AMA Analytical Ser vices, Inc. Focused On Results. CERTIFICATE OF ANALYSIS 

Chain of Cu stody: 625947 Job Name: Assignment DFPG #21-18 Oate Submitted: 3/29/2021 

Client: US Food & Drug Ad min ltratlon Job Location: Batch No. 02232021B (Batch lf28) Date Analyzed: 4/29/2021-4/30/2021 

Address: Office of Cosmetics & Colors Job Number: CLIN 0001 Report Date: 5/20/2021 

4300 River Road PO Number: 75F40119Pl0689 Da te Sampled: Not Provided 

Col ege Paril, MD 20740 Person Submitting: Martha Schwartz 

Attention : John Gasper Revised : 5/21/2021 (Revision #1) 

SUMMARY OF ANALYSIS 

TEMLOD TEM LOQ % Chrysotile by TEM % Tremolite by TEM 

AMA Sample ID Client Sample ID UsingASTM 05756 Using ASTM 05756 UsingASTM 05756 Using ASTM 05756 

Mass Calculation Mass Calculation Mass Calculation Mass Calculation 

625947-lA 02232021-12 0.00000179% 0.00000717% ND ND 

625947-18 02232021-12 0.00000253% 0.00001013% NO ND 

625947-l C 02232021-12 0.00000165% 0.00000661% ND ND 

625947-2A 02232021-13 0.00000246% 0.00000983% ND ND 

625947-28 02232021-13 0.00000251% 0.00001006% NO ND 

625947-2C 02232021-13 0.00000357% 0.00001427% ND ND 

% Total Chrysotile & 

Tremolite by TEM 

UsingASTM 05756 

Mass Calculation 

<0.00001% 

< 0.00001% 

<0.00001% 

<0.00001% 

<0.0000 1% 

<0.00001% 

Asbestos 

by PLM 

ND 

NO 

ND 

ND 

NO 

ND 

% 

Organics 

27.39% 

27.68% 

27.35% 

27.08% 

27.17% 

27.30% 

%Acid 

Soluable 

5.98% 

10.78% 

5.50% 

8.76% 

10.15% 

9.17% 

% 

Other 

66.63% 

61.55% 

67.15% 

64.16% 

62.68% 

63.53% 

Comments 

LOO = Limit of Detection LOQ= Limit of Quantification ND = Not Detected PLM = Polarized light Microscopy TEM = Transmission Electron Microscopy 

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

TEM by Modified NY ELAP 198.4/ASTM 05756 

Analyst(s): PLM b)(6) (b)(6) TEM (b)(6) 

Technical Director: "'-'-"'.,__ {b)(6) ____ ... All results are to be considered preliminary and subject to change unless 

signed by the Technical Director or Deputy 

Thlsre1»rt applltsc>ntv 10th• sa~e, or samples, lf'l\ .. stipted a.,d Is not nett$$lll'lfy indeltfvt of the qualltyorconcl lion of flPpwentlyldentictll or SlmW product·$. Au muwtit protection todl~tl, the public, and these l.abortitor1es, this repo,.1 is Mmlt11d Md acctPted for th• ex.dusfv4 use of the dlent to whom 

It Is adc:hssed and upon the oondlUon that It Is not to be used, In whole or In part, In anyadverti:sirw or ptbUc-lty matter not Shal it be reproduced, except In ~t wilhout prior written authorlzaUon from us. Sample types, locations, and collection protocols ,re based upon tte Information provided by the penons 

SWmitting t hem and, unless colec.ted bype,sonne, of these Laboratotes, we e~ressly disdai'.T'I anylcnov.ledgeand bbilityfor the accurac.y and completeness of this information and any analytical data ulcuahed based upon it. Residuals&mple material will be discarded inacoordance with the appropriate 

rculatory au1e1e1n1s, unless «h~e requested by the diem. IIVLAP~ltl tiOn 1ppl1tson1y to l)(lfWed lilffl m:<roscow 0 1 bulk$1~ts and tranvntsSiOn eJeetronmletC$O>PY or A HERA Iii' sarnp,es. ThlS repon must not be used todlllm, and does n« ln'lp)( prO<luet ccnlfleltiOn, appronit o, ~dOl"Nmtnt by 

NY ELAP,AIHA-LAP, NVLAP, NIST,orany agency of the F-ederalGovernment. Al rights reerved. AMAAnalytkalServi::es, Inc. 

4475 Forties Boulevard • Lanham, MD 20706 • (301) 459-2640/(800) 346-0961 • www.amalab.com Page 1 ofl 

Page 3 of67 
Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

625947-lA, 1B, lC/02232021-12 

Page 3 of 23 ~ - AMA Analytical Services, Inc. 

Page 14 of 67 
Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

625947-2A, 2B, 2(/02232021-13 

625947•2ft 

04/30/2021 5# 

1 02232021- .'.J 

F DA a~! 1

f>_\11: EL.AP r/ 

T EM: Bui~ ~e 

625947',:I 

21 04130/20 1:) 1 0223202 • •' 

F DA p1~ 

PL VI: ~t.A r)" 

iEM: Bui~ 

Page 4 of 23 ~ - AMA Analytical Services, Inc. 

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Case Narrative for COC 625947 

Sample Preparation 

Samples were gravimetrically reduced and filtered by(ID(ID on: April 23, 2021 through Apri l 28, 2021. PLM slide 

preparations were made by 5 6 n April 28, 2021. TEM grid preparations were made by(b)(6) on Apri l 

28, 2021. Sample preparation consisted of the following steps: 

1) Label and weigh t wo 8mL glass vials for each sample in the set - one vial for t he PLM preparation and one vial 

for the TEM preparation. 

2) Weigh out 0.1 to 0.8-grams of material and place in the 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 reagent grade hydrochloric acid. 

6) Filter acid reduced material with a pre-weighed disposable filtration apparatus onto a 47mm 0.4μm 

Polycarbonate filter. 

7) Place disposable filtration apparatus with fi lter into drying oven for 3 hours and then record Post-Acid Reduced 

weight. 

8) Make four PLM slide preparations from the PLM residue for each sample in 1.S50 dispersion oil. Make 

addit ional preparations in 1.605, 1.625, 1.680 and 1.700 dispersion oil(s) as necessary for particle identification. 

9) Weigh a portion of the material from the TEM residue and place it into the corresponding pre-weighed l00mL 

jar. 

10) Fill the l00mL jar with deionized water 

11) Sonicate the jar for "'S-minutes. 

12) Filter 0.lmL to 2mL of the solution onto a 47mm 0.22μm MCE fi lter. 

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

TEM grid preparations were examined prior to analysis and were rejected if they meet the following criteria: 

1) Less than 50% of the carbon coating was intact 

2) The grid was too dark due to incomplete dissolution of the fi lter 

3) Heavy particulate loading in excess of 25% 

4) Light particulate loading below 10% 

5) Uneven distribution of part iculate 

Problems Encountered During Preparation & Resolutions: 

No problems were encountered during sample preparation. All gravimetric data was consistent among each group of 

aliquots and all TEM grid preparations were deemed acceptable for analysis. 

PLM Analysis 

Analysis was performed in accordance with NY ELAP 198.6 prot ocols. 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; each slide preparation consisted of two (2) coverslips for a total of eight (8) coverslips. 400-

point count was performed for those samples on which asbestos was observed. If no asbestos was detected on any of 

the slides, the percentage of fibrous components was determined by visual est imation. The result s of this analysis are 

detailed below in the Discussion and Interpretation of Analytical Findings section for each individual sample. 

Point Counting 

If asbestos was observed on the slide preparations, the amount of asbestos was quantified using point count techniques. 

Point counting is form of quantifying PLM samples. One of the oculars of each PLM microscope is etched w ith a 

crosshair. When point counting, whatever is under the crosshair is counted as one point of whatever the material is. 

Four (4) slide preparat ions wit h a total of eight (8) coverslips are prepared for each sample. The microscope mechanical 

stage is used to randomly move the slide. After each movement, whatever is under the crosshair, provided the point is 

not empty, is counted. Fifty (50) non-empty points are counted on each of the eight (8) coverslips for a total of four 

hundred (400) points. The total asbestos points counted are divided by the total points counted to calculate t he 

percentage. 

M. Page S of 23 AMA Analytical Services, Inc. 

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Case Narrative for COC 625947 

Example: 

11 points of asbestos were counted out of the 400 total points 

Slide percentage= (11pts/400pts) * 100% 

Slide percentage= 2.75% 

This number is not t he final asbestos percentage. To calculate the final percentage, this number must be corrected to 

account for the material lost during gravimetric reduction preparation. See the Calculations sect ion below for addit ional 

details. 

TEM Analysis 

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

using JEOL JEM-lOOCX II and JEOL JEM-lOOCX transmission electron microscopes (TEM) equipped w ith Thermo Fisher 

NSS System 7 Energy Dispersive X-Ray Analyzers (EDXA), at magnifications of 19,000x - 20,000x. All TEM scopes are 

equipped w ith a Selective Area Electron Diffraction (SAED) setting that allows the operator to view the diffraction 

pattern of any mineral substance. Twenty (20) grid openings over two (2) grids were examined for each aliquot. 

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 0.22μm MCE filter. 

2) Any amphibole or chrysotile particle(s) observed were not quantified by visual estimation. The length and width 

of the observed particle(s) were measured, and the mass of each amphibole and chrysotile particle was 

calculated using the ASTM 05756 method. 

3) All particles identified as amphibole were included with t he counts/concentrations, regardless of size and aspect 

ratio. 

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

individual sample. 

Calculations 

ASTM D5756 Mass: Gravimetric Reduction Loss Percentages: 

M = rt/4 L * W2 * D * 10-u Organic: ((Wl - W2) * 100)/Wl 

Where: M: Mass Acid Soluble: ((W2 - W3) * 100)/Wl 

L: Length Other*: ((W3/Wl) * 100) - Calculated Asbestos % 

W: Width •other is d efined as the non-asbestos, inorganic, acid insoluble portion of the sample 

D: Density Where: Wl: Weight of sample prior to ashing/acid wash 

W2: Weight of sample after ashing 

W3: Weight of sample after acid treatment 

Asbestos Percent Calculations: 

TEM PLM 

EFA(mm2 ) * 100ml * MA(g) * RW(g) (ASB * W3)/Wl 

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

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

Where: EFA: Effective filter area Where: Wl: Weight of sample prior to ashing/ acid wash 

MA: Mass of asbestos W3: Weight of sample after acid treatment 

RW: Weight of residue ASB: Calculated Point Count Result 

VF: Volume filtered 

IW: Init ial weight of the sample 

AA: Area analyzed 

RJ: Weight of residue placed into the jar 

Note: All reported concentrations were calculated using the gravimetric data from the TEM preparations. 

Page 6 of 23 ~ - AMA Analytical Services, Inc. 

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Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

Limit of Detection and Quantification 

We used the mass of a 0.5 x 0.04-micron tremol ite fiber as the basis for our ca lculations. Limit of detection (LOO) was 

defined as 1 fiber and limit of quantification (LOQ) was defined as 4 fibers. 

Discussion and Interpretation of Analytical Findings: 

625947-lA. 18, lC/Client Sample: 02232021-12 

PLM 

All three aliquots of sample 02232021-12 were analyzed by.._5 ...... 6 _______ _, n Apri l 30, 2021. No asbestos or 

non-asbestos amphibole variants were observed during analysis. The results were calculated using the equations 

detailed in the Calculations section above. 

625947-lA 

625947-1B 

625947-lC 

No Asbestos Detected 

No Asbestos Detected 

No Asbestos Detected 

TEM 

.,_.,..._..,_ (b)(6) ___ _ nalyzed aliquot lA April 29, 2021. Andreas Saldivar analyzed aliquots 1B and lC on April 29, 2021. 

The primary particle observed was talc; barium sulfate part icles were also observed along with some silica spheres and a 

few iron particles and talc fibers. No asbestos or non-asbestos amphibole variants were observed during analysis. The 

resu lts were ca lculated using the equations detailed in the Calculations section above. 

625947-lA No Asbestos Detected 

625947-1B No Asbestos Detected 

625947-lC No Asbestos Detected 

Below are pictures, diffraction patterns, and chemistry from some of the observed particles. The copper and carbon 

peaks in the chemistry spectra are from the TEM grid. The zinc peak in the chemistry spectra is from the TEM specimen 

holder. 

Sample 625947-lA, Talc Particle 

f 

- 6269,.t,7 FDA_OOl.jpg 

'2S!M7-1a 1 "m Tate Particle HV•100l<V 

Cal: o.0054151,1mtpoc Direct Mao: 1900 X 

18:13 412IW2021 AMA Ana,ytical Services, Inc 

==~~1WX6t1, came,a: NANOSPRTS. Exponre: 800 (ffll) X 511<1. rramts, Gall: 1, 61n: 1 

Gamma: 1.00, No snaq,en1n9, ft0rrna1 con1,as 

M Page 7 of23 . AMA Analytical Services, Inc. 

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Case Narrative for COC 625947 

Hexagonal Diffraction Pattern from the Talc Particle pictured above 

- 625947 FDA_002,jpg 

625947-13 100 11/A\ Talc Particle HV=100kV 18:11 4129/2021 Cam L&n: 0.2200 m 

TEM -: Diffraction At.IA Analytical Services, Inc 

Microscopist: -){6) 

Camera: NANOSPRTS, ExPo511re: aoo (ms) x 5 std. frames, Gai: 1, Bin: 1 

Gamma: 1.00. No Sharpening, Normal Contrast 

Chemistry from the Talc Particle pictured above 

Ful scale counts: 677 625947-la(l) 

700 Si 

600 

500 

0 

Mg 

400 

300 Cu 

200 

100 

0 

I 2 3 4 5 

keV 

6 7 8 9 10 

Page 8 of 23 ~ - AMA Analytical Services, Inc. 

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Case Narrative for COC 625947 

Sample 625947-lA, Barium Sulfate Particle 

625147 FDA_009,jpg 

625147-1• 1 μm 

Barium Sulfate Particle HV=100kV 

Cal: 0.003548 μm/pix Dire<:! Mag: 29CIO x 

18:38 4/29/2021 AMA Analytical 5el'llices, Inc 

TEN Mode: lm~iOQ 

Mlcroscopls~(b)(6) carne, a: NANOSPRT5, Exposu.,e: BOO (ms} x 5 1.td. frame$, Gain: 1, Bin: 1 

Gamma: 1.00. No Sharpening, Normal Contrast 

Diffraction Pattern from the Barium Sulfate Particle pictured above 

- 6259'7 FOA_OOB.jpg 

6'159'7-1 • 100 IHAl Barium Sulfate Particle HV=100kV 18:37 412912021 Cam Len: 0.2200 m 

TEM Mode: DiJ'<•c.fion AMA Analytical Services, Inc 

Microscopist:\b)(6), 

Camera: NANOSPRTS, ExPosure: 800 (ms) x s std. frames, Glin: 1. Bin: 1 

Gamma: 1.00, No Sharpenir1g, Normal Conlfast 

Page 9 of 23 ~ - AMA Analytical Services, Inc. 

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Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

Chemistry from Barium Sulfate Particle pictured above 

Full scale counts: 1053 625947-1a(5) 

1000 

s 0 

800 Cu 

600 

400 

200 

0 

1 2 3 4 5 6 7 8 9 10 

keV 

625947-lA, Silica Sphere 

&:25~7 FDA_OH,jpg 

625947-1• 1 pm 

Silica Spher'EI HV,..100kV 

Cal: 0.003548 μmlpix Dire<:t I.lag: 2900 x 

t &:22 4129/2021 AMA Anatyticl!lt $etvices, Inc 

TEM Mode: lm~i9&-, 

Mk;roacoplat,{b)(~} J camtta: NANU~t'Klb, Exposure: aoo (ms} x s std. fl"an'les, Gai1: 1, Bin: t eamn a: 1.00, No :Sharpenmg. Normal contr§t 

M Page l Oof 23 . AMA Analytical Services, Inc 

Page21 of67 
800 

Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

Chemistry from the Silica Sphere pictured above 

Full scale counts: 1068 625947-la(2) 

Si 

1000 

600 

400 

0 

200 

0 

1 2 3 4 5 6 7 8 9 10 

keV 

625947-lA, Iron Particles 

- 0:2$947 FDA_ D11,jpg 

625947-18 

Fe PanicW:S 

Cal: 0.00102.9 μm/pi< 

15:~ 4129/2021 

~~:,_=;;~~if~s-1 

200nm 

HV=100kV 

Direct I.lag: 10000 x AMA AnatyUcal services, Inc 

camt,a: NANOSPRTS, &.posu,e: aoo (ms} x 5 std. r,:.-nes, Gai1: 11 Bin: t 

Gam n a: 1.00, No Sharpening. Normal Contrffl 

M Page 11 of 23 . AMA Analytical Services, Inc 

Page22of67 
Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

Diffraction Pattern from the Iron Particles pictured above 

- 625947 FDA_010.jpg 

625947-1 3 100 i11Al Fe Particle<; HV=1 00kV 

16:434/2912021 C.m Len: 0.2200 m 

TEM Mode: OiHraction Alt1A Analytical Services, Inc 

Nicroscopis«6}(6) 

camera: NANOSPRTS, Expcsure: 800 (ms) x 5 std. fra,11es, Gair1 : 1., Bin: 1 

Garnma: 1.00. No Sha(pel'ling. Normal Contmst 

Chemistry from the Iron Particles pictured above 

Full scale counts: 1081 625947·la(6) 

Fe 

1000 

800 

0 

600 

400 

200 

0 

1 2 3 4 5 6 7 8 9 10 

keV 

M. Page 12 of 23 AMA Analytical Services, Inc. 

Page23of67 
Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

625947-lA, Talc Fiber 

625147 FDA_007,jpg 

625147-1• 800nm Talc Flbor HV=100kV 

Cal: 0.002858 μm/pix Dire<:! Mag: 3&(10 x 

18:31 4/29/2021 AMA Analytical 5el'llices, Inc 

TEN Mode: lm~i!!9 

Microscopist ~ X6j carne, a: NANOSPRT5, Exposu.,e: BOO (ms} x 5 1.td. ,,a.me$, Gain: 1, Bin: 1 

Gamma: 1.00. No Sharpening, Normal Contrast 

Hexagonal Diffraction Pattern from the Talc Fiber pictured above 

- 625917 FDA_006.jpg 

&259"7-1 .a 100 iHAl 

Talc Flbe, HV=100kV 

16:30 4/29/2021 Cam Len: 0.2200 m 

TEM Mode: Oitfrar:ti~n AMA Analytical Services, Inc 

Microscopist{b )(6 j Camera: NANOSPRTS, ExPosure: 800 tms) ,c 5 std. f1cuTies, Gan: 1, Bin: 1 

Garnma: 1.00. No Sha(pel'lir'lg. Nonnal Conttast 

Page 13 of 23 ~ - AMA Analytical Services, Inc. 

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Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

Chemistry from the Talc Fiber pictured above 

Full scale counts: 422 625947-la(J) 

Si 

400 

0 

Mg 

300 

200 

Ou 100 C 

0 

1 2 3 4 5 6 7 8 9 10 

keV 

625947-2A. 2B. 2C/Client Sample: 02232021-13 

PLM 

All three aliquot s of sample 02232021-13 were analyzed by(6)(6) n Apri l 30, 2021. No asbestos or 

non-asbestos amphibole variant s were observed during analysis. The result s were calculated using the equat ions 

detailed in the Calculations section above. 

625947-2A No Asbestos Detected 

625947-2B No Asbestos Detected 

625947-2( No Asbestos Detected 

TEM 

..,__'---'--.,_ (15)(6) ___ _ nalyzed aliquot 2A on April 30, 2021. Andreas Saldivar analyzed aliquots 2B and 2C on April 30, 2021. 

The primary particle observed was talc; barium sulfate particles were also observed along wit h some silica spheres and a 

few iron particles, iron fibers and talc fibers. No asbestos or non-asbestos amphibole variants were observed during 

analysis. The result s were calculated using the equations detailed in the Calculations section above. 

625947-2A No Asbestos Detected 

625947-28 No Asbestos Detected 

625947-2( No Asbestos Detected 

Below are pictures, diffraction patterns, and chemistry from some of the observed particles. The copper and carbon 

peaks in the chemistry spectra are from the TEM grid. The zinc peak in the chemistry spect ra is from the TEM specimen 

holder. 

M. Page 14of 23 AMA Analytical Services, Inc. 

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Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

625947-2A, Talc Particle with Iron 

625147 FDA_G14,jpg 

625147-23 

Talc Patticle with Fo 

Cal: 0.002858 μm/pix 

10:44 4130/2021 

TEN Mode: lm~i"ll 

Mlcroscoplst((b)(6)! carne,a: NANOSPRT5, Exposu.,e: BOO (ms} x 5 1.td. frame$, Gain: 1, Bin: 1 

Gamma: 1.00. No Sharpening, Normal Contrast 

Hexagonal Diffraction Pattern from the Talc Particle pictured above 

800nm 

HV=100kV 

Dire<:! Mag: 3&(10 x 

AMA Analytical 5el'llices, Inc 

- 625947 FDA_0I 3.jpg 

625947-2'1 100 11/A\ Talc Particle with Fe HV=100kV 10:43 4/30/2021 Cam Len: 0.2200 m 

TEM Mode: Diffraction AMA Analytical Services, Inc 

Microscopist~6l Camera: NANOSPRTS. Exp,osure: B00 (ms) x 5 std. frames, Gain: 1. Bin: 1 

Gamma: 1.00. No Shatpening, Noonal Contrast 

Page 15 of 23 ~ - AMA Analytical Services, Inc. 

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Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

Chemistry from the Talc Particle pictured above 

Full scale counts: 1066 625947-2a(2) 

0 

Si 

1000 

800 

Mg 

600 

400 Fe 

Cu 

Fe 

200 

0 

1 2 3 4 5 6 7 8 9 10 

keV 

625947-lA, Barium Sulfate Particle 

0:2$947 FDA_ D10 ,j pg 

625947-2• 600nm Barium Sulfate HV=100kV 

Cal: 0.002144 μm/pi< Direct I.lag: 4$00 x 10:62 4130/2021 AMA AnatyUcal servi ces, Inc 

TEM Mode: lm1ging 

Microscopist lb)(6~ camt,a: NAN6 ~..,t<l5, &.posu,e: aoo (ms} x 5 std. r,:.-nes, Gai1: 11 Bin: t 

Gamn a: 1.00, No Sharpening. Normal Contrffl 

M Page 16 of 23 . AMA Analytical Services, Inc 

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Case Narrative for COC 625947 

Hexagonal Diffraction Pattern from the Barium Sulfate Particle pictured above 

- 625947 FDA_017.jpg 

625947-23 100 11iAl 

Barium Sulfate HV=100kV 

10:51 4130/2021 C.m Len: 0.2200 m 

TEM Mode: OiHraction AMA Analytical Services, Inc 

Microscopist: 

camera: NANOSPRTS, ExPosure: aoo (ms) , 5 std. frames, Gair.: 1, Bin: 1 

Gamma: 1.00, No Sharpel'lil'lg, Normal Contmst 

Chemistry from the Barium Sulfate pictured above 

Full scale counts: 942 625947·2a( 4) 

1000 

0 s 

Cu 

800 

600 

Ba 

400 

200 

0 

1 2 3 4 5 8 9 

keV 

6 7 

M. Page 17of 23 AMA Analytical Services, Inc. 

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Case Narrative for COC 625947 

625947-lA, Silica Sphere 

625947 FDA_016,jpg 

625947-2• 400nm Sili~ Sph8te HV=100kV 

Cal: 0.00142.9 μm/pi• Dire<:t Mag: 7200 x 10:47 4/30/2021 AMA Analytical services, Inc 

TEM Mode: lm~i!!JI 

Mlcroscoplst~ K~ camt,a: NANOSPRT5, Exposu,e: 800 (ms) x 5 std. frames, Gai1: 1, Bin: t 

Gam11a: 1.00, No Sharpening. Normal Contrast 

Chemistry from the Silica Sphere pictured above 

Full scale counts: 1189 625947-2a(3) 

1200 Si 

1000 

800 

600 

400 

0 

200 Cu 

0 

1 2 3 4 5 

keV 

6 7 8 9 10 

M. Page 18of23 AMA Analytical Services, Inc. 

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Re: FDA Office of Cosmetics & Colors 

Case Narrative for COC 625947 

625947-2A, Iron Particles 

625147 FDA_t20,jpg 

625147-23 

FePattickls 

Cal: 0.001774 μm/pix 

10:49 4130/2021 

TEN Mode: 111\~ing 

Mlcroscoplst~D)(6! carne, a: NANOSPRT5, Exposu.,e: BOO (ms} x 5 1.td. ,,a.me$, Gain: 1, Bin: 1 

Gamma: 1.00. No Sharpening, Normal Contrast 

Diffraction Pattern from the Iron Particles pictured above 

600nm 

HV=100kV 

Dire<:! Mag: SMID x 

AMA Analytical 5el'llices, Inc 

- 6259'7 FDA_019.jpg 

6259'7-2• 100 11/Al 

Fe Particles HV=100kV 

10:57 4/30/2021 Cam Len: 0.2200 m 

TEM Mode: Diffraction AMA Analytical Servi ces, Inc 

Microscopist: l6)(6! Camera : NANOSPRTS, ExPosure: eoo (ms) x 5 std. frames, Gan: 1, Bin: 1 

Gamma: 1.00, No Sharpenil'lg, Noonal Conlfast 

Page 19 of 23 ~ - AMA Analytical Services, Inc. 

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Case Narrative for COC 625947 

Chemistry from the Iron Particles pictured above 

Full scale counts: 994 625947-2a(5) 

Fe 1000 

800 

600 

0 

400 

Fe 

200 

0 

1 2 3 4 5 6 7 8 9 10 

keV 

625947-lA, Talc Fiber 

o-2$947 FDA_ D22,jpg 

625947-2• 1 pm Talc Fit>e, HV=100kV 

Cal: 0.003548 pm/pix Direct I.lag: 2900 x 

11:oa 4130/2021 AMA AnatyUcal servi ces, Inc 

TEM Mode: lm10ioo 

M1croscop1stj(b)(6J camt,a: NANOSPRTS, Exposu,e: aoo (ms} x 5 std. r,:.-nes, Gai1: 1, Bin: t 

Gam11a : Uk), No Sharpening. Normal Contrffl 

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Case Narrative for COC 625947 

Hexagonal Diffraction Pattern from the Talc Fiber pictured above 

- 625947 FDA_021.jpg 

625947-23 100 11iAl Talc Fiber HV=100kV 

11:02413012021 cam Len: 0.2200 m 

TEM Mode: OiHraction AMA Analytical Services, Inc 

Nicroscopis«6)(6)1 camera: NA..J-o::rPRl~ . ExPoStJre: 800 (ms) x S std. fra,t1es, Gairt: 1, Bin: 1 

Gamma: 1.00, No Sharpel'lir1g. Normal Contmst 

Chemistry from the Talc Fiber pictured above 

Full scale counts: 912 625947·2a(6) 

Si 

800 

0 

Mg 

600 

Cu 

400 

200 

Fe 

0 

1 2 3 4 5 6 7 8 9 10 

keV 

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QC Discussion: 

M icroscope alignment and calibration for both the PLM and TEM scopes, and EDXA unit calibration were performed on 

each day of analysis as specified by method requirements and standard laboratory operating procedures. The analytical 

balance used for gravimetric reduction is verified weekly at three (3) tare levels using three NIST-traceable weights -

10.0-g, 0.1-g, 0.5-g - and on each day of operation using the 0.1-g and 0.5-g weights tared with an 8-mL glass vial. The 

muffle furnace is verified monthly at a temperature of 480°C. All equipment was functioning within normal operating 

parameters 

Matrix blank samples were prepared at rate of 10% or greater alongside the cl ient samples w ith each series of samples 

that were put into the muffle furnace together. The matrix blank samples were prepared using Sigma-Aldrich Ta lc 

Powder 18654 (Cas No. 14807-96-6; EC No. 238-877-9, Lot 82330). Analysis of the matrix blank samples was only 

required if asbestos, or the non-asbestos versions of the regulated minerals, was found on the associated client samples 

unless otherw ise noted. Mat rix blank sample number NB21-288 was not analyzed since no asbestos was observed on 

the associated client samples. 

A talc reference control sample was randomly selected from our library of TEM grid preparations made from SigmaAldrich Talc Powder, <10 micron (Product No. 643604-SOOG; Batch No. 10830AJ) spiked with various levels of Chrysotile 

ranging from 0.4%-10%. One (1) reference control sample, sample number 625547/625947-RBl , was analyzed with this 

set. It was analyzed by (6)(6) on May 7, 2021 and found to be wit hin acceptable limits. 

Filt ration blank samples were prepared alongside the client samples with each use of the filtration apparatus. Analysis 

of these samples was only required on those blanks associated wit h a cl ient sample on which asbestos, or the nonasbestos versions of the regulated minerals, was found unless otherwise noted. Filt ration blank sample numbers DIBlank-01 and DI-Blank-02 were not analyzed since no asbestos was observed on the associated client samples. 

TEM grid preparation (EB) blank samples were prepared with each batch of carbon coated filters. AMA policy is to 

analyze these blank samples whenever asbestos, or the non-asbestos versions of the regulated minerals, is detected on 

an associated client sample or when t he laboratory blank identification number ends in a "O" or "5." Since no asbestos 

was observed on any of the client samples, only EB Blank ID 56645 was analyzed. b 6 analyzed this sample 

on April 30, 2021. No asbestos was detected on t he sample. 

Our laboratory information management system (LIMS) randomly selected samples 625947-2/02232021-13 for 

additional duplicate QC analysis. Separate preparations were made for the PLM and TEM portions of analysis. The 

duplicate QC analysis was performed by(5)(6) on April 30, 2021 for PLM and by D 6 on May 

20, 2021 for TEM. The QC result s were consistent with the original findings. 

No samples in this set were random ly selected for additional replicate QC analysis. 

Attachments: 

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

1) sample Log-In Sheet 

2) Analytical Balance Verificat ion Log 

3) Daily PLM Scope Verification Log 

4) Refractive Index Oil Verification Log 

5) Daily TEM Scope Verification Log(s) 

6) QC Results Summary for 625947 

7) NB (Matrix) Blank Preparation Log 

8) RB (Reference) Sample Bench Sheet(s) 

9) EB (TEM Grid) Blank Preparat ion Log 

10) EB (TEM Grid) Blank Bench Sheet(s) ~~~----- 11) Duplicate & Replicate QC Charts for D 6 r samples analyzed between 1/1/2021 & 4/30/2021 

12) Duplicate & Replicate QC Charts for ==6 6 =====:--- for samples - analyzed between 1/1/2021 & 4/30/2021 

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Case Narrative for COC 625947 

13) Dupl icate & Repl icate QC Charts for Andreas Saldivar for samples analyzed between 1/1/2019 & 4/30/2021 

14) Raw Dat a Sheet s 

a. PLM Gravimetric Reduct ion Bench Sheet 

b. TEM Gravimetric/Filtration Bench Sheet 

c. PLM Analysis 

d. TEM Analysis 

e. Duplicat e QC Analysis 

I certify that al l information contained in this report pertaining to laboratory events, procedures, and protocols is t rue to 

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

personnel. 

(b )(6) 5 20 2021 

b 6 Date 

Laborat ory Director 

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