PLM Validation Process Guidelines for Asbestos Data Review


Office of Superfund Remediation and Technology Innovation (OSRTI)
United States Environmental Protection Agency (USEPA)
Washington, DC 20460

October 2016

OLEM Directive: 9200.2-179

y60 ST*\

PRO^

USEPA

PLM VALIDATION

PROCESS

GUIDELINES

For Asbestos Data Review

11-196839

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NOTICE

The policies and procedures set forth here are intended as guidance to the United States
Environmental Protection Agency (hereafter referred to as USEPA) and other Governmental
employees. They do not constitute rule-making by the USEPA, and may not be relied on to
create a substantive or procedural right enforceable by any other person. The Government may
take action that is at a variance with the policies and procedures in this manual.

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TABLE OF CONTENTS

INTRODUCTION	1

DATA QUALIFIER AND REASON CODE DEFINITIONS	2

DATA PACKAGE INSPECTION	3

PRELIMINARY REVIEW	4

POLARIZED LIGHT MICROSCOPY (PLM) DATA REVIEW	5

I.	Sample Receipt	5

II.	Sample Preparation	6

III.	Microscope Alignment	7

IV.	Refractive Index Liquid Calibration	8

V.	Mineral/Fiber Identification Criteria	9

VI.	Blank Analysis	10

VII.	Reference Sample Analysis	10

VIII.	Replicate Analysis	11

IX.	Point Counting	12

X.	Overall Assessment of Data	13

APPENDIX A:	GLOSSARY

APPENDIX B:	TARGET ANALYTE LIST

APPENDIX C:	OPTICAL PROPERTIES OF ASBESTOS FIBERS

APPENDIX D:	ASBESTOS DATA REVIEW SUMMARY

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LIST OF TABLES

Table 1a. Data Qualifiers	2

Table 1b. Reason Codes	2

Table 2. Sample Receipt Actions	6

Table 3. Sample Preparation Actions	7

Table 4. Microscope Alignment Evaluation Actions	8

Table 5. Refractive Index Liquid Calibration Evaluation Actions	8

Table 6. Mineral/Fiber Identification Criteria Evaluation Actions	9

Table 7. Blank Analysis Evaluation Actions	10

Table 8. Reference Sample Analysis Evaluation Actions	11

Table 9. Replicate Analysis Evaluation Actions	12

Table 10. Point Count Analysis Evaluation Actions	13

ACRONYMS

coc

Chain-of-Custody

Rl

Refractive Index

DQO

Data Quality Objective

RPD

Relative Percent Difference

NADES

National Asbestos Data Entry Spreadsheet

SAP

Sampling and Analysis Plan

NIST

National Institute of Standards and Technology

SOP

Standard Operating Procedure

PE

Performance Evaluation

SOW

Statement of Work

PLM

Polarized Light Microscopy

SRM

Standard Reference Material

QAPP

Quality Assurance Project Plan

TR

Traffic Report

QC

Quality Control

USEPA

United States Environmental
Protection Agency

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INTRODUCTION

This document is designed to offer the data reviewer guidance in determining the usability of
analytical data generated through the Statement of Work (SOW) and/or methods applicable to
asbestos sample analysis by Polarized Light Microscopy (PLM), hereinafter referred to as the
PLM SOW. The guidance is somewhat limited in scope and is intended to be used as an aid in
the formal technical review process. It should not be used to establish specific contract
compliance. Definitive guidance is provided where performance should be fully under a
laboratory's control (e.g., blanks, calibration standards, instrument performance checks), while
general guidance is provided for evaluating subjective data that is affected by the site
conditions.

The guidelines presented in the document will aid the data reviewer in establishing: (a) if data
meets the specific technical and quality control (QC) criteria established in the PLM SOW; and
(b) the usability of any data not meeting the specific technical and QC criteria established in the
PLM SOW. It must be understood by the reviewer that acceptance of data not meeting
technical requirements is based upon many factors, including, but not limited to, site-specific
technical requirements, the need to facilitate the progress of specific projects, and availability for
resampling. To make judgments at this level requires the reviewer to have a complete
understanding of the intended use of the data. The reviewer is strongly encouraged to establish
a dialogue with the user to discuss usability issues and to answer questions regarding the
review, prior to, and after data review. It should also be understood that in all cases, data which
do not meet specified criteria are never to be fully acceptable without qualification.

The data reviewer should note that while this document is to be used as an aid in the formal
data review process, other sources of guidance and information, as well as professional
judgment, should also be used to determine the ultimate usability of data, especially in those
cases where all data does not meet specific technical criteria. While data verification and
validation are instrumental to evaluating the accuracy (i.e. absence of transcription errors) and
quality of the reported data, they are only one component of data review. The reviewer should
also be aware that minor modifications to the analytical methods may be made to meet site-
specific requirements, and that these modifications could affect certain validation criteria. A full
copy of a request for modified analysis made to the analytical method should be included in the
data package by the laboratory.

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DATA QUALIFIER AND REASON CODE DEFINITIONS

The following definitions provide a brief explanation of the data qualifiers and reason codes
assigned to results in the data review process. If the data reviewer chooses to use additional
qualifiers and/or reason codes, a complete explanation of those qualifiers or reason codes must
accompany the data review.

Table 1a. Data Qualifiers

Qualifier

Definition

The associated analyte concentrations may be inaccurate or imprecise due to the quality
of the data generated because certain Quality Control (QC) criteria were not met.

The associated analyte identification may be inaccurate and the associated concentration
represents an approximated value.

The non-detect result may be inaccurate or imprecise due to the quality of the data
generated because certain QC criteria were not met.

The sample results are unusable due to the quality of the data generated because certain
criteria were not met. The analyte may or may not be present in the sample.

Auditor defined.

NOTE: Where professional judgment is required, follow-up with the laboratory, technical knowledge and
experience, and/or outreach for professional support/guidance may be applicable.

Table 1b. Reason Codes

Code

Definition

Reported concentrations or analyte identification may be inaccurate due to improper or
infrequent scope alignment.

Identification may be inaccurate due to improper or infrequent Refractive Index (Rl) liquid
calibrations.

The reported concentrations or structure/fiber identification may be inaccurate due to
infrequent or discordant intra- and/or inter-analyst, laboratory duplicate, and/or reference
material analyses.

The reported concentration may be inaccurate due to the presence of analyte
structures/fibers in the associate contamination check or a contamination check was not
performed as required.

The reported concentration may be inaccurate due to the condition of samples upon
receipt at the laboratory and/or improper storage prior to sample preparation and/or
analysis.

The number fields of view or points counted/analyzed are insufficient to meet the required
limit of detection (LOD).

The asbestos identification and concentrations may be inaccurate because the recorded
optical properties (PLM) are not consistent with those described in SOW.

The laboratory procedure did not follow the method-specific requirements.

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DATA PACKAGE INSPECTION

If there are any concerns with the data package regarding apparent missing or incorrect
information, contact the appropriate USEPA personnel for the project.

Items typically included in a data package include:

•	Narrative

•	Traffic Report/Chain-of-Custody (TR/COC) records

•	Cross-reference to laboratory identification (ID)

•	EDD print-outs

•	Laboratory bench sheets (if applicable)

•	Calibration documents

•	Data completeness checklist

•	Communications (if applicable)

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PRELIMINARY REVIEW

This document is for the review of analytical data generated through the PLM SOW and any
future editorial revisions thereof. To use this document effectively, the reviewer should have an
understanding of the analytical method used and a general overview of the sample set or Case
at hand. The exact number of samples, their assigned numbers, their matrix, and the number of
laboratories involved in their analyses are essential information.

It is suggested that an initial review of the data package be performed, taking into consideration
all information specific to the data package (e.g., flexible analysis approval notices, airbills,
Traffic Report/Chain of Custody Records (TR/COCs), Case Narratives).

The reviewer should also have a copy of the Quality Assurance Project Plan (QAPP), SOW, or
similar document for the project for which samples were analyzed. If applicable, the reviewer
should contact the appropriate USEPA personnel to obtain copies of the QAPP and relevant site
information. This information is necessary in determining the final usability of the analytical
data.

Sample sets, or cases, routinely have unique quality control (QC) samples which require special
attention from the reviewer. These include laboratory preparation samples, field duplicates, and
Performance Evaluation (PE) samples, which must be identified. The sampling records (e.g.,
TR/COC Records, field logs, and/or contractor tables) should identify:

1.	The Region where the samples were taken;

2.	Case number;

3.	A complete list of samples, with information on:

a.

Collection and shipping dates;

b.

Preservation*;

c.

Sample matrix;

d.

Sample volumes;

e.

Field duplicates*;

f.

PE samples*;

g-

QC samples*; and

h.

Types of analysis.

(*if applicable)

The TR/COC documentation includes sample descriptions, date(s) and time(s) of sampling,
sample location, and sample matrix. The laboratory's Case Narrative is another source of
general information. The Case Narrative is required for inclusion in the data package and
should contain comments that clearly describe the analyses and any unusual problems
associated with a sample set or project, and state the limitations of the data. Unusual problems
may include:

•	Problems with matrices;

•	Insufficient sample volume for analysis or reanalysis;

•	Samples received in broken containers; and

•	Unusual events.

The reviewer should also inspect telephone or communication logs detailing any discussions of
sample or analysis issues between the laboratory and the USEPA Region.

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POLARIZED LIGHT MICROSCOPY (PLM) DATA REVIEW

The data requirements to be checked are listed below:

I.

Sample Receipt

II.

Sample Preparation

III.

Microscope Alignment

IV.

Refractive Index Liquid Calibration

V.

Fiber Identification Criteria

VI.

Blank Analysis

VII.

Reference Sample Analysis

VIII.

Replicate Analysis

IX.

Point Counting

X.

Overall Assessment of Data

I. Sample Receipt

A.	Review Items:

Traffic Report/Chain-of-Custody (TR/COC) records.

B.	Objective:

The objective is to ascertain the validity of sample results based on the condition,
packaging, and storage of the sample from time of collection to time of sample preparation
and/or analysis.

C.	Criteria:

Analyst inspection documentation must include verification that samples were properly
packaged, sealed, are undamaged, and were labeled upon receipt at the laboratory.

D.	Evaluation:

1.	Verify that the TR/COC documentation indicates that the samples were received
intact. Note in the Case Narrative if the samples were not packaged correctly, there
were any problems with the samples upon receipt, or if the sample condition could
affect the data.

2.	Verify that the information recorded on the COC records, shipping documents, and
sample containers are complete and in agreement.

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3. Verify that the COC records have been signed and dated.
E. Action

Table 2. Sample Receipt Actions

Deficiency

Action

Reason
Code

Detected Analyte

Non-Detect Analyte

Shipment and/or storage conditions
are exceeded

Qualify as estimated (J)

Qualify as estimated (UJ)

SC

COC records, shipping documents,
and sample container information
are not in agreement*

Use professional judgment

Use professional judgment

SC

COC records not signed and dated*

Use professional judgment

Use professional judgment

SC

* Follow-up with laboratory may be required.

II. Sample Preparation

A.	Review Items:

Sample preparation documentation, TR/COC, and NADES records (or equivalent).

B.	Objective:

The objective is to determine from the review of the documents whether all samples were
prepared, visual estimation procedures were applied, whether preparation procedures were
applied, and whether contamination blanks were prepared at the frequency specified in the
SOW, the laboratory's documented procedures (i.e., SOPs), or other applicable guidance
document.

C.	Criteria:

Slide (sample) preparation consists of an initial examination by stereomicroscope and the
preparation of random slide mounts from representative sub-samples of the original sample
in the appropriate refractive index (Rl) liquid. For soil and bulk matrices, a minimum of
three slide mounts are prepared.

D.	Evaluation:

1.	Verify that all samples listed on the COC for PLM analysis have been prepared for
analysis.

2.	Verify that the entire sample was examined by stereomicroscope to determine both
homogeneity and provide a visual estimate of asbestos concentration.

3.	Verify that appropriate procedures were used to prepare samples for analysis, and
that the necessary gravimetric data, if applicable, have been recorded (i.e., pre- and
post-ashing weights).

4.	Verify that contamination blank(s) were prepared at the proper frequency.

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E. Action:

Table 3. Sample Preparation Actions

Deficiency

Action

Reason
Code

Detected Analyte

Non-Detect Analyte

Stereomicroscope was not used
to examine the entire sample
for homogeneity and visual
estimate of asbestos
concentration

Qualify as estimated (J)

No action

MA

Samples were not prepared
and/or recorded using the
appropriate procedures

Qualify as unusable (R)

Qualify as estimated (UJ)

MA

Contamination blank(s) were
not prepared at the required
frequency

Qualify as estimated (J)

No action

B

III. Microscope Alignment

A.	Review Items:

PLM alignment documentation.

B.	Objective:

The objective is to determine if the PLM instrument was aligned in accordance with the
method procedure and frequency requirements. A properly aligned PLM is critical to
ensure the instrument is capable of providing acceptable data.

C.	Criteria:

The following alignment checks must be performed on a daily basis or when the
microscope is determined to be out of alignment by the individual analyst, whichever is
more frequent:

•	Centering of the stage and objectives

•	Centering the optic axis

•	Alignment of lower polar

•	Alignment of upper polar

D.	Evaluation:

Review the provided PLM alignment records to verify the microscope was properly aligned
on the day(s) on which the applicable samples were analyzed.

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E. Action:

Table 4. Microscope Alignment Evaluation Actions

Deficiency

Action

Reason
Code

Detected Analyte

Non-Detect Analyte

Alignment not performed at the
required frequency

Qualify as estimated (J)

Qualify as estimated (UJ)

IV. Refractive Index Liquid Calibration

A. Review Items:

Refractive Index (Rl) liquid calibration records and NADES records (or equivalent).

B. Objective:

The objective is to determine whether proper calibration of the Rl liquids was performed.

C. Criteria:

1. Each Rl liquid used for routine sample preparation and analysis must be calibrated
prior to initial use and as required thereafter, as specified in the appropriate method
(i.e., PLM NIOSH 9002 requires weekly calibration). Records of these calibration
activities must be maintained.

2. The difference between the calibrated Rl of the liquid and the original Rl of the liquid
must not be greater than 0.004. If the difference is greater than 0.004, the liquid may
not be used for the analysis of the samples.

D. Evaluation:

1. Verify that each Rl liquid used for routine sample preparation and analysis were
calibrated prior to initial use, and as applicable thereafter.

2. Ensure the difference between the calibrated Rl of the liquid and the original Rl of the
liquid is not greater than 0.004.

E. Action:

Table 5. Refractive Index Liquid Calibration Evaluation Actions

Deficiency

Action

Reason
Code

Detected Analyte

Non-Detect Analyte

Rl liquid calibration failed criteria

Use professional judgment in
qualifying as estimated (J) or
unusable (R)

Qualify as estimated (UJ)

Rl calibration not performed at
required frequency

Qualify as estimated (J)

Qualify as estimated (UJ)

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V. Mineral/Fiber Identification Criteria

A. Review Items:

NADES records (or equivalent), bench sheets, and raw data (i.e., calibration records).

B. Objective:

The objective is to determine whether optical properties have been recorded for reported
fibers. Positive asbestos identification requires the determination of the following optical
properties:

• Morphology

• Pleochroism

• Birefringence

• Angle of extinction

• Sign of elongation

• Refractive Indices (Rl)

Asbestos cannot be reported in any quantity, including trace, until its optical properties have
been measured and recorded.

C. Criteria:

The optical properties of fibrous material type(s) observed and recorded for samples
analyzed are consistent with those described in the applicable SOW and/or method.

D. Evaluation:

1. For fibrous materials identified as asbestos, verify that the recorded optical properties
are consistent with those provided in applicable SOW and/or method.

2. When non-asbestos fibers are observed, verify that at least one optical property that
distinguishes the fiber from asbestos is measured and recorded on the bench sheet.

E. Action:

Table 6. Mineral/Fiber Identification Criteria Evaluation Actions

Deficiency

Action

Reason
Code

Detected Analyte

Non-Detect Analyte

The recorded optical
properties are not consistent
with those of the asbestos
type reported

Between amphiboles
(i.e. WRTA)

Qualify as
estimated (N)

No action

Between serpentine
(CH) and amphiboles
(i.e. WRTA)

Qualify as
unusable (R)

Optical property not recorded
for non-asbestos fibrous
material

Qualify as estimated (N)

No action

Note: Refer to Appendix C for a list the optical properties of asbestos fibers.

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A. Review Items:

VI. Blank Analysis

NADES records (or equivalent), bench sheets, and raw data.

B. Objective:

The objective is to determine the existence and magnitude of contamination resulting from
laboratory or field activities.

C. Criteria:

The following criteria for evaluation of blanks apply to all laboratory method or preparation
blanks (contamination checks) associated with the samples.

1. Contamination checks (laboratory blanks) must be prepared and analyzed before the
analysis of each set of samples (i.e., Laboratory Job), on days when analysis is
performed.

2. Asbestos fibers must not be detected in the associated blanks.

If problems with a blank exist, all associated data must be carefully evaluated to determine
whether or not there is an inherent variability in the data, or if the problem is an isolated
occurrence not affecting other data.

D. Evaluation:

1. Verify that no asbestos was detected in the associated contamination blanks.
E. Action:

Table 7. Blank Analysis Evaluation Actions

Deficiency

Action

Reason
Code

Detected Analyte

Non-Detect Analyte

Asbestos fibers detected in
contamination blank

Qualify as estimated (J)

Qualify as estimated (UJ)

Note: If the reported sample concentration is at or below the blank concentration level, the non-detect qualifier

applies, unless otherwise specified in the applicable method, SOW, SOP, etc.

VII. Reference Sample Analysis

A. Review Items:

Reference sample analysis documentation and control charts.

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B. Objective:

The objective is to determine whether QA records are maintained for each analyst that
demonstrate the analysis of reference slides each day that samples are analyzed.

C. Criteria:

Reference slide results must be within the laboratory provided control limits. Reference
slides must be analyzed at a rate of one (1) per sampling event (i.e., one per day, per
analyst).

D. Evaluation:

Verify that a reference slide was analyzed at the proper frequency and that the results are
within the control chart limits.

E. Action:

Table 8. Reference Material Analysis Evaluation Actions

Deficiency

Action

Reason
Code

Detected Analyte

Non-Detect Analyte

Reference sample analysis not
performed at the required frequency

Qualify as estimated (J)

Qualify as estimated (UJ)

Reference sample results fall outside
of control limits

Use professional judgment
to qualify as estimated (J) or
unusable (R)

Qualify as estimated (UJ)

VIII. Replicate Analysis

A. Review Items:

NADES records (or equivalent), bench sheets, and control charts.

B. Objective:

The objective is to determine whether replicate analyses are performed at the required
frequency and meet replicate criteria requirements.

C. Criteria:

1. Replicate analyses must be performed at a frequency of one per sample set (i.e.,
Laboratory Job), one per 10 samples if the sample set exceeds 10 samples, or as
directed in the applicable SOW and/or method.

• Replicate sample analyses must meet the error rate requirement (i.e. RPD, as
specified in the laboratory's SOP) on the qualitative analysis for samples containing
chrysotile, amosite, and crocidolite. A slightly higher error rate may occur for
samples that contain anthophyllite, actinolite, and tremolite, as it can be difficult to
distinguish among the three types.

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D. Evaluation:

1. Verify that replicate analyses were performed at a frequency of one per sample set
<10 samples, one per 10 samples for sets >10 samples, or as defined in the
applicable SOW and/or method, and meet the criteria noted above (C.1).

E. Action:

Table 9. Replicate Analysis Evaluation Actions

Deficiency

Action

Reason
Code

Detected Analyte

Non-Detect Analyte

Replicate samples not analyzed
at required frequency

Qualify as estimated (J)

No Action

Replicate sample results fail
established acceptance criteria

Between amphiboles
(i.e. WRTA)

Qualify as
estimated (J)

No Action

Between serpentine
(CH) and amphiboles
(i.e. WRTA)

Qualify as
unusable (R)

IX. Point Counting

A. Review Items:

NADES records (or equivalent), bench sheets, and raw data.

B. Objective:

The objective is to determine whether the following information is documented, as specified
by the method (i.e. PLM PC-400): magnification; graticule size/type; number of slide mounts
prepared; number of empty and/or non-empty points counted; and observance of fibers in a
field of view, but not directly under a point.

If no asbestos fibers appear to be present in the sample a scanning option may be
substituted for point counting.

C. Criteria:

A minimum of 400 points per sample are required to be counted. This could include a
maximum of eight slides with 50 counts each or a minimum of two slides with 200 counts
each per sample. Accuracy and precision improve with the number of points counted.

D. Evaluation:

1. Verify that there is a minimum of 400 points counted per sample, and related
information documented as applicable.

2. If asbestos is identified during the point count, verify that the % Asbestos reported is
calculated using the equation below:

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Percent Asbestos for Point Counting

% asbestos = (A/N) x 100

Where,

A = number of asbestos counts
N = number of points counted (400 minimum)

If % asbestos = 0, report "no asbestos detected (ND)"

If 0 < % asbestos < 1, report concentration to two decimal places, as "<1%

asbestos," or as specified in the applicable method

If % asbestos is greater than 1%, report concentration to the nearest percent,
as ">1% asbestos," or as specified in the applicable method

E. Action:

Table 10. Point Count Analysis Evaluation Actions

Deficiency

Action

Reason
Code

Detected Analyte

Non-Detect Analyte

Less than 400 points counted;
improper/missing information
and/or documentation

Qualify as estimated (J)

Qualify as estimated (UJ)

DL

Percent asbestos improperly
calculated*

Qualify as estimated (J)

Qualify as estimated (UJ)

MA

* Follow-up with laboratory may be required.

X. Overall Assessment of Data

A.	Review Items:

Data package, Case Narrative, Quality Assurance Project Plan (QAPP) [specifically, the
Data Quality Objectives (DQOs)], Statement of Work (SOW), Sampling and Analysis Plan
(SAP), and any communications from the data user that concern the intended use and
desired quality of the data.

B.	Objective:

The objective of the overall assessment of a data package is to provide a brief narrative of
significant data reviewer comments, concerns, and opinions about the quality and usability
of the data.

C.	Criteria:

All method criteria apply.

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D. Evaluation:

1.	Review all available materials to assess the overall quality of the data, keeping in mind
the additive nature of analytical problems.

2.	Evaluate any technical problems that have not been previously addressed.

3.	If appropriate information is available, the reviewer may assess the usability of the
data to assist the data user in avoiding inappropriate application of the data.

4.	If particle size and/or moisture content are requested, check the calculations and
transcription of results for accuracy.

E. Action:

1.	Use professional judgment to determine if there is any need to qualify data which were
not already qualified based on the QC criteria previously discussed.

2.	Write a brief narrative to give the data user an indication of the analytical limitations of
the data. Note for EPA action any inconsistencies between the data and the Case
Narrative. If sufficient information on the intended use and required quality of the data
is available, include an assessment of the data usability within the given context.

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APPENDIX A: GLOSSARY

ACCURACY - The degree of agreement between an observed value and an accepted
reference value. Accuracy includes a combination of precision and bias.

ANALYTICAL SAMPLE - A portion of material to be analyzed that is enclosed in a single
container, received from an external source, and identified by a unique sample number.
Airborne samples are collected on membrane filters and bulk/soil samples are placed in zip-
lock bags.

ANALYTICAL SENSITIVITY - Airborne asbestos concentration represented by one fiber or
structure counted under the microscope. It is determined by the air volume collected and the
proportion of the filter examined.

ASBESTIFORM (MORPHOLOGY) - A specific type of mineral fibrosity in which the fibers
and fibrils possess high tensile strength, flexibility, or long, thin fibers occurring in bundles.

ASBESTOS - The generic name used for a group of naturally occurring mineral silicate fibers
of the serpentine and amphibole series, displaying similar physical characteristics although
differing in composition.

BIAS - A systematic error manifested as a consistent positive or negative deviation from the
known or true value.

BIREFRINGENCE - The numerical difference between the maximum and minimum
refractive indices of an anisotropic substance. Birefringence may be estimated, using a
Michel-Levy Chart, from the interference colors observed under crossed polarizers.
Interference colors are also dependent on the orientation and thickness of the grain, and
therefore are used qualitatively to determine placement in one of the four categories listed
below:

Qualitative

Quantitative (N-n)

Weak

Moderate

Strong

Very Strong

Extreme

None

<0.010
0.011-0.025
0.026-0.100
0.101-0.200
> 0.201

000 or Isotropic

BLANK - A sample designed to assess specific sources of contamination. See individual
definitions for types of blanks.

BULK SAMPLE - A sample of building material taken for identification and quantitation of
asbestos. Bulk building materials may include a wide variety of friable and non-friable
materials.

BUNDLE - Asbestos structure consisting of three or more fibers having a common axis of
elongation with each fiber closer than one fiber diameter.

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CHRYSOTILE - The most prevalent type of asbestos. Chrysotile is a fibrous mineral of the
serpentine group which has the nominal composition:

Mg3Si20s(0H)4

NOTE: In some varieties of chrysotile, minor substitution of silicon by Al3+ may occur.
Minor substitution of magnesium by Al3+, Fe2+, Fe3+, Ni2+, Mn2+, and Co2+ may also be
present.

CONTAMINATION BLANK - Daily contamination check to determine the existence and
magnitude of contamination resulting from laboratory activities.

CONTROL CHART - A graphical plot of test results with respect to time or sequence of
measurement, together with limits within which the results are expected to lie when the
system is in a state of statistical control.

DETECTION LIMIT - The smallest concentration/amount of the component of interest that
can be determined by a single measurement with a stated level of confidence. See Limit of
Detection.

DIFFERENTIAL COUNTING - The term applied to the practice of excluding certain types of
fibers from the fiber count because they do not appear to be asbestos.

DUPLICATE SAMPLES - Two samples taken from and representative of the same
population and carried through all steps of the sampling and analytical procedures in an
identical manner. Duplicate samples are used to assess variance of the total method
including sampling and analysis.

ERROR - Difference between the true and the measured value of a quantity or parameter.

EXTINCTION - The condition in which an anisotropic substance appears dark when
observed between crossed polars. This occurs when the vibration directions in the specimen
are parallel to the vibration directions in the polarizer and analyzer. Extinction may be
complete or incomplete; common types include parallel, oblique, symmetrical, and undulose.

EXTINCTION ANGLE - For fibers, the angle between the extinction position and the position
at which the fiber is parallel to the polarizer or analyzer privileged directions.

FIBER - With reference to asbestiform morphology, a structure consisting of one or more
fibrils.

NOTE: Specifically defined by the method, i.e. (adapted from ISO 10312) a particle that
is 0.5 |jm or longer, with a length-to-width ratio of at least 3:1 or greater, and with parallel
or stepped sides.

FIBRIL - A single fiber of asbestos which cannot be further separated longitudinally into
smaller components without losing its fibrous properties or appearance.

NOTE: A fiber bundle may exhibit diverging fibers at one or both ends.

FIELD - The area within the graticule circle that is superimposed on the microscope image.

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GRATICULE - A microscope slide or eyepiece that contains a grid of lines allowing the size
of objects seen under magnification to be measured.

HETEROGENEOUS - Lacking uniformity in composition and/or distribution of material;
components not uniform. Does not satisfy the conditions stated for homogeneous; i.e.,
layered or in clumps, very coarse grained, etc.

HOMOGENEOUS - Uniform in composition and distribution of all components of a material,
such that multiple subsamples taken for analysis will contain the same components in
approximately the same relative concentrations.

MATRIX - The predominant material of which the sample to be analyzed is composed.

MORPHOLOGY - The structure and shape of a particle. Characterization may be
descriptive (e.g., platy, rod-like, acicular) or dimensional (e.g., length, diameter). See
Asbestiform.

NONEMPTY POINT - The visual superposition of a point over any material in the slide
preparation.

NVLAP - National Voluntary Laboratory Accreditation Program; program administered by
NIST that accredits testing and calibration laboratories.

OFFICE OF LAND AND EMERGENCY MANAGEMENT (OLEM) - The USEPA office that
provides policy, guidance, and direction for the USEPA's solid waste and emergency
response programs, including Superfund.

PLEOCHROISM - The change in color or hue of colored anisotropic substance when rotated
relative to the vibration direction of plane polarized light.

POINT COUNTING - A technique used to determine the relative projected areas occupied
by separate components in a microscope slide preparation of a sample. For asbestos
analysis, this technique is used with PLM to determine the relative concentrations of
asbestos minerals to non-asbestos sample components.

PRECISION - The degree to which a set of observations or measurements of the same
property, obtained under similar conditions, conform to one another. Precision is often
expressed as standard deviation, variance, or range, in either absolute or relative terms.

REFERENCE MATERIAL - A material or substance, one or more properties of which are
sufficiently well established to be used for the calibration of equipment, the assessment of a
measurement method, or for assigning values to materials.

Rl - Refractive Index (Index of Refraction); ratio of the velocity of light in a vacuum relative to
the velocity of light in a medium. It is expressed as n and varies with wavelength and
temperature.

REPLICATION - Procedure in electron microscopy specimen preparation in which a thin
copy, or replica, of a surface is made.

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SERPENTINE - A group of common rock-forming minerals having the nominal formula:
Mg3Si2C>5 (OH)4

Note: Minerals from this family that are important in asbestos analysis include chrysotile,
lizardite, and antigorite.

SRM - Standard Reference Material; a reference material certified and distributed by the
National Institute of Standards and Technology (NIST).

STATEMENT OF WORK (SOW) - A document which specifies how laboratories analyze
samples under a particular Contract Laboratory Program (CLP) analytical program.

STRUCTURE - A microscopic fiber, fiber bundle, cluster, or matrix which may contain
asbestos.

TREMOLITE, ANTHOPHYLLITE, AND ACTINOLITE - The non-asbestos form of these
minerals which meet the definition of a fiber. It includes any of these minerals that have
been chemically treated and/or altered.

WALTON-BECKETT GRATICULE - An eyepiece graticule specifically designed for asbestos
fiber counting. It consists of a circle with a projected diameter of 100 ± 2 |jm (area of about
0.00785 mm2) with a cross hair having tic-marks at 3- |jm intervals in one direction and 5- |jm
in the orthogonal direction.

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APPENDIX B: TARGET ANALYTE LIST

"Asbestos" is a commercial term which applies to the asbestiform varieties of a group of
naturally occurring silicate minerals. The six minerals listed below are specifically regulated as
asbestos by the U.S. government (U.S. CFR, 2003).

Chrysotile (asbestiform serpentine)

CAS# 12001-29-5

Amosite (asbestiform cummingtonite-grunerite)

CAS# 12172-73-5

Crocidolite (asbestiform riebeckite)

CAS# 12001-28-4

Asbestiform anthophyllite

CAS # 77536-67-5

Asbestiform tremolite

CAS # 77536-68-6

Asbestiform actinolite

CAS # 77536-66-4

In addition to the regulated asbestos minerals, 388 minerals are known to occur, at least
occasionally, in fibrous form, some of which are asbestiform. The precise chemical formulation
of each species will vary with the location from which it was mined; therefore, the analytical
sensitivity that can be achieved in asbestos analyses is highly matrix-dependent (Harris, 2007).

The Libby Amphibole (l_A) solution series includes winchite, richterite, tremolite, and actinolite,
(WRTA).

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APPENDIX C: OPTICAL PROPERTIES OF ASBESTOS FIBERS

From Asbestos (bulk): Method 9002, Issue 2, dated 15 August 1994

Table 1. Optica! Properties of Asbestos Fibers





Refractive Index
i Approximate Values)



Mineral

Morphology and Color

	to

Elongation

to

Elongation

Birefringence

Chrysotile

Wavy fibers with kinks
Splayed ends on larger
bundles. Colorless to light
brown upon being heated.
Nonpleochroic. Aspect
ratio typically >10:1.

1.54

1.55

0.002-0.014

Cummingtonite-

Grunente

(Amosite)

Straight fibers and fiber
bundles. Bundle ends
appear broom-like or

1 roun u| 1 -atii u F lay
1 h *-al 1^ |ih ho

3:1.

1.67

1.70

0.02 - 0.03

Crociddite
(Riebeckite)

^trai-iht fl-cp- and fiber
11 n I*-"1 L m|(-r fibers
-.how rui iti im Splayed
<-nd orihuHi"-.
l f ar- 1t°» i-'ic h'i e cot or.
PifA n. 1 ir  tir hi t > •< -v«, '
jJm it hi ju " jx* rati >

1.61

1.63

0-019 - 0.024

T remolite-
Actinotite

Sntin 'i* cm'>«» k.1 fi' ers.

Ih ,1'k'iii iH! t

r utn M ho» -,p iv^
Hid Ti1-!! H tM |
< £fl ^ ^ ( in liV !
tip i or n4 t
II KV! ItHV HIwh is? k
A IM t r tin )tl Ht lv
10:1

1.60- 1.62
(tremoiite)

1.62- 1.67

{actinolite)

1.62- 1.64
(tremoiite)

1.64-1.68
(actinolite)

0.02 - 0.03

Table 1. Optical Properties of Asbestos Fibers (Continued)







Central Stoo Dispersion Staininq Colors

Mineral

Extinction

Sign of
Elonaation

Rl Liquid

	to

Vibration

to

Vibration

Chrysotile

Parallel to fiber

length

+ (length slow)

1.550 m

Blue

Blue-magenta

Cummingtonite-
Grunerite

(Amosite)

Cummingtonite
Grunerite

Parallel to fiber
length

+ (length slow)

1.670

Fibers subjected
to high

temperatures will
not dispersion-
stein.

1.680
1.680

Red magenta to

blue

pale blue

blue

Yellow

blue
gold

Crociddite
(Riebeckite)

Parallel to fiber
length

- (length fast)

1-700
1.680

Red magenta
yellow

Blue-magenta

pate yellow

Anthophyliite

Parallel to fitter
length

+ (length slow)

1.605 HD
1.620 HD

Blue

Blue-areen

Gold to gold-
magenta

Golden-yellow

Tremolite-
Actinolite

nhiitjiif- 10 to
^ti« fui Tiagments.
st mie! < HTiposite

	>W

extinction.

+ (length slow)

1.605 "D

Pale blue
(tremoiite)

Yellow
(actinolite)

Yellow
(tremoiite)

Pale yellow
(actinolite)

HD - high-dispersion Rl liquid series.

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APPENDIX C: OPTICAL PROPERTIES OF ASBESTOS FIBERS (Continued)

From SOP SRC-LIBBY-03 (Revision 2), dated 10 October 2008

Mineral



Refractive Indices

Brseftinpetice

nv.r... .:a

Elongation

Sign



a

,,

Tremolite7

Straight to curbed fibet> and biuiile-: C oioriess to
pale green.

1 -nn_i
1 n.4-1 hi:
1 ~^-l nil
1 -Onj.



. - ""

1 1^3."
.::-i

c 34 ^

0 Ql~-Q C2S

Obh.-ue < up

(length
slow)

Aetmolite

I JHfi-l ty2l
i *11-1 n«S
i MM rCS
t *12t



r*:;.i n:«;
c.-b-l r>55

*> ^,0 >

0.017-0 028

O^ngth

slow)

Wmchite

Straight to curved fibers or bundles. Colorless to pale

blue

PleocoiciiDi weak to moderate: X-colorless, Y=light
blue-"i Z=hght blue"

i dis-i
i si 8-i &:i-

i -20

I



0J4-

.m:

h34-
fij-

HiiiiH IHJ19'
» Ulft"

IS Mil

ii my

Oblige ::ci
15.S::

'"'bL^itK ~-

+

(length

slow)

Ri.clitet.ite

Straight to curved fibers or bundles. Colorless, pale
yellow, brown. pale to dark green, or violet8
Pleochroism weak to strong in pale yellow, orange,
and red'

1 o2M tO*

1 tO'-l c04

i ur



oiv
nj<>

Ml
•S3 *"»'*

ii iii-

ii iir-i o:

nidi ue :i-

1** -

01'1 4Ue 1-

+

(length
slow)

Magnesio-
riebeckite

Fn. inatic ic £lnri: risgteg.it?- Blue gjey-blue pale
blue to yellow. Can be pleochroic.5

1.650-1.673*



*n2-

Up to 0.015-

Obhcaue S-

40

-(fco^th

fast}*

Magnesio-
arfredsooite

Prismatic to fibrous aggregates. Yellowish green.,
brownish green. or srey-blue. Can be pleochroic.s

1.623-1.660*



»3;-

0.012-0.026-

Oblique. 18-
4:";I

- (length
fast)1

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APPENDIX D: ASBESTOS DATA REVIEW SUMMARY

ANALYTICAL TEST REPORT

Bulk Asbestos Analysis by PLM-VE

Prepared For: 	

Address:

Laboratory Name:
Address:

Report Review by:

Date

Standard Laboratory Data Package Checklist

Instructions:	For Analytical Test Reports, complete the following checklist and

attach supporting documentation as outlined below.

1	Laboratory Job No.:

2	Chain of Custody No.:

3	Date of sample receipt:

4	Number of samples received:

5	Analytical Method:

6	Test Report Correction No.:

7	Condition of samples:

8	Attachments:

Chain of Custody form(s)

Case Narrative and any modification forms

Analysis Results

Analytical Bench Sheet(s)

Verification:	Laboratory and Validator Verification signifies that all laboratory QA/QC

tasks were performed for the samples in this Laboratory Job Number and
that this Analytical Test Report is accurate and complete. Laboratory
Verification is done by the person who performed data entry and test
results and Validator Verification is done by the person who performed
the QC check of the data entry.

Laboratory Verification (Initials and Date)
Validator Verification (Initials and Date)

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