Document 7RwNQ3BYGz5JpE9wRXNqOa3no

CTPA Eipfee-if J ))( teas*: KMf.ra A S B E S T IF O R M M iN S R A L S IH C O S M E T IC T A L C S; X - r s y D i t e t i P f i SS; O p tfe i S S Ic m e c e p y a n d D ia p f8 ie n ~ S e in iR 3 M a4hod friiro d u c iio rti Th method which hsa M ort adopted for th* detection ol amphibsla rolnaraia tft cosmetic tale is tt* gerairaSy accepted method s? -ray diffraction. Methods which appeau ih tha irisraturs for tw deiaclbr cf Shies amphiboie, eh 68. transmission electron microscopy with selected area ttifftocffen* and electron mfdfoprofae,* hare ateo bs-en considered sirws ih.e gre capable uf 3 ower iovet of deiaction than by s-ray diffrsctSon. Mowevrsf, they t a s rwjt fwrar. '-y'*-':'?'-:'-'. girrce "h-y s tiff from the drawbacks, that the ambisrS of msfsrisi under sxarrJnaSsn s quo sms ftess than a mteitsgran*) m i the urne Sor analysis, expertise raqufrsct, arti! expense a? aqulpmsnt eliminates thorn a s ro u te a melhsds. Tbs m e ifirx to io ify presented Is the rrtest practical available, based on current teehnofogy.. The use qS Trarrwnliisiort Electron Microscopy with Seiiteted Area B s d ra n Diffraction offers g ra s senstlvay, tart is not presented since S is unauftabfa for marmai quality contro! s p p S w to t, Enrichm ent e>r concentration techniques using testation cells have been tiled as a means bf improving tbs detecen Ssvsi; how ever. all efforts se far Hava been unsuccessful. P rincipi ITi-s x-ray diffraction meiftod is based upon She principia that when a crystaBrw material is pfstwd in an x-ray boar?;, a portion of the x-rays are RttraetM by each set o f rito,mie ptenaa within the trysts;. The diffracted tays strike a scintiiiaficm ju n ts r as the- samp; is scannaci through a prescribed fingi with the respiting {tevsSopmant of peaks corresponding to each infarpiartar distene (d). A peak wft d value in the fangs at 8.00 to 8.8SA ' for a * sam ple sale is strong evident for the presses of am phibole in that Sale, The lave! 0? detection oC amphibole by ibis m ethod is 0.5% and ste v e . The venaiSy of detection is caused by such factors as sge and manufacturer of x-ray diffractom eters, sample homogeneity, specific am phibole minorai press}, m orphology of erriphlbbls, pastiofe six, preferred orientsiion. fife. For these reasons the level of detection should be reported for terete abac's ius% , s in t below m is Isvei ttw data has been found to be not repredudlifo. If a saHstticaiiy signffiC8rt peak found of Intensity q uel to or greater than that obtained for the 0.5% standard in rha cl range for amphibole, described above, then the ssm p te musi be put through the foltewing confirm ing schema: X-ray Didractom etry (-> U - (Acid Leach) Opticai MkKosaspy and Dispersion-Staining Coior (...) stop (ArrifthiDofo Stop (A m phibols absent.) (+ ) (- i Fibrous Morphology Sto p (As bestifc ms Amp tribale aba vnS i +> Slop (Asbestiorm Arnphtboia present) TS bs ( C :; : % ..... <!..;'}..... C JA ; X IV.-s srav;:-.- PLAIMTIFFS EXHIBIT WCD-108 CPC-BCALTRSCPT00000722 C T A W aites j P a r t I; m p h ib o te f iiln e r s is toy X -ra y D if f e m t o m a t r y A p p a ra tu s 1. X-ray diffractometer, em ploying nickel-filtered oopper K-aiptw rediatiOT, herteontaj or vertfcet gontoraetei with vaiiabte scam speed capability, suitable tats psliet sample hokisir, vsrsaM aps-ari fs o a rte tr ei-sctroaie pane! in d u in g re te m a te t and variable a ite n u a fla i andtim eoanstant setflnga 2. Hydraulic press, cap able o f attaining a pressure of i 5,008 to 25,000 its calculated on 8 3 " rare 3. Mortar and pestle or grin ding m ill (Mote 1;< 4. W aring Stendor,* erequtvatera slender 5. Spex Mixsr/Miil," or actufvalei*m eedariiiai m ix * 3. Sieve, 325-mash 7. Optical microscope (Mots 2) 8 . 1 Vs' paitet press R e a g e n ts i . Standard talc sam ple, containing no dstactabie amphibole mlnersfa ?.. standard tremoSte sam ple, a t least 80% pore Sample of tremotite standard may bs obtained by ortianrtg tram t h e C osm etic Toiletry and Ftagrane Assocfebon, Inc., U S O fifte e m b Street, N.W., W ashington, D,,C. 20005. 3. Denatured ethanol 4. Bone add The procedure consists of stow-ecannlrtg, under previously {tetenwned cowSfions, a com pressed pellet of the sample tare in Bis 11.3 to 1Q.O<5 (S-SS to 8.04 A) region tor me presence of an amphibole peak. Theta araSroas w hen ttisdKBculrto dtealrrrsaie a possible peak ?ot amphibole ove r the background no ise ievel. ,` F:5s^i.L:k'i-c TiriO-o-irio./'k rrtc ; ',1T A i - ' r V x . r \ r r - < :x . x - r - r - *.s-l .. x - . * s* . r- r CPC-BCALTRSCPT00000723  T F A Hrfeithad ,j 4.3 Ktj','3; 10-T-T S.3 Should tha.presence of a smsi* am phiboie peak above the background "noto* be in question, if wiif be necessary to statistically evaluate the scar*.. A tim ar/scalar Is roeutred on the electronic parrai of the -ray difiractcmelar. In order for a peak to Be s t a t ic a lly significant, the peak intensity must equal or exceed thrae standard deviations (3or) above the average background intensity (N); Where: N + 3n- = m inim um peak Intensity K - average background count a- -- V kF D eterm ine the region of the scan in question: in the Figure 1 seen, a peak appears to be present it? the 10.40 tu 10.50 2Sregion. S low scan with cumulative pu lse counting through the peak region three separate times and average the number of counts, D eterm ine a background count By scanning a region equal to 14 of Ihg ZB region covered by the peak, immediatsty before and after the peak. The counting time for each o f those background regions will equal Vh the total counting tim e used tor the peak. Court! each background region three times. Then average each region and add the too averages to obtain ihe background count (NJ. n7 r*:r. -. -i. t - ,, v u' - n r 'Anne CPC-BCALTRSCPT00000724 Exampi; jh Figur 1, Peak ...................... ............ Background ReqianA ........... . . . . . . . Region B . . . ___ ............ Region (*2 $ 10.40 to 10.80 10730 to 10,40 10.80 to 10,70 7iHt9 (&0.) 120 3300 ?0.40 tFoo1a0k.SO "2 3 07ns secs, courts 120 120 120 Average 80.332 59,370 SCMiB 00,102 Bckgrc und l 1i m0.aJORs seteogsi,?e0n.c4Ao0u`r2t s0 H10,'.m6R0seatcogsiJ.oOn.c7Bo0u"n2t0s 80 28,784 SO 2 8 ,9 SO 28,934 06,767 SO 26,30 SO 26,308 0 23,204 20,339 M= a- 3d- " 25\ '78W,,17.4T86i7l S42=87,12373599= 57,146 3cr = 717 S7.6S3 r ha estuai norobsf Cunf obtained for the iniagfted pa&k intensity v/as 60,102; the/sfora, ths "suspect" peak is statsScaiy praserri in fts sc&n. 1&-7-TS Pep < I rn r u ir r m v , v n ct? i r s n 'rT c c A rn T tn y iMr* . h t * hGirP+f M V W'.cMftMm-* n r ?rt(WW CPC-BCALTRSCPT00000725 CTFA M athsd J4-1 HW-iC P6JS-J S tandard preparation Optimal insiru m en t o m kM ors m ust first as datam ined with ths use of iremoflte ' standards; 1.0%, 0.75%, 0.5% tte m oilta ay weight, prepared in a standard talc which is free o f interfering peaks in id 11.Oto1Q.O5?0regk>rt. W eigh out appropriate am ounts of standard tala and tra m olte both of which have been ground to pass a 325-mash sieve. Transfer to a Waring B lender." Add 100 mi o f ethanol to the blander and blend s i low speed for 5 minutes. CarsfuSy transfer ate contents ot the Slender, w ith repeated ethanol w ashings, into a large beaker, Evaporate tt ethanol on a steam bath. S hake the sample in a plastic via! for 5 minutes on a S pex M txe riM tr to rem ove d um ps and caked sample resulting from tha evaporation of eth a n o l D eterm ine by microscopy th e homogeneity of the preps red standard previous to the x-ray diffraction analysis, P ress ths nomogsrisous standard ?mc: a 1V pallet w ith a backing of boric a d d . Transfer 2 ( 0 .2 ) g o f standard to the die-holder and evenly distrib ute on n pofshed. soratrih-free dia. D istribute 4 {* 0 .2 ) g at boric actrf e v s n iy o n ife ta lc layer. Press the mixture into a pellet under conditions sultabisfor obtaining a smooth planer surface (for exempts., a pressure c f 15,000 la 24.000 It; calculated on & 3 ' ram has bean found to produce suitable psflote). Ths mauling p a lle t must have s tale face w hich is fraa of flaws; if n o t. tha pell at meat be discordad (Mote 3). Prepare two aoceptahfe pallets from each standard. fieglESinoa TradsmaA -'r- . ................................. . v mi n r T>fif*riT< CPC-BCALTRSCPT00000726 CTFAftathe J W iRa-sd- W-?-W S&mpkJ FroprsJoft P repare two pateta Som each aampte in the m a nner described ter th e andate pa#. Wait a quafflave s c a n ' fro m 4 to SO "26 or or o f these pallet* to assertasrt the presence o f ampWboht shave the 2% lavai or the presane of miriftrsilfnpuri'Jse h a v in g ntffssrg peaks n tita 15,0 So 0.0*28(8 .65 to 8.04) regan of the seen.The p re s a n o such intstftrence w * Sminate vs* o? Use x-ray diffraction method fo r the sample, find o n e will have la proceed directly to (he mioroseoptcal procedure. fo s te r mentation Of k* ..Tstivfts f-1% standard. standardsinstrumental variables aro optim izad on the determineanalysed under the optimum conditions to Lower are then 8 tower level of detection. dabrpoesnpedmtreceoaotmpejmorceirbtataetiinmber eliesnpdpsoaewtbrrauitotrahmiv*eaceonbsmttaaacbtloiktciebngoSetrnacoddaiunBiwntiinydoitganhncsotcnctieoahsmpxeeftcpapansaebutalsierkbhollooie^mwbsretniearccuiirnosorennFdesfigattrauuirtnrrsettploee2n.e0d!.h5, e%arnostittaaahrmnsigdeahatersdarl.tostUwhnnouduaeld-r Typical instrumentai conditions employt: tor the Siemens D iffractom eter {Model No. M38S-X-A4), and Counter and Recorder Und (Type T) ara; Radiation; Divergence ad: Goniometer speed: Rscerdar Attenuation: Timo constant: Cu with K Ber at 40 KV and 24 ma T* Rscaiving sili; O 2 man ' /w*2GWnute 300 mnv'hcurr 4f x 10 impufseofeacond T (a) Statistical te r o 1, 1 % under these conditions Risa Time = 0,18 Attenuator -- 20 t n t i r r o v u t > C T r . v * w r c c o m T fn V INC 1 13J Frftosn'h Street. N.W ,, WaPtiecn. 8.C. 20005 CPC-BCALTRSCPT00000727 .5% Trem okf in Ja k ; C TFA SSsfliotf J M to a lo-y-T Psijsr 6,5 uw .: ;c> Figura 2 Kftey D iffra ction Seans Place i# standard or sam ple peRet in a suitable holder and slow ly scan between 11.0 and 10.iP The roate the pelisi 30 with re spect to Ss origina: position in the goniometer a rid rascan between 11.0 and 1C.D"2fl since pallet tentation m ay affect peak Intensity, I t prase*!? of a reproducs! peak (or pesies; is due to Ilia presence of amphibole minara! (or minerete); the absence o peaks in this re gion Iraacetes the absence of emphteote in the sample, within the Srnrt o f de te ctio n Site technics,. ' Report results as ' Mone detected* or as " Detected at approxim ately X % lavai,* when ''X " squats the aval detected. . \-r-N r-r, , , s,r r , I t TI;V.' iV ,- ! t 31 ^ , ,, ^ 1 , C u ,.. \IV / !nJ* rr,r. D f CPC-BCALTRSCPT00000728 C F & PjtSisa ) A tens* i-SS s, Part U; AMaibcrsostsiciooprmy sAnmd pDhiaibjsostresiSoSisIr-SnstraailnsirfetyijO ppili Apparatus 1. Polarising microscope. Best results wiS be obtained if tfte Instalment Includes ihs following: a. IncSviiiijflSy seirisring objectives eb.. HBeigrStrvainntdsraasnBay Ughi sounca . d. C sntsnng condenser/substage Z O ispersion-staW t^davis (Mets 4) 3. Vacuum filtration equipment, irtoiuding situar a poreeimri cone wiifr glass fiber nisrinatoraporausglaasbofioiT i cup R s a g s iriti t , Hydrochloric acid, 10% / 2, Carpe immersion fcfufei Series HO, njf ~ 1.605 (Nota S) Procedura . Acid Traatm ant Because of ib a inte ra ronce usad by sorna eattorratos jet.j. paierie} in to detec tion o asostiiorm ampniDoles n talc by optical Bsispy/diS|>fSio.`VStairt!g. il is necessary to lest remove these carbonates by a ample acid leach ing procedure: CPC-BCALTRSCPT00000729 . C T F ft tttothod <1 M taw*: 10-7-7?; - fao 9 W eigh o u t2 9 of the tafc into a 10*3 ml beaker. A dd 25 mi of 10% v/v H C i siowty {toprevent excessive evolution of gas if carbonates are p re s a ri) and heat, with occa sio nal stimng on a steam bath for 33 minutes. Fifis! with vacuum StraSen equipment, and w a sh severs! times with hot wafer. Dry the tele. O ptical M icroscopy and Dlapersloes-Stafirlrfg Carefully disperse 0. T mg of talc in on drop of Cargills HD liquid, r i j f = t .605, and ccver with a ctoon oavar stiff. Examfete the sample in the dl.spsrsion-sfaining central stop mode. The substaga diaphragm sho uld bs almost com pieteiy dosed, Sis field diaphragm may be o a rtta ly Ctosed to e nhance color contras?,' and irre p d riz a i shout b s in posilion. T w tn oliis, acBncNte and presutnebiy o t iw amphrboi rrtirwrafs, rid e r th.es ccmcSittans, wf show tha foifowirtg flspersion-stelntng octets: y s ljw changing Set blue w ith rotation of the sam ple ratativa to the polarizer o r y e lo w changing to orange with rotation The variation of tha color chartga is due to the fact that the trsm oiiie may lie in one of two p o sitkw s relative ta its principal optical oteirtaHon. Examina tha sam pte f r esbeallform fib ro u s am phlbole m inerale. ln order for an am ptiiboia minarai to be eoosicereo asbestiferm S tra u s s must meet ihe foliow ing OSHA dafinraon (to te re r 4), 1. P a ifid o s must appeas to be fibroua rafhur than ast wystas or siivors, 2. The micrimurn Cllamafar o? a fsbsr 10 ba countad in 3 rmorotts. 3. Th m axirnum langih of a ber to b oounted i* 30 nterone. 4. The length to wklth Bo muss be 5 or rposa to 1, that s, 5 firnes or m o w Nxtger tha n wts. 5. Tita separate or inriivsdua fite m inustficntairitbrils o rth e lK J rtd te o l s t e t e ' e fe e t, nniass tiw y ars a a r.ar.divisibia stage, A firil Cannes b subdividd and w ette: b s cuniad, S m e sis ih e oth e ro ite rla . Ths iength to width ratio o f 5 o r m ors io i is not m osnt to Impty tnst h e r partsciss are not hazardaus. >fkrtf\ C CPC-BCALTRSCPT00000730 GTPA J 44 teiius: 0-7-78 Page 10 i \ p o rt results ss "Asbestiform Amphibole P re s s n f or as " Asbostiform Amphibole A bsent." It Is imperative that both dispersion-staining colorane ! fibrous morphology criteria be satisfied before stfBntjfying a partiofe as asbeatiform am phiioie, since other sub stances may show colors imiter to trios de served . Motes 1, Taies to be- erwsyziKf a rri the-tfcirioliie ysed io preparo standard samples must fcs t o r than 323 mesh J.-nixi- Tekmar Companymum p a rtid e e-ize of 44microns). Trie Tekmar Aniytteal MSI (Moda! A-1) is recommended, ft Ssvelatolafrom: P.O. Box 3 7 ? Cincinnai!, Ghia 45222 . SI is im po rtan t that the homogeneity of the prepared talc-trem cliie standard sam ples b verified by optical m ic ro s c o p y , 3, This requirem ent is criticai sir.ca excessive surface scattar wil! cause abnorm ally high background counts. 4, The o n ly oo*neciaHy available dispersion-staining device is sold by. W alter C .M cC rc ne Associates, ine, 2820 South Michigan Avenu Chicago, finnois 60Q16 5, A vailable from : " -- or from laboratory suppliers. R. P. Cargrlie Laboratories. ine, C ariar Grava, New Jersey 07003 Hefarenees t . Rotti, A. 14, Iftnger, A M ., Environmental manti Perspectives 3 ,95(1974) Z. Rubin, !. 8 ., Maggiore, C. J., P rivitonm anlai Health P e rsp e ctive s8, a t [1974} 3. L S. Bints, X-Ray Spectrochsmica! Analysis, pages S4--55. intarsdenca P ublishers (1S5S) 4. 'T r e m o li and Talc." U.S. D epartment of Labor,Occupational Safety and Health Adm M stm lisn, Field Informa tion M em orandum #74-82, N ovem ber 2 1 ,1S74, COSMETIC. TO ILETRY AMD FRAGRANCE ASSOCfATtON. INC. 1133 Fifteenth Street. N.W., tahfogton. D.C. 30005 CPC-BCALTRSCPT00000731