Document r6d8dNgjJ1EBoV7LXRmo4v6ME

FILE NAME: CTFA (CTFA) DATE: 1973 Dec 10 DOC#: CTFA019 DOCUMENT DESCRIPTION: Unpublished Report to FDA e f'ffi December 10, 1973 TO: MEMBERS OR THE CTFA TALC SUBCOMMITTEE & SCIENTIFIC ADVISORY COMMITTEE; ~7kj b ^ c tjC s fia jji& A .' Attached herewith and submitted for your reading and comments ia a finalized submission of the report of the CTFA Talc Subcommittee which we wish to submit to the Food 6 Drug Administration. Please read at once and,'likewise, call me at once if you disagree with any of the content matter. In view of the very short time left to process this submission, your immediate attention is of paramount importance. Thank you, Chairman Cl FA Talc Subcommittee Goodhue WCD 000123 REPORT OF CTFA TALC SUBCOMMITTEE ON METHOD TO DETECT CHRYSOTILE AND TREMOLITE IN TALC. December 10, 1973 The Scientific Advisory Committee of the Cosmeti^, Toiletry & Fragrance Association, 1625 Eye Sttreet, 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 toy 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 Montana Talc Vermont Talc Alabama Talc No, Carolina Grade #1615 Source p Source F Grade #66 Talc Grade 643 In addition, a sample of Italian Talc spiked w/w with 1% chrysotile and 0.15% tremolite was sent to each participant. The participants were aware that the sample was spiked, but did not know the percentage of spiking. The attached table summarizes all reports submitted: Goodhue WCD 000124 -2- Sample No. of Fibers With R.I. Greater Than 1590 No. of Fibers With R.I. Less Than 1574 Status With Regard to Pro posed FDA Method 1 Mrs. Lucy McCrone, McCrone Associates for Chesebrough Spiked 320 Italian 120 Mntana-Pfizer ! 0 Alabama 0 Vermont 0 No. Carolina' 0 Montana-Ferry 0 16 Paises 0 Passes 0 Passes 0 Passes 0 Passes 0 Pa.sses. 0 Passes Mr. Harold Stanley of Pfizer Italian - /* 100 Montana-Pfizer 100 Montana-Ferry ,100 Alabama Vermont No. Carolina -100 *** 100 100 >100 >100 >100 >100 >100 >100 Fails Chrysotile Passes tremolite Fails Chrysotile Passes tremolite Fails Chrysotile Passes tremolite Fails Chrysotile Passes tremolite Fails Chrysotile Passes tremolite Fails Chrysotile Passes tremolite M r . David Hamer of Johnson & Johnson Italian 0 0 Montana-Pfizer 1 0 Montana-Ferry 25 0 Alabama 0 0 Vermont 0 0 No. Carolina 0 0 Passes Passes Passes Passes Passes Passes Spiked Italian Dr. John A. Reffner (X). of Conn,) for Avon 632 12,-930 Falls Chrysotile Passes Tremolite 220 1,114' 'Fails Chrysotile Passes Tremolite GoodhueWCD 000125 -3- Sample , No. of Fibers With R.I. Greater Than 1590 No. of Fibers With R.I, Less Than 1574 Status With Regard to FrOposed FDA Method Dr. John A. Reffner (1?, of Conn.) for Avon Cont'd Montana-Pfizer Montana-Ferry Alabama Vermont No. Carolina 0 13 26 1 41 14 5,844 9,281 15,125 165 11,852 Fails chrysotile Passes tremolite Fails chrysotile Passes tremolite Fails chrysotile Passes tremolite Fails chrysotile Passes tremolite Fails chrysotile Passes tremolite Dr. Tryfigve Baak of United Sierra Spiked Italian Montana-Pfizer Montana-Ferry Alabama Vermont No. Carolina 3,000 1*000 0 0 0 0 500 2,000 0 0 0 0 0 0 Fails Passes Passes Passes Passes Passes Passes Richard E. Stevens of Ernest F. Fullam, Inc. for Whittaker.C&D Italian Montana-Pfizer Montana-Ferry 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 Fails chrysotile chrysotile & & tremolite tremolite Fails chrysotile & tremolite Fails Fails chrysotile chrysotile & 6 tremolite tremolite Fails chrysotile & tremolite Spiked sample was not run. Goodhue WCD 000126 ..-4 - .Sample No. of-Fibers With R.I. Greater Than 1590 No. of Fibers With R.I. Less Than 1574 Status With Regard to Proposed FDA Method Mrs. Lucy McCrone of McCrone Associates; for Kolmar Italian 53 0 : Passes ' Montana-Pflzer 0 0 Passes ; Montana-Ferry Alabama Vermont 0 i o ! 0 1 0 , o 1 0 1 Passes Passes Passes *No. Carolina 0 0 Passes Spiked Sample 488 16 Passes *Sample noted to contain some fiber bundles which are rolled up talc plus some non-fibrous tremolite The following participants examined their samples but were unable conscientously-to count particles with-confidence, therefore, did not report numbers : Miss Marie Jones for Dr. G. Cohen - Bristol-Myers Products Research Labs. Mr. Salvatore DiBianca - The Mcnnen 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 alpha refractive index of talc - one of the two indices exhibited by talc plates standing on <dge - varies in value between 1.539 and 1.5501. This in combination with item 2, below, may easily result in the mis-ciassification of such plates as "fibrous, less than 1.574"'end therefore chrysotile. Dr. Refiner of the University of Connecticut, in his report to Avon, admits 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)particles. This is due in part to the fact that particles around 1J W in width approach the limi t of resolution of the human eye- when both size and contrast are considered, especially when applying the Becka line technique prescribed. This will Goodhue WCD 000127 -5- 2. cause eye fatigue'and resulting errors. Thus, a fine talc shard or plate on edge may he easily mistaken for an asbestos fiber. This applies to both the chrysotile and amphibole portions of the test. 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^. 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. D r , Refiner quotes an analysis time of about five hours per sample and at JOHNSON JOHNSON the investigator (D. H. Hamer) estimated at leas t two or three hours.' 6. Dr. Walter C. McCrone in an earlier letter to the EDA suggested that there were relatively few scientists in the country who could usethe 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 PDA 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, U.A., and Zussman, J., Rock-Forming Minerals, Vol. 3, p. 121 (1962). 2. ibid, p. 131. ***************** We have concluded that the method publishe 1 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 fa.se-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 astimation of fibrous tremolite can also be done, if necessary, as a fringe benefit, at the same time. Goodhue WCD 000128 -6- We estimate that a satisfactory method will taka 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 thej optical microscopic method. These are listed with comments.' 1. Optical Microscopic Method - may he used, with some modification. Possibly better selection of R.I. 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 threshhold of detection. It does not distinguish fibrous from non-fibrous tremolita. The simultaneous detection of chlorite makes method impractical for chrysotile. 3. X-Ray Step Scanning + Optical Microscopy - Acceptable as in if 2 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. 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 Election Microscopy - 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. Goodhue WCD 000129 -7- - The CTFA Tale Subcommittee has completed its review of the Optical Microscopic Method for the Estimation of Chrysotile and Fibrous Tremolite in Talc, which appeared in the Federal Register, voi. 38 (No. 188), (p. 27076, September 28, 1973). It recommends postponement of the finalization of the proposed regulation on talc. In addition, a collaborative effort between FDA & industry to resolve a satisfactory method of estimating chrysotile anditremolite in talc, Its recommended, with periodic liaison reviews to monitor the project stajtus. A task force of industry experts j has been designated to pursue alternate methods. We invite FDA to participate in collaboration with the task force. George W . SmidlandChairman CTFA Talc Subcommittee GWS;dd Goodhue WCD 000130 MEMBERSHIP LIST - CTFA TALC SUBCOMMITTEE G. W.. Sandland, Chairman Bristol-Myers Products (SAC) Dr. Murray Berdick (SAC) Chesebrough-Ponds, Ine. : Dr. peorge Cohen i Bristol-Myera Products | Dr. Christopher Costello Colgate-Palmolive Company Mr. Salvatore DiBianca The Mennen Company Mr. John I'acq Colgate-Palmolive Company Mr. David Hamer Johnson & Johnson Research Center Mr. Alan M. Harvey R. T. Vanderbilt, Inc. Mr. Ray R. Krammen Whittaker, Clark end Daniels Mr. Adolph Maruszewski (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, Ine. (SAC) Dr. Harold Schwartz The Mennen Company (SAC) 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. Va.iderhilt, Inc. Mr. Ronald Yakupein Kolmar Laboratories December 11, 1973 * Goodhue WCD 000131