SEPA
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
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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
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DISCLAIMER
This document has been reviewed and approved for publication by the
Office of Prevention, Pesticides, and Toxic Substances, U.S. Environ-
mental Protection Agency. The use of trade names or commercial
products does not constitute Agency endorsement or recommendation for
use.
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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.
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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).
* 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.
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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, UT84123
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 ManerRoad
Smyrna, GA 30080
A lead assessor for the American Association for Laboratory Accreditation
(A2LA).
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Mr. Peter Linger
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
VII
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VIM
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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
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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
* 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.
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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.
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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 require-
ments 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.
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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
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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 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.
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.
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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 Lead-
based 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 require-
ments 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.
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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
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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 on-
site 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.
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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).
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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:
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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
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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
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areas and other procedures to minimize sample contamination. Documenta-
tion 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:
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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,
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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.
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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.
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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).
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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
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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.
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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
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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 deter-
minations 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
verification (ICV)
Initial calibration blank
(ICB)
Continuing calibration
verification (CCV)
Interference check sample
(ICS)
Continuing calibration
blank (CCB)
Once per run after
calibration
Once per run at the
beginning of run
Before and at the end of a
sample run, as well as
every 10 samples
Beginning and end of each
run or twice every 8 hr
After each ICS and CCV
Within ±10% of known
value
Absolute value not more
than 20% of the
regulatory limit or level
of concern
Within ±10% of known
value for ICP or FLAA;
within ±20% for GFAA
Within 20% of known
value
Absolute value not more
than 20% of the
regulatory limit or level
of concern
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QC sample
Frequency
Acceptance limits
Laboratory control sample
(LCS)
Matrix spike
Duplicate sample
Method blank
1 per 20 samples or batch
(5%)
1 per 20 samples or batch
(5%)
1 per 20 samples or batch
(5%)
1 per 20 samples a batch
(5%)
Within ±20% of known
value
Within ±25% of known
value
Within ±25% relative
percent difference
(RPD)
Absolute value not more
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 abate-
ment 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.
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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.
Use of a riffle box to separate coal and coke is described in ASTM Method (D5).
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Determine the Pb background level in the "blank" wipe submitted with the
samples. Ideally, Pb background levels of wipe samples should be deter-
mined prior to sample collection. If the background level is greater than 5 ug
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 ug per wipe are insignificant at HUD clearance
recommendations of 200 ug 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 ug 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.
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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. Cross-
contamination 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.
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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 HN03 or HN03/H202
Wet digestion using a hot plate with HN03 or HN03/H202
' Microwave digestion with HN03, HN03/HCI, or HN03/H202
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 HN03
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 HCI 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.
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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 ug Pb/mL to 20 ug Pb/mL, but can be
extended by rotating the burner head.
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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 require-
ments 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 uL of sample is used for analysis,
digest volume requirements are the smallest (10-25 uL). 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) orZeeman or Smith-Hieftje background
correction schemes. Matrix enhancement or suppression of the Pb-
absorbance 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 HCI 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 irrepro-
ducible. 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.
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Range of analysis: The linear range of analysis for an intermediate sample
size is from about 0.001 ug Pb/mL to 0.1 ug 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.
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Range of analysis: The linear range of analysis for the 220.35-nm line is
from about 0.2 ug Pb/mL to 3,000 ug 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 load-
ing, 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 recom-
mended 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.
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U.S. EPA Reference Method for the Determination of Lead in Suspended
Participate 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. EPA1990C).
*U.S. EPA SW-846 Method 601OA, Metals - Inductively Coupled Plasma
Emission Spectroscopy (U.S. EPA 1990c).
* These methods do not include a digestion technique and are for digests of Pb
prepared by one of the digestion techniques listed above.
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*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 aqueous-
based SRMs from NIST and that must be used for instrument calibration. The prep-
aration 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% HN03) SRM is suitable for calibrant
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% HN03). Matrix-based
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
* 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 601OA, 7420, or 7421 for completion of analysis.
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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 SRMsfrom 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
1579a
a
a
1648
2704
2709
2710
2711
2579
Description and date
Powdered Pb-based paint, Feb. 3, 1992
Powdered Pb-based paint (in progress)
Powdered Pb-based paint (in progress)
Urban particulate matter, Nov. 16, 1978
Buffalo River sediment, July 9, 1990
Baseline agricultural soil, Oct. 16, 1992
Highly contaminated soil, Oct. 16, 1992
Moderately contaminated soil, Oct. 16, 1992
Lead paint film on Mylar sheet, set of 5, July
7, 1992
Certified Pb value
11. 995% ±0.031
4.0%
0.5%
0.655% ± 0.008
161 ug/g ± 17
18.9 ug/g ±0.5
5532 ug/g ± 80
11 62 ug/g ±31
3.53 mg/cm2 ± 0.24
1.63 mg/cm2 ±0.08
1.02 mg/cm2 ±0.04
0.29 mg/cm2 ± 0.01
< 0.0001 mg/cm2
These NIST SRMs are under development.
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2.5.11.5 Other Reference Materials—
Reference materials from other sources are available, but they are not NIST-
certified 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.
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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.
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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 cross-
contamination 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.
* Calibration requirements are both instrument and method specific. SOPs for
specific analytical methods should be followed.
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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 perform-
ing 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.
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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
Spiked samples
Spiked sample
duplicates
Reference material
(standard reference)
Type 1 water—digest as a
sample with addition of all
reagents. Should reflect the
maximum treatment given any
one sample within the batch.
A portion of a sample is
fortified with all the target
analytes before preparation
and analyzed independently.
A portion of a same sample
used for the spiked sample is
fortified with all the target
analytes before preparation.
A material of known
composition, where analyte
levels are certified by the
manufacturer. These
materials should be traceable
to NIST standards.
1 per 20 samples, a
minimum of 1 per batch
1 per 20 samples per
matrix type, a minimum of
1 per batch
1 per 20 samples per
matrix type, a minimum of
1 per batch
1 per batch of samples
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TABLE 2. RECOMMENDED INSTRUMENTAL QC STANDARDS AND SPECIFICATIONS
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 calibration.
Measured value to be less than 5 times the instrumental detection
limit.
CO
00
Calibration
standards
Used to calibrate
instrument.
Must be matrix matched to acid content present in sample
digestates.
The high standard rerun is Must be measured prior to measuring any sample digestates.
used to check for high
response rollover. Correlation coefficient of' 0.995, as measured using linear
regression on instrument response (y) versus concentration (x).
The highest level calibration standard must be measured after
calibration. The measured value to fall within ±10% of known value.
ICV—Initial
calibration
verification
Used to verify calibration Concentration of analyte to be near midrange of linear curve. The
standard levels. ICV is made from a stock solution having a different manufacturer
or manufacturer lot identification than the calibration standards.
Must be measured after calibration and before measuring any
sample digestates.
Measured value to fall within ±10% of known value.
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TABLE 2 (CONTINUED)
Name
Use
Specification
CO
CD
ICS—Interference Used to verify accurate
check sample (for analyte response in the
ICP-AES only) presence of possible
spectral interferences
from other analytes
present in samples.
CCV—Continuing Used to verify freedom
calibration from excessive
verification instrumental drift.
Concentration of analyte to be less than 25% of the highest
calibration standard, concentrations of interferant will be 200 ug/mL
of Al, Ca, Fe, and Mg.
Must be analyzed at least twice, once before and once after all
sample digestates.
Measured analyte value to fall within ±20% of known value.
Concentration to be near midrange of linear curve.
Must be analyzed before and after all sample digestates and at a
frequency not less than every 10 sample digestates.
Measured value to fall within ±10% of known value for ICP-AES or
FLAA (±20% for GFAA), run 1 every 10 samples.
CCB—Continuing Used to verify blank
calibration blank response and freedom
from carryover.
Calibration standard that contains no analyte.
Must be analyzed after the CCV and after the ICS.
Measured value to be less than 5 times the instrumental detection
limit.
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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.
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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.
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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.
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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)
43
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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 self-
evaluation 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 on-
site 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.
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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—
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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 performance-
rating 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).
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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.
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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
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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.
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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 role-
playing 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).
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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.
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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 NLLAP-
recognized 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.
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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 NLLAP-
recognized 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.
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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.
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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.
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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.
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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.
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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.
AC GIH. Industrial Ventilation, A Manual of Recommended Practices, 21 st 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.
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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.
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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), Februarys, 1992.
NIST. Certificate of Analysis, SRM 2579 (Lead Paint Film on Mylar Sheet, Set of 5),
3.53 mg/cm2 ± 0.24; 1.63 mg/cm2 ± 0.08; 1.02 mg/cm2 ± 0.04; 0.29 mg/cm2 ± 0.01;
< 0.0001 mg/cm2, July 7, 1992.
NIST. Certificate of Analysis, SRM 2704 (Buffalo River Sediment), Pb 161 ±17 ug/g,
July 9, 1990.
NIST. Certificate of Analysis, SRM 2709 (Baseline Agricultural Soil), 18.9 ug/g ± 0.5,
October 16, 1992.
NIST. Certificate of Analysis, SRM 2710 (Highly Contaminated Soil), 5532 ug/g ± 80,
October 16, 1992.
NIST. Certificate of Analysis, SRM 2711 (Moderately Contaminated Soil),
1162 ug/g ± 31, October, 16, 1992.
NVLAP: National Voluntary Laboratory Accreditation Program Procedures, NISTIR
4493, dated November 1990 (DSC Title 15, Subtitle A, Chapter II, Part 7).
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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, Wl, 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 forSRM Users. NBS (NIST) Special Publication 260-100,
September 1985.
Linger, 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.
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Vassals, John R. Psychology of Auditing. Quality Progress, September 1977, p. 37.
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APPENDIX A
ACRONYMS AND GLOSSARY OF TERMS
A-1
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A-2
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APPENDIX A
ACRONYMS
AA
A2LA
ACIL
AIHA
ANSI
AOAC
APHA
ASTM
ASQC
ASTPHLD
AWWA
CCB
CCV
CERCLA
CDC
CMD
CNAEL
CRADA
CLP
CRM
EDL
ELLAC
ELPAT
EMPC
FLAA
GFAA
GLP
ICB
ICP-AES
ICP-MS
ICV
ICS
IDL
IMVL
ISO
LCS
LOQ
LSA
MCL
MDL
ACRONYMS AND GLOSSARY OF TERMS
Atomic Absorption
American Association for Laboratory Accreditation
American Council of Independent Laboratories
American Industrial Hygiene Association
American National Standards Institute
Association of Official Analytical Chemists
American Public Health Association
American Society for Testing and Materials
American Society for Quality Control
Association of State and Territorial Public Health Laboratory Directors
American Water Works Association
Continuing Calibration Blank
Continuing Calibration Verification
Comprehensive Environmental Responsibility, Compensation and Liability Act
Centers for Disease Control
Chemical Management Division
Committee on National Accreditation of Environmental Laboratories
Cooperative Research and Development Agreement
Contract Laboratory Program
Certified Reference Material
Estimated Detection Limit
Environmental Lead Laboratory Accreditation Committee (AIHA)
Environmental Lead Proficiency Analytical Testing (AIHA/NIOSH)
Estimated Maximum (Protocol) Concentration
Direct Flame Aspiration Atomic Absorption Spectrometry
Graphite Furnace Atomic Absorption Spectrometry
Good Laboratory Practices Standards (TSCA)
Initial Calibration Blank
Inductively Coupled Plasma Emission Spectrometry
Inductively Coupled Plasma-Mass Spectrometry
Initial Calibration Verification
Interference Check Standard
Instrument Detection Limit
Interlaboratory Method Validation Study
International Organization for Standardization
Laboratory Control Sample
Limit of Quantitation
Laboratory Systems Audit
Maximum Contaminant Level
Method Detection Limit
A-3
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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-4
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Acceptance limits:
Accuracy:
Aliquot:
Analytical blank:
Bias:
Blind sample:
Calibrate:
Calibration blank:
Calibration-check:
Calibration-check
standard:
Calibration curve:
Calibration drift:
Calibration standard:
Data quality limits specified by the National Lead Laboratory
Accreditation Program for analytical method performance.
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.
See Subsample.
See Digestion blank.
The systematic error manifested as a consistent positive or
negative deviation from the known true value.
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.
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.
See Initial calibration blank.
See Calibration verification.
See Calibration verification.
The graphical relationship between the known values for a
series of calibration standards and instrument responses.
The difference between the instrument response and a
reference value after a period of operation without
recalibration. See Continuing calibration verification.
A substance or reference material used to calibrate an
instrument.
A-5
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Calibration solution:
See Calibration standard.
Calibration verification: See Initial or continuing calibration verification.
Certification:
Certified Reference
Material (CRM):
Chain of custody:
Check sample:
Continuing calibration
blank (CCB):
Continuing calibration
verification (CCV):
Control chart:
Control sample:
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.
A reference material that has one or more of its property
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.
An unbroken trail of accountability that insures the physical
security of samples, data, and records.
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.
A standard solution which has no analyte and is used to
verify blank response and freedom from carryover. The
CCB should be analyzed after the CCV and after the
Interference Check Standard (ICS).
A standard solution (or set of solutions) used to verify
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.
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).
See Laboratory control sample.
A-6
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Corrective action:
Deficiency:
Digestion blank:
Action taken to correct a deficiency noted in a technical
systems audit. See Deficiency and Technical systems audit.
Duplicate analyses or
measurements:
Duplicate samples:
External quality control:
Field blank:
Initial calibration
blank (ICB):
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.
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.
The analyses or measurements of the variable of interest
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.
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.
Activities that are routinely initiated and performed by
persons outside of normal operations to assess the
capability and performance of a measurement process.
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.
A standard solution that contains no analyte and is used
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-7
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Initial calibration
verification (ICV):
Instrument maintenance
log:
Interference check
standard (ICS):
Internal quality control:
Internal standard:
Intralaboratory precision:
Intralaboratory quality
control:
Laboratory blank:
Laboratory control
sample (LCS):
A standard solution (or set of solutions) used to verify
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.
A chronological record of preventive and emergency
maintenance performed on an analytical instrument. The
logs include record of calls, service technician summaries,
records of calibration etc.
A standard solution (or set of solutions) used for ICP-AES
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 ug/MI of Al, Ca, Fe, and Mg. The ICS
must be matrix matched to acid content present in sample
digestates.
See Intralaboratory quality control.
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.
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.
The routine activities and checks, such as periodic
calibrations, duplicate analyses, and spiked samples, that
are included in normal internal procedures to control the
accuracy and precision of measurements.
See Digestion blank.
A matrix-based reference material with an established
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-8
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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:
Method 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 performance:
Method detection limit
(MDL):
Mobile laboratory:
NLLAP requirements:
Precision:
Primary standard:
Proficiency testing:
Quality assurance (QA):
See Digestion blank.
A general term used to document the characteristics of a
method. These characteristics usually include method
detection limits, linearity, precision, accuracy and bias.
The minimum concentration of an analyte that, in a given
matrix and with a specific method, has a 99% probability of
being identified, qualitatively or quantitatively measured, and
reported to be greater than zero.
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.
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.
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.
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.
A systematic program in which one or more standardized
samples is analyzed by one or more laboratories to
determine the capability of each participant.
An integrated system of activities involving planning, quality
control, quality assessment, reporting, and quality
A-9
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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.
-------
Quality manager:
Reagent blank:
Reference material:
Reference standard:
Relative percent
difference:
The manager of the quality system. The Quality Manager is
independent of the analyst and reports directly to
management.
See Digestion blank.
A material or substance, one or more properties of which are
sufficiently well established to be used for the calibration of
an apparatus, the assessment of a measurement method, or
assigning values to materials.
See Calibration standard.
A term defined as
RDP
R, I
x 100
where | R, - R21 represents the absolute difference in two values
and R represents the average of two values.
Replicate analysis
or measurements:
Replicate sample:
Report sign-off:
The analysis or measurement of the variable of interest
performed identically on two or more subsamples of the
same sample within a short time interval. See Duplicate
analysis or measurement.
Two or more samples representing the same population
characteristic, time, and place, which are independently
carried through all steps of the sampling and measurement
process in an identical manner. Replicate samples are used
to assess total (sampling and analysis) method variance.
Often incorrectly used in place of the term "replicate
analysis." See Duplicate samples and Replicate analysis.
The Technical Manager or designee authorized to review
and sign analysis reports.
65
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Reproducibility:
Rinseate blank:
Sample log:
Sample tracking:
Secondary standard:
Site blank:
Site visit:
Site visitor:
Spiked matrix:
Spiked reagent blank:
The extent to which a method, test or experiment yields the
same or similar results when performed on subsamples of
the same sample by different analysts or laboratories.
A sample of a "used" cleaning fluid rinse solution, also
called an equipment blank. Rinseate blank examples
include a final rinse of the device used to collect soil or
vacuumed dust or to clean the scoop used to collect soil or
vacuumed dust. The rinseate blank is used in rinsing
collection media and equipment prior to use to monitor
possible cross contamination. The rinseate blank goes
through the complete analysis, including the digestion.
The document where sample identification, condition, etc is
noted when samples arrive at the laboratory. The log is part
of the sample tracking system. See Sample tracking.
A system of following a sample from receipt at the
laboratory, through sample processing and analysis, and to
final reporting. The system includes unique numbering or
bar coding labels and the use of a sample log.
A standard whose value is based upon comparison with a
primary standard.
See Field blank.
An on-site visit to a laboratory for the purpose of conducting
a technical systems audit.
A person who conducts technical system audits. The terms
site visitor, auditor and assessor are often used
interchangeably. See Technical systems audit.
See Spiked sample.
A specified amount of reagent blank fortified with a known
mass of the target analyte, usually used to determine the
recovery efficiency of the method.
66
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Spiked sample:
Split samples:
Standard addition:
Standard operating
procedure (SOP):
Standard reference
material (SRM):
Standardization:
Stock solution:
Stratification:
Subsample:
A sample prepared by adding a known mass of target
analyte to a specified amount of matrix sample for which an
independent estimate of target analyte concentration is
available. Spiked samples are used, for example, to
determine the effect of the matrix on a method's recovery
efficiency.
Two or more representative portions taken from a sample or
subsample and analyzed by different analysts or
laboratories. Split samples are used to replicate the
measurement of the variable(s) of interest.
The procedure of adding known increments of the analyte of
interest to a sample to cause increases in detection
response. The level of the analyte of interest present in the
original sample is subsequently established by extrapolation
of the plotted responses.
A written document that details the method of an operation,
analysis, or action whose techniques and procedures are
thoroughly prescribed and which is accepted as the method
for performing certain routine or repetitive tasks.
A certified reference material produced by the U.S. National
Institute of Standards and Technology and characterized for
absolute content independent of analytical method.
The process of establishing the quantitative relationship
between a known mass of target material (e.g.,
concentration) and the response variable (e.g., the
measurement system or instrument response). See
Calibrate and Calibration curve.
A concentrated solution of analyte(s) or reagent(s) prepared
and verified by prescribed procedure(s), and used for
preparing working standards or standard solutions.
The division of a target population into subsets or strata
which are internally more homogeneous with respect to the
characteristic to be studied than the population as a whole.
A representative portion of a sample. A subsample may be
taken from any laboratory or a field sample.
67
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Substrate:
Systems audit:
This term has a very specialized use in the Pb-abatement
area. It refers specifically to the material to which paint is
attached, such as wallboard, concrete, wood, steel, etc.
See Technical systems audit.
Technical systems
audit:
Trip blank:
Validation:
Working standard:
A thorough systematic on-site, qualitative review of facilities,
equipment, personnel, training, procedures, record keeping,
data validation, data management, and reporting aspects of
a total measurement system.
A clean sample, including collection media, that is carried to
the sampling site and transported back to the laboratory for
analysis without being opened. This blank is analyzed as
a regular sample through all steps. The trip blank evaluates
the integrity of the sample container.
The process of substantiating specified performance criteria.
See Secondary standard.
68
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(BLANK PAGE)
A-14
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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-1
-------
(BLANK PAGE)
B-2
-------
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-3
-------
(BLANK PAGE)
B-4
-------
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-5
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(BLANK PAGE)
B-6
-------
4.0
4.1
4.2
4.3
4.4
4.5
4.6
4.6.1
4.7
Yes
No
N/A
ORGANIZATION AND MANAGEMENT
Is the laboratory legally identifiable?
Comments:
Does the laboratory have managerial staff with the authority
and resources needed to discharge their duties?
Comments:
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:
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:
Does the laboratory have a technical manager (however
named) who has overall responsibility for the technical
operations?
Comments:
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:
Does the QA manager have the power to oversee the situation,
identify problems, and make corrections?
Comments:
Does the laboratory have deputies in case of absence of
the technical or quality manager?
Comments:
B-7
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5.0
5.1
5.1.1
5.1.2
5.1.3
5.1.4
5.1.5
5.1.6
5.2
5.2.1
5.2.2
5.2.3
Yes
No
N/A
QUALITY SYSTEM, AUDIT, AND REVIEW
Is the quality system documented in a quality manual?
Comments:
Is the quality manual and related supporting documents
available for use by laboratory personnel?
Comments:
Are the quality policies and objectives communicated to,
understood, and implemented by all laboratory personnel
concerned?
Comments:
Is the quality manual kept current under the responsibility of the
quality manager?
Comments:
Are new employees introduced to the quality manual and how
often do employees review the manual? Describe in comments
below.
Comments:
Does the laboratory have an in-house training program?
Describe the type and frequency of training in comments
below.
Comments:
Is the quality system reviewed at least once per year by
management to ensure its continuing suitability and
effectiveness?
Comments:
Does the quality manual and related supporting documents contain:
A quality assurance policy statement, including objectives and
commitments, by top management?
Comments:
Organization charts that describe the management structure
of the laboratory and its place in any parent organization?
Comments:
Job descriptions of key staff and reference to job descriptions
of other staff?
B-8
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5.2.4
5.2.5
5.2.6
5.2.7
5.2.8
5.2.9
5.2.10
5.2.11
5.2.12
5.2.13
5.2.14
Yes
No
N/A
Comments:
Identification of laboratory's approved signatories for reports?
Comments:
Procedures for achieving traceability of measurements?
Comments:
The laboratory's scope of testing?
Comments:
Procedures for reviewing methods, facilities, and resources
necessary to complete proposed new work prior to initiation of
new work?
Comments:
Standard operating procedures for instrumental analysis
techniques used?
Comments:
Procedures for sample handling?
Comments:
Reference to reagents and reference standards used?
Comments:
Standard operating procedures for instrument calibration?
Comments:
Reference to verification practices including interlaboratory
comparisons, proficiency testing programs, use of reference
materials, and internal quality control schemes?
Comments:
Procedures to be followed for feedback and corrective action
whenever testing discrepancies are detected, or departures
from documented policies and procedures occur?
Comments:
Arrangements for exceptions permitting departures from
documented policies/procedures?
B-9
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5.2.15
5.3
5.3.1
5.3.2
5.4
5.4.1
5.4.2
5.4.3
5.4.4
5.4.5
5.4.6
Yes
No
N/A
Comments:
Procedures for audit and review?
Comments:
Are audits of laboratory activities conducted to verify
compliance with the quality system?
Comments:
Are audits conducted to ensure that analysts actually follow
SOPs?
Comments:
Are all audit and review findings and any corrective actions that
arise from them documented?
Comments:
Does the laboratory ensure the quality of results by
implementing and reviewing internal quality control schemes
using, whenever possible, statistical techniques?
Comments:
Are control chart data maintained?
Comments:
Do records indicate what corrective action has been taken
when results fail to meet QC criteria?
Comments:
Does the laboratory regularly use NIST SRMs or other certified
reference materials?
Comments:
Are QC data for all analytical results retrievable?
Comments:
Are method detection limits documented?
Comments:
Are routine analyses of reagents used for dilutions and
diqestions performed?
B-10
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5.4.7
5.4.8
5.5
5.5.1
5.5.2
5.6
5.6.1
5.6.2
5.6.3
Yes
No
N/A
Comments:
Do supervisory personnel review the data calculations and QC
results?
Comments:
Are deviations or deficiencies in QC documented and reported
to management?
Comments:
Does the laboratory participate in the ELPAT proficiency testing
program for each matrix that is routinely run in the laboratory?
Comments:
Are ELPAT samples treated as regular samples and analyzed
with the same method and by the same analyst who performs
routine analyses?
Comments:
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:
Are there QC procedures (SOPs) which address the following:
Reagent and method blank analysis?
Comments:
Glassware cleaning?
Comments:
Sampling and subsampling?
Comments:
B-11
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5.6.4
5.6.5
5.6.6
5.6.7
5.6.8
5.6.9
5.6.10
5.7
5.7.1
5.7.2
5.7.3
5.7.4
5.7.5
5.7.6
Replicate/duplicate analyses?
Yes
No
N/A
Comments:
Spiked and blank sample analysis?
Comments:
Blind samples?
Comments:
Control charts?
Comments:
Calibration standards?
Comments:
Reference samples?
Comments:
Internal standards?
Comments:
Is at least the following minimum QC practiced in the laboratory:
One method blank in 20 (5% or one per batch).
Comments:
One method spike in 20 (5% or one per batch).
Comments:
One duplicate or spiked duplicate in 20 (5% or one per batch).
Comments:
One laboratory control sample (consists of a representative
matrix spiked with the target analytes) in 20 (5% or one per
batch).
Comments:
Has the laboratory established control limits for all the above
types of QC samples?
If yes, can the laboratory demonstrate the basis for the
established limits?
B-12
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6.0
6.1
6.2
6.2.1
6.2.2
6.2.3
Yes
No
N/A
Comments:
PERSONNEL
Does the laboratory have sufficient personnel, with the required
education, training, knowledge, and experience for their
assigned functions?
Comments:
Do laboratory personnel have the following minimum education,
experience and training:
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:
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:
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:
B-13
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6.2.4
6.2.5
6.2.6
6.3
6.4
7.0
7.1
7.1.1
7.1.2
7.1.3
Yes
No
N/A
Flame AA Spectroscopist
Name: Experience:
Degree: B.S. Chemistry, or related science
Recommended Experience: 1 year minimum
Comments:
Inorganic Sample Preparation Technician
Name: Experience:
Recommended Experience: 3 months minimum
Comments:
Routine Sample Analyst
Name: Experience:
Recommended Experience: 6 months minimum
Comments:
Are records maintained on the qualifications, training, skills and
experience of the technical personnel?
Comments:
Is there documented evidence of analyst proficiency for each
test method performed?
Comments:
FACILITIES AND ENVIRONMENT
Does the laboratory:
Use distilled/demineralized water that it can demonstrate to be
essentially free of lead?
Comments:
Routinely check and record the conductivity of
distilled/demineralized water (for a continuous system, check
should be per batch or daily)?
Comments:
Provide separate contamination-free work areas for sample
preparation and sample analysis?
Comments:
B-14
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7.1.4
7.1.5
7.2
7.2.1
7.2.2
7.2.3
7.3
7.4
Provide facilities for separate storage of samples, digests,
acids, reference materials, and standards with temperature and
humidity control as required?
Yes
No
N/A
Comments:
Have glassware cleaning facilities suitable for metals analysis?
Comments:
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:
Does the laboratory provide exhaust hoods for sample
digestion and vent hoods for instrumentation with sufficient flow
to prevent cross-contamination?
Comments:
Does the laboratory provide safety equipment as specified in
the Chemical Hygiene Plan, such as safety showers, eyewash
stations, chemical spill kits?
Comments:
Does the laboratory provide personal protective equipment as
specified in the Chemical Hygiene Plan, such as gloves, face
shields, acid resistant aprons?
Comments:
Are material safety data sheets readily available to the
laboratory analyst?
Comments:
Does the laboratory have documented procedures and facilities
in place for storage, and disposal of chemical wastes, including
acids and lead?
Comments:
B-15
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8.0
8.1
8.2
8.2.1
8.2.2
8.2.2.1
8.2.2.2
8.3
8.3.1
8.3.1.1
Yes
No
N/A
EQUIPMENT/INSTRUMENTATION
Note: Supplemental information on equipment should be listed
in the table at the end of this checklist.
Is the laboratory furnished with all items of equipment required
for the analysis of Pb in paint, dust, and soil?
Comments:
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
If a hot plate is used for digestion, does it have temperature
control within requirements as stated in the method SOPs?
Comments:
If a microwave oven is used for digestion, does the unit have
variable power levels that meet requirements as stated in
method SOPs?
Comments:
Has the microwave unit been calibrated according to
manufacturer's recommendations?
Comments:
How often has the unit been calibrated and does the schedule
follow that described in the SOP?
Comments:
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
If a FLAA Spectrophotometer is used, is there a detailed
SOP describing its operation and calibration?
Comments:
Does the FLAA have a monochromoter, wavelength range, and
lamps specified in the method SOP?
Comments:
B-16
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8.3.1.2
8.3.1.3
8.3.1.4
8.3.1.5
8.3.1.6
8.3.1.7
8.3.1.8
8.3.2
8.3.2.1
8.3.2.2
8.3.3
Are fuels and oxidants commercial grade?
Yes
No
N/A
Comments:
Is there a filter moisture trap between the air source and the
spectrophotometer?
Comments:
Are fuel tank pressures greater than instrument operating
pressure?
Comments:
Are flash-back arresters and heaters in use where needed?
Comments:
Are burner heads specified in the method SOP used?
Comments:
Are burner head gases removed by ventilation?
Comments:
Is the burner head clean and free of build-up?
Comments:
If the laboratory has GFAA, is there a detailed SOP describing
its operation and calibration?
Comments:
What type of GFAA background correction is used?
( ) Deuterium Arc ( ) Smith-Heiftje ( ) Zeeman
Comments:
How often is the graphite tube changed and the chamber
cleaned (every )? Is this documented?
Comments:
Lamps used for FLAA and GFAA may be of various types.
Are they: single element ; multi-element ; electrodeless
Comments:
B-17
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8.3.3.1
8.3.4
8.3.4.1
8.3.4.2
8.3.4.3
8.3.4.4
8.3.4.5
8.3.4.6
8.4
8.4.1
8.4.1.2
8.4.1.3
Are back-up lamps available as spare parts?
Yes
No
N/A
Comments:
If the laboratory has ICP-AES, is there a detailed SOP covering
its use and calibration?
Comments:
Is a background correction technique in use and documented
according to the SOP?
Comments:
Has the absence of spectral interference for analytes of interest
been checked, corrected, and documented?
Comments:
Has salt build-up on the nebulizer been controlled?
Comments:
When a matrix interference is encountered, are procedures
specified in the SOP used to correct/eliminate potential
interference?
Comments:
Is the spectrometer equipped with an argon gas supply?
Comments:
Are high purity grade or equivalent nitric and hydrochloric
acids and deionized (distilled) water used for sample
processing and standards preparation?
Comments:
General equipment requirements:
Are analytical balance/pan balances calibration covered by an
SOP?:
Comments:
Do records document regular calibration using certified
weights?
Comments:
Do records show annual servicing and calibration for all
balances?
B-18
-------
8.4.2
8.4.2.1
8.4.2.2
8.4.3
8.4.3.1
8.4.4
8.4.4.1
8.5
8.5.1
8.5.2
8.5.3
8.5.4
Yes
No
N/A
Comments:
Labware:
Does the laboratory have deionized/distilled Class A water and
an SOP describing the checks on conductivity and lead
contamination?
Comments:
Is there documentation of the lack of contamination on
glassware used for metals analysis?
Comments:
Conductivity meter:
Do records show a calibration check daily, or before each use,
whichever is less frequent?
Comments:
Autopipetors/dilutors:
Does the laboratory keep records showing delivery volumes are
checked at least monthly?
Comments:
Does the laboratory maintain records on each major item of
equipment? Do the records include:
The name of the equipment?
Comments:
The manufacturer's name, model number, and serial number or
other unique identification?
Comments:
Condition when received (e.g., new, used, reconditioned)?
Comments:
Date received and date placed in service?
Comments:
B-19
-------
8.5.5
8.5.6
8.5.7
8.5.8
8.6
9.0
9.1
9.1.1
9.1.2
9.2
9.2.1
Copy of the manufacturer's instruction manual(s) readily
available to the analyst?
Yes
No
N/A
Comments:
Dates and results of instrument calibrations and date scheduled
for the next calibration?
Comments:
Detailed maintenance SOPs, including names and telephone
numbers to call for service?
Comments:
Detailed log of preventive maintenance and service calls which
include dates and repair records?
Comments:
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:
CALIBRATION/STANDARD OPERATING PROCEDURES
Is all instrumentation having an effect on the accuracy and
validity of tests calibrated before being put into service?
Comments:
Is the initial calibration and instrument checkout documented as
instruments are brought into service, either when new or after
repair?
Comments:
Are instrument calibration records kept near the instrument and
are they used by the analyst?
Comments:
Are calibration standards traceable to NIST standard reference
materials?
Comments:
Are NIST standard reference materials used for calibration or
traceabilitv studies only and for no other purpose?
B-20
-------
9.2.2
9.3
9.3.1
9.3.2
9.3.3
9.3.4
9.3.4.1
10.0
10.1
10.1.1
Yes
No
N/A
Comments:
Are separate reference materials dedicated to calibration
purposes only and not used as LCS?
Comments:
Do SOPs that provide for method calibration contain the
following information:
Are standard curves prepared to adequately cover the
expected concentration ranges of the samples?
Comments:
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:
Are new curves prepared whenever out-of-control conditions
are indicated and after new reagents are prepared?
Comments:
When analyses are performed, is the standard curve verified
(checked) by use of at least a method blank and one standard?
Comments:
Are these checks within ±10% of the original values?
Comments:
METHODS
Method Selection. Does the laboratory:
Use recognized (EPA recommended) methodologies and
instrumentation for each analysis performed, if such methods
are available?
Comments:
B-21
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10.1.2
10.1.3
10.1.4
10.1.5
10.1.6
10.1.7
10.1.8
10.1.9
10.1.10
Select methods mandated by legal requirements, recognized
published methods, or methods developed and validated by the
laboratory?
Yes
No
N/A
Comments:
Have site-specific SOPs for sample analysis?
Comments:
Use alternative analytical techniques that have undergone an
approved validation study?
Comments:
Make available to the client fully documented and validated
non-standard method information?
Comments:
Require that modifications to test method SOPs be
documented and approved by the Technical Manager (or
however named) before being implemented?
Comments:
Make available to analysts SOPs, standards, manuals, and
reference data relevant to the work of the laboratory?
Comments:
Regularly update SOPs and document changes in the QA
manual?
Comments:
Have method performance criteria (method detection limits,
precision, accuracy, linearity, etc.) been documented in an
SOP?
Comments:
Have demonstrated acceptable performance for each analytical
test method using performance evaluation samples?
Comments:
B-22
-------
10.2
10.2.1
10.2.2
10.2.4
10.2.5
10.2.6
10.3
10.3.1
10.3.2
10.3.3
10.4
10.5
Yes
No
N/A
Standards and Calibration. Does the laboratory:
Have SOPs for standards preparation?
Comments:
Use reagent grade or higher purity chemicals to prepare
standards?
Comments:
Use NIST SRMs (SRM 3128, Pb in 10% nitric acid) as a
primary standard?
Comments:
Prepare fresh analytical standards at a frequency consistent
with good QC?
Comments:
Properly label reference materials/reagents with concentrations,
date of preparation, expiration date, and the identity of the
person preparing the reagent?
Comments:
Does the analytical run contain, where applicable:
An initial calibration blank?
Comments:
A method blank?
Comments:
A matrix-based laboratory control sample?
Comments:
Are sample pretreatment and preservation documentation
available to the analyst?
Comments:
Is the method of standard addition in use where needed?
Comments:
B-23
-------
10.6
11.0
11.1
11.2
11.2.1
11.2.2
11.3
11.4
Are method calculation and data transfers checked by
someone other than the analyst?
Yes
No
N/A
Comments:
HANDLING OF TEST SAMPLES
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:
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:
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:
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:
Does the laboratory have documented procedures for the
retention or safe disposal of samples?
Comments:
Follow documented chain-of-custody procedures, when
required by the client?
Comments:
B-24
-------
12.0
12.1
12.1.1
12.1.2
12.1.3
12.1.4
12.1.5
12.1.6
12.1.7
Yes
No
N/A
RECORDS
Has the laboratory established and maintained a records
system that ensures that:
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:
Original records are uniquely identified and traceable to the
samples to which they refer and to any analysis reports based
upon them?
Comments:
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:
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:
Records contain sufficient details of any significant departures
from specified procedures, including authorizations for such
departures?
Comments:
Records are checked for data transcription or calculation
errors?
Comments:
Records identify the person or persons responsible for their
generation and for the checking of data transcriptions and
calculations?
Comments:
B-25
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12.1.8
12.2
12.3
12.4
13.0
13.1
13.2
13.2.1
13.2.2
13.2.3
13.2.4
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?
Yes
No
N/A
Comments:
Are all records and reports safely stored, held secure and in
confidence for the client?
Comments:
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:
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:
REPORTS
Are the laboratory's results of each analysis that is carried out
reported accurately, clearly, unambiguously?
Comments:
Does each report include at least the following information:
A title (e.g., "Analysis Report")
Comments:
The name and address of laboratory and location where the
analysis was carried out, if different from the address of the
laboratory?
Comments:
A unique identification number for the report, for each page,
and the total number of pages?
Comments:
The name and address of client?
Comments:
B-26
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13.2.5
13.2.6
13.2.7
13.2.8
13.2.9
13.2.10
13.2.11
13.2.12
13.2.13
Reference to the field sampling procedure, if known by the
laboratory?
Yes
No
N/A
Comments:
A description and unambiguous identification of the sample
tested?
Comments:
A characterization and condition of the samples?
Comments:
The date of receipt of the samples and date(s) of performance
of the tests, including digestion dates, and analysis dates, if
different?
Comments:
An identification of the sample digestion and instrumental
analysis methods used?
Comments:
Description of any deviations from, additions to, or exclusions
from the SOPs, relevant to a specific analysis?
Comments:
Measurements, and derived results, supported by tables, and
graphs as appropriate, including identification of any missing
data?
Comments:
A statement of the estimated uncertainty of the analysis result?
Comments:
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:
B-27
-------
13.3
13.4
14.0
14.1
14.2
14.3
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?
Yes
No
N/A
Comments:
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:
COMPLAINTS
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:
Does the laboratory maintain records of all complaints and of
the actions taken by the laboratory?
Comments:
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-28
-------
SUPPLEMENTAL INFORMATION ON MAJOR EQUIPMENT
Instrument Manufacturer Model Serial Number Installation Date
ICP-AES
Data System
AA (Flame)
Data System
AA (GFAA)
Data System
Microwave Digestion Unit
Comments on Instruments and Data Systems:
B-29
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