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IN TADLECTEBRYMLINIGAHTTIO-ONPOTFICAASLBMESITCORSOSCOPY for WShoitutathkePrl,aiCnlfaierlkd,k NDewanJieelrss,eyInc. November 20, 1973 Report No. 1621 PLAINTIFFS EXHIBIT WCD-204 ER K EST.F, FXJk&AM -' X ` SmcCieOntRifiPcOCHoJnsLulTtaKnDts P.O. BOX 444 . 5CHCNECTAOY, N. Y, IS30I For: NPSWoaohugviteethtmaOPkbnleeaerri,n2fCi0e,lladr1,k97N&3ewDaJneireslse,y Inc, IN TADLECTBEYRMLIINGAHTTI-OONPTOIFCAALSBMEISCTROOSSCOPY Six sam ples of talc were received for analysis on October 29, 1973 as follows: : .. WH-009 WWHH--001205 WH-033 WWHH--003773 Information requested by the customer included the number of chrysotile and amphibole-type asbestos particles in each m illigram of talc. Samples were to be analyzed according to the method described on page 27080 of the "Federal Register, " Vol, 38, No. 188, Friday, September 28, 1973, One m illigram of sample was weighed out onto each of two m icroscope slides. To one slide was added 3 drops of 1.574 refractive index liquid; to the other, the same amount of a 1. 590 refractive index liquid. This procedure was repeated for all six sam ples. P articles were dispersed in the oil with the aid of a needle, capped with a 18 mm square cover gla ss, and the resulting mounts examined by phase-contrast m icroscopy at a total magnification of 430 diameters . Grossed polare were utilized as required to determine the Optical orientation and extinction characteristics of specific fibers. Report No. 1621 LoGiudice/WCD/0173 E R N E S T P, F U L L A M SmcCieOnRtiFfiOcfCtoAT.uTidltaunti P.O, BOX 4 4 4 fiCKENtCTAOY, , Y, 1 2 3 0 ! Whittaker, Clark Et D aniels, Inc. NPSoaougvteehmTPbwleaorin2fi0e,ld1,97N3ew Jersey. When the number of asbestos fibers reached 150 per m illigram , the count was stopped at a suitable location on the slide and the total number of asbestos fibers calculated from the total area of the slide divided by the area actually counted, . RESULTS AND CONCLUSIONS Particle count data are tabulated as follows: Sample No, C hrypsoertilme gf.ibers A m ppheirb omleg , WWHH--001009 WWWWHHHH----000073323375 1 ,345500 6, 075 6, 600705 5, 200 2221091388,,,,,,208228550522000505 . There are perhaps an equal number of particles in each sample which escape detection since they fall below the 3;1 aspect ratio required for positive identification. '6 jr 4/ Sfass. ^ 'l^ L O S 1/ % o ,/y 0, ( i 0, 07 0, to 9.S % ERNEST F . FULLAM, INC. R*ichard E . Stevens $o y / P-Zg- 1 *'3* i/ ? ? Report No. 1621 LoGiudice/WCD/0174 V REPORT OP CTFA. TALC SUBCOMMITTEE pN METHOD TO DETECT CHRYSOTILE AND TREMOLITE IN TALC. ' . ' December 10, 1973 The Scientific Advisory Committee of the Cosmetic, Toiletry & Fragrance Association, 1625 Eye Street, N.W., Washington, D.C. 20006 at a meeting held on September 2, 1973, designated that a subcommittee be set up to study the optical microscopic method proposed by the Food and Drug Administration. This method was published in the Federal Register of September 28, 1973. The present membership of the CTFA Talc Subcommittee is shown on an.attached sheet. ^ At the first meeting of the Subcommittee, it was agreed to.submit several samples of talc to members who volunteered to apply the FDA proposed optical microscopic method. The following talc samples were distributed without identification - except for randomly applied and ,non-duplicated code numbers: - Italian Talc Montana Talc Moptana Talc Source I Vermont Talc Source II . Alabama Talc No, Cai*rolina Talc . " and "(IT,nT5a%ddtir teimoonl,Ttea wsaamsp'lseentoftoI.teaalcihanpaTratliccisppainkte.d w/w with 1% chrysotile "The participants' were aware that the sample was spiked, but did not know the percentage of spiking. The attached table summarizes all reports submitted: Final Report LoGiudice/WCD/0175 Sample Spiked Italian Montana- I Alabama Vermont No.Carolina Montana- n No.`of Fibers ' No. of Fibers With R.I. Greater With R.I. Less Than 1590 Than 1574 Status With Regard to Proposed FDA Method Mrs. Lucy MeCrone, McCrone Associates for Chesebrough 320 120 0 0 0 0 *0 16 0 0 0 0 o: 0 * Passes Passes Passes Passes Passes Passes Passes Mr. Harold Stanley of Pfizer Italian Montana- I Montana- II,, Alabama Vermont No, Carolina Spiked ^ 100 -- 100 <~ioo ~ioo zw* 100 o. 100 <1000 >100 >100 >100 >100 >100 >100 >100 Fails Chrysotile Passes tremolite Fails Chrysotile Passes tremolite Falls Chrysotile Passes tremolite Fails Chrysotile Passes tremolite Fails Chrysotile Passes tremolite Fails Chrysotile Passes tremolite Fails Chrysotile Passes tremolite Mr. David Hamer of Johnson & Johnson Italian Montana- I Montana- II Alabama Vermont No. Carolina 0 1' 25 0 0 0 0 0 0 0 0 0 Passes Passes Passes passes Passes Passes Spiked Italian ;r Dr. John A. Reffner (U. of Conn.) for Avon 632 12,930 * " 220 1,114 Fails Chrysotile Passes Tremolite /-f^ils Chrysotile 5 Passes Tremolite LoGiudice/WCD/0176 -3- Sample, No. of Fibers ,No. of Fibers With R.I. Greater With R.I. Less ' Than 1590 . Than 1574 Status With Regard to Proposed FDA Method Dr. John A. Refiner (U. of Conn.) for Avon Cont'd Montana*-! Montana-11 Alabama Vermont No. Carolina 0 ' 13 26 41 14 * 5,844 9,281 15,125 165 . 11,852 Fails chrysbtile .Passes tremolite Fails chrysotile Passes tremolite Fails chrysotile Passes tremolite Fails chrysotile Passes tremolite Fails chrysotile* Passes,tremolite Dr. Tryggve Baak of United Sierra Spiked Italian Montanari Montana-11 Alabama Vermont a1 No. Carolina 3,000 1,000 0 0 0 0* 500 . 2,000 0 0 0 0 0 Fails Passes Passes Passes Passes Passes Passes Richard E. Stevens of Ernest F. Fullatn, In.c. for Whittaker C&D Italian Montana-I Montana-H Alabama Vermont No. Carolina 8,250 18,000 29,250 21,825 3,225 20,850 1,350 450 5,200 6,075 675 6,000 Fails chrysotile & :remolite Fails chrysotile & tremolite Fails .chrysotile & tremolite Fails chrysotile & tremolite Fails chrysotile & :remolita 'Fails chrysotile & xemolite Spiked sample was not run. 5* LoGiudice/WCD/0177 -4 Samfple No. of Fibers No. of Fibers' With R.I. Greater With R.I, Less Than- 1590 Than 1574 . Status With' Regard to. Pro posed FDA-Method Mrs. Lucy McCrone of McCrone Associates for Kolmar Italian Montana-1 Montana-H Alabama Vermont *No, Carolina Spiked Sample 53 0 0 0 0 0 488 0 0. 0 0 0 0 -16 Passes Passes Passes Passes Passes Passes `Passes 0 *Sample noted to contain some fiber bundles which are rolled up talc plus some non-fibrous tremollta The following participants examined their samples but were unable donscientiously to count particles with confidence, therefore, did not report numbers? Miss Marie Jones for Dr, G. Cohen - Bristol-Myers Products Research Labs. Mr. Salvatore DiBinca ~ The Mennen Company Liberty Mutual Insurance Co,, Research Center - for Kolmar Laboratories Mr. John Facq - The Colgate Palmolive Company, Research Center The table reveals strong inconsistency between results obtained by the different scientists applying the method to the same group of.coded talc samples. This Inconsistency is the result of problems encountered in the methodology. 1. The alph i refractive index of talc - one of the two indices exhibite l by talc plates standing on edge - varies in value between 1.539 and 1.550^. This in combination with item 2, below, m y easily result in the mls-cla'ssiflcation of such plates a;,` "fibrous, less than 1.574" and therefore chrysotile. Dr. Reffner of the University of Connecticut, in his report to Avon, admitb that this factor is paramount - "counts for chrysotile are high since (talc) edges will often be mistaken for fibrous particles',!. : "2. The immersion method for the determination of-relative refractive index becomes unreliable when applied to extremely small (ca, 1 pm)particle's. This is due in .part to the- fact that particles around 1 in width approach the limit of resolution of the human eye when both size and contrast are considered, especially when applying the Becke line technique prescribed. This will LoGiudice/WCD/0178 5- 2. cause eye.fatigu and resulting errors. Thus, a fine talc shard or plate on edge may be easily mistaken for an asbestos fiber. This applies to both'the chrysotile and amphibole . portions of the test, 3. It is quite likely that chlorite ~ a mineral of varied compo sition -commonly found in pharmaceutical grade talc - would be Incorrectly identified as tremolite. Refractive indices ` for chlorite vary in the range 1.57-1.66^. 4. The examination of a sample of one milligram dispersed on a single microscope slide presents the investigator with a preparation which is too dense for a petrographic study. 5. The method is laborious and time consuming. Dr. Ueffner quotes an analysis time of about five hours per sample and at JOHNSON & JOHNSON the investigator (D. H. Hamer) estimated at least two or three hours. f . * ` 6. Dr. Walter C.' McCrone in an earlier letter to the FDA suggested that there were relatively few scientists in the country who could use the method effectively. Scientists at Bristol-Myers, The. Mennen Company,.Liberty Mutual and Colgate-Palmolive had . great difficulty in following the method to conclusion. 7. The proposed FDA method implies that all fibrous particles in talc having optical properties similar to those of asbestos minerals are in fact asbestos. This is probably an unwarranted assumption. REFERENCES: 1. Deer, W.A., Howie, R.A,, and Zussman, J,, Rock-Forming Minerals, Vol. 3, p. 121 (1962). 2. ibid, p. 131, ***************** We have concluded that the method published in the Federal Register does not provide a truly reliable means for the detection of asbestos in talc. It results in both false-positive and false-negative findings. It is also tedious and may consume as much as one half day per sample, "The Subcommittee urges that the Food and Drug Administration defer finalizing the proposed optical microscopic method and proceed into a Phase. II program which would combine FDA and Industry in a strong effort to develop a truly reliable method for measuring chrysotile content in talc. We are confident that the detection and estimation of fibrous tremolite can also be done, if necessary, as a fringe benefit, at the same time. LoGiudice/WCD/0179 -6- . We estimate that a'satisfactory method will take at least six .months to a year to develop. We suggest a close liaison between FDA and industry in this all-out effort with updating reviews to take place as frequently as necessary. ' Review of Alternate Methods The CTFA Talc Subcommittee has reviewed several methods to detect chrysotile and treraolite in'talc, including modifications of the optical, microscopic method. These are. listed with comments.' . 1. Optical Microscopic Method ~ may be used.with some modification. Possibly better selection of R.l. liquids and reduction of sample size per slide. 2. X-ray Step Scanning - A good method for detecting tremolite if we could accept about 0.2% as the threshold of detection. It does not distinguish fibrous from non-fibrous tremolite. The simultaneous detection of chlorite makes method impractical for chrysotile. 3 X-Ray Step Scanning + Optical Microscopy - Acceptable as in if2 above but the optical method continues to present the dilemma in reliable identification of chrysotile. However, this does not rule out a major revision of the optical method to do the chrysotile identification and counting, a*' 4. X-Ray Scanning - The problem of chlorite interference in the detection of chrysotile is present in all x-ray procedures' thus far' available. It is reliable for the detection of 1% tremolite (both fibrous and non-fibrous). 5. Differential Thermal Analysis - This procedure is capable of detecting chrysotile at the 1% level, however, it will not detect'tremolite, ' 6* Scanning ElactronMicroscony - This procedure is not capable of identi fying asbestos. Even with energy dispersive analysis, completely satisfactory identification is not possible. 7. Transmission Electron Microscopy + Electron Diffraction - This appears to offer the best, most reliable method and is probably > capable of detecting-chrysotile and tremolite (fibrous), both at a level of 0,1%. It is estimated that an installation would cost about $130M +, and Is obviously prohibitive for the small manufacturer who uses talc. The amount of talc sample examined by this procedure is miniscule. ( LoGiudice/WCD/0180 -7- Smnmary .*The CTFA Talc'Subcommittee has completed its review of the Optical Microscopic Method for the Estimation of Chrysotlle and Fibrous Tremolite in' Talc, which appeared in the Federal Register, vol. 38 (No. 188),(p. 27076, September. 28, 1973). It recommends postponement of the finalization of btehtewepernopFosDeAd&reignudluasttiryon on talc. to resolve In addition, a a satisfactory collaborative effort method of estimating chrysotlle and treinolite in talc, is recommended, with periodic liaison reviews to monitor the project status. A task force of industry experts has been designated to pursue alternate methods. We Invite FpA. to participate in collaboration with the task force. George^W. Sandland Chairman CTFA Talc Subcommittee GWS:dd LoGiudice/WCD/0181 MEMBERSHIP L I S T C T F A TALC SUBCOMMITTEE G, W, Sandland, Chairman (SAC) 1 Bristol-Myers Products Dr. Murray Berdick (SAC) Chesebrough-Ponds, Inc. Dr. George Cohen Bristol-Myers Products Dr. Christopher Costello (SAC) Colgate-Palmolive Company Mr. Salvatore DiBiahca The Mennen Company Mr, John Facq Colgate-Palmolive Company Mr. David Hamer Johnson &.Johnson Research Center Mr. Alan M. Harvey R. T. Vanderbilt, Inc. Mr. Ray R. Kratunes Whittaker, Clark and Daniels Mr,' Adolph Maruszewskl- (SAC) Kolmar Laboratories, Inc. Mr. Louis D. Murino United Sierra Dr, DeWitt Petterson Johnson & Johnson Research Center Dr. Robert Rolle Johnson & Johnson Research Center Mr. Fred Roesch Whittaker, Clark and Daniels Dr. Charles Rowland Avon Products, Inc. (SAC) Dr. Harold Schwartz (SAC) The Mennen Company Dr. Joseph Simko Colgate-Palmolive Company Mr. Harold D. Stanley, Jr. Pfizer Mr.- Wallace Steinberg Johnson & Johnson (SAC) Dr. John Travers Avon Products, Inc. Dr. C. S. Thompson R. T. Vanderbilt, Inc. Mr, Ronald Yalcupcin Kolmar Laboratories Dr, Tryggve Baak United Sierra December 11, 197B LoGiudice/WCD/0182