RTI/04562/78L-F

AMERICAN INDUSTRIAL HYGIENE ASSOCIATIONBULK ASBESTOS PROFICIENCY ANALYTICAL

TESTING PROGRAM

FINAL REPORT TO LABORATORIES - TEST ROUND A78-109

Prepared for the

American Industrial Hygiene Association2700 Prosperity Avenue, Suite 250

Fairfax, Virginia 22031

Prepared by

Bruce W. Harvey, Stacy S. Doorn, J. Todd Ennis,Lisa C. Greene, Wayne G. Winstead, and Maurice Gerald

Environmental and Industrial Sciences Division

andElizabeth E. Robbins

Research Computing Division

RTI International3040 Cornwallis Road

Research Triangle Park, NC 27709-2194

April 2009

This report may contain confidential information. If you are not the intended recipient, you are herebynotified that any review, dissemination, distribution, or duplication of this report is strictly forbidden. If

you are not the intended recipient, please destroy all copies of the report and contact RTI International.

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TABLE OF CONTENTS

Section Page

I Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

II Test Material Selection and Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

III Reference Laboratory Analyses of Test Materials . . . . . . . . . . . . . . . . . . . . . . 2

IV RTI Analyses of Test Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

V Summary of the Test Round . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

VI Individual Laboratory Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

VII Analysis Problems and Suggestions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

VIII Test Method/Analytical Technique Summary . . . . . . . . . . . . . . . . . . . . . . . . 17

IX Participant Feedback . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

X Schedule for Test Round A79-209 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

LIST OF TABLES

Table Page

1 Results of Reference Analyses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

2 Optical Properties of Asbestos in Test Sample Lots . . . . . . . . . . . . . . . . . . . . 6

3 Semiquantitation Means and Ranges, and Acceptance Ranges . . . . . . . . . . 11

4 Distribution of Penalty Point Totals Incurred . . . . . . . . . . . . . . . . . . . . . . . . . 12

5 Test Sample Classification, Asbestos Identification, and Semiquantitation Errors, by Test Sample Lot . . . . . . . . . . . . . . . . . . . . . . . . 12

6 Cited Test Methods and Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

7 Analysis of Errors and Asbestos Semiquantitation, by TestMethod/Technique Used . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

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AMERICAN INDUSTRIAL HYGIENE ASSOCIATIONBULK ASBESTOS PROFICIENCY ANALYTICAL TESTING PROGRAM

FINAL REPORT TO LABORATORIES - TEST ROUND A78-109

Section I - IntroductionThe 78th test round of the American Industrial Hygiene Association (AIHA) Bulk

Asbestos Proficiency Analytical Testing Program began on February 13, 2009, with the

distribution of test samples to 239 laboratories enrolled for participation. This reflects an

increase in total enrollment of four laboratories from that of Test Round A77-408.

The program provides the means by which a participating laboratory’s proficiency

rating may be determined for the analysis of asbestos in bulk insulation materials by

polarized light microscopy (PLM). Laboratory ratings of “pass” (P) or “fail” (F) are

determined on an individual test round basis and are based on grading criteria and a

penalty point system described on page 13 of this report. The grading criteria cover both

qualitative and semiquantitative analyses.

Each laboratory received four samples, three of which contained asbestos. Lots A,

B, and C contained chrysotile. Lot D did not contain asbestos. The test round was

judged to be of moderate analytical difficulty. The relatively low asbestos content in the

three positive lots suggested that some false negative errors were possible. The

presence of a trace amount of an amphibole in the Lot C material suggested that some

semiquantitative errors due to overestimation of the amphibole mineral were possible.

Few false positive errors were anticipated.

Laboratories were asked to classify each test sample as asbestos-containing

(positive) or non-asbestos-containing (negative). For positive test samples, laboratories

were also asked to identify the type(s) and to semiquantitate the amount of asbestos

present. For all test samples, additional information about fibrous nonasbestos and

nonfibrous matrix/binder materials was also requested. Laboratory performance ratings

were based on correct classification of the test samples, correct identification of the

asbestos type(s) in the positive test sample lots, and correct semiquantitation of the

asbestos type(s) within broad acceptance ranges in those lots.

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Section II - Test Material Selection and PreparationAll four of the bulk materials used in this test round originated from the asbestos

repository at RTI. They included a textured ceiling spray (Lot A), a floor tile (Lot B), a

spray-applied fireproofing (Lot C), and a vinyl sheet flooring (Lot D). These are real-

world materials acquired from asbestos abatement or renovation projects. Detailed

descriptions of these four materials are contained in Sections III and IV of this report.

All four lots were deemed suitably homogeneous, so no mixing or blending was

performed prior to packaging. Packaging consisted of placing small portions (5-10

grams) of the material into a series of standard, plastic scintillation vials or zipper-seal

sample bags. Filled vials and bags were placed in trays, with the order of tray-filling

noted on the side of the tray. Such labeling and ordering of the test sample containers

allow for detection of possible sample bias generated during packaging.

Upon completion of packaging, a quality control check was initiated with a visual

inspection of each test sample container in each test sample lot to verify the presence

of the test material. Then the contents of 20% of the containers constituting all four lots

were examined using PLM. Chrysotile was confirmed in the contents of all the

containers examined for Lots A, B, and C. The trace-level amphibole revealed in RTI’s

subsequent detailed characterization of Lot C was not seen during the quality control

check. However, a small amount of a second, chrysotile-containing, mineral wool-based

insulation material was noted in the contents of 4 of the 53 vials examined for Lot C.

This material was judged to have been situated adjacent to the Lot C material in its

original real-world application. Although some acicular chrysotile was observed in the

mineral wool insulation, subsequent PLM analysis revealed no amphibole minerals to be

present. No asbestos was detected in the contents of any of the containers examined

for Lot D. Homogeneity was judged to be very good in Lots A, B, and D, and moderately

good in Lot C.

Section III - Reference Laboratory Analyses of Test MaterialsTwo independent laboratories, whose principals have provided reference analyses

since the inception of the program, were sent representative subsamples of each lot.

The results of their analyses, along with those of RTI’s in-house analysis, are contained

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in Table 1. The laboratories agreed on the classification of the test sample lots and on

the identification of the major asbestos types in each lot. Agreement was generally good

on the semiquantitative results for the three positive lots. Reference Laboratory Two

and RTI agreed more closely with each other than with Reference Laboratory One on

the quantitation of chrysotile in Lots A and B. The two reference laboratories agreed

more closely with each other than with RTI on the quantitation of chrysotile in Lot C.

Reference Laboratory One and RTI reported a trace of actinolite in Lot C, while

Reference Laboratory Two reported a trace of tremolite. It should be noted that RTI

analysts applied multiple quantitation methods in characterizing all three positive lots.

Laboratories are encouraged to use multiple quantitation techniques whenever possible

to refine visual estimates. Stereomicroscopy and PLM visual estimation were employed

by all three laboratories on all four test samples. Any additional techniques upon which

the reported reference values were based are listed in Table 1 by numerical code for

each laboratory and for each test sample analyzed. Details of these analyses are

contained in the following section.

Section IV - RTI Analyses of Test MaterialsRTI analysts employed a variety of techniques to characterize each of the test

sample lots for comparison to and substantiation of the findings of the reference

laboratories. These techniques included stereomicroscopy, PLM, gravimetric sample

reduction, and x-ray diffraction (XRD). Results of these analyses are summarized in the

subsections that follow.

Stereomicroscopy

Stereomicroscopy was used prior to PLM analysis and gravimetric sample

reduction to obtain a gross characterization of each test sample lot. Subsequent test

sample classification and asbestos identification (in each positive lot), using PLM, by

RTI and the reference laboratories, agreed with these stereomicroscopy analyses.

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Table 1. Results of Reference Analyses

SampleLot

SampleClassifi-cation

ReferenceLaboratory One

ReferenceLaboratory Two RTI

A + 1, 3---------------------------------- 6% Chrysotile 5% Cellulose 20% Perlite Tra Paint 69% Quartz, mica, and acid-soluble binder

3---------------------------------- 3% Chrysotile 15% Cellulose 82% Perlite, acid-soluble binder, and opaque accessories

-------------------------------- 3% Chrysotile 27% Cellulose 57% Acid-soluble binder 13% Perlite, quartz, clays, and pigments

B + 3---------------------------------- 4% Chrysotile 30% Calcite aggregate 66% Vinyl binder

3---------------------------------- 3% Chrysotile 97% Vinyl, acid-soluble binder, and pigments

-------------------------------- 3% Chrysotile 22% Vinyl binder 68% Acid-soluble binder 7% Quartz, mica, pigments, and mineral fillers

C + 1, 3---------------------------------- 5% Chrysotile Tra Actinolite 45% Vermiculite 50% Acid-soluble binder

3---------------------------------- 4% Chrysotile Tra Tremolite 31% Vermiculite 65% Acid-soluble binder

1, 3, 4, 5--------------------------------- 7% Chrysotile Tra Actinolite 30% Vermiculite and phlogopite 63% Acid-soluble binder

D

– ---------------------------------- 20% Calcite aggregate 80% Vinyl binder

----------------------------------100% Vinyl, clay, and pigments

1, 2, 4--------------------------------- 52% Organic (vinyl) binder 48% Acid-soluble and insoluble mineral matrix, and pigments

Numerical Code for Analytical Technique: 1 = Gravimetric reduction by acid dissolution 2 = Gravimetric reduction by ashing 3 = Point counting

4 = Qualitative X-ray diffraction (XRD)5 = Quantitative XRD6 = Qualitative transmission electron microscopy (TEM)Tra = Trace

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Lot B: This material consists of a self-adhesive floor tile approximately 1/16 inch (1.6millimeters) thick. The upper surface is distinguished by a textured faux stoneor marble pattern with shades of yellow, beige, brown, and rose. The tintedportion of the tile constitutes approximately one-third of the tile’s thickness. Theremaining two-thirds of the tile is off-white in color. Granular minerals such asquartz and calcite are clearly visible in the tile’s broken edges. The vinyl matrixis relatively soft. This tile is more flexible than older brittle asphaltic floor tiles.Fibrous material is not readily apparent in observation of broken edges. A thinlayer of tacky adhesive is present on the bottom surface of the tile. Theadhesive does not appear to contain fibrous components.

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Polarized Light Microscopy (PLM)

Several subsamples were randomly extracted from the repository container of each

positive test sample lot for detailed PLM analysis prior to gravimetric sample reduction.

For each asbestos component encountered in each positive lot, the following optical

properties were determined: morphology, aspect ratio, color, pleochroism, refractive

indices (RIs), birefringence, central-stop dispersion staining colors, extinction type and

angle, and sign of elongation. These properties are summarized in Table 2.

Table 2. Optical Properties of Asbestos in Test Sample Lots

Optical Property

Lot A Lot B Lot C

Chrysotile Chrysotile Chrysotile Actinolite

MorphologyWavy, curvilinear, with

“knees”Fine, wavy, with

splayed endsWavy, curvilinear, with

“knees”Straight,

needle-like

Aspect Ratio

Color

Pleochroism

RefractiveIndices

Birefringence

Central-StopDispersion

Staining Colors

Extinction

Sign ofElongation

Brief material descriptions acquired during the PLM examination are as follows:

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Lot C: Slide mounts of this material are dominated by gypsum-based matrix, amicaceous mineral, and chrysotile asbestos. The matrix, which coats all othercomponents and makes their identification difficult, is moderately effervescentin room-temperature HCl. The micaceous mineral displays a variety of colorsranging from dark brown to green, but most commonly golden brown. Thechrysotile exhibits positive sign of elongation and parallel extinction. In 1.550 RIliquid, the chrysotile displays typical blue to purple dispersion staining colors.Chrysotile is visually estimated to constitute 3% of the material. A trace amountof an amphibole mineral occurs as small needle-like fibers and bundles. Thismaterial is identified as actinolite and is inhomogeneously distributedthroughout the material.

Lot D: Slide mounts of this material reveal a homogeneous mixture dominated by fine-grained, equant-shaped mineral fragments with moderate birefringence. With the addition of gentle heat from the microscope light source, the vinyl matrixdissolves in the 1.550 RI liquid in which it is mounted. Translucent occlusionscan be observed in the oil mount. These occlusions appear to be consistentwith the stereoscopic observation of a polished top surface. No fibrous materialis visible.

Gravimetric Sample Reduction

Representative subsamples from all four lots were subjected to gravimetric sample

reduction, by way of acid dissolution and/or low-temperature ashing, to confirm

qualitative results for organic and acid-soluble components and to refine

semiquantitative results derived from stereomicroscopy and PLM examinations. The

results of these test sample reductions are described below. Unless otherwise noted,

losses are quoted as a percentage of the sample’s starting weight.

Test sample compositions rendered low-temperature ashing useful on Lots A, B,

and D. Results of this sample reduction are described below. For the reduction, a

minimum of eight preweighed subsamples were ashed at approximately 480°C for 15

hours. Each residue was allowed to return to ambient temperature (stabilize) before

reweighing.

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Lot A: The average weight loss was 26.9%, attributable to the combustion of celluloseand dehydration of mineral matrix.

Lot B: The average weight loss was 21.6%, attributable to the combustion of organic(vinyl) binders.

Lot D: The average weight loss was 51.6%, attributable to the combustion of organic(vinyl) binders.

Test sample compositions rendered acid dissolution reduction useful on all four

lots. For the reduction, a minimum of eight preweighed subsamples were treated with

3N HCl. For Lots A, B, and D, the residue after ashing was used. After the acid

treatment, each residue was thoroughly washed and allowed to dry (stabilize) before

reweighing. The approximate loss of the soluble binder/matrix was determined for each

subsample, with results as follows:

Lot A: The average weight loss was 77.3% (equivalent to 56.5% of the whole testsample), attributable to the dissolution of calcite and gypsum. The residue isdominated by perlite, fine-grained minerals, quartz, and pigments. Chrysotile isestimated to constitute approximately 15-20% of the residue, for a whole-sample equivalent of 2.5-3.3%.

Lot B: The average weight loss was 86.2% (equivalent to 67.6% of the whole test sample), attributable to the dissolution of calcite. The residue is dominated byfine-grained matrix and pigments. Chrysotile is estimated to constituteapproximately 20-30% of the residue, for a whole-sample equivalent of 2.2-3.2%.

Lot C: The average weight loss was 62.7%, attributable to the dissolution of gypsumand bassanite (both calcium sulfate minerals). The residue is dominated bymica and fine-grained matrix. Chrysotile is estimated to constituteapproximately 10-20% of the residue, for a whole-sample equivalent of 3.7-7.5%.

Lot D: The average weight loss was 97.9% (equivalent to 47.4% of the whole test sample), attributable to the dissolution of calcite. The residue is dominated byfine-grained matrix, pigments, quartz, and mica. No asbestos is visible in theresidue.

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X-Ray Diffraction (XRD)

Treated (by ashing and/or acid dissolution; see the previous section) and untreated

subsamples of all four lots were extracted for XRD analysis. All treated and untreated

subsamples were ground with a mortar and pestle, and powder mounts were prepared.

Scans were run from 5°22 or 8°22 to 62°22 at a scan rate of either 0.01°22 per second

or 0.02°22 per 0.6 second. Differences in scan rates are attributable to differences in

XRD instrumentation and have no impact on RTI’s interpretation of the diffractograms.

Following are the results of the XRD analyses:

Lot D: No asbestiform phases were detected in scans of the untreated and treatedmaterial. Confirmed nonasbestiform phases included calcite (untreated only),quartz (treated only), muscovite mica (treated only), rutile [titanium dioxide](treated only), and microcline (treated only).

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Quantitation of Asbestos in Positive Test Sample Lots

The concentration of asbestos in each of the three positive lots was determined by

point counting, quantitative XRD, and gravimetric sample reduction, each where

applicable. An abundance of fine-grained pigments in residues from gravimetric

reduction of the Lot B floor tile material adhered to

Means and standard deviations were calculated for the point counts, XRD

quantitation values, and gravimetric residue estimates for the asbestos type(s) in each

sample and used to develop two-sided tolerance limits (acceptance ranges). Limits

were chosen so as to have 99% confidence that 95% of the reported values would be

deemed acceptable. The final acceptance range for a sample used the lowest value

among the minimum values and the highest value among the maximum values for all

techniques used. Semiquantitative results and acceptance ranges are shown in Table 3.

The number of replicate analyses used in each calculation is also indicated.

Section V - Summary of the Test RoundOf the 239 laboratories enrolled, 230 submitted results of analyses for the test

round, for a response rate of . This rate was slightly higher than the 94% average

participation rate for the 55 previous test rounds conducted under the proficiency rating

format. A laboratory not returning results was deemed “failing” (F) for the test round

unless it had notified AIHA beforehand of its intent not to participate in the test round

and provided a qualifying reason for the nonparticipation. One laboratory provided such

notification to AIHA. Of the 230 participating laboratories, 227 (99%) submitted analysis

via RTI’s Web site for the program.

The eight laboratories that did not submit results by the deadline date or have an

AIHA-approved exemption were contacted by RTI to confirm their intent not to

participate. One laboratory indicated that it would submit late results but did not. One

laboratory wishes to remain enrolled but will not submit results before Test Round 80.

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Table 3. Semiquantitation Means and Ranges, and Acceptance Ranges

SemiquantitationMethod

Lot A Lot B Lot C

Chrysotile Chrysotile Chrysotile

Point CountMean (%)Range (%)

Replicates (#)

2.31.4 to 3.0

7not applied

5.13.5 to 6.3

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SemiquantitativeXRD

Mean (%)Range (%)

Replicates (#)

2.72.0 to 3.9

8

3.63.2 to 4.3

10

9.06.8 to 9.8

9

GravimetryMean (%)Range (%)

Replicates (#)not applied

2.81.6 to 3.7

20not applied

99/95 AcceptanceRange (%)

Trace to 8%,inclusive

Trace to 8%,inclusive

Trace to 15%,inclusive

One laboratory returned its test samples without explanation. The other five laboratories

did not reply to RTI’s voice messages or e-mails.

Tables 4 and 5 illustrate the total test round effort, as generated by the results of

analyses submitted by participating laboratories. Table 4 shows the penalty point totals

incurred by passing (P) and failing (F) laboratories based on the grading criteria

described on page 13 of this report. A laboratory was rated F for incurring 100 or more

penalty points or for not participating. The total numbers of P and F laboratories are also

indicated. For the test round, 203 laboratories (85% of the total enrolled, 88% of the

total participating) were rated P. Of the 35 F laboratories for the test round, 26 were

rated so for incurring classification errors, with or without other error types, and 1

resulted from a combination of asbestos identification errors and/or semiquantitation

errors, without classification errors. The eight laboratories that did not submit results by

the deadline or have an AIHA-approved exemption received F ratings for

nonparticipation. This was the first test round of participation for 3 of the 35 F

laboratories.

Table 5 lists totals of false negatives, false positives, asbestos identification errors,

and semiquantitation errors made by laboratories, by sample lot. False negatives and

false positives are denoted by “FN” and “FP,” respectively; asbestos identification and

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Table 4. Distribution of Penalty Point Totals Incurred

Total PenaltyPoints Incurred

Number ofLaboratories

Passing Laboratories 0 159

1 - 24 30

25 - 49 9

50 - 74 2

75 - 99 3

Total Passing Laboratories 203

Failing Laboratories 100 - 124 21

125 - 149 0

150 - 199 2

200 or more 4

Nonparticipants 8

Total Failing Laboratories 35

Excused Laboratories 1

Suspended Laboratories 0

Table 5. Sample Classification, Asbestos Identification,and Semiquantitation Errors, by Test Sample Lot

SampleLot

AsbestosContent

Number of Errors, by Type

FN FP ID SQ

A + 1 ---- 15 34

B + 21 ---- 2 2

C + 2 ---- 3 10

D – ---- 6 ---- ----

Total Errors Incurred 24 6 20 46

FN = False Negative FP = False Positive ID = Asbestos Identification Error SQ = Semiquantitation Error

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semiquantitation errors are denoted by “ID” and “SQ,” respectively. Totals of all error

types incurred for the test round are shown at the bottom of the table.

The following evaluation criteria were used to assign these classification,

identification, and semiquantitation errors:

Proficiency Grading Criteria Penalty Points

Failing to submit analysis results Automatic NP

Failing to report asbestos in a positive sample (FN) 100

Reporting 1% or greater asbestos in a blank sample (FP) 100

Failing to report the correct asbestos type, in a one-type sample (ID) 50Failing to report second asbestos type, in a multi-type sample (ID) 50Failing to report third asbestos type, in a multi-type sample (ID) 25

Reporting 1% or greater incorrect asbestos type (ID) 45/type

Reporting trace asbestos in a blank or trace incorrectasbestos type(s) in a positive sample No penalty

Failing to report trace asbestos when RTI QC confirmsit in all samples 25/type

Failing to report trace asbestos when RTI QC does notconfirm it in all samples No penalty

Per sample, first asbestos semiquantitation outside acceptance range 20Per sample, second asbestos semiquantitation outside acceptance range 10Per sample, third asbestos semiquantitation outside acceptance range 5

Section VI - Individual Laboratory ResultsPlease refer to the computer printout on page 14 for a tabulation of your individual

laboratory results and a comparison of those results with the reference laboratories’

analyses. The total penalty points incurred by your laboratory during this test round and

the status of your laboratory as a result of your performance this test round are listed in

the upper right-hand corner of the form. The number of penalty points per sample is

highlighted in the section entitled “Analysis Results for Laboratory _____.”

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One-page

“computer printout of graded results”

to be inserted here

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A laboratory achieved a program status of proficient (P) if two of its three most

recent test rounds were rated P. A laboratory also achieved a program rating of P if it

had participated in only two test rounds but had been rated P in each. A laboratory was

rated nonproficient (NP) for the program if it was rated F for more than one of the three

most recent test rounds. If a laboratory’s program rating is listed as not applicable (NA),

that laboratory has not participated in the number of test rounds required to establish a

program rating. Through the completion of this test round, 204 laboratories (85% of the

total enrolled) have a P program rating, 25 (11%) have an NP program rating, and 10

(4%) have no program status because they have not completed the requisite number of

test rounds.

Section VII - Analysis Problems and SuggestionsThe following appraisals are provided concerning trends or patterns seen in sample

classification, asbestos identification, and semiquantitation errors for each of the four

test sample lots.

A total of 30 classification errors were incurred, for an overall classification error

rate of 3.3%. This was only slightly higher than the program’s 3.1% historic classification

error rate. Twenty-four false negatives resulted in a false negative error rate of 3.5%;

this was slightly higher than the program’s historic false negative error rate of 3.0%. Six

false positives resulted in a false positive error rate of 2.6%; this was considerably lower

than the program’s historic false positive error rate of 3.3%.

Twenty-one of the 24 false negatives were incurred on Lot B, a vinyl floor tile

containing approximately 3% chrysotile. These false negatives were easily avoidable if

the laboratory had the ability to perform a gravimetric matrix reduction prior to looking

for and quantifying any asbestos present. Ashing and acid dissolution removed

approximately 22% and 68% of the sample’s weight, respectively. Chrysotile was easily

detected in the residue, constituting 20-30% of the remaining material.

The results on Lot B illustrate that laboratories not routinely performing gravimetric

matrix reduction on floor tiles potentially run a high risk for failing to detect asbestos

(when present) and incurring an avoidable false negative. RTI recommends that

laboratories employ a full spectrum of sample treatment processes, such as those

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described in the EPA Test Method for the Determination of Asbestos in Bulk Building

Materials, EPA/600/R-93/116. Performing ashing and acid reduction serves to

concentrate any asbestos present into the residue, where it is more easily detected and

better quantified.

If a laboratory does not have the equipment or capability to perform these sample

reductions, it may be well-advised to submit floor tile samples to another laboratory with

gravimetric reduction and/or transmission electron microscopy (TEM) capability, in order

to confirm or refute the negative PLM results. If a laboratory does this as standard

practice on all floor tiles, it may seek a permanent “floor tile waiver” from AIHA. This

waiver allows the laboratory to choose to either: 1) not submit results on any floor tile

PT sample, or 2) submit results on floor tile PT samples but not have them graded by

RTI.

Six false positives were incurred on Lot D, a sheet linoleum containing no fibrous

components. Five laboratories reported the presence of chrysotile, in amounts ranging

from 2% to 15%. A sixth laboratory reported 10% each of chrysotile and tremolite. That

laboratories would report any asbestos type at all is surprising, as RTI detected no

fibrous material to be present in the material. Three of the six laboratories also incurred

false negatives on Lot B, suggesting the possibility that analysis results for the two

samples were transposed in the process of being reported.

Twenty identification errors were incurred, for an identification error rate of 2.9%.

This was less than one-half the program’s historic error rate of 6.5%.

Fifteen of the 20 identification errors were incurred on Lot A, a textured ceiling

spray containing approximately 3% chrysotile. Nine errors were assigned for reporting

amosite or tremolite but not reporting the chrysotile known to be present; six errors were

incurred for reporting amosite or tremolite in addition to the chrysotile.

The other five identification errors were divided between Lots B and C. Both errors

on Lot B were incurred for reporting tremolite in addition to the chrysotile known to be

present. On Lot C, two errors were assigned for reporting anthophyllite but not reporting

the chrysotile known to be present. The other was incurred for reporting amosite in

addition to the chrysotile. RTI and the two reference laboratories reported the presence

of trace-level amphibole exhibiting inclined extinction.

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The number of semiquantitation errors was low compared to that in recent test

rounds, but not unexpected given the specific nature of the test samples in this test

round. On Lot B, all 34 semiquantitation errors were incurred by laboratories reporting

chrysotile in amounts exceeding the upper limit of RTI’s acceptance range for that

asbestos type. Ten errors were incurred on Lot C, all for reporting asbestos types in

amounts exceeding the upper limits of RTI’s acceptance ranges. Two errors were

incurred on Lot B, also for reporting asbestos types in amounts exceeding the upper

limits of RTI’s acceptance ranges.

Section VIII - Test Method/Analytical Technique SummaryRTI solicited information about the test methods and analytical techniques

employed by the program participants on this test round’s test samples. The cited

methods and techniques are listed in Table 6. RTI then correlated false negative, false

positive, asbestos identification, and asbestos semiquantitation errors to the

method/technique used. Based on the recommendations of its statisticians, RTI

performed two simple statistical analyses – an analysis of variance (ANOVA) and a

mean squared error (MSE) test – of the semiquantitative data on positive sample lots.

The ANOVA determines if there is a statistically significant difference among the

consensus means of the reported values, for each test method/technique. Its use is

appropriate when comparing multiple data sets of widely varying numbers of individual

measurements. If the ANOVA indicates that a significant difference exists among the

results for the methods/techniques used, the MSE test attempts to identify the

method/technique combination yielding the best semiquantitative results by comparing

the accuracy of reported values to the true value for the test sample and also factoring

in the precision of the reported values. If a statistically significant difference is found, the

results of the evaluation of the data are included in this report.

It appears that the relatively small number of errors of any type make presentation

of these comparative data on a per-sample basis to be of limited value and practicality

to participating laboratories. Therefore, and effective with Test Round A71-207, RTI has

elected to present the error type/frequency data for each test method used in

cumulative terms for all samples in the test round. These data are provided in Table 7.

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Table 6. Cited Test Methods and Techniques

Legend Method Qualitative Technique Quantitative Technique

1 EPA INT / PTCTEPA Interim Method(1982)

Polarized Light MicroscopyPoint Counting

2 EPA INT / CVE Equivalent Visual Estimation

3 EPA INT / GRAV Gravimetric Reduction

4 EPA INT / XRD X-Ray Diffraction Standards Comparison

5 EPA REV / PTCT

EPA Revised Method(1993)

Polarized Light MicroscopyPoint Counting

6 EPA REV / CVE Calibrated Visual Estimation

7 EPA REV / GRAV Gravimetric Reduction

8 EPA REV / XRD X-Ray Diffraction Standards Comparison

9 EPA REV / EM Analytical Electron Microscopy Visual Estimation

10 NYS / PTCT New York State Method198.1

Polarized Light Microscopy Point Counting

11 NYS / TEM New York State Method198.4

Transmission ElectronMicroscopy

Visual Estimation

12 NIOSH / VE NIOSH Method 9002 Polarized Light Microscopy Visual Estimation

13 NIOSH / XRD NIOSH Method 9002 X-Ray Diffraction Standards Comparison

14 OSHA / VE OSHA Method D-191 Polarized Light Microscopy Visual Estimation

15 OTHER Method Not SpecifiedAbove

The number in each row of the column with the heading “Avg. Error Points Per

Analysis” was calculated by summing the number of false negatives and false positives

times 100, the number of ID errors times 50, and the number of semiquantitation errors

times 20 and dividing that sum by the total number of analyses performed by that

method. This weighting reflects the relative penalty point values for these error types in

the actual grading criteria for the program.

Three methods that use PLM for qualitative analysis and visual estimation or

calibrated visual estimation for quantitative analysis – the 1982 EPA Interim Method,

1993 EPA Revised Method, and NIOSH Method 9002 – were, as in Test Rounds

A71-207 through A77-408, the ones most often cited by laboratories this round. In five

of those six previous test rounds, the lowest rates of false negatives, false positives,

and asbestos identification and semiquantitation errors, and the lowest average penalty

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Table 7. Analysis of Errors and Asbestos Semiquantitation,by Test Method/Technique Used

Test Round A78-109

# Method/TechniqueCited by Laboratory

Total No.of

Analyses FN

FNErrorRate(%) FP

FPErrorRate(%) ID

IDErrorRate(%) SQ

SQErrorRate(%)

Avg.Error

Points/Analysis

1 EPA INT / PTCT

2 EPA INT / EVE

3 EPA INT / GRAV

5 EPA REV / PTCT

6 EPA REV / CVE

7 EPA REV / GRAV

10 NYS / PTCT

12 NIOSH / VE

14 OSHA / VE

15 OTHER

points per analysis in each round, were achieved by laboratories using the 1993 EPA

Revised Method with calibrated visual estimation (method 6). In Test Round A73-407,

the NIOSH method with semiquantitation by visual estimation (method 12) fared the

best of the three methods most commonly used. This test round, method 6 again

yielded the lowest average penalty points per analysis.

A comparatively very small number of analyses were performed by laboratories

using either EPA method, with point counting or gravimetric reduction for quantitation

(method 1, 3, 5, or 7); the New York State PLM method, with point counting for

quantitation (method 10); the OSHA method, with visual estimation for quantitation

(method 14); and other methods not specified in Table 7. The latter are for the most part

in-house test methods developed by laboratories outside of the United States. Rates of

false negatives and false positives incurred by laboratories using these methods were

20

generally nonexistent or very low, but these method/technique combinations produced

mixed results on asbestos identification and semiquantitation errors and on penalty

points per laboratory.

The ANOVA revealed that there was no statistically significant difference in

semiquantitative results among methods for any of the three sample lots. MSE analysis

of Lot A data suggests that the most accurate and precise semiquantitation overall was

reported by laboratories using method 1, and for the three most commonly cited

methods, by laboratories using method 6. MSE analysis of Lot B data suggests that the

most accurate and precise semiquantitation overall was reported by laboratories using

method 3, and for the three most commonly cited methods, again by laboratories using

method 6. MSE analysis of Lot C data suggests that the most accurate and precise

semiquantitation overall was reported by laboratories using method 5, and for the three

most commonly cited methods, by laboratories using method 6.

Section IX - Participant FeedbackRTI welcomes comments and constructive criticism from program participants on

any aspect of this test round or RTI’s overall administration of the program. Please

direct such to Program Manager Bruce Harvey at (919) 541-6573 or bwh@rti.org.

Section X - Schedule for Test Round A79-209The following dates relating to Test Round A79-209 of the Bulk Asbestos

Proficiency Analytical Testing Program have been agreed upon by AIHA and RTI:

May 15, 2009 RTI distribution of test sample packets to laboratories.

June 15, 2009 Deadline for RTI receipt of results of laboratory analyses.

July 15, 2009 Distribution/posting of “Final Report to Laboratories - TestRound A79-209” to participants.

END OF REPORT