CERTIFICATE OF ANALYSIS

Chain of Custody: 307491 Job Name: Task 3 ‐ Analysis of Official Samples Date 

Client: US Food & Drug Adminitration Job Location: 2nd Group ‐ 10 Samples Dat

Address: Office of Cosmetics & Colors Job Number: CLIN 1 ‐ Task 3 (10 Samples) R

4300 River Road PO Number: HHSF223201810337P DatCollege Park, MD 20740 Person S

Attention: John Gasper 

TEM LOD  TEM LOQ % Tremolite by TEM % Chrysotile by TEM % Total Tremolite &  Chrysotile by TEM

Using ASTM D5756 Mass 

Calculation

Using ASTM D5756 Mass 

Calculation

Using ASTM D5756 Mass 

Calculation

Using ASTM D5756 Mass 

Calculation

Using ASTM D5756 Mass 

Calculation

307491‐12 D‐52 0 00000105% 0.00000418% 0.109% <0.000008% 0.109% ND 19.0% 17.6% 

307491‐12A D‐52 0.00000131% 0.00000526% 0.674% ND 0.674% ND 19.4% 17.2% 

307491‐12B D‐52 0.00000107% 0.00000427% 0 226% ND 0 226% ND 19.0% 16.5% 

LOD = Limit of Detection LOQ = Limit of Quantification ND = Not Detected PLM = Polarized Light Microscopy TEM = Tra

Analytical Method(s):  PLM by Modified NY ELAP 198.6

TEM by Modified NY ELAP 198.4/ASTM D5756

Analyst(s): PLM

TEM

Technical Director: Andreas 

All results are to be consideredsigned by the Technical Direct

SUMMARY OF ANALYSIS

% Acid  Soluable 

%  Organics AMA Sample ID Client  Sample ID %  Asbestos  by PLM

This report applies only to the sample, or samples, investigated and is not necessarily indicative of the quality or condition of apparently identical or similar products.  As a mutual protection to clients, the public, and these Laboratories, this report is submitted and accepted for ththe condition that it is not to be used, in whole or in part, in any advertising or publicity matter nor shall it be reproduced, except in full, without prior written authorization from us.  Sample types, locations, and collection protocols are based upon the information provided by th

of these Laboratories, we expressly disclaim any knowledge and liability for the accuracy and completeness of this information.  Residual sample material will be discarded in accordance with the appropriate regulatory guidelines, unless otherwise requested by the client.  NVLAP

samples and transmission electron microscopy of AHERA air samples.  This report must not be used to claim, and does not imply product certification, approval, or endorsement by NY ELAP,AIHA, NVLAP, NIST, or any agency of the Federal Government. All rights reserved.  AMA A

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(b) (6)
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Sample Preparation 

Samples were prepared for PLM and TEM bulk analysis by Chon Simpha on May 24, 2019 through May 31, 2019. Sample 

preparation consisted of the following steps:

1) Label and weigh two 8mL glass vials for each sample in the set – one vial for the PLM preparation and one vial 

for the TEM preparation.

2) Weigh out 0.1 to 0.8 grams of material and place in corresponding 8mL glass vial. Record weight.

3) Burn samples at 480° C for at least 12 hours.

4) Record Post-Ash Weight.

5) Treat ashed sample with concentrated hydrochloric acid.

6) Filter acid reduced material onto a pre-weighed 47mm 0.4um PolyCarbonate filter.

7) Place filter into drying oven for 30 minutes and then record Post-Acid Reduced weight. 
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8) Make four PLM slide preparations from the PLM residual ash for each sample in 1.550 dispersion oil. Make 

additional preparations in 1.605, 1.625, 1.680 and 1.700 dispersion oil as necessary for particle identification.

9) Weigh a portion of the residue from the TEM residual ash and place it into the corresponding pre-weighed 

100ml jar.

10) Fill the 100ml jar with deionized water

11) Sonicate the jars for approximate 5-minutes.

12) Filter 0.2ml to 1ml of the solution onto a 47mm 0.22um MCE filter.

13) Dry the filter for 10 minutes then collapse, carbon coat, and place on a 3 TEM grids.

PLM Analysis

Analysis was performed in accordance with NY ELAP 198.6 protocols. The analysis was conducted using an Olympus BH2 polarized light microscope (PLM) equipped with a dispersion staining objective. All four slide preparations for each 

aliquot were examined. 400-point count was performed for those samples on which asbestos or a regulated amphibole 

was observed. If no asbestos was detected on any of the slides, the percentage of fibrous components was determined 

by visual estimation. The results of this analysis are detailed below in the Discussion and Interpretation of Analytical 

Findings section for each individual sample.

TEM Analysis

Analysis was performed in accordance with modified NY ELAP Method 198.4 protocols. The analysis was performed 

using a JEOL JEM-100CX II transmission electron microscope (TEM), equipped with a Thermo Fisher Quest Energy 

Dispersive X-Ray Analyzer (EDXA), at magnifications of 19,000x. Two grids for each aliquot were examined. Twenty (20)

grid openings per sample were examined.

Modifications to the NY ELAP 198.4 Method were:

1) The residue was not placed in alcohol and prepared using the quick drop method. To obtain a more uniform 

preparation, the residue was placed in a jar and filled with 100ml of deionized water. The jar was sonicated, and 

a portion of the solution was filtered onto a 47mm 0.22um MCE filter.

2) The tremolite and chrysotile were not visually estimated. The length and width of the observed particles were 

measured and the mass of each particle was calculated using the ASTM D5756 method. All particles identified as 

tremolite were included with the counts/concentrations, regardless of size and aspect ratio.

The results of this analysis are detailed below in the Discussion and Interpretation of Analytical Findings section for each 

individual sample.

Calculations 

ASTM D5756 Mass

M = π/4 L * W2 * D * 10-12

M = mass

L = length

W = width

D = density

Percent Calculation

EFA(mm2) * 100ml * MA(g) * RW(g)

 VF(ml) * IW(g) * AA(mm2) * RJ(g) 

The calculated value is then multiplied by 100 to convert it to percent.

EFA – Effective filter area

MA – Mass of asbestos

RW – Weight of residue

VF – Volume filtered

IW – Initial weight of the sample


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Talc particle from 307491-12

Diffraction pattern for the talc particle pictured above
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Chemistry from the talc particle pictured above

Mica particle with titanium particles adhered to it from 307491-12
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Diffraction pattern for the mica with titanium particle pictured above

Chemistry for the mica with titanium particle pictured above
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Mica particle from 307491-12

Diffraction pattern for the mica particle pictured above
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Chemistry for the mica particle pictured above

Mica fiber from 307491-12
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Diffraction pattern for the mica fiber picture above

Chemistry for the mica fiber pictured above
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Talc ribbon from 307491-12

Diffraction Pattern from the talc ribbon pictured above
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Chemistry from the talc ribbon pictured above

Talc fiber from 307491-12
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Diffraction pattern from the talc fiber pictured above

Tremolite particle from 307491-12.
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Diffraction pattern from the tremolite particle pictured above

Chemistry from the tremolite particle pictured above
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Tremolite particle from 307491-12

Diffraction pattern from the tremolite particle pictured above
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Zone access diffraction from the tremolite particle pictured above

Chemistry from the tremolite particle pictured above
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Tremolite particle from 307491-12

Diffraction pattern from the tremolite particle pictured above
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Chemistry from the tremolite particle pictured above

Chrysotile fiber from 307491-12
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Diffraction pattern from the chrysotile fiber pictured above

Below are additional photos of the tremolite particles counted from aliquots 12A and 12B
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QC Discussion:

During preparation, one blank control sample and one reference control sample were prepared. These samples were 

prepared alongside the customer samples. The blank sample was prepared using Sigma-Aldrich Talc Powder, <10 

micron. No asbestos was detected on the blank sample. The reference sample was made from the same Sigma-Aldrich 

talc powder spiked with 1% Chrysotile. The reference sample was analyzed and found to be within acceptable limits.

Our LIMS randomly selects samples for additional replicate and duplicate QC. 307491-12, 12A, and 12B/D-52 were not 

selected for any additional QC analysis.

Attachments:

The following items are attached to this case narrative for your reference:

1) Sample Log-In Sheet

2) Daily PLM Scope Calibration Log

3) Refractive Index Oil Calibration Log

4) Daily TEM Scope Calibration Log

5) QC Results Summary

6) Replicate and Duplicate QC Chart for Peerawut Chaikeenee for samples analyzed 1/1/2019 through 6/30/2019.

7) Replicate and Duplicate QC Chart for Michael Greenberg for samples analyzed 1/1/2019 through 7/17/2019.

8) Raw Data Sheets

a. Gravimetric Data

b. Filtration Worksheets

c. PLM Analysis

d. TEM Analysis

e. QC Samples
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I certify that all information contained in this report pertaining to laboratory events, procedures, and protocols is true 

and accurately describes the handling of this project by AMA Analytical Services, Inc. and its personnel.

7/24/2019

Andreas Saldivar Date

Laboratory Director