

notebook PC, etc.

` Letter of introduction from the accrediting organization.

` Expense statements from the accrediting organization.

` Safety glasses and other required safety equipment.

` Sample for sample tracking as required by accreditation organization.
42

` Copies of the checklist.

` Copies of correspondence with the laboratory regarding the audit.

` Copies of the laboratory response to previous deficiencies and complaints.

` Criteria/requirements for accreditation.

` NLLAP requirements.

2.6.4 Pre-Assessment Communication to Laboratory

The assessor should open a clear line of communication with the laboratory in

order to conduct an efficient assessment with minimum disruption of laboratory

personnel. The following topics are needed for an effective assessment:

` Plan the agenda so that the laboratory knows how long the assessor will be

there and with whom the assessor needs to talk. Provide an anticipated

closing conference time. Remain flexible in scheduling.

` Send a letter of introduction from the accrediting organization and have

copies of the expense statement, the checklist, and the agenda.

` Obtain a list of key contacts from the laboratory, including phone numbers.

` Determine who will attend the opening conference. 

` Determine specific assessment plans from evaluation of previously

submitted materials.

` Request information on convenient food, lodging, and transportation from

the laboratory.

` Request the use of a copy machine to make copies of reports for the

laboratory director.

` When applicable, notify the laboratory of specific problem areas found on

the application or from client-filed complaints that will be investigated.

` Confirm, by telephone, arrival date 1 to 2 days before departure.

` Inquire about safety requirements and personal protective equipment needs.
43

2.6.5 Steps of the Assessment

The key to conducting a quality assessment with minimum disruption of

laboratory staff and maximum cooperation from laboratory management is to follow the

steps outlined below. It must be stressed that the assessor is a fact finder, not a

decision maker. The ultimate decision on accreditation is made by the accrediting

organization. The assessor is not a consultant to the laboratory. The assessor must be

thoroughly prepared and conduct himself/herself in a professional manner at all times.

2.6.5.1 Opening Conference (Entry Briefing)—

Following are suggestions for the initial conference with the laboratory personnel:

` Meet with laboratory authorized representatives.

` Confirm agenda outline (work time, breaks, lunch, etc.).

` Explain the general procedures for the assessment and emphasize that the

assessor's role is to gather facts, not make decisions.

` Confirm the accuracy of organization charts and matrices for which the

laboratory seeks accreditation.

` Request files on problems reported by clients associated with the Pb

program.

` Request current copies of SOPs and QA manuals for comparison with those

sent for pre-assessment review. (These may have been updated since the

application was submitted or after the self-evaluation checklist was sent.)

` Notify attendees of needs to evaluate areas of concerns revealed during

pre-assessment review, such as qualifications of director, problems in QA

manual, etc.

` Identify spokesperson for the laboratory.

` Request a quiet room to review documents and prepare reports.

` Request an escort.

` Obtain an attendance roster.

` Conduct a pre-assessment walk through for general orientation.

2.6.5.2 Checklist —

A checklist is used to develop the basic framework of the on-site assessment. It

is based on the general criteria required in the ISO 25 Guide (ISO/IEC Guide 25, 1990)
44

with added specifics applicable to spectroscopy (atomic absorption and ICP-AES)

procedures used for Pb paint laboratory work. The checklist should be sent to the

laboratory for a self-evaluation prior to the actual site visit. It is then returned to the

designated site assessor before the actual site visit.

The checklist serves as a specific guide to the assessor in evaluating problem

areas. Three check-offs (yes, no, and N/A) are at the top of the column, and space for

assessor comments is provided. It serves (1) as the basis for preparation of an

assessor report and (2) to document the areas of the laboratory operation specifically

evaluated by the assessor. The advantages of using this checklist include selfevaluation by the laboratory, an opportunity to correct a problem before a site visit, and

the avoidance of surprises that may arise during the site assessment. The checklist

also allows the assessor to do an independent review with less on-the-spot questioning

of technical staff during the assessment. The checklist is extensive and will require

significant time on the part of the laboratory staff to perform a self-evaluation. A copy of

the checklist is included in Appendix B. 

2.6.5.3 Documentation of Sample Tracking—

This step is used to document the flow of samples through the system and to

trace samples from their receipt in the laboratory to the data report leaving the

laboratory. The specifics of sample tracking depend on the policies of the NLLAP

accrediting organization. The assessor could bring an actual audit sample that is

observed through the system. Some accrediting organizations also perform a paper

tracking of a randomly selected sample through the system.

2.6.5.4 Interviews with Key People—

It is essential to talk to key people involved in the analysis of samples and those

responsible for quality assurance. Persons interviewed should include those who have

performed the analysis, such as the Pb technician, the metals area supervisor, the QA

person, and other specialists, as identified in the pre-assessment review and in the

opening conference. Documents should be reviewed and compared with those

provided in the pre-assessment package. 

2.6.5.5 On-site Reports—

The NLLAP-recognized accrediting organization determines the need for on-site

reports. If such reports are required, the assessor should find quiet time to prepare

draft reports prior to the closing conference. If the accrediting organization requires onsite reports, the following are recommended:

` Assessor's reports (handwritten) that include a narrative review of findings

during the site visit and the positive aspects of the laboratory operation. 

Copies of the checklist also should be included. 
45

` Deficiencies noted during the site assessment that require responses from

the laboratory within a specified time. There should be reference or citations

provided that relate to specific requirements.

` Draft reports, including deficiency reports, should be acknowledged, signed

off by both parties, and distributed to the laboratory key contact. This step is

essential to avoid surprises, provides immediate documentation of the

assessment, and allows laboratories to begin corrective actions, if needed,

right away.

Some accrediting organizations may not want the assessor to provide feedback

in written form to the laboratory until the accrediting organization has reviewed the

assessor's report. In this case, no written reports would be provided on site.

2.6.5.6 Closing Conference—

The closing conference with the same personnel that attended the opening

conference should be conducted in a firm, professional way to include positive

observations as well as observed deficiencies. Important points to include are the

following:

` There should be no surprises for the laboratory manager, if at all possible.

` Reports should be thoroughly reviewed to be sure that all parties understand

the contents. It may be necessary to actually read the report to ensure a

clear understanding. Obtain sign off from the laboratory key contact and

assessor on each copy of the reports distributed to laboratory personnel.

` Indicate that a response is required for each identified deficiency within a

specified time, as noted on the report.

` Avoid serving as a consultant. Identify deficiencies and report requirements

only. Do not recommend solutions, only requirements. 

` Discuss complaints by customers and resolution of those complaints.

` Review steps and schedule for corrective actions by the laboratory and for

decisions by the accrediting organization. (The assessor is not the decision

maker!)

` Execute other documents required by the NLLAP-recognized accrediting

organization, such as expense reports.

2.6.5.7 Final Reports and Decision by Accrediting Organization—
46

Final reports (typewritten), prepared after the site visit, are sent to the laboratory

and to the accrediting organization within a specified period of time, which is

determined by the accrediting organization. The deficiencies noted on this report that

require corrective action must have a suspense date. The laboratory must correct or

respond to the deficiencies by the suspense date. It must be emphasized that the

assessor does not make on-site decisions as to pass or failure of a laboratory.

 

The accrediting organization reviews responses to deficiencies according to their

specific policy. The assessor usually reviews the response to the deficiency report and

assists the accrediting organization in making a decision to provide/deny/revoke

accreditation, depending on accrediting organization policy. Grounds for failure include

lack of adequate, timely responses to deficiencies, lack of acceptable responses to

complaints from clients, and lack of acceptable performance in required proficiency

testing programs. A follow-up site assessment might be required before a final decision

is reached.

2.6.5.8 Assessor Performance Rating—

Assessors, to be effective, should be subjected to an objective performancerating system. The specifics are determined by the accrediting organization, but should

include the following minimum requirements:

` Feedback from the laboratories that were assessed on the competence and

thoroughness of the assessment with the precaution that ratings from

assessed laboratories are not always based on the assessors' effectiveness. 

A poorly performing laboratory could provide a biased response to a

thorough assessment.

` The accrediting organization should develop an assessor evaluation and

rating program based on the quality and timeliness of the reports submitted

and the degree of preparation prior to the conduct of the assessment.

2.7 MODULE IV. INTERPERSONAL SKILLS (4 HOURS)

The objective of this module is to provide the student with the skills and tips on

the psychology of assessment, an area equally as important as the technical aspects of

Pb analysis.

2.7.1 General Overview

This module includes the important aspects of how to conduct an assessment

(the psychology of assessment). It includes professional conduct, assessor ethics, lists

of do's and don'ts appropriate for a professional objective assessor, and pitfalls to avoid

during an assessment. There are numerous references cited in the bibliography (e.g.,

Bunker, 1984a; Bunker, 1984b; Samel, 1992; Vassals, 1977). 
47

2.7.2 Professional Conduct of the Assessor

` Maintain a positive, professional attitude at all times.

` Exhibit gentle firmness and dignity; be polite.

` Maintain objectivity at all times—be independent.

` Dress as a professional appropriate for the laboratory director or

supervisor—sweats, "tennies," golf shirts, or jeans are unacceptable.

` Observe and note rather than dictate and criticize.

` Document observations on the checklist and do not rely on memory.

` Provide constructive criticism as appropriate; provide references to NLLAP

requirements.

` Solicit constructive criticism of the assessment process.

` Adjust the agenda to meet changing needs of the laboratory, such as

increased workload, and so forth.

` Understand the assessment process and answer questions fully.

2.7.3 Assessor Ethics

` The assessor is a fact finder, not a decision maker. Observe and note; do

not serve as a consultant.

` Disclose any apparent conflicts of interest, such as assessor business

connections, prior to the visit. 

` Do not be an assessor and a consultant for the same laboratory. 

` Treat all information as confidential and do not transfer information from

laboratory to laboratory.

` Do not accept gratuities or free meals, unless there is no choice (a company

lunchroom provided as a benefit to employees with no provision for cash

payments).

2.7.4 Do

` Follow laboratory safety procedures, and leave the area when requested.
48

` Bring your own safety glasses.

` Prepare yourself for local customs, such as dress codes, meal schedules,

breaks, and so forth.

` Allow time for the laboratory to adjust to the assessment process. 

` Arrive in a fully alert, rested state. The overtired assessor or the assessor

with a hangover is unacceptable.

` Provide positive reinforcements to laboratory personnel as appropriate.

` Listen attentively and take notes.

` Express appreciation for laboratory cooperation.

` Observe and practice appropriate body language.

2.7.5 Do Not

` Criticize equipment, suppliers, or the accrediting organization.

` Become argumentative.

` Do the analysis—keep hands off laboratory equipment and personnel.

` Chew gum, use beepers or musical watches.

` Tell jokes or behave too casually.

` Smoke or chew tobacco.

` Become involved in laboratory personnel problems.

` Make specific recommendations on supplies or equipment (product

endorsement).

` Make derogatory comments about individuals.

` Discuss the assessment with personnel not involved in the assessment.

` Allow personal viewpoints to affect the assessment.

` Socialize with the client.

2.7.6 Beware of Tactics by the Laboratory to Sidetrack the Assessor
49

Reports by Bunker (Bunker, 1984a,b) provide many details on this topic. Some

of the highlights are listed.

` The "everything is beautiful" tactic, where only the positive attributes of the

laboratory are discussed. Actively seek out the weak points.

` The "name, rank, and serial number" tactic, where no information is

volunteered. Be prepared to ask specific questions in advance.

` The "bury the assessor in detail" tactic, where unnecessary detail is provided

to derail the assessment. Filter the details out and do not get sidetracked.

` The "Don't tell me how to run my lab!" tactic. Be firm, point out requirements

and deficiencies, but do not become argumentative.

2.7.7 Assessor Pitfalls

` Do not expect any one person to have complete knowledge—talk to others.

` Do not get side-tracked in areas outside the scope of the assessment, such

as regulatory policies, for example.

` Beware of the chronic complainer or lobbyist, who may use the assessor as

a tool to get a personal problem advanced to management.

` Cover all areas, using the checklist as a guide, not just those specific areas

that interest you.

` Avoid "rabbit" conclusions during a specific evaluation. Get all the facts,

including views from others, before concluding that a deficiency exists.

` Do not become part of the laboratory problem; remain detached and

professional.

` Do not accept the laboratory staff's word about a specific situation;

personally evaluate the situation. 
50

2.8 MODULE V. PRACTICAL ROLE-PLAYING EXERCISE (8-16 HOURS)

The objective of this module is to provide the student with practical, role-playing

exercises to reinforce the lecture material and to provide some insight into actual

assessments.

2.8.1 General Overview

This module discusses a role-playing, practical application of the assessment

process. A variety of approaches can be included in role-playing, such as mock site

visits could be conducted; case studies could be presented with role-playing by

students; or video cases could be presented. The objective in role-playing is to apply

skills learned in the lecture portion of the course.

The role-playing exercise provides a better understanding of the assessment

process and builds assessor confidence. The length of this module can vary from a few

hours to a full day, depending on the format of the role-playing exercise. The specific

format is intentionally left vague to encourage the development of innovative roleplaying exercises.

2.8.2 Points to Emphasize in a Role-Playing Exercise

The following points should be emphasized in a role-playing exercise:

` Entrance/exit sessions.

` Interviews of technicians and QA personnel.

` Potential conflicts/disagreements with laboratory staff.

` Preparation of a mini-report based on a presented case.

` Critique by observers of the role play.

2.8.3 Examples of Practical Role-playing Exercises

` Case studies constructed from experience and planned to illustrate actual

and potential problems.

` An actual class visit to a local laboratory. A field trip is a good role-playing

exercise, but may have a negative impact on the visited laboratory.

` Video case reports and practical role-playing exercises including the use of

the checklist and report preparation (assessor's report and deficiency lists).
51

` Mock visit to a laboratory through a variety of media, such as slides, video,

and so forth.

` Mock interviews or role-playing with laboratory personnel (director, chemist,

QA coordinator, lawyer, etc.) using student role players.

2.9 MODULE VI. WRITTEN EXAMINATION (1 HOUR)

The object of this module is to examine the student for retained knowledge and

problem-solving skills in preparation for actual on-site internship. 

2.9.1 General Overview

A written examination should be administered to document the successful

completion of the course. The examination should include essay and practical

problem-solving exercises covering all aspects of the course. The questions for the

written examination should be as objective as possible. In order to pass the course, the

student must provide acceptable understanding of each module in the course. 

Acceptable understanding cannot be rigidly defined as a percent score because tests

could be constructed so all participants get at least 70% correct on each module. If, in

the judgement of the instructor(s) or accrediting organization, the student fails any

module, the student should be given the opportunity to retake those modules. Any

student that fails more than three modules should not pass the course and should not

be given the opportunity to retake specific modules. Of course, the student could

retake the entire course with appropriate fees paid. 

The student assessor, who meets the qualifications standards in Section 2.2, will

be given a certificate of successful completion after the examination has been graded. 

Successful completion of the written exam does not qualify the student as an assessor. 

Completion of an on-site internship conducted by the NLLAP-recognized accrediting

organization is required before the student is certified as an NLLAP-recognized

assessor. 

"Observer" students, identified in Section 2.2, who are not qualified to become

assessors because of their lack of education/experience, will not be allowed to take the

examination, and will not be recognized as NLLAP assessors. No certificate of

completion would be issued.
52

2.10 MODULE VII. ON-SITE INTERNSHIP

The objective of this module is to perform actual on-site assessments as an

intern under the direction of an experienced assessor according to the policies and

procedures of an NLLAP-recognized accrediting organization.

2.10.1 General Overview

Because on-site assessments are conducted under specific rules of the NLLAPrecognized accrediting organization, actual on-site assessments are not part of this

lecture and discussion training program. However, actual on-site assessments are a

required part of the total training curriculum for recognition as an NLLAP-recognized

assessor. Certification as an experienced assessor is based on the requirements of the

NLLAP-recognized accrediting organization.

2.10.2 Minimum Requirements for On-Site Internship

The following are recommended minimum requirements for the on-site

internship:

` Two on-site visits, one as an active observer (intern), the second as a

primary assessor, with the assistance of a supervising assessor who would

accompany the intern.

` Feedback to the NLLAP-recognized accrediting organization on the

effectiveness of the assessor trainee from the assessed laboratory and from

the supervising assessor.

` Certification by the NLLAP-recognized accrediting organization following

successful completion of the internship.
53

SECTION 3

LEVEL TWO COURSE—UPDATE FOR THE EXPERIENCED ASSESSOR

3.1 COURSE OUTLINE

This course is a 12-hour course aimed at current laboratory assessors from

qualified NLLAP-recognized accrediting organizations. It includes two modules:

(1) General Overview of the Accreditation Process, and (2) Technical Aspects of Pb

Sampling and Analysis. This course is nearly identical to the Level One Course. 

However, there are different admission qualifications and examination requirements. 

The Level Two course will be restricted to current or experienced assessors who have

conducted three assessments per year in the most recent 2 years. The assessor

student must meet minimum requirements, including the conduct of recent

assessments for a NLLAP-recognized accreditation organization and a letter of

recommendation from that organization.

The course includes a 2-hour module covering the generic aspects of the

accreditation process, the history of the health effects of Pb, and the current status of

Pb-paint abatement issues and legislation. This 2-hour module is identical to the

General Overview module from the Level One course, as presented in Subsection 2.4. 

An additional 2-hour module would be required to acquaint the experienced

assessor with the specific accreditation policies and procedures for an NLLAPrecognized accrediting organization for paint, soil, and deposited dust matrices. This

program should be taught by a representative of the NLLAP-recognized accrediting

organization, because the accreditation process will be different for each accrediting

organization.

The 8-hour module on the technical aspects of Pb sampling and analysis is

identical to the Technical Aspects module from the Level One course as presented in

Subsection 2.5. It covers all aspects of laboratory issues related to sampling, analysis,

and reporting of data for Pb in paint, soil, and deposited dust matrices. 

An examination would be administered to document the successful completion of

the course. No on-site assessment would be required because the student must be a

current laboratory assessor to take this Level Two course. It is assumed that the

experienced assessor knows how to conduct an on-site assessment. An experienced

assessor may be assigned as a mentor for the new assessor at the discretion of the

NLLAP-recognized accrediting organization.
54

3.2 QUALIFICATIONS FOR ADMISSION

The qualifications for admission are 

` The general educational and experience requirements for assessors, as

specified in Section 2.2 and by NLLAP-recognized accrediting organizations.

` Experience in conducting assessments with a minimum of 3 assessments

per year for the most recent 2-year period. 

 ` A letter of recommendation from the assessor's accrediting organization.

3.3 WRITTEN EXAMINATION

The objective of the written examination is to test the student for retained

knowledge. The written examination must be administered to document the successful

completion of the course. The questions should be as objective as possible. In order

to pass the course, the student must provide acceptable understanding of each module. 

Acceptable understanding cannot be rigidly defined as a percent score because the test

could be constructed so that all participants scored at least 70%. If the student fails any

module, the student would not pass the course, and would have to retake the course

and pass another examination. 

The student assessor, who meets the qualifications standards in Subsection 3.2,

would be given a certificate of successful completion after passing the examination. 

Successful completion of the written exam should qualify the student as a Pb assessor.

No on-site assessment internship period would be required; however, an

experienced assessor from an NLLAP-recognized accrediting organization could be

assigned as a mentor to answer any questions that may arise during initial site

assessments. The experienced assessor who successfully completed the course

would then be evaluated by the NLLAP-recognized accrediting organization for possible

employment.
55

SECTION 4

CONTINUING EDUCATION REFRESHER COURSE FOR ALL ASSESSORS

4.1 OBJECTIVE

The objective of this module is to ensure that properly trained and certified

assessors have frequent opportunities to upgrade their understanding of the accrediting

process, the technical aspects of Pb methods, and practical aspects of the conduct of

an assessment. An added benefit is the opportunity to discuss problems and creative

solutions with peers.

4.2 OUTLINE OF CONTINUING EDUCATION PROGRAM (1 DAY)

Continuing education would be required of all assessors. Programs would be

offered annually and required every 2 years for assessor recertification. Programs

would be for a full day. These updates should address the following topics:

` New policies of the accrediting organization and the NLLAP.

` New or updated federal and state regulations and legislation related to both

laboratory accreditation and Pb-paint abatement.

` New findings regarding the hazards of Pb to human health, particularly

laboratory workers. 

` Technical update on sampling and analysis methods.

` Sharing of experiences of current assessors by means of case studies and

discussion groups.

The continuing education course should be documented internally at the accreditation

organization, and result in recertification from the board of directors of the accrediting

organization.
56

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57

SECTION 5

ADMINISTRATIVE ISSUES

5.1 WHO OFFERS THE COURSES?

These courses should be taught by an NLLAP-recognized accrediting

organization with their specific requirements added to a core curriculum. The course

should follow ISO Guide 25, the international standards guidelines. Alternately, the

course could be taught by a third party as a generic course. After completion of the

generic course, a supplemental course (2-hour module) would be required to familiarize

the student assessor with the policies and procedures of the specific accrediting

organization. This 2-hour module should be taught by an experienced official from the

accrediting organization. A chemist familiar with Pb analyses in paint, soil, and

deposited dust matrices should teach the technical aspects of Pb analysis. 

The on-site assessment internship, required in the Level One course, is the

responsibility of the accrediting organization. Continuing education courses are also

the responsibility of the accrediting organization.

In order for the instructors and the training organization to be recognized by

NLLAP, the training organization should submit a lesson plan, along with resumes of

the instructors, for EPA review as part of the NLLAP MOU package. Initial offerings of

courses must be evaluated by NLLAP-recognized accrediting organizations that hire

assessors as to the effectiveness of the training programs. Such constructive feedback

to accrediting organizations, and in turn to EPA, will result in improvements in the

training programs. 

5.2 HIRING, USE, AND DISMISSAL OF ASSESSORS

Assessors are employed by the NLLAP-recognized accrediting organization, thus

all decisions on personnel matters, including hiring and firing, are the responsibility of

that accrediting organization. Specific areas that the accrediting organization must

address are listed.

` The accrediting organization has the final say in all personnel matters

regarding assessors.

` The accrediting organization should provide a system of monitoring assessor

performance.
58

` The accrediting organization should develop a policy regarding the minimum

number of assessments (e.g., 1 assessment in 2 years) in order to maintain

assessor status.

` The accrediting organization should have a documented means for removal

of ineffective assessors.

` The accrediting organization should have an appeals procedure to ensure

fair and equitable treatment of grievances brought by assessors.
59

SECTION 6

LIST OF REFERENCES

Some of these references are available from the National Technical Information

Service (NTIS) at (703) 487-4650.

A2LA. General Requirements for Accreditation, March 1991.

A2LA. Environmental Program Requirements, July 1991.

A2LA. Assessor Guide, December 1991.

A2LA. Instructions for Assessor (includes copies of Assessor Report, Assessor

Deficiency Report, Estimated Assessment Cost, and Assessor Checklist: General

Criteria.) 

A2LA. Environmental Field of Testing: Assessor Checklists for Potable Water,

Nonpotable Water, and Solid/Hazardous Waste, October 1991.

A2LA. Instrument Specific Checklist: Atomic Absorption/ Inductively Coupled Plasma

Spectrophotometry, 1992.

ACGIH. Industrial Ventilation, A Manual of Recommended Practices, 21st ed., 

American Conference of Governmental Industrial Hygienists, Cincinnati, OH, 1991.

AIHA. Site Visit Plan and Model Agenda, September 7, 1982.

AIHA. Quality Assurance Manual for Industrial Hygiene Chemistry, May 1988. 

APHA, AWWA, WPCF. Standard Methods for the Examination of Water and

Wastewater. 17th ed., 1989. Standard Method 3500-Pb B, Atomic Absorption;

Standard Method 3500-Pb C, Inductively Coupled Plasma Method. 

ANSI/ASQC Q1/ISO Guide 10011, Guidelines for Auditing Quality Systems. Part 1:

Auditing (December 15, 1990); Part 2: Qualification Criteria for Auditors (May 1, 1991);

Part 3: Managing Audit Programs (May 1, 1991).

ANSI/ASQC Q90-1987 (Equivalent to ISO 9000-1987), Quality Management and

Quality Assurance Standards: Guidelines for Selection and Use. 
60

ANSI/ASQC Q91-1987 (Equivalent to ISO 9001-1987), Quality Systems: Model for

Quality Assurance in Design/Development, Production, Installation and Servicing. 

ANSI/ASQC Q92-1987 (Equivalent to ISO 9002-1987), Quality Systems: Model for

Quality Assurance in Production and Installation.

ANSI/ASQC Q93-1987 (Equivalent to ISO 9003-1987), Quality Systems: Model for

Quality Assurance in Final Inspection and Test.

ANSI/ASQC Q94-1987 (Equivalent to ISO 9004-1987), Quality Management and

Quality System Elements: Guidelines.

ASTM E 994-84 (Reapproved 1990): Standard Guide for Laboratory Accreditation

Systems.

ASTPHLD: Proceedings of the First National Conference on Laboratory Issues in

Childhood Lead Poisoning Prevention. Association of State and Territorial Public

Health Laboratory Directors, Inc., Washington, DC, 1991.

Bunker, Alan S. Dealing with Auditors: How to Take Control of an Audit Away from the

Auditors. Radiation Protection Management, April 1984a, pp. 47-58.

Bunker, Alan S. Effective Auditing: How To Be a Good Auditor. Radiation Protection

Management, October 1984b, pp. 21-36.

CDC. Preventing Lead Poisoning in Young Children: A Statement by the Centers for

Disease Control, October 1991.

CNAEL: Minutes of the June 1-2, 1992, Meeting of the Committee on National 

Accreditation of Environmental Laboratories, August 3, 1992.

HUD: Lead-Based Paint: Interim Guidelines for Hazard Identification and Abatement in

Public and Indian Housing. Appendix 5: Laboratory Testing for Lead (Pb) in Paint Film,

Dust, Air, and Soil, September 1990, pp. A5-1 to A5-37. (Appendix 13 includes quality

assurance information specific for Pb.)

HUD. NOFA for Lead-Based Paint (LBP) Risk Assessments. Federal Register. 

June 29, 1992, pp. 28910-28943. [Contains Lead-Based Paint Risk Assessment

Protocol, which includes sampling protocols (Part III, pp. 28926-28927) for dust, paint

chips, and soil.]

ISO/IEC Guide 25-1990 (E): General Requirements for the Competence of Calibration

and Testing Laboratories. International Organization for Standardization/International

Electrotechnical Commission, Geneva, Switzerland, 1990.
61

ISO/IEC Guide 58: Calibration and Testing Laboratory Accreditation Systems: General

Requirements for Operation and Recognition, November 1992.

Liabastre, A. A., K. A. Carlberg, and M. S. Miller. "Quality Assurance for Environmental

Assessment Activities," in Methods of Environmental Data Analysis, C. N. Hewitt ed.,

Elsevier Applied Science, New York, 1992, pp 259-299.

Murphy, T. J. The Role of the Analytical Blank in Accurate Trace Analysis. In Accuracy

in Trace Analysis. Vol. I, NBS Special Publication 422, 1976, pp. 509-539.

NATA: General Requirements for Registration, National Association of Testing

Authorities, Australia, 1991.

NIOSH. Manual of Analytical Methods, 3rd ed., DHHS (NIOSH) Publication 84-100,

1984.

NIST: Department of Commerce. Request for Comments on a Proposal to Establish

the Conformity Assessment Systems Evaluation Program (CASE). Federal Register 57:

10620-10621, March 20, 1992.

NIST. Certificate of Analysis, SRM 1648 (Urban Particulate Matter), Pb 0.655 ± 0.008

(weight percent), November 16, 1978.

NIST. Certificate of Analysis, SRM 1579a (Powdered Lead-Based Paint), Pb 11.995 ±

0.031 (weight percent), February 3, 1992.

NIST. Certificate of Analysis, SRM 2579 (Lead Paint Film on Mylar Sheet, Set of 5),

3.53 mg/cm ± 0.24; 1.63 mg/cm ± 0.08; 1.02 mg/cm ± 0.04; 0.29 mg/cm ± 0.01; 2222

< 0.0001 mg/cm , July 7, 1992. 2

NIST. Certificate of Analysis, SRM 2704 (Buffalo River Sediment), Pb 161 ± 17 μg/g,

July 9, 1990.

NIST. Certificate of Analysis, SRM 2709 (Baseline Agricultural Soil), 18.9 μg/g ± 0.5,

October 16, 1992.

NIST. Certificate of Analysis, SRM 2710 (Highly Contaminated Soil), 5532 μg/g ± 80,

October 16, 1992.

NIST. Certificate of Analysis, SRM 2711 (Moderately Contaminated Soil),

1162 μg/g ± 31, October, 16, 1992.

NVLAP: National Voluntary Laboratory Accreditation Program Procedures, NISTIR

4493, dated November 1990 (USC Title 15, Subtitle A, Chapter II, Part 7).
62

NVLAP: On-Site Assessment Report, Part 1 (Signature Sheet), Part 2 (General

Operations Checklist), and Part 3 (Specific Operations Checklist).

Ratliff, T. A., Jr. The Laboratory Quality Assurance System: A Manual of Quality

Procedures with Related Forms. Van Nostrand Reinhold, New York, 1990.

Registrar Accreditation Board: Certification Programs for Auditors of Quality Systems. 

Registrar Accreditation Board, Milwaukee, WI, 1992. Appendix C, "Code of 

Conduct for Auditors of Quality Systems," pp. 19-20.

Samel, Alan. Training New Quality Assurance Unit Auditors. Presented at The

American Industrial Hygiene Conference & Exhibition, Boston, MA, June 1992.

Taylor, John K. Handbook for SRM Users. NBS (NIST) Special Publication 260-100,

September 1985.

Unger, Peter (A2LA). Achieving Laboratory Accreditation: A How-To Guide. CEEM

Information Services, Fairfax, VA (1992).

U.S. EPA. Interim Guidelines and Specifications for Preparing Quality Assurance

Project Plans. QAMS-005/80 (Office of Monitoring Systems and Quality Assurance,

ORD/EPA). December 29, 1980.

U.S. EPA. Toxic Substances Control Act (TSCA); Good Laboratory Practice Standards,

Final Rule. Federal Register. Volume 54, Number 158, August 17, 1989, pp. 34031 -

34050. [40 CFR Part 792]

U.S. EPA. Manual for the Certification of Laboratories Analyzing Drinking Water: 

Criteria and Procedures for Quality Assurance, 3rd ed., EPA-570/9-90-008, April 1990a.

U.S. EPA. RCRA Quality Assurance Workshop: Outline of Mandatory and

Recommended QA Practices, Chapter One of SW-846, July 1990b.

U.S. EPA. Test Methods for Evaluating Solid Waste, Physical/Chemical Methods,

SW-846, 3rd ed., Revised, November 1990c.

U.S. EPA. Options for a Lead Analysis Laboratory Accreditation Program, Final Draft,

October 1990d. EPA/OTS/AREAL.

U.S. EPA. Laboratory Accreditation Program Guidelines: Measurement of Lead in

Paint, Dust, and Soil. EPA-747/R-92-001, March 1992a.

U.S. EPA: Pb-Based Paint: Laboratory Operations Guidelines: Analysis of Pb in Paint,

Dust, and Soil. EPA-747/R-92-006, Revision 1.0, May 1993b.
63

Vassals, John R. Psychology of Auditing. Quality Progress, September 1977, p. 37.
64

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A-1

APPENDIX A

ACRONYMS AND GLOSSARY OF TERMS
A-2

(BLANK PAGE)
A-3

APPENDIX A

ACRONYMS AND GLOSSARY OF TERMS

ACRONYMS

AA Atomic Absorption

A2LA American Association for Laboratory Accreditation

ACIL American Council of Independent Laboratories

AIHA American Industrial Hygiene Association

ANSI American National Standards Institute

AOAC Association of Official Analytical Chemists 

APHA American Public Health Association 

ASTM American Society for Testing and Materials

ASQC American Society for Quality Control

ASTPHLD Association of State and Territorial Public Health Laboratory Directors

AWWA American Water Works Association

CCB Continuing Calibration Blank 

CCV Continuing Calibration Verification 

CERCLA Comprehensive Environmental Responsibility, Compensation and Liability Act

CDC Centers for Disease Control

CMD Chemical Management Division

CNAEL Committee on National Accreditation of Environmental Laboratories

CRADA Cooperative Research and Development Agreement

CLP Contract Laboratory Program

CRM Certified Reference Material

EDL Estimated Detection Limit 

ELLAC Environmental Lead Laboratory Accreditation Committee (AIHA)

ELPAT Environmental Lead Proficiency Analytical Testing (AIHA/NIOSH)

EMPC Estimated Maximum (Protocol) Concentration

FLAA Direct Flame Aspiration Atomic Absorption Spectrometry

GFAA Graphite Furnace Atomic Absorption Spectrometry

GLP Good Laboratory Practices Standards (TSCA)

ICB Initial Calibration Blank

ICP-AES Inductively Coupled Plasma Emission Spectrometry

ICP-MS Inductively Coupled Plasma-Mass Spectrometry

ICV Initial Calibration Verification

ICS Interference Check Standard 

IDL Instrument Detection Limit 

IMVL Interlaboratory Method Validation Study

ISO International Organization for Standardization

LCS Laboratory Control Sample

LOQ Limit of Quantitation

LSA Laboratory Systems Audit

MCL Maximum Contaminant Level

MDL Method Detection Limit
A-4

MOU Memorandum of Understanding

MRI Midwest Research Institute

NATA National Association of Testing Authorities (Australia)

NIOSH National Institute for Occupational Safety and Health

NIST National Institute of Standards and Technology

NLLAP National Lead Laboratory Accreditation Program

NTIS National Technical Information Service

NVLAP National Voluntary Laboratory Accreditation Program

OSW Office of Solid Waste (U.S. EPA)

PE Performance Evaluation

PM Preventive Maintenance

PT Proficiency Testing

PQL Practical Quantitation Limit

QA Quality Assurance

QAMS Quality Assurance Management Staff

QAPjP Quality Assurance Project Plan

QAPP Quality Assurance Program Plan

QC Quality Control

QM Quality Manual

RCRA Resource Conservation and Recovery Act

RE Relative Error

RPD Relative Percent Difference 

SAP Sample Analysis Plan

SARA Superfund Amendments and Re-authorizations Act of 1986

SOP Standard Operating Procedure

SRM Standard Reference Material Produced by NIST

TCLP Toxicity Characteristic Leaching Procedure

TPB Technical Programs Branch

TQM Total Quality Management

TSCA Toxic Substances Control Act

XRF X-Ray Fluorescence

WAL Work Assignment Leader (L. K. Lowry)

WAM Work Assignment Manager (J. Scalera)

WPCF Water Pollution Control Federation

GLOSSARY 

Accreditation: A formal recognition that an organization (e.g., laboratory) is

competent to carry out specific tasks or specific types of

tests. See also Certification.

Accredited laboratory: A laboratory that has been evaluated and given approval to

perform a specified measurement or task, usually for a

specific property or analyte and for a specified period of

time.
A-5

Acceptance limits: Data quality limits specified by the National Lead Laboratory

Accreditation Program for analytical method performance. 

Accuracy: The degree of agreement between an observed value and

an accepted reference value. Accuracy includes a

combination of random error (precision) and systematic error

(bias) components which are due to sampling and analytical

operations; a data quality indicator. See Precision and Bias.

Aliquot: See Subsample.

Analytical blank: See Digestion blank.

Bias: The systematic error manifested as a consistent positive or

negative deviation from the known true value.

Blind sample: A subsample submitted for analysis with a composition and

identity known to the submitter but unknown to the analyst

and used to test the analyst's or laboratory's proficiency in

the execution of the measurement process. 

Calibrate: To determine, by measurement or comparison with a

standard, the correct value of each scale reading on a meter

or other device, or the correct value for each setting of a

control knob. The levels of the calibration standards should

bracket the range of planned measurements. See

Calibration curve.

Calibration blank: See Initial calibration blank. 

Calibration-check: See Calibration verification.

Calibration-check See Calibration verification.

standard:

Calibration curve: The graphical relationship between the known values for a

series of calibration standards and instrument responses.

Calibration drift: The difference between the instrument response and a

reference value after a period of operation without

recalibration. See Continuing calibration verification.

Calibration standard: A substance or reference material used to calibrate an

instrument.
A-6

Calibration solution: See Calibration standard.

Calibration verification: See Initial or continuing calibration verification. 

Certification: The process of testing and evaluation against specifications

designed to document, verify, and recognize the

competence of a person, organization, or other entity to

perform a function or service usually for a specified time. 

See also Accreditation.

Certified Reference A reference material that has one or more of its property

Material (CRM): values established by a technically valid procedure and is

accompanied by or traceable to a certificate or other

documentation issued by a certifying body. See Certification

and Reference material.

Chain of custody: An unbroken trail of accountability that insures the physical

security of samples, data, and records.

Check sample: An uncontaminated sample matrix spiked with known

amounts of analytes, usually from the same source as the

calibration standards. It is generally used to establish the

stability of the analytical system, but may also be used to

assess the performance of all or a portion of the

measurement system. See also Quality control sample.

Continuing calibration A standard solution which has no analyte and is used to

blank (CCB): verify blank response and freedom from carryover. The

CCB should be analyzed after the CCV and after the

Interference Check Standard (ICS). 

Continuing calibration A standard solution (or set of solutions) used to verify

verification (CCV): freedom of excessive instrumental drift. The concentration to

be near mid-range of linear curve. The CCV should be

matrix matched to acid content present in sample

digestates. The CCV should be analyzed before and after

all sample digests and periodically throughout the analyses

of sample digests.

Control chart: A graph of some measurement plotted over time or

sequence of sampling, together with control limit(s) and,

usually, a central line and warning limit(s).

Control sample: See Laboratory control sample.
A-7

Corrective action: Action taken to correct a deficiency noted in a technical

systems audit. See Deficiency and Technical systems audit.

Deficiency: A failure to fully comply with the requirements of the NLLAP

program, usually noted during a technical systems audit. 

See NLLAP and Technical systems audit.

Digestion blank: A mixture of all reagents used for the digestion of paint, soil,

or dust matrices but without the matrix. This blank, is carried

through all steps of the analysis starting with the digestion

step. This blank evaluates the process for contamination

from the laboratory.

Duplicate analyses or The analyses or measurements of the variable of interest

measurements: performed identically on two subsamples of the same

sample. The results from duplicate analyses are used to

evaluate analytical or measurement precision but not the

precision of sampling, preservation, or storage internal to the

laboratory.

Duplicate samples: Two samples taken from and representative of the same

population and carried through all steps of the sampling and

analytical procedures in an identical manner. Duplicate

samples are used to assess variance of the total method

including sampling and analysis. 

External quality control: Activities that are routinely initiated and performed by

persons outside of normal operations to assess the

capability and performance of a measurement process.

Field blank: A clean sample of matrix (e.g., paint, soil, dust, wipe) carried

to the sampling site, exposed to the sampling conditions

(e.g., bottle caps removed), returned to the laboratory,

treated as an environmental sample, and carried through all

steps of the analysis. For example, clean quartz sand,

non-Pb containing paint, or a clean wipe could be used as a

field blank. The field blank, which should be treated just like

the sample, evaluates possible site contamination sources

such as airborne contaminants.

Initial calibration A standard solution that contains no analyte and is used

blank (ICB): for initial calibration and zeroing instrument response. The

ICB must be matrix matched to acid content present in

sample digestates. The ICB should be measured during

calibration and after calibration. 
A-8

Initial calibration A standard solution (or set of solutions) used to verify

verification (ICV): calibration standard levels. Concentration of analyte to be

near mid-range of linear curve which is made from a stock

solution having a different manufacturer or manufacturer lot

identification than the calibration standards. The ICV must

be matrix matched to acid content present in sample

digestates. The ICV should be measured after calibration

and before measuring any sample digestates. 

Instrument maintenance A chronological record of preventive and emergency

log: maintenance performed on an analytical instrument. The

logs include record of calls, service technician summaries,

records of calibration etc.

Interference check A standard solution (or set of solutions) used for ICP-AES

standard (ICS): to verify accurate analyte response in the presence of

possible spectral interferences from other analytes present

in samples. The concentration of analyte to be less than

25% of the highest calibration standard, concentration of

interferant will be 200 μg/Ml of Al, Ca, Fe, and Mg. The ICS

must be matrix matched to acid content present in sample

digestates. 

Internal quality control: See Intralaboratory quality control.

Internal standard: A standard added to a test portion of a sample in a known

amount and carried through the entire demonstration

procedure as a reference for calibration and controlling the

precision and bias of the applied analytical method.

Intralaboratory precision: A measure of the method/sample specific analytical variation

within a laboratory, usually given as the standard deviation

estimated from the results of duplicate/replicate analyses. 

Intralaboratory quality The routine activities and checks, such as periodic

control: calibrations, duplicate analyses, and spiked samples, that

are included in normal internal procedures to control the

accuracy and precision of measurements.

Laboratory blank: See Digestion blank.

Laboratory control A matrix-based reference material with an established

sample (LCS): concentration obtained from a different outside source and

traceable to NIST or other reference materials. The LCS is

carried through the entire procedure from digestion through
A-9

analysis as a field sample. The purpose of the LCS is to

evaluate bias of the method. 

Laboratory systems audit: See Technical systems audit.

Matrix blank: A sample of the matrix (paint chips, soil, dust) but without the

analyte (Pb). This sample goes through the complete analysis

including digestion. 

Method blank: See Digestion blank.

Method performance: A general term used to document the characteristics of a

method. These characteristics usually include method

detection limits, linearity, precision, accuracy and bias. 

Method detection limit The minimum concentration of an analyte that, in a given

(MDL): matrix and with a specific method, has a 99% probability of

being identified, qualitatively or quantitatively measured, and

reported to be greater than zero. 

Mobile laboratory: A mobile laboratory is a self-contained, mobile facility that

moves under its own power or is conveyed on a trailer, and

does not remain at a site for more than two years.

NLLAP requirements: Requirements specified by the EPA National Lead

Laboratory Accreditation Program (NLLAP) in order to be

accredited for lead analysis in paint, soil and dust matrices

by an EPA-recognized laboratory accreditation organization.

Precision: The degree to which a set of observations or measurements

of the same property, usually obtained under similar

conditions, conform to themselves; a data quality indicator. 

Precision is usually expressed as standard deviation,

variance, or range, in either absolute or relative terms. 

Primary standard: A substance or device with a property or value that is

unquestionably accepted (within specified limits) in

establishing the value of the same or related property of

another substance or device.

Proficiency testing: A systematic program in which one or more standardized

samples is analyzed by one or more laboratories to

determine the capability of each participant.

Quality assurance (QA): An integrated system of activities involving planning, quality

control, quality assessment, reporting, and quality
improvement to ensure that a product or service meets defined standards of quality

within a stated level of confidence.

Quality assurance See Quality assurance.

program:

Quality assurance See Quality manager.

coordinator:

Quality control (QC): The overall system of technical activities whose purpose is

to measure and control the quality of a product or service so

that it meets the needs of users. The aim is to provide

quality that is satisfactory, adequate, dependable, and

economical.




A-14

(BLANK PAGE)
B-1

APPENDIX B

ASSESSOR CHECKLIST FOR LABORATORIES ENGAGED 

IN THE ANALYSIS OF Pb

 IN PAINT, SOILS, AND DEPOSITED DUST

 (INCLUDING WIPE SAMPLES AND VACUUMED DUST)
B-2

(BLANK PAGE)
B-3

ASSESSOR CHECKLIST FOR LABORATORIES

ENGAGED IN THE ANALYSIS OF

Pb IN PAINT, SOILS AND DEPOSITED DUST,

INCLUDING WIPE SAMPLES AND VACUUMED DUST

Checklist DISTRIBUTION AND INSTRUCTIONS

This checklist should be distributed to the laboratory

personnel prior to the on-site assessment. The laboratory

should perform a self-assessment and check off each item

examined. The laboratory should use an "x" for the check-off

column. Comments should be entered in the space provided

for all "no" entries and initialed. The completed checklist

should be signed by the responsible laboratory person and

returned to the assigned assessor for his/her review prior to the

scheduled site assessment. The assessor will use this

completed checklist to evaluate the laboratory. The assessor

will check each item using a tick mark ` and add comments to

each question as appropriate. The assessor will initial any

comments and sign the completed checklist. Copies of the

completed checklist should be provided to the laboratory

during the closing conference. The checklist should not be

filled out in pencil.
B-4

(BLANK PAGE)
B-5

ASSESSOR CHECKLIST

1. Background: Record comments or answers to the information-type

questions in the space provided. The numbering of the checklist follows the

corresponding paragraph numbers of ISO Guide 25-1990. 

2. Name of Laboratory: 

Address: City: State: 

Telephone: FAX: 

3. Personnel Information (Names, Education, Training, Responsibilities):

3.1 Laboratory Manager: 

 

3.2 Principal Chemists: 

 

 

 

 

3.3 Technicians: (summarize qualifications and numbers) 

 

 

 

3.4 Quality Assurance Officer: 

3.5 Manager of Sample Control: 

3.6 Statistician: 
B-6

(BLANK PAGE)
B-7

Yes No N/A

 4.0 ORGANIZATION AND MANAGEMENT

 4.1 Is the laboratory legally identifiable?

 Comments:

 4.2 Does the laboratory have managerial staff with the authority

 and resources needed to discharge their duties?

 Comments:

 4.3 Has the laboratory specified and documented in job descrip-

 tions the responsibility, authority, and interrelationship of all

 personnel who manage, perform, or verify work affecting the

quality of tests?

 Comments:

 4.4 Does the laboratory provide supervision by persons familiar

 with the test methods and procedures, the objectives of the

 test, and the assessment of the results?

 Comments:

 4.5 Does the laboratory have a technical manager (however

 named) who has overall responsibility for the technical

 operations?

 Comments:

 4.6 Does the laboratory have a quality manager (however named)

 who has responsibility for implementation of the quality system

 who functions independently from those who are responsible

 for generation of the data?

 Comments:

 4.6.1 Does the QA manager have the power to oversee the situation,

 identify problems, and make corrections?

 Comments:

 4.7 Does the laboratory have deputies in case of absence of

 the technical or quality manager?

 Comments:
Yes No N/A

B-8

 5.0 QUALITY SYSTEM, AUDIT, AND REVIEW

 5.1 Is the quality system documented in a quality manual? 

 Comments:

 5.1.1 Is the quality manual and related supporting documents

 available for use by laboratory personnel?

 Comments:

 5.1.2 Are the quality policies and objectives communicated to, 

 understood, and implemented by all laboratory personnel 

 concerned?

 Comments:

 5.1.3 Is the quality manual kept current under the responsibility of the

quality manager?

 Comments:

 5.1.4 Are new employees introduced to the quality manual and how

 often do employees review the manual? Describe in comments

 below.

 Comments:

 5.1.5 Does the laboratory have an in-house training program? 

 Describe the type and frequency of training in comments

 below.

 Comments:

 5.1.6 Is the quality system reviewed at least once per year by

 management to ensure its continuing suitability and 

 effectiveness?

 Comments:

 5.2 Does the quality manual and related supporting documents contain:

 5.2.1 A quality assurance policy statement, including objectives and

 commitments, by top management?

 Comments:

 5.2.2 Organization charts that describe the management structure

 of the laboratory and its place in any parent organization?

 Comments:

 5.2.3 Job descriptions of key staff and reference to job descriptions

 of other staff?
Yes No N/A

B-9

 Comments:

 5.2.4 Identification of laboratory's approved signatories for reports?

 Comments:

 5.2.5 Procedures for achieving traceability of measurements?

 Comments:

 5.2.6 The laboratory's scope of testing?

 Comments:

 5.2.7 Procedures for reviewing methods, facilities, and resources

 necessary to complete proposed new work prior to initiation of

 new work?

 Comments:

 5.2.8 Standard operating procedures for instrumental analysis

 techniques used?

 Comments:

 5.2.9 Procedures for sample handling?

 Comments:

 5.2.10 Reference to reagents and reference standards used?

 Comments:

 5.2.11 Standard operating procedures for instrument calibration?

 Comments:

 5.2.12 Reference to verification practices including interlaboratory

 comparisons, proficiency testing programs, use of reference

 materials, and internal quality control schemes?

 Comments:

 5.2.13 Procedures to be followed for feedback and corrective action

 whenever testing discrepancies are detected, or departures

 from documented policies and procedures occur?

 Comments:

 5.2.14 Arrangements for exceptions permitting departures from

 documented policies/procedures?
Yes No N/A

B-10

 Comments:

 5.2.15 Procedures for audit and review?

 Comments:

 5.3 Are audits of laboratory activities conducted to verify

 compliance with the quality system?

 Comments:

 5.3.1 Are audits conducted to ensure that analysts actually follow

 SOPs?

 Comments:

 5.3.2 Are all audit and review findings and any corrective actions that

 arise from them documented?

 Comments:

 5.4 Does the laboratory ensure the quality of results by

 implementing and reviewing internal quality control schemes

 using, whenever possible, statistical techniques? 

 Comments:

 5.4.1 Are control chart data maintained?

 Comments:

 5.4.2 Do records indicate what corrective action has been taken

 when results fail to meet QC criteria?

 Comments:

 5.4.3 Does the laboratory regularly use NIST SRMs or other certified

 reference materials?

 Comments:

 5.4.4 Are QC data for all analytical results retrievable?

 Comments:

 5.4.5 Are method detection limits documented?

 Comments:

 5.4.6 Are routine analyses of reagents used for dilutions and

 digestions performed?
Yes No N/A

B-11

 Comments:

 5.4.7 Do supervisory personnel review the data calculations and QC 

 results?

 Comments:

 5.4.8 Are deviations or deficiencies in QC documented and reported

 to management?

 Comments:

 5.5 Does the laboratory participate in the ELPAT proficiency testing

 program for each matrix that is routinely run in the laboratory?

 Comments:

 5.5.1 Are ELPAT samples treated as regular samples and analyzed

 with the same method and by the same analyst who performs

 routine analyses?

 Comments:

 5.5.2 Environmental lead laboratories must participate in the

 NIOSH/AIHA environmental lead proficiency analytical testing

(ELPAT) program. Please attach copies of the two most recent

 ELPAT results and provide a summary of your investigation

 and findings regarding the laboratory's handling of any "not 

 acceptable" results.

 Comments:

 5.6 Are there QC procedures (SOPs) which address the following:

 5.6.1 Reagent and method blank analysis?

 Comments:

 5.6.2 Glassware cleaning?

 Comments:

 5.6.3 Sampling and subsampling?

 Comments:
Yes No N/A

B-12

 5.6.4 Replicate/duplicate analyses?

 Comments:

 5.6.5 Spiked and blank sample analysis?

 Comments:

 5.6.6 Blind samples?

 Comments:

 5.6.7 Control charts?

 Comments:

 5.6.8 Calibration standards?

 Comments:

 5.6.9 Reference samples?

 Comments:

 5.6.10 Internal standards?

 Comments:

 5.7 Is at least the following minimum QC practiced in the laboratory:

 5.7.1 One method blank in 20 (5% or one per batch).

 Comments:

 5.7.2 One method spike in 20 (5% or one per batch).

 Comments:

 5.7.3 One duplicate or spiked duplicate in 20 (5% or one per batch).

 Comments:

 5.7.4 One laboratory control sample (consists of a representative

 matrix spiked with the target analytes) in 20 (5% or one per

 batch).

 Comments:

 5.7.5 Has the laboratory established control limits for all the above

 types of QC samples?

 5.7.6 If yes, can the laboratory demonstrate the basis for the

 established limits?
Yes No N/A

B-13

 Comments:

 6.0 PERSONNEL

 6.1 Does the laboratory have sufficient personnel, with the required

 education, training, knowledge, and experience for their

 assigned functions?

 Comments:

 6.2 Do laboratory personnel have the following minimum education,

 experience and training:

 6.2.1 Supervisory Inorganic Chemist responsible for technical effort.

 Name: Experience: 

 Degree: B.S. Chemistry or related science

 Recommended Experience: 3 years, nonacademic, 2 years

 metals analysis.

 Comments:

 6.2.2 Inductively Coupled Plasma-Atomic Emission Spectroscopist

 Name: Experience: 

 Degree: B.S. Chemistry, or related science

 Recommended Experience: 1 year minimum

 Training: Satisfactory completion of a short course on ICP.

 Comments:

 6.2.3 Flameless Atomic Absorption Spectroscopist

 Name: Experience: 

 Degree: B.S. Chemistry, or related science

 Recommended Experience: 1 year minimum

 Training: Satisfactory completion of a short course on GFAA

 Comments:
Yes No N/A

B-14

 6.2.4 Flame AA Spectroscopist

 Name: Experience: 

 Degree: B.S. Chemistry, or related science

 Recommended Experience: 1 year minimum

 Comments:

 6.2.5 Inorganic Sample Preparation Technician

 Name: Experience: 

 Recommended Experience: 3 months minimum

 Comments:

 6.2.6 Routine Sample Analyst

 Name: Experience: 

 Recommended Experience: 6 months minimum 

 Comments:

 6.3 Are records maintained on the qualifications, training, skills and

 experience of the technical personnel?

 Comments:

 6.4 Is there documented evidence of analyst proficiency for each

 test method performed?

 Comments:

 7.0 FACILITIES AND ENVIRONMENT

 7.1 Does the laboratory:

 7.1.1 Use distilled/demineralized water that it can demonstrate to be

 essentially free of lead?

 Comments:

 7.1.2 Routinely check and record the conductivity of

 distilled/demineralized water (for a continuous system, check

 should be per batch or daily)?

 Comments:

 7.1.3 Provide separate contamination-free work areas for sample

 preparation and sample analysis?

 Comments:
Yes No N/A

B-15

 7.1.4 Provide facilities for separate storage of samples, digests,

 acids, reference materials, and standards with temperature and

 humidity control as required?

 Comments:

 7.1.5 Have glassware cleaning facilities suitable for metals analysis?

 Comments:

 7.2 Does the laboratory have a Chemical Hygiene Plan as

 specified by the OSHA Laboratory Standard (29 CFR

 1910.1450, "Occupational Exposure to Hazardous Chemicals in

 Laboratories")?

 Comments:

 7.2.1 Does the laboratory provide exhaust hoods for sample

 digestion and vent hoods for instrumentation with sufficient flow

 to prevent cross-contamination?

 Comments:

 7.2.2 Does the laboratory provide safety equipment as specified in

 the Chemical Hygiene Plan, such as safety showers, eyewash

 stations, chemical spill kits?

 Comments:

 7.2.3 Does the laboratory provide personal protective equipment as

 specified in the Chemical Hygiene Plan, such as gloves, face

 shields, acid resistant aprons?

 Comments:

 7.3 Are material safety data sheets readily available to the

 laboratory analyst? 

 Comments:

 7.4 Does the laboratory have documented procedures and facilities

 in place for storage, and disposal of chemical wastes, including

 acids and lead?

 Comments:
Yes No N/A

B-16

 8.0 EQUIPMENT/INSTRUMENTATION

 Note: Supplemental information on equipment should be listed

 in the table at the end of this checklist.

 8.1 Is the laboratory furnished with all items of equipment required

 for the analysis of Pb in paint, dust, and soil?

 Comments:

 8.2 What type of equipment does the laboratory have for digestion? 

Identify types of heating units used for digestion below and

 provide complete details in equipment supplement.

( ) Hot plate ( ) Microwave Oven ( ) Other, specify

 8.2.1 If a hot plate is used for digestion, does it have temperature

 control within requirements as stated in the method SOPs?

 Comments:

 8.2.2 If a microwave oven is used for digestion, does the unit have

 variable power levels that meet requirements as stated in

 method SOPs?

 Comments:

 8.2.2.1 Has the microwave unit been calibrated according to

 manufacturer's recommendations?

 Comments:

 8.2.2.2 How often has the unit been calibrated and does the schedule

 follow that described in the SOP?

 Comments:

 8.3 What type of analytical instrument does the laboratory use? 

 Identify types of instruments below and provide complete

 details in equipment supplement.

( ) FLAA ( ) GFAA ( ) ICP-AES ( ) Other, specify

 8.3.1 If a FLAA Spectrophotometer is used, is there a detailed

 SOP describing its operation and calibration?

 Comments:

 8.3.1.1 Does the FLAA have a monochromoter, wavelength range, and

 lamps specified in the method SOP?

 Comments:
Yes No N/A

B-17

 8.3.1.2 Are fuels and oxidants commercial grade?

 Comments:

 8.3.1.3 Is there a filter moisture trap between the air source and the

 spectrophotometer?

 Comments:

 8.3.1.4 Are fuel tank pressures greater than instrument operating

 pressure?

 Comments:

 8.3.1.5 Are flash-back arresters and heaters in use where needed?

 Comments:

 8.3.1.6 Are burner heads specified in the method SOP used?

 Comments:

 8.3.1.7 Are burner head gases removed by ventilation?

 Comments:

 8.3.1.8 Is the burner head clean and free of build-up?

 Comments:

 8.3.2 If the laboratory has GFAA, is there a detailed SOP describing

 its operation and calibration?

 Comments:

 8.3.2.1 What type of GFAA background correction is used? 

( ) Deuterium Arc ( ) Smith-Heiftje ( ) Zeeman

 Comments:

 8.3.2.2 How often is the graphite tube changed and the chamber

 cleaned (every )? Is this documented?

 Comments:

 8.3.3 Lamps used for FLAA and GFAA may be of various types. 

 Are they: single element ; multi-element ; electrodeless 

 Comments:
Yes No N/A

B-18

 8.3.3.1 Are back-up lamps available as spare parts?

 Comments:

 8.3.4 If the laboratory has ICP-AES, is there a detailed SOP covering

 its use and calibration?

 Comments:

 8.3.4.1 Is a background correction technique in use and documented

 according to the SOP?

 Comments:

 8.3.4.2 Has the absence of spectral interference for analytes of interest

 been checked, corrected, and documented?

 Comments:

 8.3.4.3 Has salt build-up on the nebulizer been controlled?

 Comments:

 8.3.4.4 When a matrix interference is encountered, are procedures

 specified in the SOP used to correct/eliminate potential

 interference?

 Comments:

 8.3.4.5 Is the spectrometer equipped with an argon gas supply?

 Comments:

 8.3.4.6 Are high purity grade or equivalent nitric and hydrochloric

 acids and deionized (distilled) water used for sample

 processing and standards preparation?

 Comments:

 8.4 General equipment requirements:

 8.4.1 Are analytical balance/pan balances calibration covered by an

 SOP?:

 Comments:

 8.4.1.2 Do records document regular calibration using certified

 weights?

 Comments:

 8.4.1.3 Do records show annual servicing and calibration for all

 balances?
Yes No N/A

B-19

 Comments:

 8.4.2 Labware:

 8.4.2.1 Does the laboratory have deionized/distilled Class A water and

 an SOP describing the checks on conductivity and lead

 contamination?

 Comments:

 8.4.2.2 Is there documentation of the lack of contamination on

glassware used for metals analysis?

 Comments:

 8.4.3 Conductivity meter:

 8.4.3.1 Do records show a calibration check daily, or before each use,

 whichever is less frequent?

 Comments:

 8.4.4 Autopipetors/dilutors:

 8.4.4.1 Does the laboratory keep records showing delivery volumes are

 checked at least monthly? 

 Comments:

 8.5 Does the laboratory maintain records on each major item of

 equipment? Do the records include:

 8.5.1 The name of the equipment?

 Comments:

 8.5.2 The manufacturer's name, model number, and serial number or

 other unique identification?

 Comments:

 8.5.3 Condition when received (e.g., new, used, reconditioned)?

 Comments:

 8.5.4 Date received and date placed in service?

 Comments:
Yes No N/A

B-20

 8.5.5 Copy of the manufacturer's instruction manual(s) readily

 available to the analyst?

 Comments:

 8.5.6 Dates and results of instrument calibrations and date scheduled

 for the next calibration?

 Comments:

 8.5.7 Detailed maintenance SOPs, including names and telephone

 numbers to call for service?

 Comments:

 8.5.8 Detailed log of preventive maintenance and service calls which

 include dates and repair records?

 Comments:

 8.6 Has any equipment that has been damaged, or produces

 unacceptable results, been taken out of service until it has

 been repaired and then shown by calibration, verification, or

 test to perform satisfactorily prior to being placed back into

 service?

 Comments:

 9.0 CALIBRATION/STANDARD OPERATING PROCEDURES 

 9.1 Is all instrumentation having an effect on the accuracy and

 validity of tests calibrated before being put into service? 

 Comments:

 9.1.1 Is the initial calibration and instrument checkout documented as

 instruments are brought into service, either when new or after

 repair?

 Comments:

 9.1.2 Are instrument calibration records kept near the instrument and

 are they used by the analyst?

 Comments:

 9.2 Are calibration standards traceable to NIST standard reference

 materials?

 Comments:

 9.2.1 Are NIST standard reference materials used for calibration or 

 traceability studies only and for no other purpose?
Yes No N/A

B-21

 Comments:

 9.2.2 Are separate reference materials dedicated to calibration

 purposes only and not used as LCS?

 Comments:

 9.3 Do SOPs that provide for method calibration contain the

 following information: 

 9.3.1 Are standard curves prepared to adequately cover the

 expected concentration ranges of the samples?

 Comments:

 9.3.2 For methods using AAS, are standard calibration curves made

 up of a reagent blank, and a minimum of three standards

 covering the concentration range of the samples?

 Comments:

 9.3.3 Are new curves prepared whenever out-of-control conditions

 are indicated and after new reagents are prepared?

 Comments:

 9.3.4 When analyses are performed, is the standard curve verified

(checked) by use of at least a method blank and one standard?

 Comments:

 9.3.4.1 Are these checks within ±10% of the original values?

 Comments:

 10.0 METHODS

 10.1 Method Selection. Does the laboratory:

 10.1.1 Use recognized (EPA recommended) methodologies and

 instrumentation for each analysis performed, if such methods

 are available?

 Comments:
Yes No N/A

B-22

 10.1.2 Select methods mandated by legal requirements, recognized

 published methods, or methods developed and validated by the

 laboratory?

 Comments:

 10.1.3 Have site-specific SOPs for sample analysis?

 Comments:

 10.1.4 Use alternative analytical techniques that have undergone an

 approved validation study?

 Comments:

 10.1.5 Make available to the client fully documented and validated

 non-standard method information?

 Comments:

 10.1.6 Require that modifications to test method SOPs be

 documented and approved by the Technical Manager (or

 however named) before being implemented?

 Comments:

 10.1.7 Make available to analysts SOPs, standards, manuals, and

 reference data relevant to the work of the laboratory?

 Comments:

 10.1.8 Regularly update SOPs and document changes in the QA

 manual?

 Comments:

 10.1.9 Have method performance criteria (method detection limits,

 precision, accuracy, linearity, etc.) been documented in an

 SOP?

 Comments:

 10.1.10 Have demonstrated acceptable performance for each analytical

 test method using performance evaluation samples?

 Comments:
Yes No N/A

B-23

 10.2 Standards and Calibration. Does the laboratory:

 10.2.1 Have SOPs for standards preparation?

 Comments:

 10.2.2 Use reagent grade or higher purity chemicals to prepare

 standards?

 Comments:

 10.2.4 Use NIST SRMs (SRM 3128, Pb in 10% nitric acid) as a

 primary standard?

 Comments:

 10.2.5 Prepare fresh analytical standards at a frequency consistent

 with good QC?

 Comments:

 10.2.6 Properly label reference materials/reagents with concentrations,

 date of preparation, expiration date, and the identity of the

 person preparing the reagent?

 Comments:

 10.3 Does the analytical run contain, where applicable:

 10.3.1 An initial calibration blank?

 Comments:

 10.3.2 A method blank?

 Comments:

 10.3.3 A matrix-based laboratory control sample?

 Comments:

 10.4 Are sample pretreatment and preservation documentation

 available to the analyst?

 Comments:

 10.5 Is the method of standard addition in use where needed?

 Comments:
Yes No N/A

B-24

 10.6 Are method calculation and data transfers checked by

 someone other than the analyst?

 Comments:

 11.0 HANDLING OF TEST SAMPLES

 11.1 Does the laboratory have a documented system for uniquely

 identifying the sample to be tested, to ensure that there can be

 no confusion regarding the identity of such samples at any

 time?

 Comments:

 11.2 Upon receipt, does the laboratory record the condition of the

 sample, including the presence of debris, substrate, and any

 abnormalities that may affect the quality of the analytical result?

 Comments:

 11.2.1 If there is any doubt as to the item's suitability for analysis, or if

 the item does not conform to the description provided, or if the

 test required is not fully specified, does the laboratory consult

 with the client for further information before proceeding?

 Comments:

 11.2.2 Does the laboratory establish whether the sample has received

 all necessary preparation, or whether the client requires

 preparation to be undertaken or arranged by the laboratory

(e.g., screening out debris, grinding to a fine mesh, removing

 substrate)?

 Comments:

 11.3 Does the laboratory have documented procedures for the

 retention or safe disposal of samples?

 Comments:

 11.4 Follow documented chain-of-custody procedures, when

 required by the client?

 Comments:
Yes No N/A

B-25

 12.0 RECORDS

 12.1 Has the laboratory established and maintained a records

 system that ensures that:

 12.1.1 All observations and calculations are recorded in a permanent

 manner (such as laboratory notebooks, pro forma work sheets,

 or magnetic media) at the time they are made and that the

 units of measurement in which observations are recorded are

 stated?

 Comments:

 12.1.2 Original records are uniquely identified and traceable to the

 samples to which they refer and to any analysis reports based

 upon them?

 Comments:

 12.1.3 Records are traceable, retrievable, and legible and include

 sufficient information and explanation such that they can be

 readily interpreted by staff other than those responsible for their

generation?

 Comments:

 12.1.4 Records contain sufficient information to permit identification of

 possible sources of error and to permit, where feasible and

 necessary, satisfactory repetition of the analysis under the

 original conditions?

 Comments:

 12.1.5 Records contain sufficient details of any significant departures

 from specified procedures, including authorizations for such

 departures?

 Comments:

 12.1.6 Records are checked for data transcription or calculation

 errors?

 Comments:

 12.1.7 Records identify the person or persons responsible for their

generation and for the checking of data transcriptions and

 calculations?

 Comments:
Yes No N/A

B-26

 12.1.8 Corrections or amendments to test records are made in a

 manner that does not obliterate the original data and are

 signed or initialled by the person responsible?

 Comments:

 12.2 Are all records and reports safely stored, held secure and in

 confidence for the client?

 Comments:

 12.3 Are hard copy analysis records protected from loss damage,

 misuse or deterioration and retained for a designated period in

 a manner that permits retrieval?

 Comments:

 12.4 Are analysis records that are created and/or retained on

 magnetic media (e.g., computer disks) or photographic media

(e.g., microfiche) stored in a manner that protects them from

 the hazards that affect such media, and is provision made for

 the printing of such records when required?

 Comments:

 13.0 REPORTS

 13.1 Are the laboratory's results of each analysis that is carried out

 reported accurately, clearly, unambiguously?

 Comments:

 13.2 Does each report include at least the following information:

 13.2.1 A title (e.g., "Analysis Report")

 Comments:

 13.2.2 The name and address of laboratory and location where the

 analysis was carried out, if different from the address of the

 laboratory?

 Comments:

 13.2.3 A unique identification number for the report, for each page,

 and the total number of pages?

 Comments:

 13.2.4 The name and address of client?

 Comments:
Yes No N/A

B-27

 13.2.5 Reference to the field sampling procedure, if known by the

 laboratory?

 Comments:

 13.2.6 A description and unambiguous identification of the sample

 tested?

 Comments:

 13.2.7 A characterization and condition of the samples?

 Comments:

 13.2.8 The date of receipt of the samples and date(s) of performance

 of the tests, including digestion dates, and analysis dates, if

 different?

 Comments:

 13.2.9 An identification of the sample digestion and instrumental 

 analysis methods used?

 Comments:

 13.2.10 Description of any deviations from, additions to, or exclusions

 from the SOPs, relevant to a specific analysis?

 Comments:

 13.2.11 Measurements, and derived results, supported by tables, and

graphs as appropriate, including identification of any missing

 data?

 Comments:

 13.2.12 A statement of the estimated uncertainty of the analysis result?

 Comments:

 13.2.13 A signature and title, or equivalent identification, of person(s)

 accepting responsibility for the content of the report (however

 produced), and date of issue?

 Comments:
Yes No N/A

B-28

 13.3 Does the laboratory notify clients promptly, in writing, of any

 event, such as the identification of defective measuring or test

 equipment that casts doubt on the validity of results given in

 any test report or amendment to a report?

 Comments:

 13.4 Has the laboratory ensured the confidentiality of data when

 clients require transmission of test results by telephone, telex,

 facsimile, or other electronic or electromagnetic means, by use

 of documented procedures for electronic data transmission?

 Comments:

 14.0 COMPLAINTS

 14.1 Does the laboratory have documented policy and procedures

 for the resolution of complaints received from clients or other

 parties about the laboratory's activities?

 Comments:

 14.2 Does the laboratory maintain records of all complaints and of

 the actions taken by the laboratory?

 Comments:

 14.3 Where a complaint, or any other circumstance, raises doubt

 concerning the laboratory's compliance with the laboratory's

 policies or procedures, or with the applicable requirements, or

 otherwise concerning the quality of its tests, does the

 laboratory ensure that those areas of activity and responsibility

 involved are promptly audited according to requirements listed

 in the quality manual?

 Comments:
B-29

SUPPLEMENTAL INFORMATION ON MAJOR EQUIPMENT

Instrument Manufacturer Model Serial Number Installat```````````````````````````````````````````````````````````````````````````````````````ICP-AES Data System

AA (Flame)

Data System

AA (GFAA)

Data System

Microwave Digestion Unit

Comments on Instruments and Data Systems: