AMA Analytical Services, Inc. Focused On Results. CERTIFICATE OF ANALYSIS 

Chain of Custody: 308006 Job Name: Task 3 - Analysis of Official Samples Date Submitted: 7/24/2019 

Client : US Food & Drug Adminitration Job Location: 4th Group - 15 Samples Date Analyzed: 8/20/ 2019-9/18/2019 

Address: Office of Cosmetics & Colors Job Number: CUN 1-Task 3 Report Date: 10/3/2019 

4300 River Road PO Number: HHSF223201810337P Date Sampled: Not Provided 

College Park, MD 20740 Person Submitting: Goran Periz 

Attention: John Gasper Revi.sed: 10/11/2019 (Revision #2) 

SUMMARY OF ANALYSIS 

% Total Tremolite & 

TEMLOD TEM LOQ % Tremolite byTEM % Chrysotile by TEM Chrysotile % by TEM AMA Client % %Acid % Asbestos Comments Sample ID Sample ID Using ASTM 05756 Mass Using A5TM D5756 Mass Using ASTM D5756 Mass Using ASTM 05756 Mass Using A5TM D5756 Mass Organics Soluable other 

byPLM Calculation Calculation Calculation Calculation Calculation 

ravimetnc Loss rom Pl rep: 

308006-6 0-58 000000169% 0.00000675% ND ND ND ND 0.3% 6.7% 93.1% Organics ac 0.3"; Add Soluable a 7.1"; 

Other a 92.69' 

Gravimetric Loss from PLM Prep: 

308006-6A D-58 000000133% 0.00001485% ND <0.00001% <0.00001% ND 0.2% 19.5% 80.2% Organics :i 0.2"; Add Solu-able a 8.5"; 

Other • 91.39£ 

Gravlffletnc Loss from PLM Prep: 

308006-6B D-58 000000135% 0.00000540% ND 0.00002% 0.00002% ND 0.2% 11.2% 88.6% Organics =- 0.3"; Add Solu-able a 5.5"; 

Other a 94.2'6 

LOO = Limit of Detection LOO.= 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 HAP 198.4/ASTM 05756 

Analyst(s): PLM 

TEM -. 

Technical Director: Andreas Saldivar 

All results are to be considered preliminary and subject to change unless 

signed by the Technical Director or Deputy 

Tbis report appl.es only to the sample, or samples, investigated and is not necessarily indk atiw of the quality or condition of apparently identical or similar products. As a mutual protection to clients, the public, and these Uboratories, this report is submitted and accepted for the exdt.Wve 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 m;atter nor shall it be reproduced, except in full, without prior written authorization from us. Sample types, Jocations, and collection protocols a.re based upon the information provided by the persons submitting them 

and, ootess collected by personnel of these Laboratories, we expressly disclaim any knowledge and liability for the accuracy and completeness of this information. Residuat sample material will be discarded in acco.-da.nce with the appropriate regulatory guidelines, unless otherwise requested by the dient. NV\AP accreditation 

applies onfy to pota.rized light microscopy of bu1k samples and tran.smissio.nele-ctron microscopy of AHERA air samples. This repon must not be used to claim, and does not imply product certification, approval. or endorsement by NV flAP,AltlA, 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.aroa!ab.com Page 1 of 1 
Record Changes Report 

Client: US Food & Drug Administration 

Client Code: FDA 

Chain of Custody: 308006 

Date Description 

10/11 /2019 308006 6, 6A, 6B/D 58: 1) added initials & dates to all strike throughs and additions to gravimetric bench sheets. 2) revised handwritten TEM 

bench sheet for 6B to break up the single cluster found on Grid B, GO 18 into its 3 component fibers 3) changed the word "fiber" to "structure" on 

p. 4 of Case Narrative under LoQ discussion for 6A & 6B & updated the basis of LoQ calculation for 6B. 4) changed the word "fiber" to 

"structure" in reference to chrysotile on p.4 of Case Narrative under the TEM Discussion and Interpretation of Analytical Findings. 5) Updated 

the picture for 308006 6B Chrysotile Structure 1 on p. 6 of Case Narrative. 6) revised reported LoQ, concentration of chrysotile & total 

cocentration for aliquot 6B based off of 4 structures (original concentration was based off of 2 structures). 7) added gravimetric loss data for 

PLM preparations to comments section of the certificate of analysis. 

10/08/2019 308006 6, 6A, 6B/D58: 1) The Special Instructions section of the login sheet was revised to include the FDA's cancellation of a request for 

analyzing a 4th aliquot of D 58 (308006 6C). 2) The preparation date was added to pages 2 & 3 of the TEM gravimetric bench sheet and to 

page 2 of the PLM gravimetric bench sheet; an explanation for the date written in the right hand margin of both sets of bench sheets was added 

to them; added missing weights for 308006 16 and 308006 17. 3) The handwritten TEM Bench Sheet for 308006 6A was revised to explain that 

the 2nd Chrysotile structure was identified based upon tubular morphology; also the structure number count for the 2nd listed stricture was 

corrected to read "#2" 

4475 Forbes B vd. · Lanham, MD, 20706 · (301 ) 459 2640 · To Free (800) 346 0961 · Fax (301 ) 459 2643 1/1 
~ 

J..A AMA Analu~icQI Services, Inc. Forns.edo111fle.s,lt:. \l'IVWJil!l!-lll:ali.com (?IMse Reier To T his 308006 Nmnbt'r Fer Inquires) AlHA-LAP (1/ IOOi)?O) NVLAP (#ltll 14>-0) NY F.LAP (10920) ·CHAIN OF CU1STODY 

4475 Forbes Blvd.• Lanhum , MD 20?06 

(301)459 2640 . (800) 346-0961 ~ .FAit (301)459-2643 

t\'lofl~~gJJJU~lng .lnforruatlon: 0 Sullmitt11l Jn~cwmut~ _ ~ 'l _ \I\ \~ ~• ~~~ l , 11 ':0~~~ 

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3. Addrcss2: _______ _____________ 3. Jobi/. P.0.H:~ ,~~k)5lt' 

4. i\ddrcss3: ______________________ 4. Con(ncl Pe-rson~ :~ ~ CcU: ___________ _ 

5. Phone-#: ____________ F:i:it I;___________ 5. Co1Jcded by: _~ _______________ CeU: ____________ _ 

Rt;purtlng !Into (Results f>l'ovided as won ns tec'lmknlly f't>as,ble). U' no TAT/1Rc1>0rti:ug Info ls Jll"O'Vidcd, AMA will assign MfnuJts of 5-Dfly and etnalVfnx to ooutarts onJile. 

Nt"fl::lt UO'UICS •11111,~1 •ir ,,,.,..,...,-1,1-<1.,h·il} 0 4Uour& NOIUdAL llllSINg~s HOURS nnronTTO: 

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Asb<.'SCm, A m1ly,11i.~ .. 1CM }.jr Plelr~e lndicolc flilre1· 'J')'pe: ___ _ _ 

Q NIOSI l '74fOO _ ___ (QTY} 

Q •lritrerglas~-----(QTY} 

1'£M Air~ - Pk,.1sc !!ldii:alc Jl\llc.r1'ypc: ____ _ 

Q AfU!.RA ____ (QTY) 

0 M OSI I '7402 ____ (QTY) 

Q 0 1her ( sp~cify ) _ (QTY) 

PLM ll'lllk 

Q iflf>A 600- Visual F.~tiruat,.._ ____ (QIT)  Pos Stor> 

f.l EPA Point 0.1unt _____ {QTY} 

Q NY Stal;, P1i:ible 19lU {QTY) 

0 Cmv R~d11c1,on ().LA.P 198.6 1((J)11'll') 

0 rQ1he;r (.sp~cify _____ ) <QTY) MJs.c 

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lCM Bulk. 

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NY St11le PLMffEM \1::i , ~QT'\- )~ Rosid@I Asl1 fQT'I I 

ID Vcrmkuli1c - ---- fEM Dust* 

0 Qua!. (Jll"-slnlr..) V:w11111n/Du~1 _ ____ Q Qua,,. (,la,.:u) V11Cutmi DSi55-9S 

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Metals Analysis 

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0PbPai11tClup ____ (QTY) 

O ¥f'b Dul(! Wipe (wipe iype _____ (QTY) Q ~Pb Air _____ (QT._Y_) ___ _ 

0 PbSC)il/Snlki _____ (Q'l'YJ 

·O l'b '11.:LI'-- __ (Q"J'Y) 

,0 Drinking WuterO Pb __ (QTY) 0 Cu __ (Q'l'Y) 0 As __ ((flt') 

'0 Was1e W:iterO l'b __ (QTY) CJ Cu_(Q'fY) Cl A~ __ (Q'l'Y) 

Q Pb Fum11ce(Media ___ _ ) _ _ __ (QTY) 

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Cullccl'iD11 l\p~ratus fo.- Spore Tmps/Air Snmpl.-1: ______ _ 

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S AMJ''l, ll: IN FOIU\'1A11JON 

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 USPS Q (.'O'J!rie, ------
------------ - -------------- ---

ATTACHMENT B: CFS AN OFFICE OF COSMETICS AND COLORS CHAIN OF 

CUSTODY FORM 

CFSAN 

Office of Cosmetics and Colors 

CHAIN OF CUSTODY FORM 

Case/Lab No: 

Submitter: _ Goran Periz ____________________ _ 

Assignment No./ Contract No.: HHSF223201810337P __________ _ 

Entry No./LabNo.: ~~..,.._.~C((="""-e,,___ _____________ _____ _ Date Sealed: _7/23/2019 ___ __ Sample Type: 15 samples D-53 to D67 

Item# 

1 I 

2 1 

3 

4 

5 

6 1 

7 

8 1 

9 1 

10 1 

11 l 

12 1 

13 1 

14 

15 l 

Chain of Custody 
Item# Date Received by 

(Print Name) 

Received by 

(Si.l?Ilature) 

Comments/Location 

1-15 7/24/2019 

Page I of 2 pages (See back) 

CHAIN OF CUSTODY FORM 

(Continued) 

Chain of Costod 

Item # Date/fime Released by Received by Comments/Location 

Print Name 

Final Disposal Authority 

Authorization for Disposal 

Item(s) #: on this document is/are no longer needed as evidence and is/are authorized for disposal by ( check 

appropriate disposal method) 

D Return to Submjtter 0 Destruction 

Name of Authorizing Official: Date: 

Signature: 

Witness to Destruction of Evidence 

Item(s) #: on this document were destroyed by (Name) 

in my presence on (date) 

Name of Witness to destruction: Signature: Date: 

Adapted from: Technical Working Group on Biological Evidence Preservation. The Biological Evidence Preservation Handbook: Best Practices 

for Evidence Handlers. U.S. Department of Commerce. National lnstitute of Standards and Technology. 2013. 
Release to Lawful Owner 

ltem(s) #: _____ on this document was/were released by Evidence Custodian 

__________ ID#: ____ to 

Name -------------------------=---------------,::- Address: ______________________ City: _________ State: __ _ 

Zip Code: ___ _ 

Telephone Number: (___J -,------------c-------,--­

Under penalty of law, I certify that I am the lawful owner of the above item(s). 

Signature: __________________________ Date: ____________ _ 

Copy of Government-issued photo identification is attached. D Yes D No 

This form is to be retained as a permanent record by the Center for Food Sarety and Applied Nutrition, Office of Cosmetics and Colors. 

Page 2 of 2 pages (See front) 

Adapted from: Technical Working Group on Biological.Evidence Presen,ation. The Biological £vidence Preservation Handbook: Best Practices 

.for Evidence Handlers. U.S. Department of Commerce, National Institute ofStand_ards and Technology. 2013. 
AMA Analytical Services, 

Focused On Results 

Inc. . ~3t~~~® NY ELAP 

Lab ID 10920 

Case Narrative (I) 

.,.. .. ,, ........ 

Client Name: FDA Office of Cosmetics & Contact: John Gasper 

Colors 

PO Number: HHSF223201810337P Phone: (240) 402-1133 

Job Name/Location: Task 3 -Analysis of Email: john.gasper@fdsa.hhs.gov 

Official Samples (4th Group -

15 Samples) 

AMA COC Number: 308006-6, 6A, 68/D-58 Date Received: July 24, 2019 

AMA 

Sample No. Client Sample No. Sample Description Analytical Method 

308006-6 D-58 Slightly clumpy, white powder with 

a matte appearance 

Mod. PLM ELAP 198.6 /TEM 

ELAP 198.4 

308006-6A D-58 Mod. PLM ELAP 198.6 /TEM 

ELAP 198.4 

308006-68 D-58 Mod. PLM ELAP 198.6 /TEM 

ELAP 198.4 

Requested Analyses: PLM and TEM Analysis for asbestos fibers conducted by Modified NY ELAP Method 198.6 and 

Modified NY ELAP Method 198.4 

Sample Receipt: 

The samples were received by AMA Analytical Services, Inc. on July 24, 2019 at 1058 via in-person drop-off by FDA 

representative, Goran Periz. The set consisted of 15 (fifteen) samples submitted in "'2oz, glass jars sealed with scotch 

tape. Conditions were checked upon receipt and all sample containers were intact. Most jars were filled approximately 

1⁄2to3⁄4 full. The sample set was processed on AMA Chain-of-Custody (COC) number 308006. This COC number served as 

the internal laboratory job number for tracking purposes. The samples were entered into the AMA laboratory database 

on August 12, 2019 at 1151 by- . The samples were logged in for analysis in triplicate and each sample 

aliquot was assigned a unique laboratory identification number as shown in the table above. After the sample login, the 

set was transferred to AMA's lock-box for storage. 

The following pictures document the condition of each sample upon receipt at AMA: 

Asbestos· Leed · Mold · Nano 

4475 Forbes Bouleva rd. · Lanham, MD 20706 · (301) 459-2640/(800) 346-0961 · Fax (301) 459-2643 · www.amalab.com 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,6B/D58, Revised 10/11/2019 (Revision #2} 

308006-6, 6A. 68/058 

Page 2 of 16 ~ - AMA Analytical Services, Inc. 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,6B/ D58, Revised 10/ 11/ 2019 (Revision #2) 

Sample Preparation 

Samples w ere prepared for PLM and TEM bulk analysis by - on August 13, 2019 through September 5, 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. 

8) Make four PLM slide preparations from the PLM residua l 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 fi lter 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 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 w as performed 

using a JEOL JEM-l00CX 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 were examined per sample. 

Modifications to the NY ELAP 198.4 Method were: 

1) The residue w as 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 fi ltered onto a 47mm 0.22um M CE fi lter. 

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

measured, and the mass of each amphibole particle was ca lculated using the ASTM D5756 method. 

3) 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 = n/4 L * W2 * D * 10-12 

M = mass 

L = length 

Page 3 of 16 ~ - AMA Analytical Services, Inc. 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,6B/D58, Revised 10/11/2019 (Revision #2) 

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 mult iplied by 100 to convert it to percent. 

EFA- Effective filter area 

MA - Mass of asbestos 

RW - Weight of residue 

VF - Volume fi ltered 

IW - Initial weight of the sample 

AA-Area analyzed 

RJ - Weight of residue placed into the jar 

Limit of Detection and Quantification 

We used the mass of a 0.5 x 0.04-micron tremolite or chrysotile fiber, depending on what was found in each sample, as 

the basis for our calculations. Limit of detection was defined as 1 fiber and limit of quantification was defined as 4 

fibers. 

Some aliquots of sample D58 contained very small amounts of asbestos that were either at or below our 4-fiber limit of 

quantification. For these samples we defined our limit of quantification as follows: 

308006-6A: mass of the two observed chrysotile structures plus the mass of two chrysotile fibers measuring 

0.5 x 0.04 microns 

308006-68: mass of 4 chrysotile fibers measuring 0.5 x 0.04-micron 

Discussion and Interpretation of Analytical Findings: 

308006-6, 6A, 68 Client Sample D-58 

PLM 

All three aliquots of sample D-58 were analyzed by on September 13, 2019. No asbestos or nonasbestos amphibole variants were detected the samples. The results were calculated using the equations detailed in the 

calculations section. 

308006-6 NAO 

308006-6A NAO 

308006-68 NAO 

TEM 

Sample 6 was analyzed by on September 3, 2019. Samples 6A and 68 were analyzed byI on September 7, 2019. The primary particle observed was talc along with a few talc fibers, talc ribbons and mica 

t icles. Two Chrysotile structures were detected on the aliquot for 6A and four chrysotile structures were detected on 

the aliquot for 68. The results were ca lculated using the equations detailed in the calculations section. 

308006-6 NAO 

308006-6A <0.00002% 

308006-68 0.00002% 

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

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

Page 4 of 16 ~ - AMA Analytical Services, Inc. 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/2019 (Revision #2) 

Sample 308006-6A, Chrysotile Structures 

500nm 

HV•1CICll<V 

Dlre<:1 M"I!: 5800 X 

AMA Analytical -icee, Inc 

TEM MOde: Imaging 

Microscopist: co C.ment: NANOSPRT5, E.xposu,e: 800 (ma) a 5 std. ftames, Gaiin: 1, Bin: 1 

Gammo: 1.IIO, No Slt"'!'oning, Normal Contrnt 

Diffraction Pattern from Chrysotile Structure 1 pictured above 

30800tl FDA,_ 100,H>ll 

Clvysolile Oil 100 If/Al 308006-44o lfVa100kV 

1, ,11:1 !117/2019 Cam Len: 0.2200 m 

TEN Mode,: Dilfniction AMA Analytical S.rvica, Inc 

Microscopist CD 

Camen: NANOSPRTS, & posure: 800 (mt) ir 5 std. frames, Gain: 1, Bin; 1 

Gamma: 1.00. No Sharpening, Normal Contrast 

M. Page 5 of 16 AMA Analytical Services, Inc . 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/2019 (Revision #2) 

Sample 308006-68, Chrysotile Structure 1 

308006 FOA_ 103.jp0 

Chryaotle Cluster 400nm 

HV•111Cll<V 

-

C.I: 0.001429 llffl/plx Oim:I Mllg: 72110 X 

15:33 11/7/2019 AMA Analytical SeNic:ee, Inc 

TEM MOO@: ltnag,ng 

Mtcroscoplst co camera: NANOSPRTS, E.i:posure: 800 (me)• 5 std~ frames, Gain: 1, Bin: 1 

Gamma: 1.00, No ShOll>ening, Normal Contra1 

Diffraction Pattern from Chrysotile Structure pictured above 

30800tl FOA_ 102,jpg 

Clvy$otile Oil 10011/AI 30800611> HV• tOOkV 

16:3211/7/2019 c.,, Len: 0.2200 m 

TEM Mode,: Oillnlction AIIA Analytical S.rvicn, Inc 

Mictoscopjst CD 

Camera: NANOSPRTS, Exposure: aoo (ms) as std. frames, Gain: 1, Bin: 1 

Gamma: 1.00. NoS'-l>ening, Normal Conttnt 

M Page 6 of 16 . AMA Analytical Services, Inc . 
!:•·--

0 

. structure 2 

chrysot1le 

3osoo6-6B, 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/2019 (Revision #2) 

Diffraction Pattern from Chrysotile Structure pictured above 

- .SOIIOOI Ft>A_ 1°'4,JP!I 

Clv)sotilc Dif 10011/AI 308- HV~IOOkV 

16:03 917/2019 cam Len: 0.2200 m 

TEM Mode: Diffraction AMA Analytical Setvlca, Inc 

Microscopist CD Camora: NANOSPRTS, &posunt: 800 (ms) x S std. frames, Gain: 1, Bin: I 

Gamma: 1.00. No Sharpening. Normal Conlnlst 

308006-6, Talc Particle 

301006 FDA_062.jpg 

Talc P•ttiole 500nm Cal: O.OOITT4 1,111/pix HV'"100kV 

17:11913/2019 Direct llag: 5800 X 

TEM Mode: lm"lling AIIA Analytical S.rvica. Inc 

Microscopist MO 

Com.,., NANOSPRTS, &pooun,: 800 (ms)• S drift frames, Gain: 1, Bin: 1 

Gamma: 1.00. No Sharpening, Normal Contrast 

Page 8 of 16 ~ - AMA Analytical Services, Inc . 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/2019 (Revision #2} 

Hexagonal Diffraction Pattern from Talc Particle pictured above 

- 30800G FDA _Gsa,.jpg 

Tak Particle 100 If/Al 17: 19 9/312019 HV=100kV 

TEM Mode; Dlllractton cam Len: 0.2200 m 

Microocoplat MG AMA Analytical SOfVicea, Inc 

Cam..,,, NAHOSl'RT5, Exposure: 800 (ms) • 5 drill frames, Gain: 1, Bin: 1 Gamma: 1.00, No Sbarpening, Normal contrast 

Chemistry from Talc Particle pictured above 

Ful sc.ale counts: 377 308006-6(1) 

300 

Si 

0 

200 Mg 

100 

0 

0 1 2 3 4 5 6 7 8 9 10 

keV 

M. AMA Analytical Services, Inc . Page 9 of 16 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/2019 (Revision #2) 

306008-6, Mica Particle 

JOSOOI FtlA_054.JP9 

Mica Parto<:le 400nm Col: 0.001'29 l'ffllpiJl HVe100kV 

17:21 9/312019 Direct Yag: 7200 X 

TEM Mode: Imaging AMA AnaJyllcal 5enrlc:U, Inc 

Microscopist: MO 

Camora: NANOSPRTS, Exposun,: 800 {ms) x S drill frames, Gain: 1, Bin: 1 

Gamma: 1.00, NoShatponlng, Normal Contrast 

Diffraction Pattern from Mica Particle pictured above 

- 308~ FDA. OSGJpg 

Mica P1rt1c1e 1nn t11A\ 

17:22 !113/2019 HV•100kV TEM _ , Dilrnoction c.im Len: 0.2200 m 

Microac.opiat: MG AMA Analytical SefYicu, Inc 

Camera: NANOSPRTS, Exposure: 800 {ms) x 5 drill frames, Gain: 1, Bin, 1 

Gamma: 1.00, No Sll.ltpeflirlQ, NOltnal Contrast 

M Page 10 of 16 . AMA Analytical Services, Inc . 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/2019 (Revision #2} 

Chemistry from Mica Particle pictured above 

Ful scale counts: 337 308006-6(2) 

0 

300 

Mg 

200 

Si 

Al 

100 

0 

0 1 2 3 4 5 6 7 8 9 

keV 

308006-6, Talc Fiber 

308006 FD"-057 Jpg Talcflbe< 200nm Cal: 0.7:14t21 nm/pix HV~100kV 

17:27 9/3/2019 Direct llag: 14000 X 

TEM lilodo, Imaging AMA Analytical S.rvk:es, Inc 

Microseopist: MG 

Comer.a, NANOSPRT5, bposuro: 800 (ms) a 5 drin frames, Gaon: 1, Bin: 1 

Gamma: 1.00, NoS!wpening, Normal Conlnlot 

M Page 11 of 16 . AMA Analytical Services, Inc. 

10 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/2019 (Revision #2) 

Diffraction Pattern from Talc Fiber pictured above 

308006 FDA_058.jpg 

'Tale Fiber -

100 If/Al 17:28 91312019 HV=100kV 'TEM _ , Dlllractlon cam Len: 0.2200 m 

Microacoplsl! MG AMA Analytical Son,ic••· Inc 

ca.,,.ta: NAHOSPRTS, Exposure: 800 (ms) • 5 drill ftames, Gain: 1, Bin: 1 

Gamma: 1.00, NO S barpenirlg, Normal contrast 

Chemistry from Talc Fiber pictured above 

Ful scale counts: 235 308006-6(3) 

0 Si 

200 

1SO 

Mg 

100 

so 

0 

M. AMA Analytical Services, Inc. 

5 

keV 

6 7 8 9 10 

Page 12 of 16 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/ 2019 (Revision #2) 

308006-6, Talc Ribbon 

JOIOOI RIA_059,jpg 

Talc Ribbon 500 nm Col: 0_001n, l'ffllpu HV~100kV 

17:37 9/3/2019 Direct ... g: 5800 X 

TEM Mode : Imaging AIIA Analytical Servlc:U, lne 

Microscopist: MG 

came111: NANOSPRTS, EJtposunt: 800 (me) • 5 drill frames, Gain: 1, Bin: 1 

Gamma: 1.00, NoShatponing, Normal ConlJUt 

Diffraction Pattern from Talc Ribbon pictured above 

308006 FDA_O&O.jpg 

Talc Ribbon -

1nn111A1 17:38 913/2019 HV•100kV 

TEM - : Dillnlclion cam Len: 0.2200 m 

Microacopiat: MG AMA Analytical Senrices, Inc 

Came,a; NANOSPRTS, Exposure: 800 (ms) it I d rift frames, Gain,; t, Bin: 1 

Gamma; 1.00, No 511arpaning, Normal C0nlraSI 

Page 13 of 16 ~ - AMA Analytical Services, Inc . 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/2019 (Revision #2} 

Chemistry from Talc Ribbon pictured above 

Ful scale counts: 155 308006-6(4} 

0 Si 

150 

Mg 

100 

50 

0 

0 1 2 3 4 5 6 7 8 9 10 

keV 

308006-6, Talc Fiber 

~-~OS1,jplj 

Talc Fiber -200nm Cal: 0.001029 llffl/plx HVe100kV 

17:50 ll/3/2019 Direct IAag: 10000 X 

TEM Modoc Imaging AMA Anal_yllcal Services, Inc MocroSCOl)ISt MG 

Camen: NANOSPRT5, Exposure: IIO0 (ms) a 5 drill lramtt, Gaon: 1, Bin: 1 

Gamma: 1.00, NoS""'1>oning, Normal Conlnlst 

M Page 14 of 16 . AMA Analytical Services, Inc . 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,68/D58, Revised 10/11/2019 (Revision #2) 

Diffraction Pattern from Talc Fiber pictured above 

-

100 11/AI HV=100kV 

cam Len: 0.2200 m 

Mlcroacopl&t MG AMA Analytical Son,icH, Inc 

C.Ometa; NANOSl'RT5, Exposure: 800 (ms)• 5 drift ftames, Gain; 1, Bin: 1 

Gamma: 1.00, No Sl\arponil'lg, Normal contrast 

Chemistry from Talc Fiber pictured above 

Ful scale counts: 264 308006-6(5) 

250 

200 -

150 

100 

50 

Si 

0 

Mg 

0 

0 1 2 3 4 5 6 7 8 9 

keV 

M Page 15 of 16 . AMA Analytical Services, Inc . 

10 
Re: FDA Office of Cosmetics & Colors 

COC 308006-6, 6A,6B/D58, Revised 10/11/2019 (Revision #2) 

QC Discussion: 

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

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

micron, and was analyzed by on September 18, 2019. No asbestos was detected on the blank samples. 

The reference sample was m t e same Sigma-Aldrich talc powder spiked with 10% Chrysotile. The reference 

sample was analyzed by on September 18, 2019 and found to be within acceptable limits. Additionally, 

fi lter blanks were prepared with each batch of carbon coated filters. Filter blank number EB-54155 was associated with 

the carbon coating for samples 308006-6, 6A, 68/D-58. No asbestos was detected on the filter blank sample. 

Our laboratory information management system (LIMS) randomly selected samples 308006-2/D-54 and 308006-15/D-67 

for addit ional replicate QC analysis. Separate preparations were made for PLM and TEM analysis. The replicate QC 

analysis was performed by-on September 13, 2019, 2019 for PLM analysis and by on 

September 18, 2019 for TEM analysis. The QC results matched the original 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 & Duplicate QC Chart for for samples analyzed between 1/1/2019 and 

9/18/2019 

7) Replicate & Duplicate QC Chart for for samples analyzed between 1/1/2019 and 9/18/2019 

8) Replicate & Duplicate QC Chart for for samples analyzed between 1/1/2018 and 9/18/2019 

9) Raw Data Sheets 

a. Gravimetric Data 

b. Filtration Worksheets 

c. PLM Analysis 

d. TEM Analysis 

e. QC Samples 

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. 

10/11/2019 

Andreas Saldivar Date 

Laboratory Director 

Page 16 of 16 ~ - AMA Analytical Services, Inc. 
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Login Sheet 

Client: 

Date Submitted: 

Due Date: 

US Food & Drug Adm n s ra on 

07/24/2019 

09/13/2019 5:00 pm 

Job Name: 

Job Location: 

Job Number: 

Task 3 - Ana ys s of Off c a Samp es 

4 h Group - 15 Samp es 

CUN 0001 

Chain of Custody: 

PO Number: 

308006 

SF225201810337P 

AMA Sample Number Client Sample Number Analysis Type(s) and Sample Type(s) 

4475 Forbes B vd. · Lanham, MD, 20706 · (301 ) 459 2640 · To Free (800) 346 0961 · Fax (301) 459 2643 1/4 
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AMA Sample Number 

308006-6 

308006-6A 

308006-68 

308006-6C 

Client Sample Number 

D-58 

D-58 

D-58 

D-58 

Analysis Type(s) and Sample Type(s) 

PLM: ELAP 198.6 NOB 

TEM: Bu k Upgrade 

PLM: ELAP 198.6 NOB 

TEM: Bu k Upgrade 

PLM: ELAP 198.6 NOB 

TEM: Bu k Upgrade 

PLM: ELAP 198.6 NOB 

TEM: Bu k Upgrade 

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- 4475 Forbes B vd. · Lanham, MD, 20706 · (301) 459 2640 · To Free (800) 346 0961 · Fax (301) 459 2643 2/4 
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AMA Sample Number Client Sample Number Analysis Type(s) and Sample Type(s) 

Special Instructions: 

Use FDA Protocols. Samples are in Asbestos Sample Lock Box (See for Key). ALL PLM & TEM Analysts: Please record the date & amount 

of time spent analyzing each sample in the comments section of the bench sheet. Please save all pictures, graphs, etc. to L:\Case Narratives\FDA 

Project\308006 

4475 Forbes B vd. · Lanham, MD, 20706 · (301 ) 459 2640 · To Free (800) 346 0961 · Fax (301 ) 459 2643 3/4 
9/30/2019 byl: Client requested that we analyze a 4th aliquot for sample 308006 6/D58; this was added as 308006 6C 

10/1/2019 by : Client requested that we cancel their request to analyze 308006 6C, Preparation was mostly complete by the time we received the 

cancellation ce, but no analysis was performed. 

4475 Forbes B vd. · Lanham, MD, 20706 · (301) 459 2640 · To Free (800) 346 0961 · Fax (301 ) 459 2643 4/4 
Daily Calibrations for PLM Scope ff __ 2.-=---- Date: 'i t ltl. I lj__ 

Anal){st Initials: ___ 

Cleaning: 

Oculars r Objectives._ / _ _ Field Lcns. __ r-_ Meehat1ical St.age._ /,,_ __ Main Body_....:;./ __ 

Alignment: 

~ Kohler lllumiru1tion (or flH close to it a.1 scope e.Ilow~) 

/ PoJnrizcr &Ana lyzer nl 90 degrees to one llllother 

~olru izer & A.11a ly1er oligned with reticule cross hc1irs 

r Axis of rotation of stage centered in field of view 

7 Central stop of the D.S. objective aligned with condenser aperture 

Refractive Index. Colors of Permanent 1,680 Amosile: 

ltte-Parallcl w:,vclcnglh ~6£......Pt:rpe.ndicular wavele1:1gth 

Comments/other procedures performed: 

Daily Calibrations for PLM Scope#_......:£_ _ _ _ Date: 'f l l3 / t;L_ 

Analyst .[uitids:--

Cleaning: 

Oculars. ____ ,, __ Objectives_✓ __ Field Lens ,, Mechanical Stage. _ _£_/ __ Main Body_---=✓-

Alignment 

_ ,._Kohler Illumination (or as close Lo it as ~cope allows) 

_ ,_ Polarizc::r & Am1l)'2er al 90 degre,es tn one anotJ1cr 

, Yolarizer & Analyzer aligned with reticule cross hairs 

,. Axis of rotation of stage centered in field of view 

/ Central stop of the O,S. objective nligned with condenser nperturc 

Refractive lndex. Colors of Permanent 1,680 Amosite: 

~arallel wavelength t-., h',erpendicular wawfonglh 

C',.ommenL-./ other procedures pcifo1mcd: 

Daily Calibralions for PLM Scope #-""L=--- Date:9 I I /, / ( t..._ 

Analys,t limitials:--

C leaning: 

Oculars__£" _ Objectives ,, Field Lens ;- Mechanical Stage , Main Body_ ,-

Alig;nment: 

~Kohler lllum.ination (or as close to it as scope allows) 

~Polarizer & AnaJyzer at 90 degrees to one another 

_, _ Polarizer & Analyzer alignoo with reticule cross hairs 

_ , _Axis of rotation of stage centered in field of view 

__..L_ Central stop oflhe D.S. objective flligned with condenser aperture 

Refractive lndcx Colors of Permanent 1,680 A.mosite:_ ~ Pnmllel wnvefoJtgth 1,p4Perpendici1lar wavelength 

( Comments/other procedu(es perfom1ed: 

Revisiou P,Jssued 12/1&'10; approvcrl: PC 

Di1-ecl01y: UloeJDaily 111icl'Osco1,,-o log sl1ec:1S 
REFRACi!Vt: INDfX , OIL C/\LIBRP,ilON 

I DATE II ANALYST ]I RIOIL 

11 BOTT(E 1011 LABID II RI BEAD I TEMP Dispersion Staining Color/ lv1atching Measured 

( De~. C} Becke Une ObseK1ations Wavelength R.I. 

q-3-Jq t;so • (. S'~DK} I I.K' .ir-· Xs-J R/11e,. . H" ~ ~~D !, n-i,s-

; J.l,~ I. ~So"<? /.bY 'r cRl\.tt. Gv-uvi V hz0 / . fJS'/l, 

; (.'l,tf f. b..,sx, I .b0 ~ Oi1A,,. L,~+i~,11 bl,t> /. l:,o<f./ 

, 

' I, i,z;( J.bi·n<J /. bZ. t 1,~ LI t-: l'lti~e~~ ~ ,-

"' , . 'foO f .~>;1 1:·r0 ~ I< "I t.-- &,~ k -. ~ - I 

I I l ..; 

I 

I 

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I 

Re11isior11 2, February '19, 2,0())7 
DATE NAME 

,SY ST.EM/ 

ALIGN . CHECK 

,1,(,q oA 

BCTUA.k..''BEAM TIME" USED · 

TOTAL TOTAL# 

ON OFF MINUTES SAMPLES TYP.E 

oioo 

~h\ ~ 6i \i~ 11-----'--+=::=::--l----~ \1 A 

(~I~ ' ,.+ ' 

Ver-sion 2-l;.9/90 

l ,~\5\t!i~\ <' 1 ~J.1d ~~. 'dc?JcA 

l\:=llm'! illU~\!o'Jt~ml 

.~ 

,: .. 

mUL'l TEW CALIIBRA'lIO~ LOG 

ti'' 

E:vary analyst should confirm alignmenl prior: to. analyzing saroples. 

X-ray analyzer must ue calibrated prior to eaoh d~y-~s use . . 

Dewer for x-ray detector is to Ls filled each Tues day and Friday. 

Note! Please I enter oode letters in TJ~a Col~m~ 

Type of Analysis: Routine Analysis A j Quality Control QC 

Training T 

Research R 

other (Expl ain) o .. 

I 

rr==============::;::===::;=============:;f,:;;==::::;;==:::::;;=aii 
Chain Of Custody +Add CoC #308006 

General Samples Documents QC Results 

QC Samples 

Original Original PLM PLM Original Original TEM 

Date Sample PLM PLM QC PLMQC R TEM TEM QC TEMQC TEMR 

Analyzed Number Analyst Result Result Analyst Value Analyst Result Result Ana.lyst Value Comments 

09/09/2019 308006- (6Jl6f. 0.00 SW 0.00 MG 0.00 0.00 CD 0.00 Analysis 

1 6RQC 9/18/19 

09/09/2019 308006- 0.00 SW 0.00 MG 0.00 0.00 CD 0.00 Analysis: 

17RQC 9/18119 

Reference Samples 

Sample Number 

Talc Ref 

 

TIie# 

Talc Ref 10% 

Analyst 

(6) (,-...------w 

Asbestos Type 

Chrysotile 

Percent Asbestos 

10.00 

Result 

Pass 

Created Date 

0911812019 

Comments 

 

Blanks 

Blank Number 

NB19-646 

NB19-645 

Date 

09/18/2019 

0911812019 

(t5) 6 

Asbestos Percentage 

0.0 

0,0 

Asbestos t ype Comments 

NB19-647 09/1812019 0.0 

PLM Error(s) 

No Results 

TEM NOB Error(s) 

No Results 
2 

PLM QC Chart 

QC Type: Duplicate 

Analyst: ~b) (6 ) 

Dates Analyzed: 01/01/2019 - 09/18/2019 

Q) 

> -fil 0 

d:. 

-1 

·2 

~~ ':, '1., ~'? ~ ~ ~ ~ I;) ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ 

Original Asbestos Result 

R = [Original Result] - [QC Result)/ (Average] 

4475 Forbes Blvd. · Lanham, MD, 20706 · (301) 459-2640 • Toll Free (800) 346-0961 · Fax (301) 459-2643 1 /1 
2 

PLM QC Chart 

QC Type: Replicate 

AnaJyst: (b) (6) 

Dates Analyzed: 01/01/2019- 09/18/2019 

Q) 

:::, 

ro o > 

d: 

-1 

-2 

~~ <6> " 'v,'y ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ 

Original Asbestos Result 

R = [Original Result] • [QC Result] / (Average) 

44 75 Forbes Blvd. · Lanham, MD, 20706 · (301) 459-2640 · Toll Free (800) 346-0961 • Fax (301) 459-2643 1 /1 
2 

NOB QC Chart 

QC Type: Duplicate ~ ---- Analyst 15) 6 

Dates Analyzed: 01/01/2019 - 09/18/2019 

V" ................................. . 

-1 

-2 

TEM Or g na Asbestos % 

R = [Or g na Resu t) - [QC Resu t] / (Average] 

4475 Forbes B vd. · Lanham, MD, 20706 · (301) 459 .2640 · To Free (800) 346 0961 · Fax (301) 459 2643 1/1 
2 

NOB QC Chart 

QC Type: Replicate 

Analyst: (b) (6) 

Dates Analyzed: 01/01/2019 - 09/18/2019 

(I) 

:, 

~ 0 

d: 

-1 

-2 

TEM Or g na Asbestos % 

R = [Or g na Resu t] - [QC Resu t] / [Average] 

4475 Forbes B vd. · Lanham, MD, 20706 · (301 ) 459 2640 · To Free (800) 346 0961 · Fax (301 ) 459 2643 1/1 
2 

NOB QC Chart 

QC Type: Duplicate 

Analyst: (b) (6) 

Dates Analyzed: 01/01/2019 - 09/18/2019 

·1 

·2 

~-······················ 

TEM Or g na Asbestos % 

A= [Or g na Resu t) - [QC Resu t] / [Average] 

4475 Forbes Bvd. · Lanham, MD, 20706 · (301) 459 2640 · To Free (800) 346 0961 · Fax (301) 459 2643 1/1 
2 

NOB QC Chart 

QC Type: Replicate 

Analyst: (b) (6) 

Dates Analyzed: 01/01/2019 - 09/18/2019 

(I) 

::, 

~ 0 

d: 

-1 

-2 

,§, ~~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ ~ 

,'1-· ~- ~- ~-

TEM Or g na Asbestos % 

R = [Or g na Resu t] - [QC Resu t] / [Average] 

4475 Forbes B vd. · Lanham, MD, 20706 · (301) 459 2640 · To Free (800) 346 0961 · Fax (301) 459 2643 1/1 
1 

».At( AMA Analytical Services, Inc ~ - FoclJsP.d On Result s. 

coc 1t: 3Q&90(o 

Olent:_l).S_"F_bA_ ..._._______ _ Gravimetric Reductfon Wefgnts 

Mm(ii) Massie) • M>5'M 

Pi;,>tA,h Vial Vl&I & S11mμI~ Vi;,l l!I S•111pk, 

\ 

GravJ.lnet ric Reductfon and Filtration Bench Sheet for Modified ELA:P 198.4 

TEM Prep·arations 

Prep By; 

,f,1,,s (el .M»1(8) l'o~t 11dd W.>sh Fjter & 1'<'111 flls~ FTltu & IP~trl tliJh 

o.-~'&!)l"\ 

F11tr,atlorn Weights 

Ma»{t) · M&Jl Isl 1O0m'l .lir w/ lid 100ml br w/ li<I & Sample Rc._,idtJe 

Page _j_ of ,3 

1 Filter Type: 47 mm, 0.22 μm, MCE EFA: 1047 mn 

Filtered By:(b) 6 lot II: R"\ CAO~\~~::~:~ 

Flltratlon Volumes ~~ 

~.,..i DlluUcn Se-rl~I lllll>don Serlal Dtlu1Ian 

lfllllaJVolllf'!l~ 1/ol•me ~ill<t1"ct lnlll•IVol«n>o Vol.,me riltet<I rlnalVo l11m• 

(ml) (mU t11•ll tntll t1nt.t I ' t-;.n ti.:;,._ ; II) .,t,t,., ( I ,,, t;.n, ~, r.wt.-1 (!fll.,ft bf'.,,,._ ,io 1e.~! 

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coc fl: 30 ~OOG, 

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AMA S1m11le ID 

Focused On Result:,. 

Gravlmetrlc Reduction Weights 

Mass(gJ 

V-,4 &5-.mplr 

M•n (a) 

r~tA,h 

1/ial Ii Son,ple 

Gravimetric Reduction and Filtration Bench Sheet for Modified ELAP 198.4 

TEM Preparations 

..... 1b\l¥>.~ 

Prep By: {b) (S) - \ · 

Ma,s(c) 

fllttr It. Petri fll•~ 

MMs(g} 

P<>ll At Ill With 

f ,ter & Pe111 o·is1, 

Filtration Weights 

M.m(cl 

tooortL~fW/ Ud 

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l"ll.'IIVdume 

(mlj 

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ln,OelVoluffl<! 1/ol-f ilterd 

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Jk1. AMA Analytical Services, Inc. Gravimetric Reduction and f Utration Be,nch Sheet for M odif ied ELAP 198.4 

coc n: ,3oicoeo 

Client: tJSP})A 

Focused On Res ul!s . 

Gravimetric Reduction Weights 

M•u (II) 

Vlal 

. • "1•5$ (&) 

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Mm (g) 

Pr'31Mh 

Via/ &5amplo 

iEM Preparations 

OM" ,J~ .... Plep B {tj) (0} "" '"' \,' 

f iltrntlon We ights 

lv'I~» 1B) 

tlfter ~ ~elrl Dlsl1 

1 

Mrn(a) 

P<»t4cld Wnsh 

FIilo, & r,,t,IDl•h 

M•» (1) 

100,nL A r w/ lid 

IM~u/g) 

lOOml far w/ Lid 

& Sample Residue 

. l•>it••I 1f<1lu11t<! 

lillll 

Page _3.__ of 3 

Filtration Volumes 

S<!r!• I D\lut!<>n S~rM Ollullon Serl:ol Olluelon 

Vdfl!rna~,l<•« d 11111!al volum~ \lol.umc f llll!rd t inol \l()lume 

(ml) (,<1 LI (,~~) (mLI Olftf\Lt-.\)..MM11l1I 'tlf .. tt Cl11• 1 n • .s,Hht '-1 f hill:Oo'"#n~, rA1•l•• 

dtfud:n ~ floffllc\tl ijj uhn lla,1''o1ni«t} lllfudoo aertoona:JI 

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----------

---------

AMA Analytko Gravimetric Reduction Bench Sheet l Services , Inc:. F::icu~erl On llt!~ult:., Modified ELAP 198.6 

PLM Preparations Page 1 ol' -2 

<:oc #; 3og:ooc, Date: filt3/2ofl 

Prep l:ly: (b) (S) Client: VS Eh.A 

AMA Sample ID 

Mass.(g) 

Via1 

Mass {el • Mass (g} 

Filter & Petri Dhh 

- l 

I 

Mass {g) 

I 

' 

., 32 1 

2 l 05 
--

Gravimetric Reduction Bench Sheet M. 

AMA Analytical Services, Inc. 

FocU!;ec1 On Rei.ulli.. Modified ELAP 198.6 

PLM Preparations 

h - .., ,, COC #: 3 O<[OO(o Date: __.~ ~~-=---Llb (6) C lJ5FbA-- Prep By: lient: 

Mass (g) Mass {g) Mass (g) Mass (R) Mass (g) AMA Sample ID Post Ash Post Acid Wash 

Vial Vial & Sample 1 ter ~tr s 

Vial & Sample 

. ,oS'5 t:,. ~o 1 

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Edit Sample #308006-6 (0•58) 0 

PLM: ELAP 198.6 NOB TEM: Bulk Upgrade 

Initial Sample Weight Post Ash Weight Post Acid Treatment 0 

Vial Weight 1.252 Vial+ A&hod Sample Weight 1.6833 Fllt«Tare 6.0877 

Vial+ Sample Weight A&hod Sample Weight 0.431 Groll FIiter Weight 6.49<12 

lnKial San,ple Weight OA32 0.402 

Visual Estimations Final Asbeslos Per<:enls Final Non-Asbeslos % 

Estlm- AIMltOI PLM 0.0 Perceni AsbHIOI PLM NAD 0.254 

Estlm- AIMltOI TEM 0.0 Perceni AsbHIOI TEM NAD Percent Acid Solubi. 6.66 

Pwc.ntOther 93,085 

Sample Type Material Type San,ple Color 

Whole • 

Grid Box Row and Slots 

A19-433 lab 

Worltlng Mag, High Working Mag, Low Accelerating Voltage (ICY) 

(l(j lKl 100 

15 

• 

Structure Chrystallographic and Photographic Data 

$o,,,cru,-1 um a ....... ..... 5 Hex Mg,Si, Talc Fib..- 10 

Neg Mg,Si• Talc Ribbon 5.8 • • 

3 Hex Mg,Si, Talc Fib..- 14 

2 Hex Mg,AJ,Si,Fe• Mica~ 7 .2 • • 

... Mg Si• Talc Partido 5.8 • • 

Add Row 

Grid #1 Estlmaled Asb .. tos Grid #2 Estimated Asb .. tos Estimated Aabl-atos o/o 

0.0 0 .0 0.0'6 

Anatyst Comments 

f aiontation. 250, 115 

Grid A anely.md 9/a/19, Grid 8 analymd !1/,4/19, 

Analytical time ~ 1.Sln. 
....... ,.. • ..._ID•SIJO 

, ..... , ...... , 

~--I'd•~ 

....... 

, $ott1T19~..-.~" 

~•.dNl'fcaurt 

.ml'<ilrtOoU't 

,.~,oo.o 

--

...... , "'· ......... 

•1•• ·-· .,.. ...... • •• , 111-• •••• .. _, •••• "-· •••• .. _, • •• , ·-· ·-·· 111-• 

-

--

- . .,... 
• • 

• • 

• • 

• • 

15 

Edit Sample #3D8006-6A (D-58) 0 

PLM: ELAP 198.6 NOB TEM:. Bulk Upgrade 

Initial Sample Weight 

Vial Weight 

Vial• Sample Weight 

lnKial San,ple Weight 

T.1414 

0.486 

Visual Estimations 

Est imated AIMStOI PLM 

Estimated AIMStOI TEM 

0.0 

0.0t 

SampleTyp• 

Whole • 

Grid Box 

at9•433 

Wor1<Ing Mag, High 

(l(j 

Mat.,ial Typ• 

Row and SI<>!• 

2ab 

Working Mag, Low 

(K) 

Post Ash Weight 

Vial • A1h• d Sample Weight 

A1h• d Sample Weight 

Final Asbeslos Percenls 

Perceni Asbostos PLM 

Perceni Aabostos TEM 

Sample Color 

MlcrolC"I)• # 

Accelerating Voltag• (ICY) 

100 

Structure Chrystallographic and Photographic Data 

Sci,.,cru,-1 um e,..,...,. 

5 hex 

...... 

4 ulo (0.4x0.05) Grib UID 101 

3 pos (1.75'<0.06) Gri Si Mg 100 

2 neg 

hlK 

T.6324 

0.485 

NAD 

0.008 

Grid #1 E111m .... d Asb .. tos Grid #2 Esllmat• d Asb .. tos Estimated Aabl-atc,a o/o 

0.01 0.01 0.01% 

Analyst Comment& 

AM!y,,is: 9/7/19, time ; 1~r 10 mins 

F Orienla\ion: 285,40 

Post Acid Treatment 0 

Fill« Tar• 6.08~ 

Groll Fllt.,W.lght 6 .4791 

Weigl!< Resldu• 0.390 

Final Non-Asbeslos % 

0.226 

Percent Acid Solubi. 19.543 

Perc.nt Other 80,222 

5.8 Cllry>lolile 

0.22/5.8 Cllry>lolile • • 

Add Row 
__ 

Fiber Count Sheet for Transmassio:n Electron Microscopy )_.( AMA Analytical Services, Inc. .CIEr.). F<>cusect On Results, 

Page-\-of -l- dicnt 10: ...:;;._.:....;;;;__ t) ... 5s ________ _ FllterSiz~/Type/Porosity47mm MCE 0.22 μm 

COC#; '3Qf!,0Qk) AMAID#: 3~ ... E:A, 

Analys _ _ _ Working Mag: \ S: I( Acee! Voltage: l'0 0 !kV Orientation of Letter F: '( J: 

Grid Box#: A \ <\ ·· \.\"!:,,3 Grid Acceptable@ N Volume FIitered: 0~:1. ml• 

___ Row #: ... -2 ..... , _ __ Grld:.hJ~-- ,Grid OIPenings lo Observe: ?-.O 

Method: Mod. NY ELAP 198.4 [FDA Procedures) 

Grid Opelllng S1rvr.tvre L,mgth & Wld\h £le111efl\s ll>'d fllN!fi'lcr.11' SA'E<DNe@• Maar,lficatton .or 

I/ Location N (ltt r,lltrOII!) SAfl) Uflows Minero! Tvpo lt:J'-1',,,;, ..... a,;,dwer,, e•ii.r1 t.inln,,,...,, c,.,,t,a L&n,gth ~,.,,., . .__~,...::tc,-.tflt\lf'f~J .,_..1~\ .... ... ,_) fllrl1 blri, ,oph:>..,w..l•krn, 

( !l. ~ \ . \.-is I o.0o t>b!:) {'_J\~~i\t., ~;.\Ma \0\ \© 5 .~ l( CiYI 

t!l ~ 1.. o. "\ 10.05 Vka r h~i \.t ......i· ,,o\ 5"·S l( cm 

L ; I i K • cm ' L ' i K ! cm 

L ' i 

i K cm 

L I 

i 

! K cm 

L K cm 

L -_ 

' K i cm 

L 1 

I i 

; K I cm 

L I 

K cm 

l_ K cm 

L ! 

i I( I cm 

I_ ! 

i K cm 

L I 

! K cm 

L i 

I K cm 

L ; i K ! cm 

L i 

I K cm 

L I 

I K cm 

L ! 

i 

i I( cm 

L l 

I 

I I( cm 

L I 

I > K I cm 

L l 

~ . . .K cm 

L i 

i . . I( ; cm 

L i 

' K ; cm 

L ; 

i 

! .. K cm 

~<111d : HSO c N<> Struclllt'Cs r>ctcetc.tl UTO ,. Unable IC Obu In LJ • 1st Crfd l_lLl• 2nd Grid 

Total 

Mineral Type: C h<''(~j 1⁄2,. = :2 

Mln~ralType: ______ = _ _ _ 

Mineral Type: ______ ; __ _ 

Mineral Type: ______ = __ _ EM Sef(al #:_:s/,v I 
--

Edit s.mp1o , ......... s (0•58) 0 

...... .... ,. 

0 .243 

....... ~. w ... 

~--1'1011•,wyz,lld 

....... 

, &otrn19~..-.~" 

~•.dNrtcaurt 

.mNrtOoU11 

,.~,oo.o 

...... , "'· ............ 

•... •... . .. , •... •... •... . .. , ·-·· ,_, ,..... "-' .. _, "-· .. _, ·-· "-' 

-

--

-
• • 

15 

Edit Sample #308006-6B (D-58) 0 

PLM: ELAP 198.6 NOB TEM:. Bulk Upgrade 

Initial Sample Weight 

Vial Weight 

Vial+ Sample Weight 

lnltial San,ple Weight 

1.16$1 

0.495 

Visual Estimations 

Estlm- AIMltOI PLM 

Estlm-AIMlt0I TEM 

0.0 

O.Ot 

Sampl<oType 

Whole • 

Grid Box 

A19-433 

Wor1<1ng Mag. High 

(l(j 

Material Type 

Row and Sl<>ts 

3ab 

Working Mag. Low 

(K) 

Post Ash Weight 

Vial+ Ash..:! Sampl<o Weight 

Ash..:! Sampl<o Weight 

Final Asbeslos Percents 

Perceni AsboslOs PLM 

Perceni A•boslOs TEM 

San,pl<o Color 

Mlcro"""P•# 

Accelerating Voltage (ICY) 

100 

Structure Chrystallographic and Photographic Data 

Scr,,,crur.l um a ........ 

5 hex 

neg • 

...,,. 

3 hex 

2 pos (1.0>0.05, MatJ Si MgAJ 104 

pos {1.6>0.05, Cb, Si Mg 102 

1.45622 

0.494 

NAD 

0.009 

Grid #1 e.tlmaled AlbHtOI 

0.01 

Grid #2 Esllmat..:i Asbestos 

0 .01 

Estlmat..:i Aabo1101 % 

0.01'6 

Anatyat Comment& 

Anaty,,is: 09/0712019, Time; 1hr 10 mins 

F Orientation: 120,230 

AJ peak on lhe chrysolile malrix is lik.,y rom lhe 

Report Comments. 

Post Acid Treatment 0 

Flll«Tare 6.09<l3 

GroH FIil« We lght 6.5285 

0.438 

Final Non-Asbeslos % 

Percent Organ~ s. 0.243 

Percent Acid Solubl<o 11.178 

Percent Other 88,57 

CMltftL<WIQd'I I ..... -L . • 

. • 

0 .22/10000 C~olile . • 

0.2217800 C~olile . • Add Row 
Fiber Count Sheet fo:r Tranismlss!IOn Ellectron Mk ros-oopy )All AMA Analytical Services, Inc. fE.l. Focui.ed On Results. 

Page--1-otL 

Date; Client iD: t)-5'o Filter Size/Type/ Powsltv 47mm MCE-0 .. 22 μrn 

coc tt: 30W:l!'o AMA ,on: So'6CD6-b~ 

Working Mag:_1_5 __ K Actel Voltage:__\DQ__kV Orlent_atlon of Letter F: ~ 

Grid Sox ti: A:\~Lf~~ Grid Acceptable(j; N Volume F,iltened : 0,1 ml 

:'3 Glid:_A}_AJ__ •Grid •Openings to Observe: ,g,o 

~!Cll'ICIIU ID'tf · F11>ar t14g II ~l;O!il-'i!1t f,ilnsnl ~utlnn or 

Mlncr81Typ!! ,.,ir...,-. • ......, \ll'htiM)c",11111-W.t+ Comer~ t1mslh 

w•a•l.:ilf.f O.\odJ nJ (:Mtlt 11411'11:, M ri/llAIOWJ;S 1.\hf'lt 

\ -b \10 ,i. 7 .;j .• K cm 

\.\ \ O,t. 'l,'Z.. K cm 

0.,5 I 12.. 1 o.oL-\ '10 I( an 

\ •O b.o,- \OLJI \0 I( cm ! 

I( cm 

l( cm 

I( cm 

K cm 

I< cm 

K cm 

K cm 

K cm 

K l."tfl 

K cm 

K cm 

K cm 

I< cm 

K cm 

K Cllit 

K cmi 

I< Cllll 

.K Cl'l'l 

I( cm 

K cm 

K cm 

Legend: NSD • Ho Slfuclures-t'letec:ud UTO = Uaobla lo Obhln = l $t <lrld ! - lr,,fGrid 

, ToUI -

Mineral Type: C.~n~,\t. ,: ~ Total ti of Grid Openings Observed: 1o 

Mineral Type: = M ean Grid Opening Are;i: o.oJ~ mml 

Mineral Type: = 

Mineral Type: :: EM Serial#: 

R:1111i1r.r~ ,~ 1,,:\Hlcf Af;11 l01• by O!el ,. 
Edit TEM NOB B~an'k ResuU 

Blank Number 

NBl 9-645 

Ana~yst 

(b) (6 

P,e11ce,nt Asbestos 

0.0 

Asbestos Type 

,, 

Comments 

Save Changes 

ii 
Edit TEM NOB 

1B~an'k Resu!lt 

Blank Number lti4B1'9-646 

Anallyst 

(ti) (6) 

oa,~e Anally.Hd 

109-18-2019 ii 

Percent Asbestos 

0.0 

Asbestos Type 

,, 

Comments 

Save Changes 
Edit TEM NOB B~an'k Result 

Blank Number 

INBl9-647 

.Ana~yst 

[fl) 6 T 

109-18-2,Q 119 ii 

Perrcent Asbestos 

0.0 

Asbestos Type 

,, 

Comments 

Save Changes 
10 

Edit NOB Reference Sample Result 

Sample Number Analytt Retim,nee Sample 

Talc Ref Christopher C .. 

Refer•nc• Value A1be1toa Type 

Chrysotile 

0.0 

,.o 

Vial and Ashed S1.111ple Welgt,t 1.0 

lnltlal Sa,npkl Weight 

Comments 

Save Changes 

Tile fl 

Talc Ref 10% ' 

Lower Limit Upper Limit 

5 25 

,.o Asbesto1 Type Chrysotle y 

Filter-TaN 0.0 Eltlmeted AlbHtOS 100 

Ashed Weight F>erc:ent A1bestos 10 

RHult Pass 
l 

AKA Analytical Services, rnc .. Laborat-0ry Blank Log 

( 

stank ID# Ini t ials 

EB•1⁄2 '1 I 4lf 

L 'ftlJ EB- ) , 

EB- ~ t,{ I H 

it.t l~l. 

EB· 

EB· ~'t If 1 

Prep 

Date 

Chain of 

Custody# 

AMA or Client 

Sa~le Numbers 

Analysis Asbestos 

Date 1Domc .. 

Cl iient )Jame Archive 

Box ff 

EB _5~J6{) 

( E8§ 4/I/ 

Ver:1•3 (4/91) 

lw\ ->i 6n o 1 \:'>~\ et\- ·~ce~ 
EcUt Air Blank Resuh 1Blaf11,k Number 

Analyst 

ll>) < ) ... [Date Analyz,ed 

09-1,8-2019 

AreaAna.lyzed 

0.07 

As be,stos Structut>e!s 

As be·s,tos Type 

... 

R&iSUlt 

< 14 .. 286 

Comments Save Changes 

ii