CERTIFICATE OF ANALYSIS

COC:  305281 Job Name: Task 2 ‐ Analysis of Demonstration Samples Date Submitted: Client: US Food & Drug Administration Job Location: Talc (x000756) A TK4428 FDA Date Analyzed: 

Address: Office of Cosmetics & Colors Job Number: Not Provided Report Date: 

4300 River Road PO Number: HHSF223201810337P Date Sampled: 

College Park, Maryland 20740 Person Submitting: 

Attn: John Gasper Revised: 

ISO 22262‐2 ASTM D5756 ISO 22262‐2 ASTM D5756

305281‐3 D‐18 0.00000057% 0.00000090% 0.00000229% 0.00000359% ND ND ND <0.00000229% <0.00000359% 305281‐3A D‐18 0.00000059% 0.00000093% 0.00000236% 0.00000371% ND 0.00412% 0.00647% 0.00412% 0.00647% 305281‐3B D‐18 0.00000056% 0.00000088% 0.00000225% 0.00000353% ND ND ND <0.00000225% <0.00000353% 

305281‐4 D‐30 0.00000684% 0.00001074% 0.00002734% 0.00004295% ND 9.86344% 15.49345% 9.86% 15.5% 305281‐4A D‐30 0.00000330% 0.00000519% 0.00001322% 0.00002076% ND 1.35083% 1.82317% 1.35% 1.82% 

305281‐4B D‐30 0.00000453% 0.00000712% 0.00001813% 0.00002848% ND 2.75310% 4.32456% 2.75% 4.32% 305281‐5 D‐31 0.00000103% 0.00000161% 0.00000410% 0.00000644% 0.00183% 0.15435% 0.24245% 0.156% 0.244% 1305281‐5A D‐31 0.00000146% 0.00000229% 0.00000583% 0.00000916% 0.00035% 0.17068% 0.26810% 0.171% 0.268% 1305281‐5B D‐31 0.00000075% 0.00000117% 0.00000298% 0.00000468% 0.00012% 0.13368% 0.20999% 0.134% 0.210% 1305281‐6 D‐96 0.00000084% 0.00000132% 0.00000335% 0.00000526% ND ND ND <0.00000335% <0.00000526% 1

305281‐6A D‐96 0.00000047% 0.00000074% 0.00000190% 0.00000298% ND ND ND <0.00000190% <0.00000298% 1305281‐6B D‐96 0.00000073% 0.00000114% 0.00000290% 0.00000456% ND ND ND <0.00000290% <0.00000456% 1LOD = Limit of Detection LOQ = Limit of Quantification ND = Not Detected PLM = Polarized Light Microscopy TEM

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

TEM by Modified NY ELAP 198.4/ASTM D5756/ISO 22262‐2

Analyst(s): PLM

TEM , Andreas Saldivar

(b) (6)(b) (6)

Technical Director: AndAll results are to be considered preliminaby the Technical Director or Deputy

SUMMARY OF ASBESTOS IN TALC ANALYSIS

TEM LOD Range TEM LOQ Range

AMA 

Sample ID

Client 

Sample ID

% Chysotile by 

TEM

% Tremolite by TEM % Total by TEM

% O

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 Laborathe exclusive use of the client to whom it is addressed and upon the condition that it is not to be used, in whole or in part, in any advertising or publicity matter not shall it be reproduced, except in full, without prior written autho

collection protocols are based upon the information provided by the persons submitting them and, unless collected by personnel of these Laboratories, we expressly disclaim any knowledge and liability for the accuracy and compmaterial will be discarded in accordance with the appropriate regulatory guidelines, unless otherwise requested by the client.  NVLAP accreditation applies only to polarized light microscopy of bulk samples and transmission electmust 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 Analytical Services, Inc.

 4475 Forbes Boulevard • Lanham, MD 20706 • (301) 459‐2640/(800) 346‐0961 • www.amalab.com   
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305281-4, 4A, 4B, Client Sample D30

PLM

All three aliquots of sample D30 were analyzed by on January 31, 2019. Tremolite was observed 

on aliquot 4a but no points were counted. No tremolite was detected on 4 and 4b. No other asbestos was detected.

305281-4 NAD

305281-4A <0.13% Tremolite detected

305281-4B NAD

305281-4A Tremolite 100x

TEM

Sample 4 was analyzed by Andreas Saldivar on January 11, 2019. Samples 4A and 4B were analyzed by 

 on January 25, 2019 and January 31, 2019 respectively. Talc is the main constituent in all three aliquots. The 

talc is primarily in plate form but there are also some talc fibers and ribbons. Tremolite was detected on all three 

aliquots. At least 100 tremolite particles were documented for each aliquot. The length and width of each particle was 

recorded and the mass was calculated using both the ASTM D5756 and ISO 22262-2 methods. The percentage of 

tremolite was calculated using the mass from both calculations and the range was reported. 

305281-4 9.86% to 15.5%

305281-4a 1.35% to 1.82%

305281-4b 2.75% to 4.32%

The range of tremolite in aliquot 4 is substantially higher than 4a and 4b. One large particle, #24, accounts for 85% of the 

total mass of tremolite counted in aliquot 4. When the mass of that particle is removed from the total the range of 

tremolite is 1.54% - 2.41%. The dramatic effect of this one particle on the total percent is a result of the dilution factors 

from preparation. The tremolite particles varied in morphology from small blocks to very long, high length to width 

aspect ratio fibers. The length to width aspect ratio of particles counted ranged from 1.27 to 113.9. The mean aspect 

ratio is 11.5. The chemistry of the tremolite observed consisted of O, Mg, Si, and Ca. A few particles had small amounts 

of Al and Fe. One chrysotile fiber was counted on sample 305281-4a.

The following chart is a plot aspect ratio vs length for all the particles counted over all three aliquots.

(b) (6) (b) (6) (b) (6)
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Below are pictures, diffraction patterns, and chemistry from some of the counted particles. The unidentified peaks in 

chemistry spectra are copper, zinc, and carbon. Those peaks are from the TEM specimen holder and specimen grid.

305281-4 Particle 2 8.9 x 0.35 microns Tremolite

 
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Element

 Line

Weight % Weight %

 Error

 O K 51.41 ± 2.37

 Mg K 18.09 ± 0.54

 Al K 1.98 ± 0.29

 Si K 25.57 ± 0.35

 Si L --- ---

 Ca K 2.96 ± 0.19

 Ca L --- ---

Total 100.00
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305281-4 Particle 3 1.6 x 0.2 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 53.11 ± 1.38

 Mg K 16.92 ± 0.30

 Si K 27.08 ± 0.30

 Si L --- ---

 Ca K 2.89 ± 0.09

 Ca L --- ---

Total 100.00
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305281-4 Particle 4 3.0 x 1.2 microns Tremolite

 

Element

 Line

Weight % Weight %

 Error

 O K 48.04 ± 1.69

 Mg K 17.67 ± 0.35

 Si K 30.30 ± 0.38

 Si L --- ---

 Ca K 3.99 ± 0.13

 Ca L --- ---

Total 100.00
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305281-4 Particle 5 2.7 x 1.3 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 50.90 ± 1.56

 Mg K 16.75 ± 0.34

 Si K 28.70 ± 0.35

 Si L --- ---

 Ca K 3.65 ± 0.12

 Ca L --- ---

Total 100.00
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305281-4 Particle 6 1.2 x 0.8 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 49.72 ± 1.38

 Mg K 17.25 ± 0.29

 Si K 29.30 ± 0.30

 Si L --- ---

 Ca K 3.74 ± 0.10

 Ca L --- ---

Total 100.00
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305281-4 Particle 7 2.3 x .8 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 49.62 ± 1.60

 Mg K 17.26 ± 0.35

 Si K 29.41 ± 0.37

 Si L --- ---

 Ca K 3.71 ± 0.12

 Ca L --- ---

Total 100.00
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305281-4 Particle 8 5.6 x 0.18 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 55.70 ± 2.05

 Mg K 16.34 ± 0.44

 Si K 25.17 ± 0.42

 Si L --- ---

 Ca K 2.79 ± 0.13

 Ca L --- ---

Total 100.00
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305281-4 Particle 9 5.8 x 1.3 microns Tremolite (#9 is the large particle. Particle 10 is also pictured to the left of 9)

Element

 Line

Weight % Weight %

 Error

 O K 50.52 ± 1.60

 Mg K 18.00 ± 0.35

 Si K 27.86 ± 0.35

 Si L --- ---

 Ca K 3.63 ± 0.12

 Ca L --- ---

Total 100.00
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305281-4 Particle 11 20.5 x 0.18 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 54.02 ± 3.07

 Mg K 14.93 ± 0.54

 Si K 27.96 ± 0.56

 Si L --- ---

 Ca K 3.09 ± 0.18

 Ca L --- ---

Total 100.00
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305281-4 Particle 12 4.5 x 1.7 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 48.73 ± 1.26

 Mg K 17.21 ± 0.28

 Si K 29.82 ± 0.30

 Si L --- ---

 Ca K 4.24 ± 0.10

 Ca L --- ---

Total 100.00
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305281-4 Particle 13 & 14 4.4 x 1.3 microns 15.6 x 0.8 Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 52.28 ± 1.64

 Mg K 17.40 ± 0.35

 Si K 27.41 ± 0.36

 Si L --- ---

 Ca K 2.92 ± 0.11

 Ca L --- ---

Total 100.00
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305281-4 Particle 15 2.7 x 0.26 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 59.21 ± 2.63

 Mg K 17.88 ± 0.68

 Si K 19.08 ± 0.52

 Si L --- ---

 Ca K 3.84 ± 0.14

 Ca L --- ---

Total 100.00
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305281-4 Particle 51 4.8 x 0.2 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 52.86 ± 2.32

 Mg K 17.64 ± 0.46

 Si K 26.86 ± 0.48

 Si L --- ---

 Ca K 2.64 ± 0.13

 Ca L --- ---

Total 100.00
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305281-5, 5A, 5B, Client Sample D31

PLM

All three aliquots of sample D31 were analyzed by on January 31, 2019. Tremolite was observed 

on all three aliquots but no points were counted. No other asbestos was detected. The results were calculated using the 

equations detailed in the calculations section. 

305281-5 <0.18% Tremolite detected

305281-5A <0.18% Tremolite detected

305281-5B <0.18% Tremolite detected

305281-5 Tremolite 100x

305281-5A Tremolite 100x

(b) (6)
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305281-5B Tremolite 100x

TEM

Samples 5, 5A and 5B were analyzed by on January 15-17, 2019. Talc is the main constituent in all 

three aliquots. The talc is primarily in plate form but there are also some talc fibers and ribbons. Tremolite and chrysotile

was detected on all three aliquots. 20 grid openings were analyzed on all three aliquots. Sample 5 had 43 tremolite and 

7 chrysotile particles counted. Sample 5A had 43 tremolite and 5 chrysotile particles. Sample 5B had 55 Tremolite and 9 

chrysotile particles. The length and width of each particle was recorded. The mass of the tremolite was calculated using 

both the ASTM D5756 and ISO 22262-2 methods. The mass of the chrysotile was calculated using the ASTM D5756 

method. 

305281-5 0.156% to 0.244%

305281-5A 0.171% to 0.268%

305281-5B 0.134% to 0.210%

The tremolite particles varied in morphology from small blocks to very long, high length to width aspect ratio fibers. The 

length to width aspect ratio of particles counted ranged from 1.40 to 58.33. The mean aspect ratio is 11.0. The chemistry 

of the tremolite observed consisted of O, Mg, Si, and Ca. The chrysotile particles were high length to width aspect ratio 

fibers. The aspect ratio ranged from 6.5 to 280. The mean aspect ratio was 41.8. The chemistry of the chrysotile was O, 

Mg, Si, Fe. 

The following charts are a plot of the aspect ratio vs length for all the particles counted over all three aliquots, for the 

tremolite only, and for the chrysotile only.

(b) (6)
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0.00

50.00

100.00

150.00

200.00

250.00

300.00

0 2 4 6 8 10 12 14 16 18

Aspect Ratio

Length microns

Tremolite and Chrysotile

Tremolite

Chrysotile

0.00

10.00

20.00

30.00

40.00

50.00

60.00

70.00

0 2 4 6 8 10 12 14 16 18

Aspect Ratio

Length microns

Tremolite

Tremolite
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Below are pictures, diffraction patterns, and chemistry from some of the counted particles. The unidentified peaks in 

chemistry spectra are copper, zinc, and carbon. Those peaks are from the TEM specimen holder and specimen grid.

0.00

50.00

100.00

150.00

200.00

250.00

300.00

0 2 4 6 8 10 12 14 16

Aspect Ratio

Length microns

Chrysotile

Chrysotile
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305281-5 Particle 3 8.0 x 0.40 microns Tremolite

 

Element

 Line

Weight % Weight %

 Error

 O K 59.45 ± 1.68

 Mg K 16.67 ± 0.51

 Si K 22.15 ± 0.47

 Si L --- ---

 Ca K 1.73 ± 0.09

 Ca L --- ---

Total 100.00
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305281-5 Particle 4 12.0 x 0.60 microns Tremolite

 

Element

 Line

Weight % Weight %

 Error

 O K 59.77 ± 1.60

 Mg K 17.11 ± 0.51

 Si K 21.58 ± 0.45

 Si L --- ---

 Ca K 1.54 ± 0.09

 Ca L --- ---

Total 100.00
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305281-5 Particle 5 12.0 x 0.60 microns Tremolite

Element

 Line

Weight % Weight %

 Error

 O K 59.22 ± 1.53

 Mg K 17.13 ± 0.47

 Si K 22.06 ± 0.43

 Si L --- ---

 Ca K 1.60 ± 0.09

 Ca L --- ---

Total 100.00
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305281-5 Particle 6 1.70 x 0.25 microns Tremolite

 

Element

 Line

Weight % Weight %

 Error

 O K 58.34 ± 2.26

 Mg K 17.65 ± 0.67

 Si K 22.56 ± 0.63

 Si L --- ---

 Ca K 1.45 ± 0.12

 Ca L --- ---

Total 100.00
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305281-5B Particle 49 1.40 x 0.15 microns Chrysotile

 

Element

 Line

Weight % Weight %

 Error

 O K 55.89 ± 1.44

 Mg K 24.04 ± 0.49

 Si K 20.07 ± 0.42

 Si L --- ---

Total 100.00
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305281-5B Particle 56 2.50 x 0.06 microns Chrysotile

 

Element

 Line

Weight % Weight %

 Error

 O K 60.28 ± 3.44

 Mg K 22.85 ± 1.17

 Si K 16.86 ± 0.96

 Si L --- ---

Total 100.00