United States EPA Science Advisory EPA-SAB-RAC-03-009
Environmental Board (1400A) June 2003
Protection Agency Washington DC www.epa.gov/sab
&EPA MULTI-AGENCY
RADIOLOGICAL
LABORATORY
ANALYTICAL
PROTOCOLS (MARLAP)
MANUAL: AN SAB
REVIEW
REVIEW OF THE MARLAP
MANUAL AND APPENDICES
BY THE MARLAP REVIEW
PANEL OF THE RADIATION
ADVISORY COMMITTEE OF
THE US EPA SCIENCE
ADVISORY BOARD (SAB)
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
June 10, 2003
EPA-SAB-RAC-03-009
OFFICE OF THE ADMINISTRATOR
SCIENCE ADVISORY BOARD
The Honorable Christine Todd Whitman
Administrator
U.S. Environmental Protection Agency
1200 Pennsylvania Avenue, NW
Ariel Rios Building, Mail Code 1100
Washington, DC 20460
Subject: An SAB Review of the Multi-Agency Radiological Laboratory
Analytical Protocols (MARLAP) Manual
Dear Governor Whitman:
The Office of Radiation and Indoor Air (ORIA) requested that the Radiation Advisory
Committee (RAC) establish a panel to review the Multi-Agency Radiological Laboratory
Analytical Protocols (MARLAP) Manual. The MARLAP Manual is intended to provide
consistent technical guidance for planning, implementing, and assessing projects that require the
generation of radiological data. As such, it compliments the Multi-Agency Radiation Survey
and Site Investigation Manual (MARSSIM) developed through a similar process during the
1990s. The MARLAP Manual was developed over as seven year period by a by a partnership of
seven federal agencies, departments, and commissions, and two states.
The Panel wishes to bring to your attention that the partnership that produced this
Manual, which was led by Dr. John Griggs of ORIA and involved technical staff from different
government entities working together, represents the very best in government practices. Such
collaboration brings collective wisdom, together with the practical application of consistent and
comprehensive science methodologies, into harmony with a variety of regulatory and
compliance practices. We believe that this effort deserves special mention for the common sense
approach it brings to the implementation of government programs and guidelines.
Through the auspices of ORIA, the federal MARLAP Work Group posed three charge
questions to the Panel regarding:
1) the effectiveness and clarity of the overall approach,
2) the technical accuracy of the guidance on laboratory operations, and
3) the technical accuracy and clarity of the guidance on measurement statistics.
The MARLAP Review Panel added a fourth charge question pertaining to:
4) the overall integration and implementation of the Manual's guidance.
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The MARLAP Review Panel found the Manual to be well conceived and expects that it
will be a valuable reference, particularly helpful to analytical laboratories and users of laboratory
services working with radioanalytical data and protocols. The primary recommendations from
the Panel involve reorganization of the Manual to make it user friendly and facilitate its intended
use. The comments and recommendations offered by the Panel should be construed as
constructive criticism as they are intended solely to assist in improving a document that is
already very comprehensive and thorough.
In response to Charge Question #1 (relating to the effectiveness and clarity of the overall
approach), the Panel finds that the performance-based, flexible approach in MARLAP is
appropriate and, for the most part, presented clearly and logically in the draft MARLAP Manual.
The Panel agrees with the guidance provided with regard to a graded approach for projects of
different size and scope, as well as with the emphasis on data quality, that is adequate and
reasonable for the decision being supported. The linkage of the planning, implementation, and
assessment phases of projects involving radioanalytical data is effective. However, the Manual
is consequently massive, and finding the information needed for a specific radioanalytical
project is difficult at this stage, especially for a novice or infrequent user. In its attempt to make
the various chapters stand alone, the MARLAP Work Group may have introduced excessive
redundancy. The Panel also identified some guidance requiring greater definition and detail.
The Panel recognizes that a lack of consensus between different members of the MARLAP Work
Group may be inevitable, due to the multi-agency input to this document and the different
governing regulatory requirements under which those agencies must operate. Nonetheless, the
Panel recommends that a well-defined "consensus" solution be adopted in making
recommendations to the users. In addressing these and other questions, the Panel proposes
several specific suggestions for reorganizing and editing the document and improving its overall
usefulness and accessibility.
In response to Charge Question #2 (relating to the technical accuracy of the guidance),
the Panel finds that the document is an impressive compilation of information and
recommendations that should be immensely useful to radiochemical analysis practitioners. It
also finds the guidance to be, on the whole, reliable and well thought out; however, as would be
expected with such a large compendium of information, some technical inaccuracies and
inconsistencies are identified. The Panel includes the most important of these issues in the text
of its Review Report and recommends some changes or additions to several of the chapters. It
also suggests some changes in the organizational structure of the Manual to add clarity and
usefulness. The bulk of the Panel's specific concerns are addressed in appendices to its report.
In response to Charge Question #3 (involving the guidance on measurement statistics),
the Panel finds that statistical issues are addressed very well in the MARLAP Manual but offers
several suggestions for reorganization and clarification to enhance its value, specifically for
laboratory directors and staff. In particular, both the terminology used in the MARLAP Manual
as well as the treatment of uncertainty propagation in measured values require some re-
evaluation, and possible revision.
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In response to Charge Question #4 (related to self-initiated Panel questions on the issue
of overall integration and implementation), the Panel suggests that in addition to better
integration with the earlier MARS SIM (2000) document, it might be useful to devote a short
section at the beginning of the Manual to show how the performance-based approach is suitable
for decisions regarding the cleanup of radioactively contaminated sites. Although the Panel
recognizes that MARLAP is not limited to site cleanup decisions, these represent some of the
most important drivers for the creation of MARLAP. The proposed new section would also help
elucidate the areas of overlap between MARLAP and MARSSEVI, as well as emphasize their
differences in scope and coverage.
Finally, the Panel offers some suggestions beyond the charge given by the federal
MARLAP Work Group, regarding implementation of the Manual's recommended protocols after
its completion and release:
Due to the complexity of the issues addressed in MARLAP, the Panel recommends that
EPA undertake a program to train laboratory personnel and users of radio-analytical data in
much the same manner as occurred for the MARS SIM activity.
The Panel also recommends that the agencies, departments, and commissions involved in
the development of MARLAP support a professional education program to generate a new
generation of experts in radioanalytical techniques, to offset the trend towards a diminishing pool
of available experts. Such a program might include scholarships, fellowships, research grants,
and teaching grants geared to encourage students and faculty to develop and maintain
proficiency in the application of radioanalytical protocols.
The MARLAP document should be maintained as a "living document" and involve an
iterative process whereby user suggestions can be incorporated into future revisions.
The success of this and a previous multi-agency effort (i.e., MARLAP and MARSSIM)
in addressing complex multidisciplinary environmental issues leads us to recommend that multi-
agency approaches be extended to other EPA activities.
The Panel also wishes to express to you that one of its main concerns with the draft
MARLAP does not involve its technical content but rather the ease and practicality of its use as a
tool. User implementation of its recommendations to use a performance-based approach may be
frustrated by the fact that the selection of specific radiochemical protocols is often driven by the
requirements of existing methods set as standards by different organizations. Until these
methods are revised, and commitments from EPA and other authoring organizations are
obtained, the radiochemistry community may be in conflict over the application of MARLAP
guidance. The Panel therefore encourages you to establish a time table and funding to conduct a
review of your agency's existing regulations and guidance on radioanalytical protocols and to
revise those documents as appropriate to reflect the MARLAP performance-based approach.
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We appreciate the diligence and cooperative spirit in which this ambitious project has
been undertaken and congratulate its participants. On behalf of members of the RAC and the
MARLAP Review Panel, we wish to thank you for your consideration and look forward to your
response.
Sincerely,
/Signed/ /Signed/
Dr. William H. Glaze, Chair Dr. Janet A. Johnson, Chair
EPA Science Advisory Board Radiation Advisory Committee
and MARLAP Review Panel
EPA Science Advisory Board
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NOTICE
This report has been written as part of the activities of the EPA Science Advisory Board,
a public advisory group providing extramural scientific information and advice to the
Administrator and other officials of the Environmental Protection Agency. The Board is
structured to provide balanced, expert assessment of scientific matters related to problems facing
the Agency. This report has not been reviewed for approval by the Agency and, hence, the
contents of this report do not necessarily represent the views and policies of the Environmental
Protection Agency, nor of other agencies in the Executive Branch of the Federal government, nor
does mention of trade names or commercial products constitute a recommendation for use.
Distribution and Availability: This EPA Science Advisory Board report is provided to the EPA
Administrator, senior Agency management, appropriate program staff, interested members of the
public, and is posted on the SAB website (www.epa.gov/sab). Information on its availability is
also provided in the SAB's monthly newsletter {Happenings at the Science Advisory Board).
Additional copies and further information are available from the SAB Staff [US EPA Science
Advisory Board (1400A), 1200 Pennsylvania Avenue, NW, Washington, DC 20460-0001; 202-
564-4533].
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ABSTRACT
The EPA Science Advisory Board's Radiation Advisory Committee and the MARLAP Review
Panel (the Panel) reviewed technical aspects of the draft Multi-agency Radiological Laboratory
Analytical Protocols (MARLAP) Manual dated August 2001. This document was developed
collaboratively by seven federal agencies, departments, and commissions having authority for
regulating radioactive materials, and two states.
The Panel finds that MARLAP effectively addresses the need for a nationally consistent,
performance-based approach for planning, implementing, and assessing radioanalytical
measurements to address regulatory concerns. The Manual's graded approach encourages a user
to select a set of analytical procedures, with associated precision and reliability, suited to the
complexity and importance of the problem being addressed. It does a thorough job of explaining
how decision makers should make choices in the selection of hypotheses that help determine the
confidence levels associated with the results obtained from analytical laboratories. The
Manual's guidance on laboratory operations is generally technically sound although highly
variable in scope and level of detail provided. Guidance on measurement statistics is also
technically sound but perhaps overly detailed. The Panel recommends reorganization and a
thorough technical edit of the Manual to improve its flow, add clarity and logic, and reduce
redundancy so as to make it easier to use. The Panel also stresses the need to include more
explicit examples to better illustrate the application of each step in the performance-based
approach to activities of differing size and complexity. The Panel recommends that the EPA
undertake a training program for MARLAP users and that it use the classes as a mechanism for
seeking input that can be incorporated into future revisions of the Manual.
Key Words: Analytical Protocols, Protocol Assessment, Protocol Implementation, Protocol
Manual, Radiological Analytical Protocols
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U.S. Environmental Protection Agency
Science Advisory Board (SAB)
Radiation Advisory Committee (RAC)
Multi-Agency Radiological Laboratory Analytical Protocols (MARLAP)
Review Panel
CHAIR
Dr. Janet A. Johnson, Senior Technical Advisor, Shepherd Miller, Inc, Fort Collins, CO
SAB MEMBERS
Dr. Lynn R. Anspaugh, Research Professor, University of Utah, Salt Lake City, UT
Dr. Bruce B. Boecker, Scientist Emeritus, Lovelace Respiratory Research Institute, Albuquerque, NM
Dr. Gilles Y. Bussod, President, Science Network International, Santa Fe, NM
Dr. Thomas F. Gesell, Professor of Health Physics, Department of Physics, Idaho State University,
Pocatello, ID
Dr. Helen Ann Grogan, Cascade Scientific, Inc., Bend, OR
Dr. Richard W. Hornung, Director, Division of Biostatistical Research, IHPHSR, University of
Cincinnati, Cincinnati, OH [Subcommittee chair: Charge Question #3: Guidance on Measurement
Statistics, Measurement Uncertainty, and Detection and Quantification Capability1
Dr. Jill Lipoti, Assistant Director, Environmental Safety, Health and Analytical Programs, Radiation
Protection Program, New Jersey Department of Environmental Protection, Trenton, NJ
Dr. Genevieve S. Roessler, Radiation Consultant, Elysian, MN
CONSULTANTS
Dr. Vicki M. Bier, Professor of Industrial Engineering, College of Engineering, University of
Wisconsin, Madison, WI
Dr. Stephen L. Brown, Director, R2C2 (Risks of Radiation and Chemical Compounds), Oakland, CA
[Subcommittee chair: Issues Beyond the Charge 1
Dr. Michael E. Ginevan, Proprietor, M.E. Ginevan & Associates, Silver Spring, MD
Dr. Shawki Ibrahim, Department of Radiological Health Sciences, Colorado State University, Fort
Collins, Colorado
Dr. Bernd Kahn, Professor, School of Nuclear Engineering and Health Physics, and Director,
Environmental Resources Center, Georgia Institute of Technology, Atlanta, GA [Subcommittee chair:
iii
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Charge Question #2: Guidance on Laboratory Operations]
Dr. June Fabryka-Martin, Staff Scientist, Group EES-6, Hydrology, Geochemistry and Geology, Los
Alamos National Laboratory, Los Alamos, NM [Subcommittee chair: Charge Question #1: Overall
Approach for Planning and Implementation]
Dr. Bobby R. Scott, Staff Scientist, Lovelace Respiratory Research Institute, Albuquerque, NM
SCIENCE ADVISORY BOARD STAFF
Dr. K. Jack Kooyoomjian, Designated Federal Officer, U.S. Environmental Protection Agency,
Science Advisory Board (1400A), 1200 Pennsylvania Avenue, NW, Washington, DC, 20460
Ms. Mary L. Winston, Management Assistant, U.S. Environmental Protection Agency, Science
Advisory Board (1400A), 1200 Pennsylvania Avenue, NW, Washington, DC, 20460
IV
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TABLE OF CONTENTS
1. EXECUTIVE SUMMARY 1
2. INTRODUCTION AND CHARGE 5
2.1 Background About the MARLAP Manual 5
2.2 Charge Questions 5
2.3 RAC Review Process 6
2.4 Report Organization 7
3. RESPONSE TO CHARGE QUESTION #1: TECHNICAL ACCEPTABILITY, PRESENTATION, AND EASE
OF IMPLEMENTING THE PLANNING, IMPLEMENTATION AND ASSESSMENT PHASES 8
3.1 Overall Response to Charge Question #1 8
3.1.1 Response to Charge Question #la 8
3.1.2 Response to Charge Question #lb 9
3.1.3 Response to Charge Question #lc 9
3.2 Detailed Comments on Organization and Presentation of Part I 9
3.2.1 Organization 9
3.2.2 Presentation Style 10
3.2.3 Technical Edit 12
3.3 Detailed Comments on Technical Content of Part I 14
3.3.1 Technical Issues 14
3.3.2 Use of Examples 18
4. RESPONSE TO CHARGE QUESTION #2: TECHNICAL ACCURACY OF GUIDANCE ON LABORATORY
OPERATIONS 23
4.1 Overall Response to Charge Question #2 23
4.2 Detailed Comments on Organization and Presentation of Part II 25
4.3 Detailed Comments on Technical Content of Part II 25
4.3.1 Chapter 10: Field and Sampling Issues That Affect Laboratory Measurement 26
4.3.2 Chapter 11: Sample Receipt, Inspection and Tracking 28
4.3.3 Chapter 12: Laboratory Sample Preparation 28
4.3.4 Chapter 13: Sample Dissolution 28
4.3.5 Chapter 14: Separation Techniques 28
4.3.6 Chapter 15: Nuclear Counting Instrumentation 30
4.3.7 Chapter 16: Instrument Calibration and Test Source Preparation 30
4.3.8 Chapter 17: Data Acquisition, Reduction and Reporting 31
4.3.9 Chapter 18: Laboratory Quality Control 32
4.3.10 Chapter 20: Waste Management in a Radioanalytical Laboratory 32
5. RESPONSE TO CHARGE QUESTION #3: GUIDANCE ON MEASUREMENT STATISTICS 33
5.1 Overall Response to Charge Question #3 33
5.2 Detailed Comments on Organization and Presentation of Chapter 19 33
5.2.1 Organization 33
5.2.2 Terminology 34
5.3 Detailed Comments on Technical Content of Chapter 19 35
5.3.1 Statistical Approximations of Uncertainty 35
5.3.2 Treatment of Negative Analytical Values 36
5.3.3 Use of Examples 38
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6. RESPONSE TO CHARGE QUESTION #4: OVERALL INTEGRATION AND
IMPLEMENTATION ISSUES 39
6.1 Integration Issues 39
6.2 Implementation Issues 40
6.2.1 Composition of the Planning Team 40
6.2.2 Availability of a Trained Workforce 41
6.2.3 User Training 41
6.3 Future Enhancements of MARLAP 43
7. SUMMARY OF FINDINGS AND RECOMMENDATIONS 49
7.1 Overall 49
7.2 Charge Question #1: Effectiveness and Clarity of the Overall Approach in Part I 49
7.2.1 Comments 49
7.2.2 Recommendations 49
7.3 Charge Question #2: Technical Accuracy of the Guidance in Part II 50
7.3.1 Comments 50
7.3.2 Recommendations 51
7.4 Charge Question #3: Guidance on Measurement Statistics 52
7.4.1 Comments 52
7.4.2 Recommendations
52
7.5 Charge Question #4: Overall Integration and Implementation Issues 53
REFERENCES CITED R-l
APPENDIX A - DETAILED DESCRIPTION OF THE SAB PROCESS AND ITS CHARGE A-l
A.I Charge Questions and Subcommittee Assignments A-l
A.2 Panel Review Schedule and Process A-3
APPENDIX - B - ACRONYMS AND ABBREVIATIONS B-l
APPENDIX C - TECHNICAL REVIEW COMMENTS C-l
VI
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1. EXECUTIVE SUMMARY
The MARLAP Manual is intended to provide consistent guidance for laboratories and
users of laboratory services, for the planning, implementation, and assessment of projects
entailing radioanalytical data and protocols. The MARLAP Manual was developed in
partnership by seven federal agencies, departments, and commissions: the U.S. Environmental
Protection Agency (EPA), Department of Energy (DOE), Department of Defense (DoD),
Nuclear Regulatory Commission (NRC), National Institute of Standards and Technology
(NIST), U.S. Geological Survey (USGS), and U.S. Food and Drug Administration (FDA). State
participation in the development of the Manual involved contributions from representatives from
the State of California and the Commonwealth of Kentucky. For the purpose of the Radiation
Advisory Committee (RAC) review, this group is termed the federal "MARLAP Work Group."
The RAC finds that the development of the MARLAP Manual is an excellent example of
interagency cooperation in line with a similar effort that produced the Multi-agency Radiation
Survey and Site Investigation Manual (MARSSIM). Use of an interagency partnership to
produce the MARLAP Manual represents the very best in government practices by involving
technical staff from different government entities working together. Such collaboration brings
collective wisdom and practical application of consistent and comprehensive science
methodologies into harmony with a variety of regulatory and compliance practices. The RAC
believes that this effort deserves special mention for the common sense approach it brings to the
implementation of government programs and guidelines. The multi-agency authorship of
MARLAP and the apparent consensus on a single overall "performance-based" approach gives
the reader confidence in the reliability of the guidance and the logical foundation that underlies
it.
Through the auspices of EPA's Office of Radiation and Indoor Air (ORIA), the federal
MARLAP Work Group posed three charge questions to the RAC regarding: 1) the effectiveness
and clarity of the overall approach; 2) the technical accuracy of the guidance on laboratory
operations; and 3) the technical accuracy and clarity of the guidance on measurement statistics.
To respond to the charge, the RAC established the MARLAP Review Panel ("the Panel") as a
RAC subcommittee, augmented by consultants. Following a planning conference call, the Panel
added a fourth charge question pertaining to overall integration and implementation issues.
With regard to Charge Question #1 (relating to the effectiveness and clarity of the overall
approach), the Panel finds that the performance-based and flexible approach in MARLAP is
appropriate and, for the most part, presented clearly and logically in the draft MARLAP Manual.
The essence of a performance-based approach is the selection of radioanalytical protocols and
the development of acceptance criteria for radioanalytical data based on project-specific
analytical data requirements, as opposed to the use of prescribed methods. The Panel finds the
guidance to be reasonable with regard to application of a graded approach for projects of
different size, scope, and complexity, as well as the emphasis on data quality sufficient for the
1
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decision being supported. The linkage of the planning, implementation, and assessment phases
of projects involving radioanalytical data is effective. However, the draft Manual is
consequently massive, and finding the information needed for a specific radioanalytical project
may be difficult, especially for a novice or infrequent user. In its attempt to make each chapter
relatively self-contained, the federal MARLAP Work Group may have introduced excessive
redundancy. The Panel identified some guidelines which require greater definition and detail.
Although the Panel recognizes that a lack of consensus among members of the federal MARLAP
Work Group may be inevitable due to the different governing regulatory requirements for each
of the participating agencies, the Panel recommends that a well-defined "consensus" solution be
adopted in making recommendations to the users. To address these and other concerns, the
Panel proposes several specific suggestions for reorganizing and editing the document to
improve its overall usefulness and accessibility.
The Panel also recommends the inclusion of more examples to illustrate the planning
process and the graded approach, so as to bring these to life for the reader. A variety of clearly
presented and realistic scenarios will be critical to the success of MARLAP and should
emphasize the potential benefits of planning and using a graded approach. The Panel recognizes
that policies are often implied in the assumptions that are adopted as part of the planning
process, and that it is difficult for a multi-agency document to address this nontechnical aspect.
The Panel also recognizes the concern of the federal MARLAP Work Group that case studies or
scenarios in the Manual could be interpreted by some users as setting or endorsing a precedent.
Nonetheless, the Panel recommends that this concern be addressed upfront. Furthermore, to
address the concern that regulatory agencies may try to apply the entire MARLAP process to
situations and organizations for which a full-scale effort would not be appropriate, the Panel
suggests the inclusion of more explicit guidance, including examples, on how to scale back the
process to a level appropriate to the decision under consideration.
In reference to Charge Question #2 (relating to the technical accuracy of the guidance),
the Panel finds that the draft Manual is an impressive compilation of information and
recommendations that should be immensely useful to radiochemical analysis practitioners. The
Panel also finds the guidance to be, on the whole, reliable and well thought out; however, as
would be expected with such a large compendium of information, numerous technical
inaccuracies and inconsistencies are identified. The Panel includes the most important of these
issues in the text of its Review Report and recommends some changes or additions to the
discussions in specific chapters. The Panel also suggests some changes in organizational
structure so as to streamline and add clarity to the discussions, improve the logic of its flow, and
in general increase its usefulness as a reference. The bulk of the Panel's specific concerns are
addressed in Appendices C and D to its report.
With regard to Charge Question #3 (involving the guidance on measurement statistics),
the Panel finds that statistical issues are addressed very well in the MARLAP Manual but offers
several suggestions for reorganization and clarification to enhance its value, specifically for
laboratory directors and staff. In particular, the terminology used in the draft MARLAP Manual
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and the treatment of uncertainty propagation in measured values require some re-evaluation and,
perhaps, revision.
In terms of Charge Question #4 (related to the self-initiated Panel question on the issue of
overall integration and implementation), the Panel suggests that, in addition to better integration
with the earlier MARS SIM (2000) document, it might be useful to devote a short section at the
beginning of the Manual to show how the performance-based approach is suitable for decisions
regarding the cleanup of radioactively contaminated sites. Although the Panel recognizes that
MARLAP is not limited to site cleanup decisions, these represent some of the most important
drivers for the creation of this Manual. The proposed new section would also help elucidate the
areas of overlap between MARLAP and MARS SIM, as well as emphasize their differences in
scope, coverage, and guidance.
In general, the Panel emphasizes that its comments and recommendations are intended to
facilitate the use, and enhance the user-friendly construct, of an already superior product. The
comments and recommendations offered by the Panel should be construed as constructive
criticism intended solely to assist in improving a document that is already very comprehensive
and thorough. Some of the main concerns with the draft MARLAP do not involve the technical
content but rather the ease and practicality of its use as a tool. User implementation of its
recommendations to use a performance-based approach may be frustrated by the fact that the
selection of specific radiochemical protocols is often driven by the requirements of existing
methods set as standards by different organizations. Until these methods are revised, and
commitments from the authoring organizations are obtained, the radiochemistry community may
be in conflict over some applications of MARLAP guidance.
The Panel emphasizes the need for a thorough technical edit, the main objectives of
which should be to: 1) remove the considerable amount of redundancy, 2) ensure internal
consistency among the chapters in presentation style and formatting, 3) make wider and more
consistent use of effective techniques for presenting information, such as the inclusion of a
Manual roadmap, reduced use of acronyms, development of a good overview figure, and
reinforcement of key text information with tables and figures, and 4) verify and proofread all
references, web-site addresses, equations, tables, figures, and examples. To aid in this effort, the
Panel notes several presentation and formatting techniques in the draft Manual that it found to be
particularly effective in emphasizing important points.
Finally, the Panel offers some suggestions beyond the charge given by the federal
MARLAP Work Group regarding implementation of the Manual after its release:
1. Due to the complexity of the issues addressed in MARLAP, the Panel
recommends that EPA undertake a program to train laboratory personnel and
users of radioanalytical data in much the same manner as occurred for the
MARS SIM activity.
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2. The Panel also recommends that the agencies, departments, and commissions
involved in developing MARLAP support a professional education program to
generate a new generation of experts in radioanalytical techniques, to offset the
trend towards a diminishing pool of available specialists. Such a program might
include scholarships, fellowships, research grants, and teaching grants geared to
encourage students and faculty to develop and maintain proficiency in the
application of radioanlytical protocols.
3. The MARLAP document should be maintained as a "living document" and
involve an iterative process whereby user suggestions can be incorporated into
future revisions.
4. The success of MARLAP and MARSSIM in addressing complex
multidisciplinary environmental issues leads the Panel to recommend that multi-
agency approaches be extended to other EPA activities.
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2. INTRODUCTION AND CHARGE
The EPA's Office of Radiation and Indoor Air (ORIA) requested that the Radiation
Advisory Committee (RAC) of the Science Advisory Board (SAB) review the Multi-Agency
Radiological Laboratory Protocols (MARLAP) Manual. The RAC review was initiated in
August 2000 while the MARLAP was still under development, at which time the RAC initiated
action to establish a MARLAP Review Panel comprised of RAC members and consultants. The
draft Manual was made available to the Review Panel in September 2001. The Panel's review
was completed in September 2002. Its report was adopted and approved by the RAC in
November 2002 and transmitted in December 2002 for an Executive Committee review.
Appendix A describes the details of the RAC review schedule and process. Appendix B defines
the acronyms and abbreviations used in this report.
2.1 Background About the MARLAP Manual
The MARLAP Manual provides "guidance for the planning, implementation, and
assessment of projects that require the laboratory analysis of radionuclides." The intent of the
Manual is to "provide the guidance necessary for national consistency in the form of a
performance-based approach for meeting a project's data requirements" and to help "ensure the
generation of radioanalytical data of known quality, appropriate for its intended use." The
MARLAP is not intended to be a "cookbook;" the Manual contains guidance but not specific
laboratory procedures.
The MARLAP Work Group that developed the Manual consists of representatives of the
Environmental Protection Agency (EPA), Department of Defense (DoD), Department of Energy
(DOE), Nuclear Regulatory Commission (NRC), National Institute of Standards and Technology
(NIST), U.S. Geological Survey (USGS), U.S. Food and Drug Administration (FDA), the
Commonwealth of Kentucky, and the State of California.
2.2 Charge Questions
The specific charge questions posed to the RAC by the MARLAP Work Group through
the auspices of ORIA were as follows:
Charge Question 1: Is the overall approach present in Part 1 of MARLAP for the planning,
implementation and assessment phases of projects which require analysis for radionuclides
technically acceptable?
la. Is the performance-based approach presented clearly and logically ?
Ib. Is the approach reasonable in terms of ease of implementation?
Ic. Does the approach effectively link the three phases (planning, implementation,
assessment) of a project?
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Charge Question 2: Is the guidance on laboratory operations in the Part II chapters technically
accurate? Does it provide a useful resource base of information for a laboratory's
implementation of a performance-based approach?
Charge Question 3: Is the guidance on measurement statistics - specifically measurement
uncertainty and detection and quantification capability - technically accurate, clearly presented,
and useful for implementation by appropriately trained personnel?
2.3 RAC Review Process
The MARLAP was introduced to the RAC at its August 1, 2000 meeting in Washington,
DC and the RAC conducted a planning meeting on MARLAP and other topics on December 12-
14, 2000. The RAC determined that additional expertise would be needed for the review.
Consequently, several consultants were added to the MARLAP Review Panel to assist in
addressing the organizational aspects of the Manual as well as the accuracy of its radiochemical
and statistical guidance.
The sequence and scope of the Review Panel's conference calls and meetings, and its
interactions with the MARLAP Work Group (who were responsible for the Manual's content),
are described in Appendix A. Two aspects of the review process are particularly worthy of the
reader's attention. First, during its April 23-25, 2002 public meeting, the Panel subcommittee
responding to Charge Question #1 (relating to the effectiveness and clarity of the overall
approach) employed a tool that is unique to this review, at least for the RAC. In order to get a
sense of how a laboratory manager or other critical users might perceive MARLAP, the
Subcommittee engaged in a role-playing exercise with members of the MARLAP Work Group.
This exercise was very enlightening, particularly in identifying and clarifying areas where
MARLAP may be confusing and/or not a practical guide for the user. The exercise subsequently
served as the basis for one of the Panel's recommendations on MARLAP training techniques.
Secondly, although not unusual among RAC reviews of EPA products, the cooperative
process between the Panel and the federal MARLAP Work Group proved to be very useful. It
facilitated the flow of information from the federal MARLAP Work Group to the Panel as well
as providing an opportunity for the federal MARLAP Work Group to hear and understand the
concerns of the Panel. Questions that might have been posed in the Panel's draft Review Report
were addressed at the time they were raised, thus saving much effort and reducing the need for
later corrections. The RAC very much appreciates the time and effort the federal MARLAP
Work Group devoted to explaining aspects of the Manual and the rationale behind its
organization. While the Panel worked in close cooperation with the federal MARLAP Work
Group, that process did not compromise the independence of the peer review.
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2.4 Report Organization
Responses to specific charge questions are contained in Sections 3, 4, and 5 of this report.
In addition to responding to the specific charge questions, the Panel addressed several issues
that went beyond the charge. These issues are presented in Section 6. Section 7 summarizes the
Panel's most important findings and recommendations. Appendix C to this report compiles the
Panel's comments on technical aspects of the Manual, relating to the accuracy, completeness,
and clarity of MARLAP's technical discussions. Appendix D lists the Panel's editorial
comments that address the need for more precise or succinct wording, additional detail in the
guidance, corrected references, cross-referencing, and clarification of statements or terminology
used in the Manual.
Names of subcommittee chairs and members, and a list of the MARLAP Manual chapters
and appendices assigned to each Panel subcommittee, are included in Appendix A of this report.
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3. RESPONSE TO CHARGE QUESTION #1: TECHNICAL
ACCEPTABILITY, PRESENTATION, AND EASE OF IMPLEMENTING
THE PLANNING, IMPLEMENTATION AND ASSESSMENT PHASES
Charge Question #1: Is the overall approach presented in Part 1 of MARLAP for the planning,
implementation and assessment phases of projects which require analysis for radionuclides
technically acceptable?
la. Is the performance-based approach presented clearly and logically ?
Ib. Is the approach reasonable in terms of ease of implementation?
Ic. Does the approach effectively link the three phases (planning, implementation,
assessment) of a project?
3.1 Overall Response to Charge Question #1
Compiling and organizing information and guidance related to the acquisition and use of
radioanalytical analyses is a formidable but worthy task to be undertaken by a multi-agency
committee. The federal MARLAP Work Group is largely successful in achieving its goal of
developing a consensus document on this complex topic. Overall, the MARLAP Manual is a
very impressive document with almost encyclopedic amounts of useful information. Chapters 1
to 9 in Part I are well prepared and thoughtfully organized, making this document very useful for
persons needing to obtain or provide radioanalytical services for large-scale projects. The
Manual does a thorough job of explaining how decision makers should make choices in the
selection of hypotheses that help determine the confidence levels associated with the results
obtained from analytical laboratories. Finally, the multi-agency authorship of MARLAP and the
apparent consensus on a single overall approach gives the reader confidence about the reliability
of the guidance.
The Panel strongly supports the graded approach advocated for the implementation of
MARLAP, in which resources applied to a problem are appropriate to the size and complexity of
the project. The Panel also strongly endorses MARLAP guidance that the planning process be
viewed as an iterative process, rather than linear or stepwise, to ensure that the final product
precisely meets all the requirements associated with data needs and a decision-based approach.
An iterative process also permits the incorporation of new information as it is received, allowing
the planners flexibility to modify or change earlier decisions as required, so that the most
resource-effective approach to the problem can be developed and implemented.
3.1.1 Response to Charge Question #la
With only a few reservations about explaining the context in which MARLAP will
operate, the performance-based and flexible approach is well designed and appropriate, and is
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presented clearly and logically in the draft document. The exposition is generally better than
that typical of such large and complex draft technical documents at this stage of review.
3.1.2 Response to Charge Question #lb
Although some of the guidance in MARLAP may challenge the capabilities of those who
must plan, manage, and conduct radiochemical analyses (see detailed discussion in Sections 3.2
and 3.3), the approach is reasonable, especially in light of the graded approach for projects of
different scope and importance, and the emphasis on data of quality sufficient for the decision
being supported rather than on specific requirements for analytical procedures or data precision
and accuracy.
3.1.3 Response to Charge Question #lc.
The linkage of the planning, implementation, and assessment phases is largely effective
as well. However, the Panel recommends that MARLAP provide guidance or recommendations
to the end user who receives the analytical data that are generated through MARLAP, with
regard to traceability, compilation and archiving of the data. For certain types of projects the
assembled data may be useful in the future in the context of a different project. However, such
data will be useful only to the extent that they are compiled and stored with sufficient
information regarding sampling location, method, sampling time, analytical procedure, and
quality assurance and control aspects. Inclusion of a statement regarding this issue could
provide very timely advice to project planners and managers in the early stages of a project.
3.2 Detailed Comments on Organization and Presentation of Part I
The following comments are offered in the hope of further improvement, not as a
criticism of this important effort. The comments are classified into the following categories:
organization, presentation style, and the need for a thorough technical edit.
3.2.1 Organization
The organization of the draft MARLAP document is complicated, and it is not obvious
how the user should most effectively make use of this thick two-volume manual. The present
draft is wordy, with information being scattered and repetitive. The goal of producing stand-
alone chapters is ineffective in practice because this repetition is distracting to those who are
reading more than one chapter at a time, with the result that the reader very quickly loses
interest. The following suggestions are made to address these shortcomings:
a) The goal should be to make Part I a stand-alone volume, replacing the goal of
stand-alone chapters. The Panel envisions Part I as including the information
presented in Chapters 1 to 9 and Appendices A to E.
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b) Chapters should be thinned down and focused. Information in the chapters should
be limited to that which the majority of users are likely to need to know, with the
reader being referred to an appendix or references for extended discussions of
exceptions, alternative options, or less common aspects.
c) In order to improve usability and reduce repetition, the Panel suggests that
Appendix B should be incorporated in its entirety into Chapter 2. As it now
stands, neither Appendix B nor Chapter 2 give the total picture, and the different
numbering of steps in these two parts of the Manual adds to the confusion. If for
some pressing reason the two cannot be merged, then at a minimum
cross-references to appropriate sections of Appendix B should be sprinkled
throughout Chapter 2 in order to tie the two together. Attachment B-l to
Appendix B also provides information that is important for understanding the
underpinnings of a performance-based laboratory process; it may not need to be
elevated to chapter status, but technically oriented readers should be encouraged
to read it.
d) Instead of discussing all planning process options, the main body of the Manual
should stick with one model (Data Quality Objectives) and discuss the
alternatives only in an appendix.
e) Problems associated with navigating efficiently through the document could be
minimized through the use of a decision tree to guide the user to sections that are
relevant to a particular issue.
f) In the future, navigation through the document could also be made easier through
the use of hyperlinks in a computerized version of MARLAP.
g) In general, the document eventually answers almost every question that occurs to
the reader while reading it. However, it is so extensive that questions that arise in
one section may be answered only in another section well removed from it.
Although the document has extensive cross-referencing, it could do even better in
that regard. Examples are provided in the specific comments compiled in
Appendices C and D.
h) The utility of the Manual would benefit from the inclusion of an index similar in
design, use of key words, and level of detail to the one in MARSSEVI (2000).
3.2.2 Presentation Style
During one of the Panel's subcommittee sessions, a member of the federal MARLAP
Work Group observed that the emphasis of key points and redundancy were already built into the
document, but that key points were nonetheless still being overlooked by new readers. Why is
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that the case? In its role as new readers, the Panel feels that the presentation style is often
ineffective, and that it takes too long for the reader to "catch on" and to "see the big picture."
The following suggestions are made to address that problem:
a) A well-written Executive Summary or Roadmap [such as the one in MARSSIM
(2000)] could provide a means to unify MARLAP by using clear, simple text and
figures to show the linkages among the chapters without the distracting repetition
that is currently present. This summary of the major components of the
MARLAP Manual should use figures and tables in the place of extensive text, as
appropriate, to summarize sequential steps and/or interrelationships.
b) Acronyms are likely to be a major stumbling block at first for most readers.
Although training and time may make some readers more comfortable with use of
acronyms, the document is acronym-heavy and plain language should be used
more often. Numerous acronyms appear to be good candidates for being dropped
from the Manual and replaced with their full terms, such as ADC (analog to
digital converter), AL (action level), ASL (analytical service laboratory), ATD
(alpha track detector), BOA (basic ordering agreement), CC (charcoal canister),
CL (central line of a control chart), COC (chain of custody), COR (contracting
officer's representative), DL (discrimination limit), EDD (electronic data
deliverable), GUM [Guide to the Expression of Uncertainty in Measurement
(ISO, 1995)], and NIM (nuclear instrument module), to name but a few.
c) A good overview figure is needed at the outset, a figure that lays out the entire
planning process and shows the interrelationships among the steps. Figure 1
(appearing at the end of Section 3 of this report) is a suggestion for such a figure.
d) Figures and tables should be designed so as to reinforce the text, or to help reduce
the need for lengthy discussions. For example, Figure 1.1 is particularly helpful
in presenting the concept of a Data Life Cycle without a lot of words. In many
cases, however, the flow charts and other illustrations or tables are not always
particularly useful and are sometimes even confusing, with the important ideas
covered better in the text. For example, the text essentially repeats information in
Table 3.1 without providing any added value. In these cases, the authors or
technical editor should consider deleting one or the other. As an aside, the Panel
noted that the text used in the flow charts is too small in many cases and even
unreadable in a few cases.
e) The MARLAP text is clear about the very non-linear and iterative nature of the
planning process, even at its first step. However, this aspect is not reinforced by
the figures and tables. Figures 1.2 and 1.3 are static and linear; these figures
should include feedback loops to more clearly convey the sense of the process of
continual reassessing and fine-tuning the objectives and approaches. The
11
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repeating spirals used in MARSSIM's Figure D.2, "Repeated Applications of the
DQO [Data Quality Objectives] Process Throughout the Radiation Survey and
Site Investigation Process" (MARSSIM, 2000) illustrate one approach for
capturing this aspect in a graphic format.
f) The draft Manual's Table of Contents indicates that a glossary will be provided.
In this glossary, it may be useful to place terms in italics in each definition to
indicate those terms that are further defined in the glossary, as has been done in
MARS SIM (2000).
3.2.3 Technical Edit
In order to make the Manual more user-friendly, efficient and effective, it should receive
a thorough technical edit. The main objectives of this edit should be to remove the considerable
amount of redundancy, ensure internal consistency among the chapters in presentation style and
formatting, and make wider and more consistent use of effective techniques for presenting
information. The Panel found the following presentation and formatting techniques to be
particularly effective in emphasizing important points:
a) The boxed summaries of Recommendations at the end of Chapters 2 to 7 and
Chapter 9 are useful and easy to understand. However, the number of
recommendations for some chapters appears to be too few relative to the large
amount of detail given in that chapter. Suggestions for additional
recommendations to include in the chapter summaries are provided in Appendix
C of this report (e.g., see comments for sections 2.2, 2.3.1, 2.3.3, 2.4, 2.4.1, 2.5,
2.7.1, 2.7.2 and 3.5).
b) The short discussions on uncertainty and error (MARLAP Section 1.4.7), and on
precision, bias, and accuracy (MARLAP Section 1.4.8) are admirably concise and
focused, saying no more and no less than is appropriate for this introduction to
MARLAP terminology.
c) MARLAP Section 2.2 is another effectively written section, with just the right
level of detail, good pacing, and an effective mix of presentation styles (short
paragraphs, bulleted lists, boxed example).
d) The design and content of Table 2.1 effectively summarizes the planning process
and the role of the radioanalytical specialist in this process.
e) Although the text in MARLAP Sections 2.5.1 to 2.5.4 covers the same topics as
does MARLAP Table 2.1, it does not duplicate the table entries but rather adds
value beyond the information presented in the table. The discussions largely
support one another in a complementary fashion that is not overly repetitive
12
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(although comments in Appendices C and D of this report note some
discrepancies).
f) The specification of inputs and the explicit inclusion of an "Output" statement at
the end of the discussion of each Analytical Planning Issue in MARLAP Section
3.3 are very helpful in understanding the value and importance of each item
discussed.
g) MARLAP Section 3.3.7.1 reinforces critical but subtle guidance by including a
short clear example immediately following the paragraph that describes how to
establish a Measurement Quality Objective (MQO) for method uncertainty.
h) The well-designed checklist formats used in Chapters 7 and 18 are particularly
noteworthy as effective ways to organize and communicate information. Section
7.4.2.2, which addresses on-site audits, is effective in telling the reader what to
look for. This approach is equally useful for the laboratory and the client in that it
identifies for both parties the key aspects to be examined during an audit and thus
facilitates communication between them about expectations. Similarly, the
chapter on Laboratory Quality Control (Chapter 18) provides succinct lists of
potential causes for specific types of analytical problems, which is an effective
way to convey some of the lessons learned from many years of practical
experience by the MARLAP co-authors.
i) Section 8.5 guides the reader through the data verification and validation process
by spelling out the criteria to be met, and the approach to first verify, and then
validate, that the data meet the specified criteria. MARLAP is unusual among
guidance documents on laboratory data acquisition in that it clearly distinguishes
the different issues to be identified and resolved in the data validation and
verification steps.
j) The format used in Chapter 18 subsections is particularly user-friendly: first
defining and summarizing the importance of the issue at hand, then expanding on
its subtleties in a more extended discussion, briefly mentioning excursions as
appropriate, and finally ending with specific examples.
In contrast, reference citations in the document are particularly problematic in the draft
Manual, for being incomplete, inconsistent, and sometimes outdated. Federal regulations cited
in the text should be included in the list of chapter references so that the reader can judge their
potential applicability to specific situations. For example, U.S. Department of Transportation
(DOT) regulations may not be applicable to material transport on roads that are closed to public
access, such as is commonly the case for some DOE laboratories. To the extent possible, cited
references should refer to current editions. Reference citations that include web-site addresses (a
practice which the Panel wholeheartedly supports) also need to be checked prior to publication.
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For example, the web-site address listed for MARSSIM (2000) at the end of Chapters 1 and 3 is
incorrect.
Finally, based upon suspected errors found in some equations, the Panel recommends a
rigorous check of all equations throughout the Manual in order to ensure that they are correct.
Furthermore, the MARLAP Work Group is encouraged to establish a quality assurance/quality
control (QA/QC) plan in order to ensure that the equations, tables, and figures do not get
corrupted during the process leading to final publication.
3.3 Detailed Comments on Technical Content of Part I
3.3.1 Technical Issues
No significant technical errors were found during the Panel's review. However, the
Panel recommends that the MARLAP Work Group consider addressing the following points, at
least in a cursory fashion, in the Manual. Additional technical points are raised in Appendix C to
this report.
a) MARLAP clearly should not be expected to cover every situation involving the
collection and evaluation of radioanalytical data, but it might be useful for the
Manual to state more clearly and directly the types of decisions to which it
applies. Examples of topics beyond its scope include radionuclide speciation in
the environment, demonstration of regulatory compliance, and evaluation of some
innovative radioanalytical approach, such as for analyzing a short-lived and
volatile radionuclide. The Panel refers the federal MARLAP Work Group to
Table 1.1, Scope of MARSSIM, in MARSSIM (2000) as one way to convey
information to the reader on the limits of the Manual's coverage. Table 1 in this
report suggests the types of entries that may be appropriate for an analogous table
in MARLAP.
b) Radionuclides released in the environment from a source can be present in
different physico-chemical forms varying in size, valence, and charge properties.
Although it is outside the current scope of MARLAP to include specific guidance
on analysis of speciation and oxidation states of radionuclides, it nonetheless
should discuss the significance of speciation for proper utilization of
radioanalytical data. Several radionuclides (e.g., plutonium, americium and
uranium) are known to coexist in multiple oxidation states which are each
susceptible to different complexation and hydrolytic reactions and consequently,
result in different physico-chemical properties. Thus, knowledge about the total
concentration of radionuclides in environmental samples is important but may be
insufficient to assess potential ecological mobility and risks to humans.
Prediction of contaminant transport in the environment can be significantly
improved if their physico-chemical associations are well defined. The action
14
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level (e.g., the derived concentration guidance level [DCGL]) often, if not always,
will be set under the assumption that the nuclide is in the worst possible state as
far as risk is concerned (e.g., soluble if the exposure pathway is ingestion).
However, if the nuclide is in fact in a different state, then its presence at levels
slightly above the action level may be inconsequential. If specified as part of the
analytical plan, a laboratory should report the levels of the nuclide in each of its
possible states, but in practice, meeting such a request may not be feasible for
many radionuclides. Protocols for sample collection and preservation and for
speciation measurements are the subject of intense research at the present time.
The MARLAP report should acknowledge the importance of this topic and
mention the complexities associated with it. The MARLAP authors should be
prepared to address the issue of speciation in further detail in future revisions; this
effort may require close coordination with the MARSSIM authors on protocols
for sample collection and preservation.
c) Specific examples of clearly defined DQOs and associated MQOs would be
instructive, particularly for illustrating the application of a graded approach. As
an example, the Manual could discuss how DQOs and MQOs would differ for
analysis of tritium in a liquid sample, depending upon whether the issue being
addressed involves site cleanup, drinking water standards, risk analysis, bioassay
for worker exposure, leak testing, waste acceptance criteria for a specific
treatment facility, effluent monitoring, background survey, or a groundwater
tracer study.
d) In its discussions of DQOs and MQOs, the Panel suggests that MARLAP include
some realistic examples of considerations for developing an optimized strategy
using a performance-based approach. The following examples could be used to
illustrate that, from the perspective of statistical power, it is often better to obtain
many data of only modest quality (e.g., ±30%) than a few data of high quality
(e.g., ±1%). (See comments in Appendix C relating to MARLAP Sections 2.5.4,
3.3.1, 6.4, B3.8, and C.3 for suggested locations in which to make this point)
1) Data collected for reconnaissance purposes, such as screening an area for
hot spots or conducting a preliminary assessment of an area about which
little is known.
2) Data collected for a purpose that does not require great precision or the
prescribed use of a precise method.
3) Data collected when it is known or suspected that uncertainties related to
field sampling (e.g., representativeness of the sample, sample outgassing)
may overwhelm analytical uncertainties.
15
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4) Calibrated air flow measuring devices on air sampling stations (MARLAP
Section 10.5.1, line 1221) offer high precision but maintaining calibrated
instruments can be labor-intensive. An alternative which may be a little
less accurate, but far more reliable, is to simply measure the flow after
placing a new filter on the device and then just before it is removed, and
averaging the results. This average flow rate is multiplied by the run time
(sampler should be equipped with a simple run-time meter) to get the total
flow through the filter. The same flow rate meter, which is taken from
station to station and checked frequently for calibration, provides good
station to station precision in airflow.
5) Along similar lines, some guidance would be useful relating to the use of
data that do not have a good QA/QC pedigree but that are otherwise
believed to be credible.
e) The document makes it clear that the radioanalytical specialist is essential
throughout the planning, implementation, and assessment phases. However, the
skill set for this position differs from that for the generic "health physicist" as
described in most job specifications. It thus may be useful for MARLAP to
include a sample job specification or Statement of Work (SOW) that could be
used by small radioactive materials licensees or small regulatory programs to hire
a radioanalytical specialist to help with writing a project-specific SOW,
evaluating the bids, and assessing the data. In addition, the Manual should note
areas in which individuals with related backgrounds could also conduct some of
the tasks, noting that the role of the "radioanalytical specialist" need not be filled
by a single person with a specific title but rather may be jointly covered by the
expertise and experience of the other team members, e.g., industrial hygienist,
laboratory personnel, scientist, project manager.
f) Timely review of data packages is a very important point that cannot be
emphasized enough. Without feedback from this review process, the whole
process could suffer because needed changes would not be identified in a timely
or effective manner. Although stated clearly in MARLAP Section 5.4.3.3, this
recommendation should be reiterated in the summary section of that chapter as
well as in Chapter 8.
g) The Panel agrees with the approach taken by the authors to seek and identify
points on which consensus could be reached, such as an overall approach (or
structure or framework) to be taken rather than details on the specific steps or the
order in which they should be taken. Nonetheless, it would be useful for the
Manual to openly acknowledge that many areas exist in which agency guidance
or requirements are currently not uniform or consistent, such as in the
establishment of action levels, reporting uncertainties, assessment of penalties if
16
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specifications are not met by the contracted laboratory, differences in number of
significant figures reported, attention given to estimating yields, and treatment of
negative data.
h) There is a need to check generalizations that may not apply to a significant
proportion of the target audience or to the samples with which they may be
dealing, and to assess whether exceptions to these generalizations are sufficiently
important to warrant at least a brief mention. Several examples are given from
Chapter 11:
1) Guidance on line 207 of page 11-8 is to treat contaminated packing
material and packages as radioactive waste; however the possibility that
there may be non-radioactive hazardous contaminants that would require
the contaminated material to be classified as mixed waste is not
mentioned.
2) Similarly, page 11-6 seems to mandate a designated receiving location for
all samples, and page 11-14 states that sample storage areas must be
posted as Radioactive Materials storage areas. For small projects or those
limited to the analysis of very low levels of radioactivity, these apparent
"mandates" may not be applicable or may even be counter-productive
(e.g., by storing low-level samples together with high-level samples).
3) Page 11-4 (lines 73-75) states that laboratory facilities that handle
radioactive materials are required to have a radioactive materials license
issued by the NRC or the Agreement State in which the laboratory
operates, with the exception of certain DOE and DoD laboratories.
However, it is important to make clear that the latter facilities themselves
cannot handle unrestricted levels of radioactive materials. They operate
under similar types of regulation-driven restrictions, which are
administered internally.
i) Chapter 9 of the Manual focuses on verification, validation, and assessment of the
laboratory measurements. Somewhere in that chapter, perhaps in Section 9.2, the
selection of the verification, validation, and assessment personnel should be
discussed. Can some of them come from the performing laboratory? From the
sponsoring organization (e.g., EPA, DOE, or DoD)? From the financially
responsible parties? From an outside organization contracted to do the work?
What qualifications are essential?
j) The example on page 3-16 (lines 458 ff) implies that data are unacceptable if the
uncertainty does not meet the a priori MQO. This is not necessarily the case. For
example, if an action level is 0.1 Bq/g (as in the MARLAP example), the
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uncertainty should be less than 0.01 Bq/g. However, data for a sample with a
concentration of 0.02 Bq/g and an uncertainty of 0.02 Bq/g are still valid and
useful even though the reported uncertainty exceeds the MQO of 0.01 Bq/g. The
MARLAP should make a distinction between the a priori MQO and the validity
of the actual data.
3.3.2 Use of Examples
More examples are needed to illustrate the planning process and the graded approach, so
as to bring these to life for the reader. A variety of clearly presented and realistic scenarios will
be critical to the success of MARLAP and should emphasize the potential benefits of planning
and using a graded approach. The Panel suggests the following aspects be considered for adding
more examples:
a) References to good examples of process outputs (e.g., Statements of Work) from
different agencies would be helpful. Specific examples or case studies would also
be helpful, such as how to analyze a volumetrically-contaminated sample (e.g.,
scrap metal) in order to decide its disposition. Specific scenarios or case studies
could be carried through each chapter to illustrate and contrast how a particular
step would be implemented in those particular cases.
b) The MARLAP process appears to be designed for, and is applicable to, large
projects encompassing a team and a relatively large number of samples.
However, it is not clear that it would be practical to implement for small projects.
Although the document refers to a graded approach, insufficient explicit guidance
is provided for small projects. The detailed process described in the MARLAP
Manual requires intensive use of resources. This is appropriate for large-scale
environmental projects but not for small-scale evaluations and other activities.
Therefore, it would be useful if the Manual could advise users on circumstances
for which a much simpler approach would be appropriate, e.g., similar to the brief
example discussed in Appendix B in MARSSEVI (2000), which applies to certain
users of sealed sources, short half-life materials, and small quantities. The limited
number of references to a "graded approach" in MARLAP (e.g., Sections 2.3.1
and 4.5.3, and the first recommendation on p. 4-18) do not provide guidance that
is clear or complete. For example, the Manual could expand upon its statement in
Section 2.3.1 that the concept of a graded approach extends to the representation
of the planning team by using this opportunity to provide a few concrete examples
of simple activities in which only a few people would need to be involved in the
planning. Examples of the graded approach could also be provided in the
discussion on selection of contract services (Appendix E).
c) The federal MARLAP Work Group should consider whether a simpler version of
MARLAP could be prepared, that would be applicable to the $10,000 to $50,000
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projects that involve taking no more than 10 to 20 samples and that cover a small
area. This is an important point. Regulatory agencies may try to apply the entire
MARLAP process to situations and organizations for which a full-scale effort
would not be appropriate. Some "out" must be available for small projects that
are being required to respond to radiological situations with minimal potential for
real impact. Suppose, for example, an entity had a small site with the potential
for very low levels of contamination. This type of project could be a short-term
decommissioning project, involving a health physicist and a few field and
laboratory personnel. The health physicist would be responsible for site safety as
well as the development of the sampling and analysis plan and production of the
final report. The entire budget could be expended in writing the Project Plans
described in MARLAP. A simpler outline could be developed that would give
reasonable assurance that the DQOs would be met but without the myriad of
written plans and reviews. A limited version of MARLAP could cover the
development of DQOs, sampling and analysis plans, and verification and
validation of data, but would not necessarily go into great detail in the selection
and evaluation of a laboratory. Contract laboratories can be selected just on the
basis of past experience.
d) The Panel recognizes that policies are often implied in the assumptions that are
adopted as part of the planning process, and that it is difficult for a multi-agency
document to address this non-technical aspect. The Panel also recognizes the
concern of the federal MARLAP Work Group that case studies or scenarios could
be interpreted by some users as setting or endorsing a precedent. However, the
Panel recommends that this concern be addressed upfront and that the MARLAP
Work Group not be discouraged from including realistic or complex case studies
or scenarios in the Manual.
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Project Planning Team
Ptlll'tl?
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*NOTE: Planriing, asse-ssrne-rH and iinplesi'trrtatioi'i of protocols for ;i.:?i»olc collection ate-
i'iot shown In this figure ihis asi>2« is oyistcfetlMf scope of MAfiLAft
ld«ally, however. sampling protocols iolto^ a parallel process {MAKSIM, 2000).
Figure 1. Schematic of die MARLAP asKesgrnt-irt mipleiiientation process for
radioanalytical analyse?, Solid arrow? advancement to the step,, while dotted arrows
te feedback loops to steps.
20
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Table 1. Scope of MARLAP
Topic
Within Scope of MARLAP
Beyond Scope of MARLAP
Regulatory guidance
Describes an approach that is
generally consistent with those
required by various federal and state
agencies responsible for managing
radiological contamination
• Does not establish or propose new
regulations for radioanalytical protocols
• Does not address how to demonstrate
compliance with regulations
Applicability to specific
projects
Broadly applicable to any project
requiring the acquisition of
radioanalytical data. Emphasizes a
"graded approach" to data
acquisition, in which the extent of
application is based on the intended
use of the data and the degree of
confidence needed in the quality of
the results
• Does not specify whether or not
MARLAP is applicable to a specific project
• Not intended to address research and
development projects requiring acquisition of
radioanalytical data
• Would be difficult to apply to pre-
existing data, in the absence of detailed
information on the protocols used for sampling
and analysis
Contaminants of
concern
Applicable to any radionuclide for
which action levels are, or can be,
defined
• Does not address analytical protocols
for nonradioactive chemical constituents
• Does not address the determination of
radionuclide speciation or oxidation state
• May be difficult to apply to a
radionuclide for which an action level does not
exist or is irrelevant (e.g., studies of groundwater
recharge and solute transport rates based on
concentrations of natural atmospheric
radionuclides like tritium or carbon-14)
Sampling procedures
Discusses how sampling protocols
can affect the analytical results
Does not provide detailed guidance on sample
collection
Types of media
Addresses analytical issues for a
wide range of media typically
encountered in environmental
sampling studies
Does not contain guidance on sampling or
analyzing fixed contamination on surfaces, i.e.,
radioactive contamination that cannot be readily
removed from surfaces by nondestructive means
such as wiping or washing
Data Quality Objectives
(DQOs) and
Measurement Quality
Objectives (MQOs)
Presents a systematic approach for
developing qualitative and
quantitative statements of the
analytical data requirements for a
project
Does not provide prescriptive or default DQO or
MQO values
Action levels
Describes how action levels are used
to establish quantitative data
requirements adequate to support
decisions
Assumes that action levels will be provided
rather than specified by MARLAP
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Topic
Within Scope of MARLAP
Beyond Scope of MARLAP
Analytical procedures
Guidance given in MARLAP is
performance-based and directed
towards acquiring data adequate to
meet a project's specific data needs.
The Manual should be viewed as a
toolbox with many
components—some of which are
discussed explicitly in MARLAP
and others by reference.
• Does not contain step-by-step
descriptions of analytical procedures
• Does not recommend the use of specific
analytical equipment or procedures
• Does not include novel analytical
procedures that are not yet widely accepted by
the radioanalytical community
• Does not establish specific procedures
for sample storage and disposal
• Does not contain guidance on the
analysis of fixed contamination on surfaces
• Provides only cursory discussions on
laboratory health and safety, and waste
management
Use of analytical data
Discusses how to translate a
decision into a testable hypothesis
with an associated decision error
rate, and provides a set of statistical
tests for evaluating data against the
stated hypothesis
• Does not discuss how measured data are
translated into doses or risks
• Does not discuss how measured data are
compared against release criteria for contaminated
components, equipment or property
• Does not recommend the use of specific
hypotheses, decision error rates, or statistical tests
Non-technical issues
Recognizes that non-technical
factors (e.g., costs, stakeholder
concerns) can impact the selection
of analytical protocols
• Does not discuss non-technical issues
(e.g., legal or policy) in detail
• Does not address public involvement
• Does not address training issues for
analytical protocols
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4. RESPONSE TO CHARGE QUESTION #2:
TECHNICAL ACCURACY OF GUIDANCE ON LABORATORY
OPERATIONS
Charge Question #2: Is the guidance on laboratory operations in the Part II chapters technically
accurate? Does it provide a useful resource base of information for a laboratory's
implementation of a performance-based approach?
4.1 Overall Response to Charge Question #2
MARLAP is an impressive compilation of information and recommendations that should
be immensely useful to radiochemical analysis practitioners. The document addresses the entire
reach of radiochemical analysis from project design to final report of results. Each section
appears to have been prepared by competent specialists in the topic, and little appears to have
been ignored or misinterpreted. The MARLAP document matches the MARSSIM document for
providing guidance for the laboratory analyses of field samples collected under the MARSSIM
approach.
The following discussion focuses on Chapters 10 to 20 (excluding Chapter 19) of Part II
because they specifically discuss the actual laboratory operations of analytical processing and
measurement. Because these chapters are integrated into the entire text, some comments refer to
related aspects in other chapters. On the whole, guidance in these chapters is reliable and well
thought out. However, as would be expected for such a large document, the Panel found
numerous errors. While many of the errors are typographical, they can be misleading, such as
errors involving a chemical formula or technical terminology. Suggested corrections are
compiled in Appendices C and D of this report.
The document is an encyclopedic resource. Chapters 10, 11, 12, 16, 18 and 20 are
particularly well written, technically straightforward, and very useful. For the sake of clarity,
Chapters 13 and 15 require more important revisions because some of the information is either
incomplete, not useful or repetitious. Most of the suggested changes are organizational or
editorial in nature, although they affect the technical clarity of the document and its internal
consistency. Specific parts that would benefit from revisions are identified in Section 4.3 of this
report.
The Panel concludes that the performance-based approach for the MARLAP document is
appropriate and presented clearly and logically. The Panel suggests some reorganization of the
presentation to the user, as described in recommendations provided in this review. Subject to the
caveats listed in this section, Part II of the MARLAP document provides a much needed resource
base for laboratory operations.
The Panel spent considerable time discussing the issue of how to report measured values
that are below the minimum detectable concentration (MDC) as determined from counting
23
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statistics or even negative (due in the latter case to the subtraction of non-negligible background
concentrations). The Panel agrees with the MARLAP authors that the laboratory must report "as
measured" values, whether or not negative or below the MDC, in the product intended for the
scientists who will compile and statistically analyze the results for decision-making and who
must evaluate the reliability of measurements near the limit of detection. The Panel was divided
on the issue as to whether or not the lay public and nontechnical decision makers would be better
served by tables that use "less than" values or statements of nondetectability for such
measurements, in order to provide a better picture of the prevalence of results reliably different
from zero. Reporting in that form will seem more familiar to many users, and doing so also
eliminates the need to explain why the laboratory appears to have measured a physically
impossible value. However, several Panel members strongly objected to the proposal to "dumb
down" results for managers and the public. That practice increases the likelihood that the non-
numeric results will be misused in further analyses and decisions, including the danger of
generating mixed data sets with inconsistent treatment of low-level measurements. The Panel
recommends that the MARLAP Manual address this issue in more depth and attempt to find a
solution that will allow reports to the public and decision makers to be easily understood without
being easily misused. A compromise solution to this quandary is proposed in Section 5.3.2 of
this report.
The Panel also discussed the relationship of uncertainties in the results of laboratory
analyses with the generally much larger uncertainties associated with:
a) derivation of an action level (e.g, a DCGL) from a risk-reduction policy goal, and
b) design of an effective sampling strategy to decide whether the action level is
exceeded.
The federal MARLAP Work Group made it clear orally that its intent was to specify
analytical procedures whose uncertainties would not add significantly to the uncertainties from
other steps of the decision process. To the Panel, that intent is less clear in the written Manual,
and it should be clarified there, perhaps in what is now Section B-1.3. Moreover, some Panel
members are concerned that the user's interpretation of "significant" might not recognize that
there are strategic tradeoffs between the precision of the analytical procedures and the coverage
of the sampling plan. These two steps compete for resources; whether larger sample size with
less analytical precision or smaller sample size with greater analytical precision is best for a
given situation undoubtedly depends on situation-specific factors. Again, the Manual should
devote greater attention to this issue, perhaps in Section B-1.3 and possibly in Section 1.4.7 as
well.
In summary, guidance to the designers and managers of analytical laboratory projects
should be as complete and direct as possible to avoid misuse of the MARLAP process. The
Panel strongly supports the initiation and maintenance of a training program and implementation
of a web site to enhance dissemination of the points raised above, as well as others.
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The MARLAP Manual should emphasize the identification and treatment of data that are
crucial for making decisions. Analyses that influence the overall performance results should be
evaluated and, if necessary, redone prior to the completion of the decision process. Similarly,
this point could also apply to the selection of the null hypothesis. This issue needs to be
addressed in more detail in MARLAP. The most conservative approach may not be the optimal
one. Failure to thoroughly evaluate the null hypothesis in the early stages of a project may lead
to the wrong policy decisions, i.e., that a relatively "benign" site requires remediation. The
Panel expects that this and other aspects of the technical implementation of MARLAP's
performance-based approach will be greatly improved by user feedback as the document is tested
through time.
4.2 Detailed Comments on Organization and Presentation of Part II
The Panel suggests that Part II be divided into two parts to facilitate convenient use in the
laboratory. A reasonable separation may be between Chapters 10 to 14 and Chapters 15 to 20.
Dividing Part II into two parts would make the document more convenient for use by
radiochemists and by radiation detection and quantification users. Such a division would also
help with the unwieldy physical size of the document in its present form, and in locating the
needed information more quickly by the users. This suggested logical division is described in
more detail below.
Partlla. Chapters 10 to 14. These chapters contain information on sampling considerations,
sample receipt and inspection on laboratory premises, sample preparation and pretreatment, and
various separation techniques. All these topics are related and are likely to be used mainly by
the radiochemistry laboratory staff (except possibly Chapter 10, Field and Sampling Issues).
Part lib. Chapters 15 to 20. The remainder of the document, i.e., Chapters 15 to 20, includes
information on nuclear counting, instrumentation, calibration and test sources, data acquisition
and reporting, quality control, statistical considerations, and waste management. These topics
are somewhat related (except Chapters 19 and 20, which are stand-alone chapters) and are likely
to be used mainly by the counting laboratory staff.
Appendices should be rearranged for inclusion with the respective volumes, so as to
facilitate the ease of use. At present, all appendices for Parts I and II are placed at the end of
Part II.
4.3 Detailed Comments on Technical Content of Part II
Note: Additional comments related to these chapters are compiled in Appendices C and D.
Some of these specifically address complexities associated with analytical methods and
techniques.
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4.3.1 Chapter 10: Field and Sampling Issues That Affect Laboratory
Measurement
Overall this chapter is straightforward and useful. Although not necessarily a bad thing,
a disproportionate amount of space is devoted to radon. It is all good information, but invites the
question why there are not analogous sections such as "Selecting Tritium Sampling Methods
Based on Data Quality Objectives" or for any other radionuclide as well? A table summarizing
the known problems related to container and type of acid preservative for the various
radionuclides, matrices, and analytical methods would be a useful addition to Chapter 10. For
example, USGS documents usually indicate hydrochloric acid rather than nitric acid as a
preservative for water. Is there a good reason for this? [Note: These sampling concerns could
logically be addressed in either Sections 10.3.3.1 or 14.10.9.]
Several instances are noted in which the compilation of sampling methods or sampling
data needs is incomplete:
Section 10.4.1. The Manual should remind users that the laboratory needs to document the
amount of vegetative material removed from a sample so that environmental concentrations can
be estimated appropriately for the exposure scenario(s) of interest. Also, sampling soil profiles
and sediment cores for determining total inventory is an important technique that is not presented
in this section of MARLAP. For example: soil at specified depths can be removed and analyzed
separately. A plot of activity as a function of depth can be prepared, and the activity integrated
over a particular depth of soil can be determined [c.f DOE (1990)].
Section 10.4.2.1. This section implies total reliance on models for description of initial mixing
and dispersion of radionuclides discharged to water. The use of dyes or other tracers to quantify
dispersion in studies of complex situations should be acknowledged.
Section 10.4.3.2. In selecting foods and locations for food sampling, it is tempting to limit
consideration of consumption habits to those of European-descended populations. The
consumption and lifestyle habits of native peoples and other ethnic minorities can be quite
different. MARLAP should recommend consideration of these differences. The use of inedible
plants and non-game species as indicator organisms should also be mentioned in this section.
Section 10.5.4.2. Noble gases in air have also been collected for laboratory analysis by
compressing air into Self-Contained Breathing Apparatus (SCBA) tanks, by collecting in
impermeable plastic bladders (e.g., Tedlar) for later compression, or by cryogenic methods.
Radon isotopes do not present an issue as interferents if laboratory analysis is delayed
sufficiently for their decay.
Section 10.5.4.3. Electrets can also be used for monitoring tritium at relatively high levels. The
use of electrets was discussed with regard to radon so a discussion of that technology in the
tritium section would also be appropriate (e.g., Surette and Wood, 1993). Although mentioned
earlier, the molecular sieve technique is not identified as a method for collecting tritium.
26
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Molecular sieves are being used increasingly because of favorable properties such as less water
retention following bakeout and better collection properties in environments with fluctuating
temperatures.
Section 10.5.5.2. Methods for measuring radon flux should be mentioned in this section. In
addition, 220Rn analysis methods should be addressed. Also, it would be appropriate to note here
that MARSSIM Section 6.9 provides extensive guidance on radon measurement methods and
instrumentation.
Section 10.6.2. It would be very useful to indicate or reference suitable combinations of liquid
scintillation fluids (cocktails) and filters for the liquid scintillation method of wipe testing.
The Panel also notes an exception to the general guidance provided on labeling of
samples submitted to analytical laboratories. The statement in Section 10.2.4 (lines 173-176)
provides guidance on ensuring that laboratory data are not influenced by prior knowledge of the
origins of the samples. This is certainly an important consideration and needs to be discussed.
However, the wording implies, perhaps unfairly, that laboratory personnel might take deliberate
actions in this regard. In addition, there are many situations in which a laboratory would need to
be aware of samples with relatively high levels of activity as these may require separate
treatment to prevent cross-contamination, as is reflected in the statement on lines 313-314 in
Section 12.2.4. The statement in Section 10.2.4 could be reworded as follows: "Theproject
manager needs to determine whether the sample numbering scheme is appropriate. It is
advantageous to number samples to be submitted to a laboratory in such a way as to prevent
inadvertent bias on the part of the analyst. However, in some cases, laboratories need to be
aware of "hot" samples because these may require the use of separate areas or labwarefor
processing (see Section 12.2.4). "
Some technical inaccuracies in guidance or in generalizations are noted in this chapter:
Page 10-8. lines 217-219. The time to date of analysis is usually captured in pre-established
holding times, not left to the judgment of field sampling personnel who make entries in the log
or on the data form.
Page 10-21. lines 660-661. "...radionuclides that are highly insoluble, such as isotopes of
uranium, thorium, andplutonium... " This is an invalid premise. Uranium is somewhat soluble
and occurs dissolved in some groundwaters. Thorium and plutonium are better described as
relatively immobile in the environment rather than insoluble, because thorium nitrate, for
example, is certainly soluble.
Page 10-24. line 766. The statement "...paperpulp has been shown to remove more than 95
percent ofradionuclidesfrom solution... " seems too general. Tritium, for example, would not
likely be removed by paper pulp.
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Page 10-27. line 839. The following sentence is much too simplistic as guidance for selecting
milk sampling sites: "Raw milk should be obtained from the closest cows or goats downwind
from a source. " For example, background sites should also be selected, and processed milk may
have to be collected to fully characterize the impact on the general public. Significant iodine
releases are much more likely to result from accidental exposures, which may be short term, than
from continuous routine releases. Relying on a single "downwind" sampling location could
potentially result in underestimating the impact of an episodic event.
4.3.2 Chapter 11: Sample Receipt, Inspection and Tracking
The relationships among various recommended documentation (e.g., bench sheets,
laboratory logbook, "separate paperwork obtained before sample receipt," and "documents
listing requests for specific analyses") need to be made clear. Good examples of these
documents would be useful.
4.3.3 Chapter 12: Laboratory Sample Preparation
Overall, this chapter is straightforward and useful. Note that tritium may also be a
problem for cross-contamination if low-level measurements are made in an environment where
higher-level tritium sources are analyzed or in use. Tritium from leaking exit signs may also be
a problem in certain laboratories. Similarly, background levels of radon progeny from natural
sources in soil or possibly in the building's construction materials may create a problem in low-
level counting laboratories. Short-lived radon decay products can become attached to surfaces,
particularly where a static charge has been induced.
4.3.4 Chapter 13: Sample Dissolution.
In general, this chapter should be reorganized so as to discuss the issues from the
simplest to the most complex. In addition, Section 13.6 (Special Matrix Considerations), Section
13.7 (Total Dissolution and Leaching), and Section 13.8 (Examples of Decomposition
Procedures) should be presented differently. The style in these sections is inconsistent, and the
text is either too general or overly specific with direct quotes from published papers. An
alternative approach would be to refer the reader to specific publications for each special case.
4.3.5 Chapter 14: Separation Techniques
A table summarizing the characteristics of alpha, beta, and gamma radiation should be
inserted at the beginning of Section 14.2 to illustrate that the extent of radiochemical separation
is impacted, in part, by the type of radionuclide emission (e.g., see Table 2 as an example of such
a table). This information relates directly to the understanding of the required chemical
separation for each type of emission.
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Table 2. General Characteristics of Alpha, Beta and Gamma Radiation
Characteristic
Identity
Mass (g)
Charge
Energy characteristic (initial emission
energy)
Penetrating power (relative)
Required radiochemical separation
Alpha
Particles
Helium nuclei
~io-24
2+
Discrete
1
Extensive
Beta Particles
Electrons
Positrons
~io-28
1+
Continuous or
discrete
100
Modest
Gamma Radiation (Photons)
High-energy electromagnetic
radiation (e.g., gamma or x-
rays)
0
0
Discrete
10,000
Minimal or not required
Section 14.10 would benefit from some reorganization and revised headings. This
section would be more appropriately titled "Analysis of Specific Radionuclides," which is its
subject, rather than "Radiochemical Equilibrium," which does not describe its contents. The
presentation would be better balanced by placing current Sections 14.10.1 to 14.10.8 as
subheadings in a new Section 14.10.1 called "Introduction" or "Overview." This overview
should also include a brief explanation concerning the selection of the specific radionuclides that
follow. The selection makes sense but should be justified. Finally, the analytical aspects of
individual radionuclides in current Sections 14.10.9.1 to 14.10.9.12 would be renumbered as
Sections 14.10.2 to 14.10.13.
The citation of references in subsections 14.10.9.1 through 14.10.9.12 is problematic for
the Manual's users. Each of these 12 subsections has 8 sub-subsections, beginning with
"Isotopes" and ending with "Methods of Analysis." The properties of radionuclides that permit
chemical separation are discussed throughout these sub-subsections, but the references that
underlie the presentation for each radionuclide are all bunched in the last sub-subsection,
"Methods of Analysis." It would be far more convenient for the reader if each discussion of a
property that permits separation and purification were associated with the reference on which it
is based. At present, the reader who wants to follow up a particular separation has to guess
which of the references are pertinent. This comment pertains to each of the 12 subsections.
Detailed descriptions of certain aspects of chemical behavior in current Sections 14.10.1
to 14.10.8 should be referred to in the specific radionuclide sections to avoid repetition
concerning matters such as hydrolysis and polymerization. For specific radionuclides discussed
in Section 14.10.9, extensive paragraphs that describe the occurrence, properties, and preparation
of minerals and the metallic state should be deleted unless they are pertinent to the purpose at
hand. Furthermore, some of the discussion on the environmental behaviors of specific
radioelements such as plutonium and uranium is misleading and overly generalized (see specific
comments in Appendix C of this report, relating to Section 14.10.9). For such topics, it might be
best to direct the reader to appropriate up-to-date references rather than to provide detailed
descriptions of aspects that are largely outside the scope of MARLAP. Similarly, the discussion
of toxicity and radiotoxicity in Section 14.10.9 is not appropriate except when advising on
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sample handling, in which case any warning to analysts should include specific information
about use, quantity, and speciation in order to place amounts and effects in perspective. If the
reference to toxicity is intended to explain the purpose or required sensitivity of an analysis, the
reader should be referred to a radiation protection text. In a large tome such as this, the authors
should limit themselves to pertinent information.
4.3.6 Chapter 15: Nuclear Counting Instrumentation
This chapter is a strange presentation of two writing styles: Sections 15.2 to 15.6 and
Sections 15.7 to 15.10. In addition, much of the material in the first part is repeated in the
second part. Although this chapter is admirably concise, it (especially Sections 15.2 to 15.7) is
not consistent with the rest of MARLAP, which is much more detailed. Because of its
conciseness, there is missing information in parts of the chapter. This material appears later in
the chapter and even in Chapter 16 but there needs to be a better organization. The Panel learned
that the reason that Chapter 15 is confusing and/or repetitive is because at least part of it was
taken directly (and with permission) from an American Society for Testing and Materials
(ASTM) text, but its order was reversed. This chapter needs to be rewritten. The material in
Chapter 15 would be more efficiently presented if it were to describe proportional counters and
scintillation counters (or even each of the various types of detectors) first and then describe
specific radiation types. This reordering of material would avoid the need to repeat the
description for each type of radiation.
Section 15.7 is redundant with much of the early material but is written more in the style
of the rest of MARLAP. This section answers many of the questions raised in reading the earlier
sections. It might be worthwhile for the earlier sections to be merged into section 15.7. Perhaps
much of the overlap and difference in presentation in this chapter could be overcome by
reorganizing the chapter. Starting on page 15-26, the chapter reads very well. This section
should be used as a guideline for the earlier parts of the chapter. Pages 15-31 and 32 are
redundant with Chapter 16 and should be deleted. On page 15-39, the writing suddenly becomes
very specific and prescriptive. Consider whether some of the material in Attachment 15 A,
"Field Measurements," is redundant with other chapters on calibration or quality assurance.
The federal MARLAP Work Group should review Chapter 15 to be sure that the
terminology used is consistent with current practices. For example, in Section 15.2 (lines 133
ff), photomultiplier tubes are referred to as "multiplier phototubes." This is not the usual
terminology and is confusing to the reader.
4.3.7 Chapter 16: Instrument Calibration and Test Source Preparation
Chapter 16 seems to be straightforward and unambiguous with a good balance between
the general performance and the prescriptive. There are numerous reference citations. Some of
the instrument descriptions in this chapter are better than the ones in Chapter 15. There are
instances of overlap with other chapters; and although this repetition probably cannot be
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avoided, it is suggested that a better integration of Chapters 12, 13, 15 and 16 be sought. This
may be accomplished in part by including suitable references in the chapters preceding pertinent
discussions in Chapter 16. In general, a better "road map" to these chapters is required for
clarity.
Chapter 16 deals with two topics, instrument calibration and test source preparation.
Because instrument calibration is intimately linked to Nuclear Counting Instrumentation
(Chapter 15), the question arises as to whether this topic should be included in Chapter 15
instead of Chapter 16. In contrast, test source preparation deals with converting the collected
and processed samples to a suitable form for introduction to the counting instrument; hence, this
topic is the bridge to Chapter 15 from:
a) Chapter 12, Laboratory Sample Preparation (for samples that need minimal
preparation),
b) Chapter 13, Sample Dissolution (for samples that need moderate preparation), and
c) Chapter 14, Separation Techniques (for samples that need radiochemical
preparation).
The Panel suggests that the federal MARLAP Work Group consider making Test Source
Preparation a separate chapter either before or following the current Chapter 15. The common
thread between the two parts of Chapter 16 (instrument calibration and test source preparation) is
that both the test samples and the calibration samples should be prepared in the same, consistent
manner. These two topics could be separated, with a note in the test source preparation chapter
that samples need to be consistent for the calibration to apply to all the samples. A note could
also be inserted in the calibration section stating that the calibration sources need to simulate the
geometry and composition of the test samples. The chapter as written flows well and it currently
uses some of the material already introduced in Chapter 15. At a minimum, the document should
be reviewed to ensure that the wording in Chapters 12, 13, and 14 and at the beginning of the
Test Sample Preparation part of Chapter 16 recognizes and facilitates the linkages described
above.
It is not clear what the role for commercial, plated alpha and beta sources is, particularly
for alpha spectrometry. MARLAP should discuss the considerations, cautions, correction
factors, etc. should a laboratory choose to purchase commercial sources rather than custom
making sources from calibrated solutions.
4.3.8 Chapter 17: Data Acquisition, Reduction and Reporting
In general, the text is very well written, with the exception of some repetitions and
redundancies and editorial points as listed in Appendices C and D of this report. The Panel
compliments the authors on the thorough technical job done for this chapter.
-------
One shortcoming is that the advice to laboratories on how to check their own data is not
adequate (discussed in Sections 7.3 and 7.4 and tie-in of Chapter 17 with Chapters 8 and 9).
MARLAP presents consumer advice on how to verify and validate data, but provides no parallel
advice to laboratories on how to check their own data. Verification is possible but not
validation. MARLAP should provide advice on data verification by the laboratory as well as by
the consumer.
4.3.9 Chapter 18: Laboratory Quality Control
This chapter is very well written and the presentation of the material is very accessible.
The Panel compliments the authors for the thorough technical presentations in this chapter. The
MARLAP authors might want to include the International Atomic Energy Agency (IAEA) along
with NIST as a source of certified reference materials [IAEA Analytical Quality Control
Services (AQCS), 2002].
The greatest problem resides in the presentation of the references in the text, which
should be accompanied by a date of publication to distinguish these from earlier versions of the
same documents. The reference section needs work and the format needs to be consistent
throughout the section as well as throughout the MARLAP document (i.e., from chapter to
chapter).
Attachments ISA and 18B are very useful additions to Section 18.3.2, "Statistical Means
of Evaluating Performance Indicators—Control Charts." Attachment ISA serves as a guide to the
various control charts and their use in the statistical evaluation of data sets. The solutions to the
problems given in the section should be verified using an internal QA procedure for all statistical
and numerical problems and equations throughout the MARLAP document. The only problem
noted in Attachment 18B is the equation indexing. Problems and their solutions are well
presented and the section is very useful as an illustration of additional statistical methods
available to the user of control charts.
NOTE: The Panel's comments on Chapter 19 are addressed under Charge Question #3 in
Section 5 of this report.
4.3.10 Chapter 20: Waste Management in a Radioanalytical Laboratory
The chapter has good flow and is well written. The second paragraph in the introduction
is a nice road map that tells what the chapter is all about. The chapter, out of necessity, gives
general guidelines and then lists specific references to lead readers to more detailed information.
Section 20.8, "Useful Web Sites," is an excellent addition to the chapter. However, just before
final publication someone should verify that these sites are all still correct and active.
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5. RESPONSE TO CHARGE QUESTION #3:
GUIDANCE ON MEASUREMENT STATISTICS
Charge Question #3: Is the guidance on measurement statistics - specifically measurement
uncertainty and detection and quantification capability - technically accurate, clearly presented,
and useful for implementation by appropriately trained personnel?
5.1 Overall Response to Charge Question #3
The Panel finds that the issue of measurement statistics is addressed very well but could
benefit from some revision in specific areas (described below) to enhance its value to laboratory
directors and staff. Review comments on Chapter 19 and its attachments have been divided into
four areas: organization, terminology, technical issues, and use of examples. The comments that
follow represent a consensus on issues addressed by the Panel members.
5.2 Detailed Comments on Organization and Presentation of Chapter 19
5.2.1 Organization
Overall the Panel finds that too much material is included in Chapter 19, and that the
material is not presented in the most logical order. The Panel suggests several changes to
address these problems:
a) Divide the chapter into two sections. The simpler concepts of measurement,
detection, and quantification should be discussed in the first section, followed by
a section on the more complex issues regarding uncertainty evaluation and
expression.
b) Provide the most important material at the beginning of the chapter. For example,
there is a good discussion of counting statistics starting on page 19-44. This
discussion should be moved to (or near to) the start of Chapter 19.
c) Attachment 19E contains some good examples. These examples should be
brought into the body of the text in appropriate places.
d) Avoid duplication of examples (e.g., the example on page 19-121 is an exact
duplicate of the one on page 19-69).5. Number the examples to facilitate
reference in the text.
e) Bullet the important points in boxes. The box on the top of page 19-25 is a good
example. It is, however, critical that these boxed "important points" be clear. For
example, the box on 19-25 states: "A measurement result should not be
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compared to the minimum detectable concentration to make an analyte detection
decision. A detection decision may be made by comparing the gross signal, net
signal, or measured analyte concentration to its corresponding critical value."
This important recommendation should also be illustrated at this point by an
example.
f) Eliminate Attachment 19B, "Multicomponent Analyses."
5.2.2 Terminology
The Panel finds the technical presentation to be statistically sound but too complex for
the target audience of laboratory directors and staff. This chapter and several of the attachments
would be more understandable to non-statisticians if an attempt were made to use more
colloquial language for presentations of concepts that will be easier to understand by the target
audience. For example, the presentation of statistical independence vs. correlation provided on
page 19-5, lines 122-127, is unnecessarily complicated and probably not needed. Similarly,
Attachment 19C on coverage factors should either be deleted or revised. As currently written, it
is doubtful that anyone without a Ph.D. in statistics and experience in laboratory uncertainty
analysis could implement this methodology.
Many of the terms used in the measurement statistics chapter may be commonly
employed in the jargon of laboratory science, but these terms are confusing when read by
statisticians. The Panel recognizes that this is a deliberate attempt to distinguish some of the less
rigorous concepts involving laboratory uncertainty from those employed in a more strict
statistical interpretation. Examples are "standard uncertainty" for "standard deviation" and
"coverage factor" for "uncertainty interval" or "confidence interval". For example, on page 19-
10, lines 240-241, a statement is made that: "The uncertainty in x is expressed in the form of a
standard deviation, called the standard uncertainty...". However, on page 19-29, the standard
uncertainty of an input estimate using the sample mean of n observations is given in equation
19.4 as the standard error, which is the standard deviation of a mean of size n. Therefore it is not
clear whether the original definition of standard uncertainty is intended to mean the standard
deviation of the distribution (which does not depend upon sample size) or the standard error, i.e.
standard deviation of a sample statistic which does depend upon the sample size. Perhaps what
should be stated is that the standard uncertainty is the standard deviation of whatever statistic is
chosen as an estimator of the input parameter as actually used in the analytic method, i.e. do not
use the standard error of a mean of size n if the method only uses one replicate for that input
parameter.
The MARLAP Manual frequently uses the word "uncertainty" to describe the inability of
any procedure to measure some value exactly. Sometimes, however, a decision depends on the
true variability of values for a parameter, as with variable soil concentrations over a
contaminated site. In that case, the important uncertainty may be about the value of, say, the
mean, and depends on the sampling strategy as well as the analytic procedure. Moreover, the
variability of measurement results over a set of nominally identical samples can be used to
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characterize the uncertainty in the next measurement of a similar type of sample, and the
variability of measurement results over samples taken from a site can be used to characterize the
uncertainty about the mean soil concentration over that site. The federal MARLAP Work Group
surely recognizes such distinctions between uncertainty and variability. The Panel recommends
that the distinction be discussed early in the document, perhaps directing the reader to a more
detailed discussion later, for example in Chapter 19.
Other examples include vague definitions of "Type B" evaluations and counting
efficiency. Although strictly correct, the former term should not simply be defined as "any
evaluation of standard uncertainty that is not a Type A evaluation" but rather should include a
reference and a more helpful statement that Type B evaluations are typically based upon expert
judgment. Similarly, counting efficiency should be defined in terms such as the ratio of analyte
measured to the amount of analyte present.
The Panel realizes that the MARLAP Manual is directed at laboratory personnel who
may be familiar with the terminology used in the current version. The Panel suggests, however,
that statements be included to inform statisticians, who are likely to get involved, that many of
the terms used are not directly translatable to corresponding statistical parameters or concepts
with which statisticians may be more familiar.
5.3 Detailed Comments on Technical Content of Chapter 19
5.3.1 Statistical Approximations of Uncertainty
The Manual needs to clarify its use of statistical approximations. The discussion of
uncertainty propagation in subsections 19.5.3 (Combined Standard Uncertainty), 19.5.5.1
(uncertainty propagation for nonlinear models), and 19.5.5.2 (Bias) is incomplete and potentially
misleading. In particular, the methods presented are only approximate but this caveat is not
always clearly stated. For example, Equation 19.11 on page 19-33, for combined standard
uncertainty, is only an approximation, not equality. However, the presentation does not clearly
stress the approximate nature of the formula, nor does it indicate the conditions under which this
approximation would be valid. Both the use of an equal sign in the equation as well as the use of
terminology such as "the uncertainty propagation formula" or the "law of propagation of
uncertainty" give the impression that the relationship in Equation 19.11 is equality rather than an
approximation.
In general, it would be helpful if the terminology and notation throughout Chapter 19
clearly indicated the approximate nature of most calculations. For instance, Table 19.1 shows all
results as equalities, even though most formulas in the table are only approximate (except those
for sums and differences). By contrast, in the last row, the table uses an "approximately equal"
sign to indicate that (In 10)2 is only approximately equal to 5.302. This latter result is at least
accurate to four significant figures, while in some cases, the results presented as equalities might
not be accurate to even a single significant figure.
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Similar problems appear throughout Chapter 19. Admittedly, when uncertainties are
small, the errors associated with the first-order Taylor polynomial are likely to be small.
However, the Manual should clearly state whether a formula is an approximation when it is first
introduced, and misleading notation and terminology should be avoided.
Section 19.5.5.2 is described as a discussion of bias. However, this section does not
seem to use the term in the usual statistical sense, as discussed on pages 19-5 and 19-6, but rather
refers to the potential inaccuracy of the Taylor polynomial approximation. Instead of providing
an estimate of the error from use of the Taylor polynomial, the Panel suggests a qualitative
discussion of situations in which this approximation is not accurate (e.g., when the uncertainties
span a range sufficiently large that the function of interest is not approximately linear over that
range).
The discussion in Attachment 19D, "Low-Background Detection Limits," should be
revised to explain when someone should consider formulas A, B, and C, the Stapleton
approximation, or the exact test. If MARLAP intends to suggest a preferred method, it should be
clearly stated, along with recommendations for situations when one of the other methods is
preferable.
The Manual should incorporate discussion on the use of Monte Carlo analysis as an
alternative means for estimating total uncertainties, such as in the situation mentioned above
when the Taylor polynomial approximation would be inaccurate. Section 19.5.5.1 shows how to
include higher-order terms in the uncertainty propagation formula. However, the version of the
uncertainty propagation formula presented in this subsection assumes that "all the input
estimates xt are uncorrelated," and no mention is made of Monte Carlo simulation as an
alternative to the uncertainty propagation formula when uncertainties are substantial. The Panel
believes that when uncertainties are large and it is important to have a good estimate of their
magnitude, Monte Carlo analysis is generally preferable to the use of Taylor series
approximations. Even a second-order Taylor polynomial can be inaccurate when uncertainties
are large and the function of interest is significantly nonlinear. Monte Carlo simulation does not
have this drawback and can achieve any desired level of accuracy simply by increasing the
number of realizations. The Manual should note this and provide one or more references.
Comprehensive references on Monte Carlo simulation include Simulation and the Monte Carlo
Method (Rubinstein, 1981) andMonte Carlo: Concepts, Algorithms, and Applications (Fishman,
1996). Briefer summaries are given in Uncertainty: A Guide to Dealing With Uncertainty in
Quantitative Risk and Policy Analysis (Morgan and Henrion, 1990) and Statistical Models in
Engineering (Hahn et al., 1994).
5.3.2 Treatment of Negative Analytical Values
The treatment of laboratory data in Chapter 19 could benefit from a better distinction of
"a priori" and "a posteriori" data analysis. In the case of "a priori"data, to which Chapter 19 is
devoted, the Panel agrees with the recommendation on page 19-13 that laboratories should report
negative values when they are obtained, even though such values are physically impossible. It is
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clear that the measurement process itself can create negative values, even though the physical
process cannot. Analytical measurement errors are ubiquitous and caused by random and
systematic effects, as well as spurious errors. Whereas random errors are inevitable, and
spurious errors (e.g., operator errors) can be generally avoided by good laboratory practices,
systematic errors can vary greatly between laboratories. For example, systematic errors that
result from an imperfect mathematical model for the relationship between the measurands and
the measurable input quantities on which their values depend, can have significant effects on the
measurement values obtained. Input quantities such as instrument background corrections can
be optimized for a suite of analyses, but can still lead to systematic measurement errors and
mathematically negative values for the measurand because instruments typically show a positive
reading even for samples that are known to contain none of the element of interest. The positive
background reading occurs for many reasons, including but not limited to interfering excitation
energies, external radiation, instrument noise, or other problems, as discussed in MARLAP. In
the case of radionuclides, an additional complication is associated with the presence of
background radiation in the sample (e.g., naturally occurring radiation), a topic which is
addressed in MARSSIM and other risk management documents. Therefore, even after
instrument background has been subtracted out, a set of samples all having zero actual
concentration will be represented analytically, in the vicinity of the detection limit, as a
distribution of values, about half of which will be negative. Large negative values and/or
departures from an equal distribution of negative and positive values can therefore be useful in
that they are indicative of the adequacy and quality of the background correction methodology
chosen by the operator. In other words, the negative values for the measurand are in part a
measure of the suitability and limitations associated with the background correction technique
adopted, even though the negative number is not "physically" real.
For these reasons, the Panel supports the recommendation in MARLAP that negative
analytical results be reported for any and all "a priori" analytical laboratory results, and that the
associated uncertainties always be included, as is the case for any measured value reported.
These data need to be readily available for future reexamination, QA review, and numerical
manipulations such as averaging, trending, and isopleth plotting. In addition, the Panel
recommends that MARLAP authors consider extending the Manual's guidance on the reporting
of negative values and values that fall within the measured uncertainty limits, by suggesting that
(1) these results should be accompanied by the initials "n.d." to indicate a "nondetect," and (2)
further explicatory information should be provided for negative values, such as in footnotes,
because reporting of physically impossible negative values may be confusing to nontechnical
audiences.
Conversely, in the case of the "a posteriori" use of analytical data, the Panel advises that
the application of Bayesian statistical methods be envisioned by MARLAP and documented in
future renditions of this report (Borak, 2000; Miller et al., 2000). It may be too early to judge the
extent to which a Bayesian approach may be beneficial because of the paucity of peer-reviewed
publications on Bayesian analysis of radioanalytical data. However, it appears to be a promising
area of research, particularly for cases in which sources of uncertainty are not initially
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recognized and cannot therefore be quantified using the material based on assumptions about "a
priori" distributions as presented in Chapter 19. One recent example involved data generated by
a whole-body bremsstrahlung counter that was used for decades (Kozheurov et al., 2002). This
counter was subject to a variety of unanticipated influences, such as varying absorption of radon
by different types of cloth, seasonally dependent values of radon contamination, and cesium-137
in global fallout. These various sources of uncertainty were recognized only after the collection
of an extensive set of "a priori" data. Thus, it was more realistic to reevaluate the uncertainties
in the data on the basis of "a posteriori" data analysis, rather than by using the existing "a priori"
uncertainty distribution assumptions.
5.3.3 Use of Examples
Much of the material presented in Chapter 19 is at the limit or beyond the comprehension
of laboratory personnel, managers, and planners. Although the material is generally technically
sound, it is often too complex and presented with so much mathematical content that the targeted
user will have much difficulty in trying to implement the estimation procedures. While the
federal MARLAP Work Group may be reluctant to provide a "cookbook" approach to every
procedure, an ordered set of steps in producing each estimate should be given. After each
estimation procedure is outlined, it should be followed by a numerical example in which each
step is worked out with data values typical of radiological assays. The temptation to make the
examples too simple should be avoided. For example, in Attachment 19E "Example
Calculation," the uncertainties for each input parameter are provided in the calculation of the
combined uncertainty when it is doubtful that most laboratories would have already obtained all
of these values. On the other hand, examples should not include factors that are unlikely to
occur or have negligible effect. For example, is it necessary to include the effects of buoyancy
during weighing and other errors associated with pipettes?
Another potential problem with the current examples is that they seem to imply that the
combined uncertainties associated with radiological measurements are small, particularly when
compared to uncertainties often encountered in field sampling. For example, the total combined
standard uncertainty in Example 19E is only about 14% of the estimated measurand. Perhaps
such a small uncertainty is typical of radiological measurements, but the Panel suspects that
there may be considerably larger combined uncertainties. Examples of scenarios where one
source of uncertainty may dominate and how this situation should be handled would be useful.
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6. RESPONSE TO CHARGE QUESTION #4:
OVERALL INTEGRATION AND IMPLEMENTATION ISSUES
Charge Question #4: What are the overall integration and implementation issues?
6.1 Integration Issues
Careful reading of the MARLAP Manual reveals considerable attention to integrating it
with the earlier MARSSIM document (MARSSIM, 2000). However, it might be useful to
devote a short section early in the Manual showing how the whole process is integrated for
decisions regarding the cleanup of radioactively contaminated sites. Although the Panel
recognizes that MARLAP is not limited to site cleanup decisions, they are probably the most
important drivers for creating MARLAP. The proposed new section should also elucidate the
areas of overlap between MARLAP and MARSSIM as well as their differences in scope and
coverage. The addition of a table summarizing this comparison and linkage is a possible vehicle
for this purpose (e.g., see Table 3 at the end of Section 6 as an example).
What is the relationship of MARLAP to other analytical planning guidance issued or
required by federal agencies? Primary sources of radiochemical methods for several of the
authoring organizations are listed in Table 4 at the end of Section 6. It may be useful to include
an appendix in MARLAP that lists "source methods" for specific radionuclide methods,
including brief descriptions of the contents of each document, similar to the compilation and
description of available guidance on sampling methods in Appendix M of MARSSIM (2000).
Unfortunately, few of the method resources listed in Table 4 fully reflect the proposed
MARLAP guidance. However, many of the authoring organizations for the methods are also
participants in writing MARLAP. Therefore, these same organizations are well-positioned to
revise these methods in a timely fashion following the finalization of MARLAP. The issue is not
so much that existing guidance specifies methods incompatible with MARLAP as it is that
existing guidance may be too prescriptive about procedures. Without the freedom to use the
graded, performance-based MARLAP approach, laboratories may be inhibited from finding the
most cost-effective methods for providing the data needed for a decision. Unless the existing
guidance is revised to encourage the MARLAP approach, the radiochemistry community will not
be able to enjoy all the benefits that MARLAP offers. [Note: The list in Table 4 is based
principally on the public comments of Mr. Donivan Porterfield, augmented and reorganized
slightly by the Panel. It's completeness and accuracy have not been assessed by the Panel,
which offers it simply as a starting point for an effort by the federal MARLAP Work Group to
respond to the Panel's recommendation.]
The Panel believes that it would be useful to show, perhaps through a table of
connections, how the MARLAP Manual interfaces with, augments, or replaces existing guidance
on radiochemical analyses. Where existing guidance appears to limit the full implementation of
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MARLAP, or even to conflict with MARLAP guidance, the source agency should be encouraged
to amend its published guidance or at least to acknowledge in a footnote the potential for
conflicts between MARLAP guidance and published agency guidance. MARLAP may wish to
recommend that those participating agencies that currently attempt to control the quality of
analysis by specifying methods, as in the regulations for the Safe Drinking Water Act, use
MARLAP to control by protocol instead of method, and leave method selection to the analyst.
The Panel encourages each of the authoring organizations to initiate a review of its existing
guidance and to withdraw or revise them if necessary to reflect the MARLAP guidance.
Otherwise, a mixed message will be sent to the user community: on the one hand, advocating the
right way to do radiochemical analyses, while on the other hand likely legally requiring the
usage of radiochemical methods that follow outdated practices.
The documents listed in Table 4 provide a good start as references for well-established
and widely-accepted analytical procedures that have been developed over the past 50 years for
various radionuclides. The Panel suggests that the federal MARLAP Work Group consider
including this information in the Manual, and that it expand the list to include other sources of
information and references that could assist users in searching and locating individual
radiochemical procedures. Some examples of such resources are (1) the Nuclear Sciences Series
of monograms on individual radioelements, that is published by the National Academy of
Sciences, (2) specific journal articles in Analytical Chemistry, Health Physics, Radioactivity and
Radiochemistry, Radioanalytical and Nuclear Chemistry, and Chemical Abstracts., and (3)
specific specialized books, reports, manuals and symposium proceedings of interest to
radioanalytical chemists. Although MARLAP advocates a performance-based approach to
analyses and is not intended to be a "cookbook" of analytical "recipes," users nonetheless will
need to seek specific laboratory procedures that could best meet the given requirements of a
project. If such a list were to be provided in the Manual, then a simple disclaimer may be
included with it, stating that the various participating organizations consider the listed documents
to be valuable information sources on specific radiochemical procedures (without sanctioning
any specific method).
6.2 Implementation Issues
6.2.1 Composition of the Planning Team
Section 2.4 in MARLAP discusses the composition of the planning team. The first
paragraph of that section states "MARLAP recommends that the planning team consist of all of
the parties who have a vested interest in, or who can influence, the outcome (stakeholders)." In
the following paragraph, the Manual presents a list of potential representatives that does not
explicitly include the parties paying for the analyses and potentially for remedial actions
afterwards (e.g., the Potentially Responsible Parties for a Superfund site). This disconnect may
or may not have been intentional; the Panel can think of reasons for including and for excluding
that class of stakeholders, likely depending on the specific decision for which the analyses are
being conducted. The Panel strongly recommends that the issue be discussed in Section 2.4 and,
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if there is consensus among the federal MARLAP Work Group, the MARLAP recommendation
be made clear. In some cases, moreover, it may be appropriate to include representatives from
the candidate performing laboratory(ies).
6.2.2 Availability of a Trained Workforce
The MARLAP Manual recommends that planning teams include "radioanalytical
specialists." Because any individual will rarely have substantial expertise in all the areas of
interest to radioanalysis (e.g., wet chemistry, spectrometry, statistics, QA/QC), the teams may
need either to include several such individuals or to recruit an individual with general knowledge
of radioanalytical issues AND specially trained in the MARLAP process. In doing so, the
widespread use of MARLAP may create a demand for such individuals that substantially
exceeds the current supply. Declining interest in nuclear power and less emphasis on nuclear
weapons as the centerpiece of U.S. national security has allowed the pool of radioanalytic
specialists to diminish. The MARLAP agencies may need to stimulate a new generation of such
experts through scholarships, fellowships, research grants, teaching grants, or other means in
order to implement MARLAP as envisioned.
A significant decline in research support for nuclear science in general and
radiochemistry in particular has made it difficult to maintain the university faculty base needed
to ensure a steady supply of educated nuclear scientists and radioanalytic specialists that will still
be needed into the future. A decline in fundamental nuclear research, in the number of nuclear
degree-granting programs and in the number of nuclear research reactors on campus facilities, as
well as a decline in research support that would encourage faculty to study the nuclear science
field, have all contributed to a decline in the pool of nuclear scientists and radioanalytic
specialists. Many of the currently retiring generation of nuclear scientists obtained their training
through Atomic Energy Commission (AEC) Special Fellowships in Nuclear Science and
Engineering. DOE continues to support the training of Health Physicists through fellowships
and scholarships, and also administers a "Radiochemistry Education Award Program" and other
education programs through its Office of Nuclear Energy, Science and Technology
(http://www.NE.doe.gov/). However, the DOE's programs focus mainly on nuclear engineering.
To the best of our knowledge, there is no program today for generally trained scientists and
particularly for radioanalytical personnel. This issue is being further explored by the SAB's
RAC in a proposed self-initiated study on the broad topic of education and training related to
guidance developed by EPA and multi-agency work groups.
6.2.3 User Training
Although the planning process is straightforward and logical, the learning curve is steep
at first. Well-designed training courses would be an efficient approach to get new users
comfortable with the process more quickly. In designing these courses, the Panel recommends
that the federal MARLAP Work Group meet with the federal MARS SIM Work Group to find
out the lessons learned by this team over the last couple years. For example, how has
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MARSSIM dealt with the highly variable starting points of prior experience and expertise among
the course attendees? MARLAP is more likely to succeed if separate training courses are
tailored for different audiences: managers, radioanalytical specialists, laboratory personnel,
perhaps auditors. However, it will also be important for the courses to overlap at least slightly
in coverage so as to enhance communication among user groups by ensuring that participants
speak a common language and that all see how each fits into the "big picture." The federal
MARLAP Work Group could also consider offering or coordinating some of the MARLAP
training through the National Environmental Laboratory Accreditation Conference (NELAC).
The stated purpose of this voluntary association of State and Federal agencies, which first
convened in 1995, is to establish and promote performance standards for environmental
laboratory operations (EPA, 2002). NELAC provides a well-established forum for the private
sector to interact with, and provide input to, regulatory agencies in the environmental arena.
Moreover, it is important to take advantage of user feedback not only on the effectiveness of
training but also on MARLAP itself. Users may be able to identify requirements in MARLAP
that are infeasible or counterproductive or, by contrast, identify additions to MARLAP that
would result in data products better suited to the needs of specific decisions. MARLAP could
then become a dynamic document that could respond to users' comments in future revisions.
The MARLAP web site could serve as one place to receive suggestions for improvement, for
example by offering a bulletin board. The Panel recommends that the authoring agencies
commit to the implementation of training and outreach programs with the goal of achieving
better use of the current version of MARLAP and improvements in future versions.
The Panel also recommends that role-playing exercises be part of the user training
courses. The Panel subcommittee addressing the overall approach, i.e., responding to Charge
Question #1, employed this tool at its April 24, 2002 work session. In order to get a sense of
how a laboratory manager or other critical users might perceive MARLAP, the Subcommittee
engaged in a role-playing exercise with members of the federal MARLAP Work Group. The
scenario that was posed was based on a real situation in which elevated alpha activity had been
detected in an unofficial groundwater sample collected from one of the monitoring wells
adjacent to a privately-owned landfill. Subcommittee members took on the roles of the county
administrator, landfill owner, a representative of the State environmental regulatory agency, and
a concerned citizen from the neighborhood adjacent to the landfill. The federal MARLAP Work
Group members adopted the roles of various types of "radioanalytical specialists" that included
an analytical laboratory manager, an independent advisor for the county, and legal advisor to the
landfill owner. The assignment to this group was to work through the MARLAP planning
process described in Part I of the Manual. The radiochemical specialists were asked to direct the
Panel members to the appropriate pages in the Manual that best described each step of the
process.
The exercise only lasted a half hour, during which time the group was able to come to
consensus on the problem definition, decision identification, data inputs, and decision
boundaries. Due to lack of time, the exercise did not proceed as far as developing decision
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rules, specifying limits on decision error rates, or developing DQOs, MQOs, APSs, or a SOW.
Nonetheless, this cooperative exercise was invaluable for focusing attention of the group upon
relevant advice provided in MARLAP. It not only facilitated the flow of information from the
federal MARLAP Work Group to the Subcommittee, but also provided an opportunity for the
Work Group to hear and understand the concerns of the Subcommittee, particularly in
identifying areas where MARLAP guidance may be confusing, scattered, or not a practical guide
for the user. Participants gained an appreciation for the critical importance of the appendices for
key information needed to work through the planning process. Subcommittee members also
became more cognizant of the very nonlinear and iterative nature of the planning process, even
starting at its first step. The exercise raised the awareness of the MARLAP Work Group with
respect to several training issues: how to conduct training, what to include in it, how important it
will be, and assumptions about the prior level of knowledge of the user community. All
participants appreciated the highly variable "starting points" of prior experience and expertise,
and recognized the challenge of designing training that takes this variability into account. The
consensus was that scenarios and training will be critical to the success of MARLAP, by
illustrating the planning process, driving home the potential benefits of the process, and
"bringing it to life."
Finally, user training may be enhanced through the provision of workbooks allowing
trainees to work through example exercises illustrating the various major tasks of MARLAP.
These examples should be neither so simple as to hide the true complexities of implementing a
laboratory project within the MARLAP guidance nor so complicated that judging the adequacy
of the trainee's answers would be difficult. These workbooks would not strictly be a part of the
MARLAP Manual but could be considered appendages useful in training or available for
reference prior to undertaking an unfamiliar type of project.
6.3 Future Enhancements of MARLAP
Many of the changes recommended by the Panel could require considerable effort to
implement in full, and it is not the Panel's intent that release of the Manual be held up to do so.
The value of the Manual to the user community will best be realized if it is managed as a "living
document" with a mechanism in place for its ongoing maintenance and continual improvement
as a multi-agency consensus product. The essence of the MARLAP Manual is to promote a
flexible approach that permits a wide range of analytical procedures, from which a few are
selected to meet the specific needs of a project. It is likely that different procedures will be
developed to meet different DQOs, with a secondary objective of minimizing the cost of
analysis. Additional analytical techniques will be developed for a variety of analytical needs,
including speciation of the radionuclides of interest. Hence, a mechanism should be developed
to promote the exchange of analytical procedures among laboratory personnel, perhaps using
MARLAP user groups to instigate, facilitate, and document the results of such exchanges.
The following list reiterates some of the longer-term enhancements envisioned by the
Panel for the Manual, as described elsewhere in this report:
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a) Better integration with MARS SIM guidance on developing and implementing
sampling and analysis plans,
b) Guidance on the use of Monte Carlo approaches to estimate uncertainties,
c) Guidance on the application of Bayesian analysis to a posteriori data,
d) Up-to-date and indexed list of method resources that describe advances in
sampling, separation, and analytical techniques for radionuclides, including
speciation and oxidation states in the environment,
e) Up-to-date list of relevant regulations and other documents issued by regulatory
agencies, including web-site addresses,
f) Development of companion workbooks for target audiences,
g) Development of appendices containing examples of good planning,
implementing, and reporting documents,
h) Development of a simpler version of MARLAP geared for the planning and
implementation of small projects,
i) Development of a computerized version of MARLAP that includes hyperlinks for
navigation, and
j) Development of updated scenarios and examples that reflect the real-world
experiences of users.
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Table 3. Comparison of MARLAP and MARSSIM Approaches
Issue
MARLAP
MARSSIM
Performance-based
approach
Underlying basis and recurring theme
throughout Part 1, involving 3 major steps:
planning, implementation, and assessment.
(Section 1.4.3)
Uses the data life cycle as the basis for
its performance-based approach, but
does not explicitly define this term
Directed planning
process
Briefly describes several directed planning
processes suitable for projects requiring the
collection of radioanalytical data, and presents
the DQO process in detail (Chapter 2,
Appendix A); detailed discussion of role of
radioanalytical specialist in this process
(Section 2.5)
Uses the DQO process (which is one
type of directed planning process)
(Section 2.3.1, Appendix D)
Graded approach
Recommends the use of a graded approach
(Section 2.3.1), and discusses its application to
planning (Sections 4.3 and 4.5.3) and data
assessment (Section 9.3)
Emphasizes the use of a graded
approach for sampling contaminated
areas (Section 2.2, 2.3) and provides
example of a graded approach
(Appendix B)
Data life cycle
Defines three phases: planning,
implementation, assessment (Section 1.4.1)
Defines four phases: planning,
implementation, assessment, making
decision (Section 2.3, Appendix D,
Appendix E)
Data Quality Objective
(DQO) process
Defines 4 elements for this directed planning
process in Section 2.3.3; 7 steps described in
detail in Appendix B.
Defines 7 steps in the DQO process
(Section 2.3.1, Appendix D)
Data verification and
validation
Extensive discussion of the verification and
validation process (Chapter 8)
Very brief discussions in Section 9.3.
Provides example of data validation
using 6 data descriptors (Appendix N)
Data Quality
Assessment (DQA)
process
Defines 4 steps in the DQA process: review
project plan document (including DQOs),
assess whether samples are representative,
assess data accuracy, assess whether decision
can be made (Section 9.6)
Defines 5 steps in the DQA process:
review DQOs and survey design,
conduct preliminary data review, select
statistical test, verify test assumptions,
draw conclusions (Section 2.3.3, 8.2,
Appendix E)
Sampling design
Sampling design is outside scope
Extensive discussion of survey
planning and design (Chapters 4-5)
Field sampling
Extensive discussion of field sampling,
focusing on those issues that affect laboratory
measurements, such as sample size,
containers, filtering, preservation, storage, and
transport (Chapter 10)
Extensive discussion of field sampling
protocols, mostly focusing on field
surveys (Chapter 6), but also including
sampling for laboratory measurements
(Chapter 7). Provides list of sources of
sampling methods (Appendix M)
Radiation field
equipment and
measurement protocols
Brief discussion of field measurements from
perspective of how conditions under which
these measurements are obtained differ from
those in a laboratory (Attachment 15A)
1-2 page descriptions of common types
of field survey equipment (Appendix
H.2)
Equipment summary tables organized
by type of radiation to be surveyed
(TablesH.I to H.5)
Brief discussions on measurement
protocols (Chapter 6)
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Issue
Radon field
measurements
Radiation laboratory
equipment and
measurement protocols
Obtaining and
evaluating laboratory
services
Action level
Statistical tests for data
evaluation
QA/QC for
measurements
Decision rules and
decision errors
Reporting data
Laboratory or field
health and safety
Laboratory waste
management
Regulations requiring
radioanalytical data
MARLAP
Brief overviews of radon sampling methods
(Section 10.5.5)
Major focus of Part 2, which covers sample
preparation, dissolution and separation
techniques, instrumentation, calibration, and
data acquisition in depth (Chapters 12 to 17)
Selecting and evaluating laboratories are
covered in depth, including contractual
specifications (Chapters 5 and 7; Appendix E)
Discusses use of generic "action level" to
formulate and test hypothesis about
contamination (Appendix C)
Detailed discussion of statistical tests suitable
for testing hypotheses about contaminant
(Chapter 19 and its attachments, Appendix C).
Provides statistical tables (Appendix G)
Discusses performance indicators for
radiochemical and instrumentation steps of
radioanalytical procedures (Chapter 18)
Extensively discussed (Appendix B)
Stresses importance of reporting actual data,
including negative values. Data reports
should include appropriate number of
significant figures, and combined or expanded
uncertainties (Section 19.3.9).
Briefly mentioned, but no extensive
discussions (Sections 10.2.11 and 14.10.9)
Discussed in very general terms in Chapter 20
Outside scope
MARSSIM
Extensive discussion of radon
measurement methods (Section 6.9,
Appendix H.2.4, Table H.4)
1-2 page descriptions of common types
of laboratory instrumentation
(Appendix H.3), Equipment summary
table of systems that measure atomic
mass or emissions (Table H.5)
Laboratory selection is briefly reviewed
(Section 7.4); evaluation of laboratory
services is outside scope
Defines action level as the derived
concentration guideline level (DCGL),
which is used to formulate and test
hypothesis about contamination
(Sections 2. 2 and 4. 3)
Describes tests suitable for use
depending upon whether the
contaminant is absent or present in the
background (Chapter 8, Appendix E).
Provides statistical tables and brief
descriptions of specific statistical
procedures (Appendix I)
Brief discussion of quality assurance
project plan (QAPP) and data
assessment procedures (Chapter 9);
discusses use of Data Quality Indicators
(DQI) (Section N.6)
Extensively discussed (Appendix D.5
and D.6)
Stresses importance of reporting actual
data, including negative values and
results with large uncertainties. Data
reports should include appropriate
number of significant figures,
uncertainties, and applicable method
detection limit (MDL). Recommends
reporting results in same units as
DCGL. (Section 2.3. 5)
Briefly mentioned
Not discussed
Summarizes applicable regulations
(Appendix C). Describes relationship
of MARSSIM to CERCLA and RCRA
Corrective Action process (Appendix
F)
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Table 4. Analytical Planning Guidance Issued or Used by Agencies and Organizations
Authoring MARLAP*
U.S. Environmental Protection Agency
EPA (1916) Interim Radiochemical Methodology for Drinking Water, EPA 600/4-75-008 (revised), March 1976.
EPA (1979) Radiochemical Analytical Procedures for Analysis of Environmental Samples, March 1979.
EPA (1980) Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA 600/4-80-032.
August 1980.
EPA (192,1) Radiochemistry Procedures Manual, EPA 520/5-84-006, December 1987.
EPA (1991) Manual for the Certification of Laboratories Analyzing Drinking Water, EPA 815-B-97-001, March
1997.
40 CFR 61 National Emission Standards for Hazardous Air Pollutants, Part B radiochemical methods.
U.S. Geological Survey
USGS (1976) Selected Methods of the U.S. Geological Survey of Analysis ofWastewaters, Open-File Report
76-177.
USGS (1977) "Methods for Determination of Radioactive Substances in Water and Fluvial Sediments", Chapter A5
in Book 5, Techniques of Water-Resources Investigations of the United States Geological Survey.
U.S. Department of Energy
DOE (1982) RESL Analytical Chemistry Branch Procedures Manual, IDO-12096, U.S. Department of Energy,
Idaho Falls, ID.
DOE (1990) EML Procedures Manual, 27th Edition, Volume 1, HASL-300. Environmental Measurements
Laboratory, New York, NY. [N.B.: As of September 2002, this reference is no longer available in hard copy but is
available on CD and on the internet at: http://www.eml.doe.gov/publications/procman.cfm]
DOE (no date) Methods for Evaluating Environmental and Waste Management Samples.
States:
State of New York (1982) Determination ofRa-226 andRa-228 (Ra-02), January 1980, Revised June 1982.
Radiological Institute Center for Research, New York State Department of Health, Albany, NY.
State of New Jersey (1980) Determination of Radium 228 in Drinking Water, August 1980. New Jersey
Department of Environmental Protection, Division of Environmental Quality, Bureau of Radiation and Inorganic
Analytical Services, Trenton, NJ.
American Society for Testing and Materials (ASTM) International:
ASTM (1994) Annual Book of 'ASTM Standards, Vol. 11.02. American Society for Testing and Materials, West
Conshohocken, PA.
47
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American Public Health Assocation (APHA)
APHA(1971, 1989, 1992, 1995) Standard Methods for the Examination oj'Water and Wastewater, 13th edition
(1971), 17th edition (1989), 18th edition (1992), and 19th Edition (1995). American Public Health Association,
Washington, D.C.
* Based on a list provided by Mr. Donivan Porterfield, and amended by the Panel. Most of these documents are
referenced on the EPA website at http://www.epa.gov/safewater/methods/rads.html
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7. SUMMARY OF FINDINGS AND RECOMMENDATIONS
7.1 Overall
The MARLAP Manual is comprehensive and provides answers—or citations to
documents with answers—to virtually all of the questions that might be asked about
radiochemical analyses in support of environmental decisions. Moreover, its graded and flexible
approach allows a user to select a set of analytical procedures suited to the complexity and
importance of the problem being addressed. The Manual in general provides a convincing
rationale for its recommendations, showing how decisions can be supported with sufficient but
not excessive attention to analytical precision and reliability. It does a thorough job of
explaining how decision makers should make choices in the selection of hypotheses that help
determine the confidence levels associated with the results obtained from analytical laboratories.
One of the major drawbacks of the draft MARLAP document is the sheer size of its two
volumes. Furthermore, the individual volumes are not self-contained because all appendices
have been relegated to the back of the second volume. The Panel suggests that a more efficient
goal would be to reorganize Part I to include Appendices A to E, and to consider dividing Part II
into two parts to facilitate convenient use in the laboratory. A reasonable separation may be
between Chapters 10 to 14 (with Appendix F), which focuses on radiochemistry, and Chapters
15 to 20 (with Appendix G), which focuses on radiation detection and quantification.
7.2 Charge Question #1: Effectiveness and Clarity of the Overall Approach in Part I
7.2.1 Comments
a) The performance-based and flexible approach in MARLAP is appropriate and, for
the most part, presented clearly and logically in the draft MARLAP Manual.
b) The guidance provided with regard to a graded approach for projects of different
scope, as well as the emphasis on data quality sufficient for the decision being
supported, is reasonable.
c) The linkage of the planning, implementation, and assessment phases of projects
involving radioanalytical data is effective.
7.2.2 Recommendations
The following recommendations are listed in order of the priority placed on them by the Panel.
a) The Manual should undergo a thorough technical edit, the main objectives of
which should be to (1) remove the considerable amount of redundancy, (2) ensure
49
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internal consistency among the chapters in presentation style and formatting, (3)
make wider and more consistent use of effective techniques for presenting
information, (4) proofread all references, equations, tables, figures, and examples,
and (5) reduce the use of acronyms.
b) Provide a well-written Executive Summary using clear, simple text, and figures to
unify the document and show the linkages among the chapters.
c) A good overview figure is needed at the outset, a figure that lays out the entire
planning process and shows the interrelationships among the steps.
d) More examples should be included in the Manual to illustrate the planning
process and the graded approach, so as to bring these to life for the reader. A
variety of clearly presented and realistic scenarios will be critical to the success of
MARLAP and should emphasize the potential benefits of planning and using a
graded approach.
e) To address the concern that regulatory agencies may try to apply the entire
MARLAP process to situations and organizations for which a full-scale effort
would not be appropriate, the Panel suggests the inclusion of more explicit
guidance on how to scale back the process to a level appropriate to the decision
under consideration.
f) Figures and tables should be designed so as to reinforce the text, or to help reduce
the need for lengthy discussions. In particular, the very nonlinear and iterative
nature of the planning process should be indicated by feedback loops in figures to
more clearly convey the sense of the process of continual reassessing and fine-
tuning the objectives and approaches.
g) An appendix containing good examples of process outputs (e.g., DQOs and
Statements of Work) for projects differing in scope and complexity would be
helpful.
7.3 Charge Question #2: Technical Accuracy of the Guidance in Part II
7.3.1 Comments
a) Subject to caveats listed in this review, Part II of the MARLAP document
provides a much needed resource base for laboratory operations, and its guidance,
on the whole, is reliable and well thought out.
b) Numerous technical inaccuracies and inconsistencies in the Manual are identified,
as well as incomplete compilation of sampling methods or sampling data needs
50
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and additional complexities associated with specific analytical methods and
techniques. These detailed comments are listed in Appendix C.
c) Some of the main issues with MARLAP do not concern the content but the ease
of its use as a practical tool. The implementation of radiochemical analyses is
often driven by the requirements of existing methods set as standards by different
organizations. Until these methods are revised, and commitments from the
authoring organizations are obtained, the radiochemistry community may be in
conflict over the application of MARLAP guidance.
7.3.2 Recommendations
As with the recommendations in Section 7.2.2, the following recommendations are given
in order of priority.
a) The Panel strongly supports the initiation and maintenance of a teaching program
and the implementation of a web site to enhance dissemination of guidance on
issues related to MARLAP.
b) Restructuring some of the chapters in Part II could add clarity and usefulness to
the document by providing more consistency in the level of detail, employing a
more logical order of presentation, and inserting appropriate cross-references
between chapters to reduce confusion and repetition. Discussion of limited value
should be deleted, with the reader referred to specific publications (e.g., special
matrices and radionuclide behavior in the environment).
c) Although the Panel agrees that the laboratory must report values "as measured"
when below the limit of detection—or even negative through subtraction of
background—presentations of the data annotated with qualitative indicators of
non-detectability or less-than notation may be desirable to include in reports to
the lay public and to decision makers. The Manual should address this issue and
attempt to find a solution that would maximize lay understanding while
minimizing the potential for misuse.
d) The federal MARLAP Work Group has provided guidance on laboratory analyses
with the intent of ensuring that the uncertainties in their results do not contribute
significantly to the overall uncertainty of the decision process, including those
from the sampling design and those from translating risk-reduction policy goals to
action levels. This intent should be further clarified in the Manual, and the issue
of tradeoffs between sampling coverage and laboratory precision should also be
discussed.
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7.4 Charge Question #3: Guidance on Measurement Statistics
7.4.1 Comments
a) From a technical perspective, statistical issues are addressed very well in the draft
MARLAP Manual. From a presentation perspective, however, too much material
is included in Chapter 19, the material is not presented in the most logical order,
the technical discussions are too complex for the target audience of laboratory
directors and staff, and the terminology differs from that most commonly used by
statisticians.
7.4.2 Recommendations
The recommendations on statistical issues are presented in the order of importance.
a) Many of the terms used in the measurement statistics chapter may be commonly
employed in the jargon of laboratory science, but these terms are confusing when
read by statisticians. Statements should be included to inform statisticians, who
are likely to get involved, that many of the terms used are not directly translatable
to corresponding statistical parameters or concepts with which statisticians may
be more familiar.
b) The Panel recommends that the distinctions and connections between uncertainty
and variability be discussed early in the section on measurement statistics.
c) The terminology and notation throughout Chapter 19 should clearly indicate the
approximate nature of most calculations and clearly state whether a formula is an
approximation when it is first introduced. It should also indicate the conditions
under which each approximation would or would not be valid. If MARLAP
intends to suggest a preferred method, it should be clearly stated, along with
recommendations for situations when one of the other methods is preferable. For
example, Attachment 19D should provide recommendations regarding which of
formulae A, B, C, the Stapleton approximation, or the exact test are preferred and
under what conditions.
d) The Manual should incorporate discussion on the use of Monte Carlo analysis as
an alternative means for estimating total uncertainties. Given recent advances in
desktop computers and work stations, computational restrictions on the use of
Monte Carlo methods are no longer a concern. In this case, however, the user
needs to be reminded that assumptions about parameter distributions are critical.
e) The steps used for each statistical estimate should be clearly laid out in
chronological order so that users of MARLAP will know how to begin and how
52
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to progress through the estimation process. After each estimation procedure is
outlined, it should be followed by a numerical example in which each step is
worked out with data values typical of radiological assays.
f) The potential use of Bayesian analysis should be explored, particularly as a way
to address the problem of negative values resulting from background-corrected
laboratory data.
g) The current statistical examples seem to imply that the combined uncertainties
associated with radiological measurements are small, particularly when compared
to uncertainties often encountered in field sampling. Examples of scenarios
where one source of uncertainty may dominate and how this situation should be
handled would be useful.
7.5 Charge Question #4: Overall Integration and Implementation Issues
The following recommendations are given in priority order:
a) The Panel believes that scenarios and training will be critical to the success of
MARLAP, by illustrating the planning process, driving home the potential
benefits of the process, and "bringing it to life" for the user community. The
Panel recommends that role-playing exercises be part of the user training courses.
b) The Panel recommends that the MARLAP Work Group meet with the MARS SIM
Work Group to find out the lessons learned by this team over the last couple years
for developing well-designed training courses.
c) The Panel recommends that the MARLAP Work Group take advantage of the
training sessions to obtain user feedback not only on the effectiveness of training
but also on MARLAP itself. Users may be able to identify requirements in
MARLAP that are infeasible or counterproductive or, by contrast, identify
additions to MARLAP that would result in data products better suited to the needs
of specific decisions.
d) It might be useful to devote a short section early in the Manual to showing how
the MARSSIM and MARLAP processes are integrated for decisions regarding the
cleanup of radioactively contaminated sites.
e) It would be useful to show, perhaps through a table of connections, how the
MARLAP Manual interfaces with, augments, or replaces existing guidance on
radiochemical analyses.
53
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f) Although it is outside the scope of the Panel's charge, the Panel recommends that
each of the authoring organizations seek to establish a time frame for reviewing
and revising the radiochemical method resources issued by their organizations to
fully reflect the MARLAP guidance. Otherwise, a mixed message will be sent to
the user community: on the one hand, advocating the right way to do
radiochemical analyses, while on the other hand likely legally requiring the usage
of radiochemical methods that follow outdated practices.
g) The MARLAP agencies may need to stimulate a new generation of such experts
through scholarships, fellowships, research grants, teaching grants, or other
means in order to implement MARLAP as envisioned. A decline in fundamental
nuclear research, in the number of nuclear degree-granting programs and in the
number of nuclear research reactors on campus facilities, as well as a decline in
research support that would encourage faculty to study the nuclear science field,
have all contributed to a decline in the pool of nuclear scientists and radioanalytic
specialists. To the best of our knowledge, there is no nuclear science program
today for generally trained scientists and particularly for radioanalytical
personnel. This issue is being further explored by the SAB's RAC in a proposed
self-initiated study on the broad topic of education and training related to
guidance developed by EPA and multi-agency work groups.
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the Measurement of Radioactivity, Annual Book of ASTM Methods., Vol. 11.02. West
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Borak, Thomas B. (editor) (2000) Application of Probability and Statistics in Health Physics.
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Filistovich, V.J., Nedveckaite, T.N., and Styra, BJ. (1986) Activation analysis of 1291. J.
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Ibrahim, S.A., Webb, S.B., and Whicker, F.W. (1994) A semiautomated approach for processing
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(2002) Reference Materials Catalogue, 2002 - 2003. AQCS, IAEA, PO Box 100, A-1400
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Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA 600/4-
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520/5-84-006. December 1987.
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Water and Fluvial Sediments, Chapter A5 in Book 5 of Techniques of Water-Resources
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APPENDIX A - DETAILED DESCRIPTION OF THE SAB PROCESS AND
ITS CHARGE
The EPA Office of Radiation and Indoor Air (ORIA) requested that the Radiation
Advisory Committee (RAC) of the Science Advisory Board (SAB) review the Multi-Agency
Radiological Laboratory Protocols Manual (MARLAP). The MARLAP was introduced to the
RAC at its August 1, 2000 meeting in Washington, DC. The Manual was still in early draft form
at that time and was not available for the RAC to study, beyond the Table of Contents.
The SAB Staff recruited Dr. Jan Johnson, Executive Committee Member of the SAB and
Chair of the SAB RAC, to serve as Chair of the MARLAP Review Panel. The RAC determined
that additional expertise would be needed for the review to assist in addressing the accuracy of
its radiochemical and statistical guidance. Working with the Chair, other SAB members and
consultants, Agency Staff, and suggestions from the public, the SAB Staff identified scientists
and engineers ("Wide Cast") whose expertise appeared to be relevant to answering the questions
in the Charge. Subsequently, the Chair, the Staff Director, and the Designated Federal Official
(DFO) reviewed the list in some detail and identified individuals ("Narrow Cast") to contact
regarding their interest and availability to participate on the Panel. Based on this information
and the importance of having a balanced range of views on the technical issues represented on
the Panel, the Chair and the DFO made recommendations for membership to the Staff Director,
who made the final decision on the composition of the Panel. This process included assigning
Lead and Associate responsibilities to specific Panel members for each of the Charge questions.
The draft Manual was made available to the MARLAP Review Panel in September 2001.
The Panel completed its review in November 2002. This Appendix describes the details of the
Panel's review schedule and process.
A.I Charge Questions and Subcommittee Assignments
Members of the MARLAP Review Panel addressed the specific charge questions posed
by ORIA by organizing into subcommittees for each question, and allocating specific chapters
and appendices to each subcommittee.
Charge Question #1 :Is the overall approach presented in Part 1 of MARLAP for the planning,
implementation and assessment phases of projects which require analysis for radionuclides
technically acceptable?
la. Is the performance-based approach presented clearly and logically?
Ib. Is the approach reasonable in terms of ease of implementation?
Ic. Does the approach effectively link the three phases (planning, implementation,
assessment) of a project?
A-l
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Subcommittee chair: Dr. June Fabryka-Martin
Subcommittee members: Dr. Steve Brown, Dr. Bruce Boecker, Dr. Jill Lipoti, Dr. Helen
GroganApplicable MARLAP chapters:
Primary review materials: Chapters 1-9; Appendices A, B and C
Secondary review materials: Chapters 11 and 18
General review: all chapters and appendices
Charge Question #2:Is the guidance on laboratory operations in the Part II chapters technically
accurate? Does it provide a useful resource base of information for a laboratory's
implementation of a performance-based approach?
Subcommittee chair: Prof. Bernd Kahn
Subcommittee members: Prof. Tom Gesell, Dr. Gilles Bussod, Prof. Genevieve Roessler1, Prof.
Shawki Ibrahim
Applicable MARLAP chapters:
Primary review materials: Chapters 10-18 and 20
Secondary review materials: Chapters 1, 2, 5, 6 and 8
General review: all chapters and appendices
Charge Question #3:
Is the guidance on measurement statistics - specifically measurement uncertainty and detection
and quantification capability - technically accurate, clearly presented, and useful for
implementation by appropriately trained personnel?
Subcommittee chair: Dr. Richard Hornung
Subcommittee members: Dr. Vicki Bier, Dr. Mike Ginevan, Prof. Lynn Anspaugh, Dr. Bobby
Scott
Applicable MARLAP chapters:
Primary review materials: Chapter 19; Appendices B and E; Attachment B-l
Secondary review materials: Chapters 1, 3, 5, 6, 8, 17 and 18.3
General review: all chapters and appendices
Charge Question #4: The MARLAP Review Panel added this fourth charge question during a
planning conference call:
What are the overall integration and implementation issues?
Subcommittee chair: Dr. Steve Brown
Subcommittee members: All MARLAP Review Panel members and consultants
1 Dr. Genevieve Roessler chaired this activity in the absence of Dr. Kahn at the April 23-25,
2002 meeting. She was assisted by Drs. Bussod, Gesell, and Ibrahim and others as appropriate.
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Applicable MARLAP chapters: All materials, and possibly additional supplemental items from
other sources.
A.2 Panel Review Schedule and Process
The RAC was introduced to the MARLAP topic at its publicly-accessible Federal
Register-noticed planning meeting on August 1, 2000 and a subsequent public planning meeting
on MARLAP and other topics on December 12-14, 2000. At the December 12-14, 2000 RAC
planning meeting, the RAC determined that additional expertise would be needed for the review.
Consequently, several consultants were added to the widecast list as candidates for the
MARLAP Review Panel to assist in addressing the organizational aspects of the Manual, as well
as the accuracy of the radiochemical and statistical guidance contained in the Manual. The
RAC's MARLAP Review Panel held its first formal meeting on MARLAP as a public
conference call on April 8, 2002. The goal of this information-gathering conference call meeting
was to clarify any questions that the MARLAP Review Panelists might have, to identify any
gaps in the review materials and any other information sent to the Panel, and to identify areas
that the Agency and the federal MARLAP Work Group should be prepared to clarify at the face-
to-face meeting. The RAC's MARLAP Review Panel added a fourth charge question during this
April 8, 2002 planning conference call dealing with the topic of overall integration and
implementation issues.
On April 23 through 25, 2002 the Panel convened a in the EPA Headquarters Building,
EPA East Building Hearing Room 1153, Washington, DC. The federal MARLAP Work Group
participating in this review included technical staff from the following agencies, departments and
commissions: the U.S. Environmental Protection Agency (EPA), Office of Radiation and Indoor
Air (ORIA), the Department of Energy (DOE), the Department of Defense (DoD), the Nuclear
Regulatory Commission (NRC), the National Institute of Standards and Technology (NIST), the
U.S. Geological Survey (USGS), and the U.S. Food and Drug Administration (FDA). State
participation in the development of the Manual involved contributions from representatives from
the Commonwealth of Kentucky and the State of California.
During the April 23 - 25, 2002 public meeting, the SAB's MARLAP Review Panel heard
presentations from the Agency and the federal MARLAP Work Group staff on the first day.
Public comments were received from Mr. Donivan Porterfield in advance of the meeting. No
additional public comments were received at this meeting. The presentations were followed by
detailed discussion by the MARLAP Panelists on the four charge questions in break-out sessions
held in smaller rooms adjacent to or in close proximity to the EPA Hearing Room, in which all
participants were invited to participate. The second day saw continued break-out session
discussions, a re-convening of the MARLAP Review Panel to discuss its progress and next tasks,
and the making of additional writing assignments by the subcommittee chairs. The discussion in
the break-out sessions focused on key points within each charge question, as well as re-writing
of the pre-meeting written comments by the Panelists to their assigned charge questions, and
teaming in groups by the Panelists to develop merged language edits.
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By the end of the second day, the individual comments and merged edits were discussed
by the Panelists within each of the Working Groups. The third day was engaged with more
refinements of the written materials and focused discussions within each of the subcommittees.
The MARLAP Review Panel decided to exercise its option to conduct a planned technical
editing public conference call in June 27, in which the public can follow the Review Panel's
discussions on the working draft, which is not yet a public consensus report. The Review Panel
anticipated that a public consensus draft would be completed at the end of August, and planned
to hold a second public face-to-face meeting at the end of September to reach closure on edits to
that draft report. The first "working" public draft was developed on August 29, 2002 and posted
on the SAB web site (www.epa.gov/sab under "draft reports") for discussion at the MARLAP
Review Panel's Sept 24-26, 2002 meeting. It is important to note that early on in the process,
the MARLAP Review Panel identified the need for two face-to-face public meetings to resolve
issues, have extensive discussions, and reach a point where closure could be achieved on this
complex and detailed topic.
The MARLAP Review Panel held its planned second public meeting to reach closure on
September 24 -26, 2002 in which the first public draft report, dated August 29, 2002 was shared
with all parties and on which public comments were solicited on the August 29, 2002 public
draft report. Following receipt of Panel and public comments, a revised working draft dated
was prepared and the Panel convened a technical editing (non-FACA) work session on to
complete the edits. Following work session, the edits were incorporated into a second public
draft report dated December 18, 2002. This draft was provided to the SAB's Executive
Committee and the MARLAP Review Panel, and was posted on the SAB web site
(www.epa.gov/sab under "draft reports") for access by the public (including the Agency). A
public closure meeting was held on January 14-15, 2003 in which the SAB's Executive
Committee and the public was given an opportunity for closure comments. At the January 14-
15, 2002 SAB Executive Committee meeting the public was invited to comment by the Chair of
the SAB Executive Committee. The Chair of the MARLAP Review Panel conferred with the
SAB Executive Committee discussants and completed the edits to this advisory, resulting in this
final version being submitted to the Administrator.
NOTE: Throughout the process, the SAB has provided announcements in the Federal Register.
as well as posting notices, agendas, and the publicly-available draft reports on the SAB web site
(www.epa.gov/sab). along with related efforts to reach out to all potentially affected and
interested parties. This also included a public conference call meeting prior to the April, 2002
face-to-face public meeting to discuss and negotiate the charge, determine if the review materials
are adequate, and begin the pre-meeting review and writing process. The MARLAP Work
Group also provided a URL site for the MARLAP Manual and received extensive public
comments as well as comments from all the Agencies, departments and commissions involved,
including review materials, appendices, background briefings and related materials.
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APPENDIX - B - ACRONYMS AND ABBREVIATIONS
[NOTE: Bracketed references following each definition represent
the location in which the acronym first appears.]
• • probability of making a Type I error, i.e., false positive [Appendix C]
• • alpha particle (type of radiation) [Table 2]
• • probability of making a Type II error, i.e., false negative [Appendix C]
• • beta particle (type of radiation) [Table 2]
• • total standard deviation [Appendix C]
• • standard deviation of the sampled population [Appendix C]
• m micrometer [Section 4]
ACE U.S. Army Corps of Engineers [Appendix C]
ADC analog to digital converter [Section 3]
AEA Atomic Energy Act [Appendix C]
AEC Atomic Energy Commission (U.S.)
AL action level [Section 3]
Am americium, as an element or one of its isotopes (e.g., 241Am) [Appendix C]
ANSI American National Standards Institute [Appendix C]
AOAC Association of Official Analytical Chemists [Appendix C]
APHA American Public Health Association [Section 6]
APS analytical protocol specifications [Section 3]
ASL analytical support laboratory [Section 3]
ASTM American Society for Testing and Materials [Section 6]
AQCS Analytical Quality Control Services [Section 4]
ATD alpha track detector [Section 3]
Ba barium, as an element [Appendix C]
Be beryllium, as an element or its isotopes (e.g., 7Be) [Appendix C]
BOA basic ordering agreement [Section 3]
Bq becquerel [Section 3]
c counts [Appendix C]
C celsius temperature scale [Appendix C]
CC charcoal canisters [Section 3]
CD compact disk [Appendix C]
CDF cumulative distribution function [Appendix C]
CERCLA Comprehensive Environmental Response, Compensation, and
Liability Act [Table 3]
cfm cubic feet per minute [Appendix C]
CFR Code of Federal Regulations [Appendix C]
Ci curie [Appendix C]
Cl chlorine [Appendix C]
CL central line (of a control chart) [Section 3]
CLIA Clinical Lab Improvement Act [Appendix C]
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cm centimeter [Section 4]
COC chain of custody [Section 3]
COR contracting officer's representative [Section 3]
cps counts per second [Appendix C]
Cr chromium, as an element [Appendix C]
Cs cesium, as an element or its isotopes (e.g., 137Cs)
d disintegrations [Appendix C]
DC direct current [Appendix C]
DCGL derived concentration guideline level [Section 4]
DFO Designated Federal Official [Appendix A]
DL discrimination limit [Section 3]
DoD U.S. Department of Defense [Section 1]
DOE U.S. Department of Energy [Section 1]
DOT U. S. Department of Transportation [Section 3]
dps disintegrations per second [Appendix C]
DQA data quality assessment [Table 3]
DQO data quality objective [Section 3]
EDD electronic data deliverable [Section 3]
EML Environmental Measurements Laboratory (DOE) [Section 6]
EPA U.S. Environmental Protection Agency [Section 1]
Eu europium, as an element or one of its isotopes (e.g., 155Eu) [Appendix C]
F fluorine, as an element [Appendix C]
FACA Federal Advisory Committee Act [Appendix A]
FDA U.S. Food and Drug Administration [Section 1]
FWFDVI full width of a peak at half maximum [Appendix C]
g gram [Section 4]
Ge germanium, as an element [Appendix C]
GEDD general electronic data deliverable [Appendix C]
GM Geiger-Mueller detector [Appendix C]
GUM Guide to the Expression of Uncertainty in Measurement
(ISO, 1995) [Appendix C]
HASL Health and Safety Laboratory (renamed the Environmental Measurements
Laboratory [EML]) [Appendix C]
H hydrogen, as an element or one of its isotopes (e.g., 3H) [Appendix C]
HPGe high-purity germanium (semi-conductor) [Appendix C]
I iodine, as an element or its isotope (e.g., 129I) [Appendix C]
IAEA International Atomic Energy Agency [Section 4]
IEC International Electrotechnical Commission [Appendix C]
ISO International Organization for Standardization [Appendix C]
IUPAC International Union of Pure and Applied Chemistry [Appendix C]
K potassium, as an element [Appendix C]
LET linear energy transfer [References]
In natural logarithm [Section 5]
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m meter [Appendix C]
M metal ion [Appendix C]
M molar concentration [Appendix C]
mm millimeter [Section 4]
MARLAP Multi-Agency Radiological Laboratory Analytical Protocols (Manual) [Section 1]
MARS SIM Multi-Agency Radiation Survey and Site Investigation Manual [Section 1]
MCA multichannel analyzer [Appendix C]
MDC minimum detectable concentration [Section 4]
Mg magnesium, as an element [Appendix C]
MQC minimum quantifiable concentration [Appendix C]
MQO measurement quality objective [Section 3]
MR moving range [Appendix C]
n neutron [Appendix C]
Nal(Tl) Sodium Iodide (Thallium) ( crystal photon detector) [Appendix C]
NAREL National Air and Radiation Environmental Laboratory (U.S. EPA)
NBS National Bureau of Standards (renamed NIST) [Appendix C]
NCRP National Council on Radiation Protection and Measurements [Appendix C]
nd nondedect [Section 5]
NELAC National Environmental Laboratory Accreditation Conference [Section 6]
NIM Nuclear Instrument Module [Section 3]
NIST National Institute of Standards and Technology [Section 1]
Np neptunium, as an element or its isotope (e.g., 237Np) [Appendix C]
NRC U.S. Nuclear Regulatory Commission [Section 1]
O oxygen, as an element [Appendix C]
ORIA Office of Radiation and Indoor Air (U. S. EPA) [Section 1 ]
OSL optically stimulated luminescence [Appendix C]
p used variously in MARLAP to indicate parameter, percentile,
probability [Appendix C]
PDF probability density function [Appendix C]
pH negative log of hydrogen ion concentration [Appendix C]
Pb P2 photopeaks [Appendix C]
PMT rjhotomultiplier tube [Appendix C]
PTFE rjolytetrafluoroethylene (i.e., Teflon) [Appendix C]
Pu plutonium, as an element or as an isotope (e.g., 238Pu, 239Pu, 240Pu) [Appendix C]
QA quality assurance [Section 3]
QAPP quality assurance project plan [Table 3]
QC quality control [Section 3]
Ra radium, as an element or its isotopes (226Ra, 228Ra) [Section 6]
RAC Radiation Advisory Committee of the EPA Science Advisory Board [Section 1]
RCRA Resource Conservation and Recovery Act [Table 3]
Rn radon, as an element and its isotopes (220Rn, 222Rn) [Appendix C]
ROI region of interest [Appendix C]
s second (time) [Appendix C]
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SAB
SCBA
SI
SNAP
SOW
Sr
Tc
TENORM
Th
TLD
Type A
TypeB
Type I
Type II
U
C]
UBGR
URL
US
USGS
xc
Xp,
sulfur, as an element [Appendix C]
specific activity of material added to a sample for an isotope dilution analysis
[Appendix C]
specific activity of material measured in a sample using isotope dilution analysis
[Appendix C]
Science Advisory Board (U.S. EPA) [Section 2]
Self-Contained Breathing Apparatus [Section 4]
International System of Units [Appendix C]
Systems for Nuclear Auxiliary Power [Appendix C]
Statement of Work [Section 3]
strontium, as an element or its isotopes (88Sr, 89Sr, 90Sr) [Appendix C]
technetium as an element or one of its isotopes (e.g., "Tc) [Appendix C]
Technologically Enhanced Naturally Occurring Radioactive
Material [Appendix C]
thorium, as an element or its isotopes (e.g., 229Th, 230Th, 232Th) [Appendix C]
thermoluminescent detector [Appendix C]
method of evaluation of uncertainty by the statistical analysis of a series of
observations (ISO, 1995) [Section 5]
method of evaluation of uncertainly by means other than the statistical analysis
of a series of observations (ISO, 1995), e.g., based on expert judgment
[Section 5]
decision error that occurs when the null hypothesis is rejected when it is true. The
probability of making a Type I decision error is called alpha (a).
[Appendix C]
decision error that occurs when the null hypothesis is accepted when it is false.
The probability of making a Type II decision error is called beta (|3).
[Appendix C]
standard uncertainty, also known as "one-sigma" uncertainty and expressed as a
standard deviation [Appendix C]
Uranium, as an element or its isotopes (e.g., 233U, 234U, 235U, 236U, 238U) [Appendix
upper bound of the gray region [Appendix C]
uniform resource locator (protocol for specifying a unique address of a file on a
specific computer accessible by other computers) [Appendix A]
United States [MARLAP Roster and Executive Summary]
U.S. Geological Survey [Section 1]
critical value [Appendix C]
minimum detectable value [Appendix C]
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APPENDIX C - TECHNICAL REVIEW COMMENTS
This master list of comments is intended to be limited to technical comments and
some major editorial comments. Editorial comments are compiled in Appendix D. Comments
compiled in this appendix are not consensus comments. They represent the opinions of
individual members of the Review Panel and should not be construed as formal comments of the
RACortheSAB.
Some of the comments in this appendix have also been included in the main body
of this report. In this case, they can be considered to represent the consensus of the Panel
members and formal comments of the RAC and the SAB. The following criteria were used to
identify these comments:
a) Does the comment relate to organization of a chapter or the MARLAP as a
whole?
b) Does the comment relate to the credibility of the MARLAP or its
usefulness to the user?
c) Does the author of the comment feel strongly that it belongs in the body of
the report?
Review comments are listed in order of the chapter to which they pertain.
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