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*-------- -------- ------ 1 FY: 1974 DATE: 9/6/73 "-ogram: COSMETICS PPE USE ONLY 00679 # Subprogram: Aerosols & Hair Preparations rroject litle: Asbestos and Other Contaminants in Talc Project Manager 6 Mailing Symbol : John Stuart (BF-446) Statement of Obi active: Develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concen trations at which such contaminants present a potential health hazard. -- ------- * The inhalation of certain asbestiform minerals is a known health hazard. The results of the determination of asbestos by x-ray diffraction in 200 commercial cosmetic talc samples by consultant to the FDA were in disagreement with those obtained by others through microscopy. This project will provide the in-house capability to perform reliable asbestos analyses and resolve the controversi on.th asbestos content of the 200 commercial talc samples. Description of Work: The 200 commercial cosmetic talc samples evaluated by Dr. Lewin will be tested for asbestos by refractory optical microscopy. After installation of the automated x-ray powder diffractometer and the high-temperature differential thermal analyzer, instrumental analytical methodology will be perfected to a degree that asbestos can be determined reliably and speedily at concentrations of less than one percent. The perfected methods will be published. C MILESTONES: 1.Evaluation of Talc Samples by Optical Microscopy 2. Installation of High Temperature Thermal Analyzer 3. Installation of x-ray Diffractometer 4. Establishment of Analytical Method 5. Analysis of Talc Samples by Instrum. Method First Quarter Second Third ;Fourth ' x s x TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT 1. ram COSMETICS 4. Project Title 2. Sub-Program Aerosols and Hair 3. Quarter/FY ------------- Braparat inns-- 1st FY 74'___ 5. Project Number Asbestos and Other Contaminants in Talc 00679 6. Description of this Quarter's Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, the relationship of this quarter's work to that of previous and future quarters. If more space is needed, use blank paper). The objective of this program is to develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations at which such contaminants present a potential health hazard. This 1st quarter efforts have been directed to establishing a good technical base for meeting the program objectives. As a first milestone, the installation of the High Temperature Differential Thermal Analyzer was scheduled for completion. This has been accomplished. Further, the X-Ray Diffractometer has arrived and arrangements are underway for its installation Procedures are being set up for making a rough estimate of the amount of talc powinhaled by an infant during powdering. A literature and technical review of Serpentine, Amphibole and Talc mineralogy is in progress. For This purpose, the work of Lewin, on the examination of asbestos in 200 talc products has been reviewed. A trip was made to the Smithsonian Insti- -- tution-tg-- examine-tape 5 p._he above mineraJLs__and arrange for the use of facilities/ Co 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them, If more space is needed, use blank paper). Milestones not achieved NONE (8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions xf Yes / / No (if no, explain) !9 , Project Manager's Signaj?ure JO. Date 7 and yHfrtptf. John(^uart, BF-446 9/26/73 1 1 . P r o g i Manager's Signature |^2 Date Heinz J. Eiermann, BF-440 9/26/73 CONTINUATION OF ZTEM #6 jram: COSMETT-CS h Sub-Prograin : Aerosols and Hair Preparations 1st qtr. FY 741 Project Title: Jbebestos and Other Contaminants in Talc Project Number: 00679 Techniques are being developed for concentration of the asbestos fraction of talc products to be essmined. Among these are the use of heavy liquids for density separations. kind of approach may lead to a lessening of the requirements for instrumental sene-- bivity while maintaining detection sensitivity. Efforts in the neurt quarter will continue in the areas outlined above. Also, Lewin's "talc samples" wn.1.1 be examined by optical microscopy and crystallography. ! i TECHNICAL PLAN \ QUARTERLY PROJECT PROGRESS REPORT rogram COSMETICS 2. Sub Program Aerosols and Hair Preparations 3. Quarter/FY 2nd FY 74 4. Project Title Asbestos and Other Contaminants in Talc 5. Project Number 00679 6 Description of this Quarter's Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, tbe relationship f this quarter's work to that of previous and future quarters. If more space ie needed, use blank paper). The objective of this program is to develop methods of sufficient sensitivity and reliability to permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations at which such contaminants present a potential health hazard. The necessary equipment for the talc inhalation study has been received. Exper imental work for the purpose of estimating the amount of talc powder inhaled by an infant during powdering will commence shortly. The differential thermal analyzer has been performance-checked and standardized. As of 12/21/73 approximately 50 thermograms (including 18 talc samples which Dr. Lewin had investigated) were prepared and analyzed. No asbestos minerals were detected. ra investigational samples of commercial talc products were analyzed by DTA and optical microscopy. No asbestos minerals were detected. The literature and technical review of serpentine, amphibole and talc mineralogy is continuing. (Continued on next page) 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why. Aiso indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more apace Is needed, use blank paper). Installation of x-ray diffractometer has been delayed. GSA did not make the necessary utilities installation. The other project phases are essentially on target. 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions / yj Yes / / No (if no, explain) activity in the future. 9 Project.Manager's Signature 10. Date / II o Program Manager's Signature ^ 2 Date John Stuart HFF-446 i h j 7 / Heinz J. Eiermann HFF-440 Asbestos and Other Contaminants in Talc 00679^ Examination of talc samples by optical microscopy according to the method published in the Federal Register (39 FR 27076) is proceeding. As of 12/21/73, samples (Lewin's identification) # 29, 58, 60, 84, 87, 131, 133, 134, 135, 136, 137, and 138 were analyzed for mineral content.All contained large quantities of talc, small amounts of carbonates, and minor amounts of hematite, quartz and diatomaceous earth. Sample # 84 contained 107 filers of tre:crlite/actinolite per mg. Sample # 87 contained 66 fibers per mg- Standard sliuSes were prepared with 1% and 0.1% tremolite and chrysotile in talc. TremoILitie is readily detectable to 0.1%. Detection of chrysotile at the 0.1% LswelL is questionable. Less than one in 20 fibers are visible at 400X. This; evaluation was made using Congo Red dye which preferentially stains the charysattile fibers. -- -- ........ ...... ... .. ............................................. ..... ----- ------ TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT 1. -rogram Cosmetics 4. Project Title 2. Sub-Progratn Aerosols & Hair Preparations 3 - 9 ^ f ? r/ F 5. Project Number Asbestos & Other Contaminants in Talc 00679 6. Description of this Quarter's Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,,where relevant, the relationship f this quarter's work to that of previous and. future quarters. If more space is needed, use blank paper) The objective of this program is to develop methods of sufficient sensitivity and reliability to permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations at which such contaminants present a potential health hazard. A study was undertaken to determine the amount of talc an infant may inhale when powder is applied to the child during diaper change. The use conditions were simulated and exaggerated to obtained data reflecting the most severe circum stances. Baby talc was sprinkled Ctoto a platform at a rate of 200g per approxi mate half hour, and air was sucked through a filter fitted with a pre-weighed filter paper at a rate of 0.5 liters per minute reflecting approximate respiration rate of a child. The air filter funnel was positioned in such a way that it would be located near the mouth of the child under actual use conditions. . total of 24 experiments of dispensing 200g of talc was performed. An average of 1.2 mg it 0.5 mg of talc was collected. The average time, for dispensing the 200g of talc was 30 min jt ^7 min. Considering extreme conditions (highest amount of talc dispensed during the shortest time period, both at the 95% level of confidence) and the 0.5 1/min. air flow, the amount of talc collected on the (con't.) 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more space is needed, use blank paper). Because of the delay in the installation of x-ray diffractometer and the analysis of commercial cosmetic talc samples by optical microscopy, establishment of the analytical method for determination will be delayed beyond the fourth quarter. 8, Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. F J Yes U No (if no, explain) ! 9, P ro je c t Manager' s/Signature 10. Date y^and M ai)/ Sym bol f o / t S j J fa a ir 1 1 . Program M a n a g e r's S ig n a t u r e ^2 Date tiAR 2 8 797<| Hdinz J . tiiermann HlT-440 -2 / '/ filter would be 0.275 x 10 ^ mg/ml. Taking into consideration OSHA standards for permissible levels of asbestos fiber contamination of air (29 CFR 1910.93a) of 5 fibers / ml air on a continuous basis (8 hours per day per 5-day week) and 10 fibers / ml air as temporary exposure (15 min. per hour per 5-hour day per 5-day week) and assuming that the difference of 5 fibers per ml air may be inhaled by an infant, and furthermore considering the equation that 1000 fibers are equivalent to 0.1% of 1 mg of talc, the following condition exists: The 5 fibers per ml of air is equivalent to 5 x 10"6 mg of asbestos / ml air. Consequently, the 275 x 10" mg of talc may contain 5 x 10"^ mg asbestos, which is equivalent to 1.8%. Since the OSHA standard permits inhalation of up to 10 fibers of asbestos per ml air which is equivalent to 10,000 fibers (or 10 x 10"^ mg) per liter, of 10 x 10"6 mg asbestos per ml, the maximum asbestos fiber concentration may' be 3.6%. Using a safety factor of 100 would reduce the allowable level of asbestos to 0.036%. In essence this may be interpreted to mean that talc used for cosmetic purposes should contain less than 0.036% (360 fibers/mg) asbestos fibers and that analytical methodology to be developed for regulatory purposes should be sufficiently sensitive to detect asbestos in talc at this level. On the other hand, applying OSHA standards somewhat more liberally and being primarily concerned about the maximum total daily intake of asbestos fibers, and not so much about the maximum exposure of 10 fibers/ml at any time, one may extrapolate that OSHA permits an exposure time of 10 x 5 = 75 min. per day to the excess amount of 5 fibers/ml. Since the infant is exposed to talc approximately 10 x 1 min. per day, the 1.8% asbestos level may be increased to 1.8 x 70/10 = 13.5%. With a safety factor of 100, the allowable level of asbestos fibers would be reduced to 0.135% (1350 fibers/mg). The examination by optical microscopy of the commercial cosmetic talc samples which Dr. Lewin had tested by x-ray diffraction was continued. The following samples were analyzed according to the proposed method published in the Federal Register (39 FR 27076): #61, 88, 89, 90, 92 and 93. Our determination showed that all contained tremolite (amphibole) but none showed chrysotile. With the exception of sample #61 which was found to be free of asbestos fibers, Dr. Lewin reported A - 5% chrysotile and 3 - 5 % tremolite. Because the fiber count for a given weight percentage of tremolite varies significantly, it is impossible to establish accurate correlation between fiber count and weight. It may, however, be stated that the high counts of tremolite observed in these samples appear to confirm the results Dr. Lewin reported for this type of asbestos fiber. The x-ray diffractometer has finally been installed. Work on the development of a method for the determination of asbestos with this instrument, however, has been delayed because of the analysis of some of the Lewin samples by optical microscopy. Vo commercial talc products were analyzed for mineral and asbestos content oy optical microscopy. No chrysotile was detected, however, tremolite (amphibole) was found in one sample at a level of 1,100 fibers/mg. Program C0SMETICS 4. Project Title TECHNICAL PLAN QUARTERLY PR0JEC1 PROGRESS REPORT 2. Sub-Prcgram Aerosols and -- Hair. Pr,,enaxai_QiLS________ 3. Quart er/'EY' ___ 4th/74 __ 5. Project Number Asbestos and Other Contaminants in Talc 00679 6. Description of this Quarter's Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, the relationship of this quarter's work to that of previous and future quarters. If more space is needed, use blank paper). The object of this program is to develop methods of sufficient sensitivity and reliability to permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concen trations at which such contaminants present a potential health hazard. The examination by optical microscopy of the commercial talc samples which Dr. Lewin had analyzed by x-ray diffraction was continued. As of 6/14/74 the following samples were analyzed according to the proposed method published in the Federal Register (39 FR 27076): 26, 37, 42, 63, 70, 71, 72, 74, 77, 80, " 85, 94, 95, 99, 100, 101, 107,.143, 144, 145, 148, 149, 151, 152, 153, 154, 163, and 164. DCST's results by optical microscopy tend to confirm in a general way, Dr. Lewin's findings for tremolite. Chrysotile, however, which was reported in samples 95, 143, 145, 163, and 164 could not be detected by optical microscopy by DOST. As of 6/14/74, four collaborative and two commercial samples were also analyzed for asbestos fibers by optical microscopy. Statistical analysis of the talc inhalation data reported in the (continued) 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as plannedE reschedule them. If more space Is needed9 use blank paper). Milestones Not Achieved: Although the x-ray diffractometer was installed during the third quarter FY 74, it is presently malfunctioning. Development of x-ray analytical method will commence when instrument is repaired. ! 8-. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. / yl Yes _! No (if no. explain) 9 , Project Manager's Signature and,,.Mail Symbols.,/ Ronald *L. Yates ' HFF-446 i. nate 7/4/7? pj_# rrogram nager /A ! . J Heinz J. Eiermann s Signatu^w ms * S'** HFF-440 'rosols and Hair Preparations (00679) 2 third quarter FY 74, suggested that further data be accumulated to arrive at statistically significant conclusions concerning talc concentration in ait. At the suggestion of the Division of Mathematics, DOST has obtained 30 additional sets of data. Regression and correlation analyses will now be carried out to determine the degree of dependence of experimental variables. FY : 1975 TECHNICAL PLAN PROJECT DESCRIPTION DATE: May 16, 1974 PPE USE ONLY 0067 9 am: COSMETICS , Project Title: Determination of Asbestos in Talc Subprogram: Chemical Analysis and Methods Development Project Manager & Mailing Symbol : Ronald L. Yates (HFF-446) Statement of Objective: Develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations at which such contaminants present a potential health hazard Justification: The inhalation of certain asbestiform minerals is a known health hazard. This project will provide the necessary in-house capability to perform reliable asbestos analyses. Description of Work: Instrumental analytical methodology will be developed and perfected to a degree that asbestos can be determined reliably at concentrations in the range of 0.1% or less. At least two instrumental techniques will have to be developed because no single method is sufficiently specific, sensitive, and accurate to accomplish the objective. Samples of commercial talcs and cosmetic talc products will be examined for asbestos at random and as needed in conjunction with the development of analytical methodology. MILESTONES : 1. Establishment of Analytical Method Quarter First Second Third Fourth , Program [U- Cofimp.rirs 4. Project Title TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT 2. Sub-Program Chemical Analysis 3. Quarter/FY and Methods Tievp1opment ____ ____ 1/-L5____ 5. Project Number Determination of Asbestos in Talc 00679 6. Description of this Quarterns Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, the relationship of this quarter's work to that of previous and future quarter-. If more space is_needed, use blank paper). The purpose of this project is to develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations at which such contaminants present a potential health hazard. Work started on a method for the determination of chrysotile in talc by differential termal analysis (DTA). Pure talc samples were spiked with various levels of chrysotile. DTA data on these samples indicate a lower detection limit of 0.5%. For a series of samples containing the same con centration of chrysotile neither the endotherms nor the exotherms were of equal intensity. This indicates that the accurate determination of chrysotile will depend upon measurement of peak areas. As of September 25, 3 compliance program surveillance (CPS) samples and one consumer complaint sample were analyzed for asbestos by optical microscopy. One CPS sample contained 1,100 tremolite fibers/mg. Asbestos was not detected in the remaining samples. 7. Milestones Not Achieved? (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more space is needed, use blank paper). No milestones were scheduled for completion during 1st quarter/FY 75. 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. A 7 Yes / / No (if no, explain) Lr-> J> TECHNICAL PLAN ' QUARTERLY PROJECT PROGRESS REPORT ^ ,rogram 0 COSMETICS |4. Project Title 2. Sub-Program Chemical Analysis 3. Quarter/FY and Methods Development 2nd/75 5. Project Number Determination of Asbestos in Talc 00679 6. Description of this Quarterns Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, the relationship f this quarter's work to that of previous and future quarters. If more space is needed, use blank paper). The purpose of this project is to develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations at which such contaminants present a potential health hazard. Work, continued on the development of a method for the determination of chrysotile in talc by differential thermal analysis (DTA). Although DTA is reasonably specific for chrysotile, certain minerals, such as large amounts of chlorite (ca 10%), cause problems when determining small amounts of chrysotile (0.5-1%). Efforts to remove interferences by chemical means have had limited success. Treatment of talc samples with dilute hydrochloric acid removed interfering carbonates. 'covery studies were done on spiked talc samples containing from 0.5 to 5% .nrysotile. Exotherm intensities were not as reliable as peak areas for quantitative calculations. Recoveries were approximately +_ 20% of true values. Samples of chrysotile from 10 different geographic locations were examined by DTA. ___________________ -- ___ __ (continued next page)_________ _ 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them, If more space is needed, use blank paper). No milestones were scheduled for completion during 2nd quarter/FY *75. 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions /_&/ Yes / / No (if no s explain) 9 . Project Manager's Signature 10. Date and Mail .Symbol / Ronald L. Yatg^ (HFF-446) 1/ 7 /7 r 11. Program Manager5s Signature 1 2 . Date Heinz J. Eiermann (HFF-440) 1/ 7/7r ~ 2- & ( o emical Analysis and Methods Development 2nd/75 00679 It was found that there was wide variation in the intensities of the dehydroxylation endotherm and the recrystallization exotherm from sample to sample. These results are not unexpected because chrysotile, being a mineral, varies slightly in com position and crystalline structure. This would mean that any quantitative results obtained would be suspect because the chrysotile in the sample would not necessarily relate to the calibration standard in a chemical and structural context. The CTFA submitted three more round-robin samples of talc for chrysotile analysis by DTA and optical microscopy. By DTA, sample A contained in excess of 5% chrysotile, sample B contained 1% and in sample C chrysotile was not detected. Analysis by optical microscopy has not been completed. , Program Cosmetics h . Project Title TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT 2. Sub-Program Chemical Analys;iiss 3. Quarter/FY ____ ____rZZS____ 5. Project Number Determination of Asbestos in Talc 00679 6 Description of this Quarter's Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Includewhere relevant, the relationship f this quarter's work to that of previous and future quarters. If more space is needed use blank paper). The purpose of this project is to develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations at which such contaminants present a potential health hazard. Work is continuing on a method for the determination of chrysotile in talc by differential thermal analysis (DTA). Present work involves determining at what level chlorite interferes with this determination. Preliminary data indicate that chlorite levels of 50% can be tolerated in most talc samples. In other cases, depending on the degree of grinding and purity, chlorite can interfere at levels of 15% due to shifts in the endotherms at approximately 650 and 850C. A more definitive answer to this problem will be obtained by spiking pure talc with chrysotile and various grades of chlorite. Zinc, calcium and magnesium stearate have been studies by DTA to determine if these compounds interfere with the determination of chrysotile in talc. The zinc and magnesium stearates do not interfere; the calcium compound is potentially troublesome. A similar study done on laboratory grade (continued) 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as planned reschedule them. If more space is needed use blank paper). Insufficient progress has been made in method development due to unforeseen scientific complexities to assure completion of work during FY 4/75. > / 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. /X/ Yes / / No (if no, explain) Project Manager's Signature 10. Date -2- f 7 magnesium carbonate indicates no interference from this compound. Mineral specimens of magnesium carbonate will be examined by DTA when obtained. Nearly all commercial samples of cosmetic talc analyzed by DTA contain an endotherm at 740C. The mineral responsible has not yet been identified. As of 3/28/75, DTA of approximately 75 (ca. 20 during FY 3/75) of Dr. S. Z. Lewin's talc samples were analyzed for the purpose of comparing analytical data. Two samples, Lewin's #96 and #143 indicated serpentine by DTA. It has not been determined whether that serpentine is chrysotile or antegorite. As of 3/28/75, five Field Activity Surveillance samples have been analyzed for chrysotile. None was detected. E Program IHO JE r e j e c t Cosmetics T itle TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT 2. Sub-Program Chemical Analysis 3. Quarter/FY and Methods Development 4th/75 5. P r o j e c t Number Determination of Asbestos in Talc 00679 6 Description of this Quarters Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,,where relevant, the relationship g>f this quarter's work to that of previous and future quarters. If more space is needed, use blank paper). The purpose of this project is to develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations at which such contaminants present a potential health hazard. Work continued on development of a method for the determination of chrysotile in talc by differential thermal analysis (DTA). DTA data was obtained on seventeen minerals known or suspected to occur in talc. Data will be used to: 1) Identify minerals present in cosmetic talc samples. 2) Determine which minerals may interfere with determination of chrysotile in talc. \s of 6/27/73, 49 Field Surveillance samples have been analyzed for chrysotile. .one was detected at limit of method (Q.5%). Thirty-two FAS samples were analyzed for tremolite using light microscopy. None was detected. 7. Milestones Not Achieved; (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more space is needed, use blank paper). Insufficient progress has been made in method development due to unforseen scientific complexities to complete project during FY 75. K t i 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions fjJ ^ es / / No (if no, explain) LFDH Project Manager's Signature 10. Date and Mail SyphaJ/2 I Ronald L. YatefefHFF-A L ----------------------y 7 /z/r 1 1 . Program Manager's Signature 12. Date I si TECHNICAL FLAK PROJECT DESCRIPTION T77 1976 ?R<KrJHT DATE; May 19, 1975 Cosmetics PPES USE ONLY: 00679 SUBPROGRAM? Chemical Analysis _______and Methods Development PROJECT TITLE ? Determination of Asbestos in Talc PROJECT MANAGER & MAILING SYMBOL: Ronald L. Yates (HFF-446) STATEMENT OF OBJECTIVE! Develop analytical methods for the determination of asbestos in talc-containing cosmetic products at concentrations of 0.1% or less. JUSTIFICATX&i: The inhalation of certain asbestiform minerals is a known health hazard. This project is expected to provide the necessary in-house capability to perform appropriate asbestos determinations and the analytical methodology for proposal of a regulation on asbestos in talc. INSCRIPTION OF WORK: DCST has methods for the determination of serpentine (chrysotile and antigorite) by differential thermal analysis at a level of 0.5% and of tremolite by step-scanning x-ray diffraction at a level of 0.3%. Floatation methods will be developed to concentrate sepentine and tremolite in order to be able to determine these minerals at 0.1% concentration.. T0S USE ONLY MILESTONES: % Method for concentration of chrysotile -and tremolite by floatation L FDH 2853 TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT .ogram ^smetics 4. Project Title 2. Sub-Program Chemical Analysis 3. Quarter/FY and Methods Development lst/76 5. Project Number Determination of Asbestos in Talc 00679 ! 6. Description of this Quarterns Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, the relationship of this quarter's work to that of previous and future quarters. If more space is needed, use blank paper). The purpose of this project is to develop one or several methods for sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations at which such contaminants present a potential health hazard. Due to separation of John Stuart from government service, no methods development investigations were done during 1st quarter/FY 76. DOST has continued the differential thermal analysis (DTA) of Compliance Program Surveillance samples of ccmmercial cosmetic talcs for serpentine (chrysotile) minerals. As of 9/19/75, 28 of these samples have been analyzed. Serpentine was not detected in any samples. tiation of investigation to develop floatation methods for the concentration of chrysotile in talc samples will depend on manpower availability and project priorities. 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why. Aiso indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more space is needed, use blank paper). No milestones were scheduled for completion during lst/76. 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. / / Yes /y/ No (if no, explain) below budget due to resignation. 9. Project Manager's Signature 10. Date MaU/Sxmbj ad^L. 'Yates/HFF-446 10/3/75 TECHNICAL PLAN i QUARTERLY PROJECT PROGRESS REPORT i. Program Cosmetics 4. Project Title 2. Sub-Prograin Chemical Analysis 3. Quarter/FY and Methods Development 2nd/76 5. Project Number Determination of Asbestos in Talc 00679 6. Description of this Quarter's Activities: (Discuss accomplishments this quarter end indicate their significance to the program or project. Include,where relevant, the relationship of this quarter's work to that of previous and. future quarters. If more space ie needed, use blank paper). The purpose of this project is to develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations of which such contaminants present a potential health hazard. Due to lack of specialized personnel and certain necessary instrumentation, no significant work was done on methods development during 2nd quarter/FY 76. Routine analysis of consumer talc samples by differential thermal analysis (DTA) continued. Serpentine was not detected in any of these samples. Some x-ray diffraction data was obtained from talc, chrysotile and tremolite samples. The main purpose of this effort, however, was to familiarize a staff member with the peration of the computerized x-ray diffraction unit. Because of limited resources in regard to instrumentation and trained personnel, the only project planned relating to methods development is sample enrichment by floatation in order to detect lower levels of serpentine by DTA. Initiation of this project will depend on manpower availability and project priorities. 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more space is needed, use blank paper). No milestones were scheduled for completion during 2nd quarter/FY 76. 3. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. / / Yes /X/ No (if no, explain) j */ell below budget due to resignation of principal investigator.. !9 . Project Manager's Signature 10. Date and ^ / A * Ronald LL Yates, HFF-446 !& / / f / 7 5 " 11 Progfi&wltenagefc/B Signature p 'Heinz J. Eiermann? HFF-440 Date r- / .rogram Cosmetlcs 4. Project Title TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT 2. Sub-Program Chemical Analysis 3. Q ^ e r / F Y and Methods Development 5. Project Number Determination of Asbestos in Talc 00679 6. Description of this Quarter's Activities; (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, the relationship f this quarter's work to that of previous and future quarters. If more space is needed, use blank paper). The purpose of this project is to develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations of which such contaminants present a potential health hazard. During the 3rd quarter/FY 76 an investigation into the use of x-ray diffraction for the detection and determination of tremolite, anthophyllite and chrysotile was initiated. The principal investigator on the project was unfamiliar with the operation of the computerized x-ray diffractometer so that several weeks of operational study was necessary. Initial talc studies were done on talc samples that had been previously analyzed by S. Z. Lewin and DCST and known to contain tremolite. Initial analytical results were disappointing. After instrument alignment and a change in the divergence slit, consistent analytical results -ere obtained. Quantitative values, however, differed from those reported by S. Z. Lewin. An examination of our tremolite standard by x-ray diffractometry revealed large amounts of anthophyllite and talc which probably accounts for the difference in quantitative results. 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them, If more space is needed, use blank paper). No milestones were scheduled for completion during the 3rd quarter/FY 76. 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions !_J Yes /x/ No (if no, explain) Somewhat below budget due to resignation of principal inye.stigator Project Manager's Signature 10. Date M a il SypiboJU 11. ^ o m Manager/s Signature maid L. Ypt-oc ^FF-446 6. continued: Presently, an investigation is being conducted to evaluate the effect that divergence slits of 0.5, 1.0 and 4.0 have on resolution, sensitivity and reproducibility. Preliminary data indicates that the 0.5 slit, at low and intermediate values of 28, is the slit of choice. Future work will involve investigation in the following areas: 1. Sample preparation techniques It is important when preparing samples for analysis by x-ray diffractometry to achieve reproducible results. Three sample preparation techniques will be evaluated. 2. Completion of investigation of the effect that different divergence slits have on resolution, sensitivity and reproducibility. 3. Investigation and analysis of selected talc samples by x-ray diffraction. Line profiles of 10 talc samples obtained from Dr. Arthur Langer of Environmental Sciences Laboratory will be run to obtain an overall qualitative picture. Selected talcs of the 76 FAS samples will also be analyzed. When suitable standards of anthophyllite and tremolite are obtained, quantitative analyses will be conducted by step-scanning through selected values of 20. TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT Program Cosmetics 4. Project Title 2. Sub-Program Chemical Analysis, 3. Quarter/FY ana Methods Development 4th/76 5. Project Number Determination of Asbestos in Talc 00679 6. Description of this Quarter's Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,,where relevant,, the relationship this quarter's work to that of previous and future quarter;. If more space is needed# use blank paper). The purpose of this project is to develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations of which such contaminants present a potential health hazard. The main purposes of the present investigation are two-fold; 1. Determine which instrumental operating parameters and sample preparation techniques provide optimum conditions for the detection and determination of asbestos minerals by x-ray diffraction. 2. Periodically analyze conroercial cosmetic talc products for presence of asbestos minerals. Analyze samples that other investigators have implicated as containing asbestos minerals. Investigation was completed on evaluation of the combination of divergence and receiving slits which would provide maximum sensitivity and resolution. 7. Milestones Not Achieved; (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more space is needed, use blank paper). Method for floatation concentration of chrysotile and tremolite was not completed. Project was discontinued when data obtained indicated that lew levels of chrysotile could not be significantly concentrated using floatation methods. 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. /__/ Yes /X/ No (if no, explain) Scmewhat\ below allocation due to resignation of principal investigator. 9 Project Manager's Signature 10. Date 11. Program Manager's Signature Date PonalcT L. Yates, F-446 6. continued The following sets of slits were evaluated: Analytical Group Divergence Slit Receiving Slit Mt. Sinai CTFA FDA 4 0 1.0 0.5 4.0 0.2 ran 0.3 ran The combination of 0.5 divergence slit and 0.3 ran receiving slit gave most sensitivity. Conditions recommended by CTFA were found to be nearly as good. The slit combination used by Mt. Sinai Hospital were found to give a very high background, thus requiring a much higher net count to be statistically significant. FDA analyzed by x-ray diffraction ten samples of commercial cosmetic talcs which were collected and analyzed by Dr. Langer of Mt. Sinai Hospital. Dr. Langer reported anthophy11ite in five of the ten samples analyzed. FDA confirmed the presence of anphibole in these samples but identified the anphibole as tremolite in three of the samples. In addition, FDA detected anthophy11ite in one sample where Dr. Langer (Mt. Sinai) reported anphibole was not detected. Samples of standard tremolite were obtained from the U.S. Geologic Survey and Cape Asbestos Co. of London. These samples, originating in Fowler, N.Y. and South Korea respectively, were pure by x-ray diffraction. Talc standards containing 1% and 3% of the above tremolite were prepared and analyzed using the step-scan node. A malfunction of the goniometer has prevented further study of these samples. Different sample preparation techniques have been investigated. In our opinion the method used by Dr. Langer, where a slurry of talc is deposited on a millipore filter, is too tedious and requires a sample holder of unusual design. We have been unable to evaluate the sample preparation technique recommended by CTFA because of the present unavailability of suitable sample holders. A number of cosmetic talc samples collected by FDA for the cosmetic surveillance program were examined by x-ray diffractometry. No anphibole or serpentine minerals were detected. Future work on this project involves activity in the following areas: 1. Preparation of standard calibration curves for the determination of tremolite, anthophyllite and chrysotile. 2. Continued study of sample preparation techniques. 3. X-Ray diffraction analysis of aomnercial cosmetic talcs to deter mine anphibole and serpentine content. ... . -- 1. Program 4. Project Title TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT -- 2. Sub-Program Chemical Analysis and Methods Development - ------------ -------------- 3. Quarter/FY 5th/76 5. Project Number Determination of Asbestos in Talc 00679 6. Description of this Quarterns Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, the relationship of this quarter's work to that of previous and future quarters. If more space is neededB use blank paper). The purpose of this product is to develop one or several methods of sufficient sensitivity and reliability which will permit the determination of asbestos and I other contaminants in talc-containing products with the necessary degree of accuracy and at concentrations of which such contaminants present a potential health hazard. | The main purposes of the present investigation are two fold: 1. Determine which instrumental operating parameters and sample preparation techniques provide optimum conditions for the detection and determination of asbestos minerals by x-ray diffraction. 2. Periodically analyze commercial cosmetic talc products for presence of asbestos minerals. Analyze samples that other investigators have implicated as containing asbestos minerals. In response to an EDPO research request, the New York District Office has offered to provide assistance in the development of analytical methods for the detection and determination of asbestiform minerals in talc. In response to their request, 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more space is needed, use blank paper). As stated in report for 4th/76, project to develop floatation methods for the concentration of chiysotile was discontinued. 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. /__/ Yes fx/ No (if no, explain) Somewhat below allocation due to resignation of principal investigator. 9/30/76 Determination of Asbestos in Talc o i 7V C'^ !*'& L'JO ?C/ 2 6. DCST is preparing a m u t e r of talc samples containing known amounts of chrysotile and tremolite. These samples will be sent to the New York office by October 4, 1976 During the 5th quarter/FY 76 most investigative work was devoted to the study of techniques for sample preparation for analysis by x-ray diffraction. The standard technique, which involves manual packing of the sample against a smooth surface, was found to give variable results in terms of sensitivity and quantitative reproducibility. These vari ations are caused by differences in packing density and background count. In an effort to obtain a talc sample with reproducible density, the pressed pellet technique was investigated. Talc samples containing known amounts of tremolite were prepared using pellet dies and a hydraulic press. X-Ray diffraction examination of the pelletized talc samples indicated the technique was superior to the standard method in respect to limit of detectability and reduced background count. On one sample tremolite was detected at the 0.1% level. On another sample containing 0.1% tremolite a net count was obtained but was not statistically significant; that is, net count did not exceed 2 V n , where N = background count. The main disadvantages of the pellet method are preferred orientation and 29 shifts of the tremolite peak. Preferred orientation, which is nonrandom alignment of crystals, causes errors in quantitative measurements. Shifts in 29 values are due to a decrease in crystal lattice d spacing which, in our opinion, is caused by high hydraulic pressure. The shift in 20 values places the main diffraction peak of tremolite in the region of anthopbyllite, thus creating a potential identification problem. Future work will involve continued investigation of sample preparation techniques, collection of statistical data, and analysis of selected FAS and consumer samples. TECHNICAL PLAN PROJECT DESCRIPTION -- m -------------- - DATE: 1 1977 August 12, 1975 PRRM:7 Cosmetics PROJECT TITLE? . PPES USE ONLY: 00679 SUBPROGRAM: Chemical Analysis and Methods Development PROJECT MANAGER & MAILING SYMBOL: Determination of Asbestos in Talc Clifton H. Wilson, Ph.D., (HFF-446) STATEMENT OF (BJECTXE: Develop a method to determine with the highest analytical sensitivity and accuracy asbestiform minerals in cosmetic talcs by means of x-ray diffraction. Analyze cosmetic talcs and talc products for asbestos by means of x-ray diffraction and differential thermal analysis. JUSTIFICATION: The inhalation of certain asbestiform minerals is a known health hazard. This project is expected to provide the necessary in-house capability to perform appropriate asbestos determinations and the analytical methodology for proposal of a regulation on asbestos in talc. INSCRIPTION OF WORK: DCST has methods for the determination of serpentine (chrysotile and antigorite) by differential thermal analysis at a level of 0.5% and of amphibple (tremolite) by step scanning x-ray diffraction at a level of 0.3%. The level of detection of serpentine (chrysotile) by x-ray diffraction varies with fiber dimensions and ranges from 0.5 to 2%. TOS USE ONLY DCST will investigate various sample preparation techniques and instrumental operating procedures for the determination of asbesti form minerals in talc products by x-ray diffraction. The method with the highest analytical sensitivity and accuracy will be subjected to a collaborative revise study for adoption as an official analytical method for possible regulatory purposes. Samples of cosmetic talcs and talc products will be investigated by x-ray diffraction and differential thermal analysis for the determination of asbestiform minerals. MILESTONES: Develop x-ray diffraction method for asbestos FDH 2853 1234 X 1. Program Cosmetics 4c Project Title TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT 2. Sub-Program Chemical Analysis 3. Quarter/FY _______ and Methods Development st/77 5. Project Number Determination of Asbestos in Talc 00679 6- Description of this Quarter's Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, the relationship f this quarter's work to that of previous and future quarter?. If more space is needed, use blank paper). The purpose of this project is to develop a method to determine with the highest analytical sensitivity and accuracy asbestiform minerals in cosmetics talcs by means of x-ray diffraction. Analyze cosmetic talcs and talc products for asbestos by means of x-ray diffraction and differential thermal analysis. Investigations have been completed on sample preparation techniques and instrumental operating conditions for the x-ray diffraction detection and determination of amphibole minerals in talc. These minerals can be detected and determined at levels of 0.1%. After these investigations were completed, analysis of a number of standard samples were done to develop a standard calibration curve for the quantitative analysis of amphibole in talc. For this purpose, samples of talc containing 3.03, 1.05, 0.52 and 0.11% of Korean treamolite were prepared. The samples were then prepared as pressed pellets using a hydraulic press. Samples were then analyzed by x-ray diffraction. To muniroize error due to preferred orientation, net counts were obtained at one position and the sample was then rotated 90 and a second net count was obtained. Two samples of each 7. Milestones Not Achieved; (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more space is needed, use blank paper). No milestones were established for this quarter 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions, /x/ Yes / 7 No (if no, explain) 10. Date |116 ] 1/5/77 6. continued: OC-C- 4h 7? concentration were prepared. A munirrium of eight determinations were done on each sample. These values were averaged and then plotted (Figure I). Although differences in mass adsorption coefficients between tremolite and talc would predict a non-linear plot, it is apparent from the figure that the relationship between concentration and net count is linear over the range studied. The above procedure was then repeated using a CTFA tremolite standard. Analytical data is summarized in Table I. Ten FAS talc samples provided to Dr. Danger of Mt. Sinai Hospital for analysis are in the process of being reanalyzed in our laboratory using the proposed diffraction procedure. Dr. Langer reported that one talc sample contained approximately 1% tremolite. Our analysis of this sample using the Korean and CTFA tremolite standards indicate 1.75 and 0.65% tremolite respectively. One other talc of the group contained a trace (less than 0.1%) of tremolite. The remaining eight samples will be analyzed using the proposed procedure. The CTFA is conducting a round robin analysis of consumer talc products and our laboratory has agreed to participate. These sanples have arrived and will be analyzed during the second quarter/FY 77. In the 5th quarter/FY 76, a number of talc sanples containing added tremolite or chrysotile were sent to the New York District Office for optical microscopic analysis. The request by the New York office was in response to an EBRD research problem request. The results of their analyses have been recently received. Analysis of the data is pending. Table I O /V / -cV'-K 77 X-Ray Diffraction Data for Korean Tremolate Standards (Fibrous) Trem. Cone.(%) 3.03 1.05 0.52 0.52 0.11 0.11 Count Time (Sec) 5.0 5.0 7.5 5.0 20.0 5.0 Peak Max. 1084 374 325 217 194 48.5 Net Count Peak Area 6911 2125 1730 1153 600 150 3.14 1.13 1.39 0.75 0.75 0.16 0.16 CTFA Tremolite Standard (Massive) 5.0 5.0 5.0 7.5 5.0 20.0 5.0 2716 1436 1446 933 622 639 160 15,367 7469 7923 5276 3517 2774 694 TECHNICAL PLAN 1 QUARTERLY PROJECT PROGRESS REPORT 1. Program Cosmetics 4. Project Title 2. Sub-Program Analysis ana Methods Development 3 - W f /FY 5. Project Number Determination of Asbestos in Talc D 0/679 6* Description of this Quarter1s Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project. Include,where relevant, the relationship f this quarter's wcrk to that of previous and future quarter If more space is needed, use blank paper). The purpose of this project is to develop a method to determine with the highest analytical sensitivity and accuracy asbestiform minerals in cosmetic talcs by means of x-ray diffraction. Analyze cosmetic talcs and talc products for asbestos by means of x-ray diffraction and differential thermal analysis. Analysis of the ten FAS talc samples mentioned last quarter was completed. One sample contained tremolite, one a trace (less than 0.1%) of tremolite and the remaining eight were free of amphiboles by x-ray diffraction. Our laboratory participated in a round robin analysis conducted by CTFA. Nine samples, including seven commercial talc products and two containing 0.5% tremolite and 3.5% anthophy11ite were analyzed. This analysis included x-ray diffraction and optical microscopy. The analysis has been completed and results sent to the CTFA committee. Our x-ray diffractometer has tetter sensitivity (about 0.1%) than the CTFA method specifies. As a result, three samples were found to contain less than the 0.5% tremolite cut-off point specified in the CTFA method. 7. Milestones Not Achieved; (Identify any of this quarter's milestones not met and briefly explain why. Aiso indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them. If more space is needed, use blank paper). No milestones were established for this quarter. 8. Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. /X/ Yes / / No (if noB explain) F ____________ 9. Project Manager's Signature 10. Date c y i: ?ton H. WilsonymPtoDT 3/29/77 _1 11. P* c^rarn Manager's Signature 22 Date 6. continued C V C o lfi &/ yy Seventeen new FAS talc samples were received and eleven given a preliminary analysis (continuous scan). The results indicate the possibility of an amphibole in several samples. Nine of those eleven will be analyzed further (line-profile scan and optical microscopy). All of these samples would be completed by now except for instrument malfunction which resulted in four weeks of down time. Future work involves further analysis of FAS samples. TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT 1. Progran Cosmetics 'roject Title 2. Sub-Program Chemical Analysis 3. Quarter/FY and Methods Development Jrd/77 5. Project Number Determination of Asbestos in Talc 0 Q6679 6. Description of this Quarter's Activities: (Discuss accomplishments this quarter and indicate their significance to the program or project, Include,where relevant, the relationship of this quarter's work to that of previous and future quarters If more space is needed, use blank paper). The purpose of this project is to develop a method to determine with the highest analytical sensitivity and accuracy asbestiform minerals in cosmetic talcs by means of x-ray diffraction. Analyze cosmetic talc and talc products for asbestos by means of x-ray diffraction and differential thermal analysis. Seventeen talc products collected under the Cosmetic Compliance Program were ana lyzed by X-ray diffractcmetry and two of the products were found to contain tremolite. One of these products contained 0.1% tremolite and the other product contained trace amounts of tremolite and anthcphyllite. The products containing tremolite will be examined later by optical microscopy. Two samples of raw talcs were also examined for asbestiform minerals. One raw talc which was scheduled to be re-packaged and sold as a cosmetic talc product was found by X-ray diffractcmetry to contain approximately 65% trsralite and a significant amount of anthcphyllite. The presence of tremolite fibers was verfied by optical TLcroscopyo A meeting was convened by the CTFA Talc Sub-Ccmmittee for the purpose of discussing with participants the results of their round robin analysis of coded talc samples for .Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why. Also indicate how this will affect project progress. If future m ilestones will not be accomplished as planneds reschedule them. If more space Is needed, use blank paoer),, No milestones were established for this quarter. 8o Latest RUS Report Indicates Compatibility Between Planned and Used YTD Positions. P J Yes / / No (If no, explain) asbestiform minerals. Results indicated major differences with the optical microscopic technique. A second round robin analysis is planned using a modified microscopic technique. TECHNICAL PLAN QUARTERLY PROJECT PROGRESS REPORT ,'rogram Cosmetics 4. Project Title 2. Sub-Program Chemical Analysis 3. and Methods Development r/FY p. Project Number Determination of Asbestos in Talc 0 ^ 9 & 7' 6 Description of this Quarter's Activities: (Discuss accomplishments this qiuarter and indicate their significance to the program or project. Include,where relevant, the relationship f this quarter's work to that of previous and future quarters. If more space ig needed, use blank paper). The purpose of this project is to develop a method to determine with the highest analytical sensitivity and accuracy astestiform minerals in cosmetic talcs by means of x-ray diffraction. Analyze cosmetic talc and talc products for asbestos by means of x-ray diffraction and differential thermal analysis. The second round robin analysis in cooperation with CTFA Talc Sub-Committee was completed. Five samples were examined and no tremolite or anthophyllite was detected based upon the guidelines set forth in the CTFA method. One sample did contain about 0.3% tremolite. The dispersion staining method recommended by CTFA failed in my opinion. Comments which were forwarded to CTFA on this method included: 1. The magnification of the dispersion staining device on our microscope was such that fiber size was difficult to determine since fibers meeting the definition were so small. 2. Parts 1 and 5 of the definition for a fiber are very subjective and can easily vary with the analyst. 7. Milestones Not Achieved: (Identify any of this quarter's milestones not met and briefly explain why Also indicate how this will affect project progress. If future milestones will not be accomplished as planned, reschedule them, If more space is needed, use blank paper). The milestone established for this project has been met. 8. L a t e s t R U S R e p o r t I n d i c a t e s C o m p a t i b i l i t y B e t w e e n P l a n n e d and U s e d Y T D P o s i t i o n s . Yes / / No (if no, explain) i ^ ^ P r o ^ g ^ i g ^ e ^ ^ ^ ^ g n a tur e 10. D a t e tlii^ton H. r n l n , p h . D . ^ H F F " 4 4 6 11. ? rjftr a m M a s t e r ' s S i g n a t u r e 12. D a t e $4A/1 -- .ECHNICAL PLAN: No. 6. continued: 3. The method was slow and tedious for the type of results one obtains. It seems to me one could spend this kind of time on a scanning electron microscope and obtain more information. The x-ray diffraction method developed in our laboratory is being prepared for publication. This will conclude work on this project.