Document gDJj2OyOq357z4B9n4nYQBdya

FILE NAME Talc TALC DATE 1973 DOC TALC170 DOCUMENT DESCRIPTION FDA Memo on Summary & Comments on Prof. Lewin's Analytical Results for Asbestos in Talc with Final Report EMORANDUM EMORANDUM EMORANDUM EMORANDUM EMORANDUM EMORANDUM DEPOA F HER ALTT H EDM UCATE IONN ANDT WELFAREWELFARE PUBLIC HEALTH SERVICE FOOD AND DRUG ADMINISTRATION F 620 Dr. Robert M. Schaffner Director Office of Technology 400 Rab - DATE Rab7/31/73 Rab 7/31/73 7/31/73 7/31/73 July 31 1973 . OM Dr. Alfred Weissler Acting Director Division of Color Technology 430 JJECT Summary and in Talc Comments on Prof. Lewin's Analytical Results for Asbestos 1 The purposes of this memorandum are to present a summary of the analytical results for asbestos in Cosmetic talcum powders obtained by Prof. Seymour Z. Lewin of New York University in his role of consultant to FDA to compare his results with those obtained by other laboratories on some of the same samples and to make some comments on the gen- eral question of suitable techniques for the analysis of asbestos in tale 2. asked Dr. Lewin in December 1971 to undertake asbestos analyses in 100 samples of cosmetic powders the scope was expanded on two subsequent occasions to include a total of 195 samples I chose Dr. Lewin for this work because he is an internationally expert on mineralogical chemistry and because he is a member of the academic community and therefore likely to be impartial in a confrontation between industry and government by industry appeared to Furthermore his competence had previously been recognized by virtue of their own use of him as a consultant which confer ^ desirable immunity against possible industry attacks on the validity of the results . 3 Dr. Lewin's findings are shown in Table 1 the key to the identities of the numbered samples is given in Table IV Please note also the explanatory comments in Dr. Lewin's meno of July 10 1973 which is an Attachment to Table I. No varieties of asbestos other than chrysotils a serpenting or tremolite an amphibole were found by Dr. Lewin in the 195 samples which he examined As shown in Table I Dr. Lewin found definite indications of chrysotile in 17 of the samples many of these also had tremolite and definite indications of tremolite but not chrysotile in an additional 18 of the samples These results were obtained primarily by means of Ray diffraction supplemented in some cases by optical microscopy and other tecliniques However Dr. Lewin points out on page 2 paragraph 1 of the Table I Attachment that the chrysotile he has identified in commercial products shows several significant dif- ferences from classical chrysotile in the location of its Ray dif- fraction peaks in its appearance under the microscope in its reactivity toward dilute acid and in its behavior with respect to differential thermal analysis HHS00000197 Page 2 - Dr. Robert M. Schaffner 4. In Table II I have compared Dr. Lewin's results for tremolite with those obtained for some of the same samples at FDA by means of optical microscopy and at the Pfizer Minerals Pigments and Metals Division by meanosf Ray diffraction This comparison which was undertaker in order to obtain additional information on the samples shows good quantitative agreement among the three laboratories Whatever quantitative differences exist in the amounts of tremolite found can be understood readily on the basis of such factors as a preferred orien- tation of plates and fibers in the packing of the Ray diffraction sample and b inhomogeneities in sample composition caused for example by air elutriation within the container when it is shaken , .5 In Table III I have compared Dr Lewin's results for chrysotile with those obtained for some of the same samples by four other labora- tories the additional two laboratories included in this part of the study are Columbia Scientific Industries of Austin Texas who sell the Stone apparatus for differential thermal analysis and the Health Protection Branch of the Department of National Health and Welfare of the Canadian government in Ottawa The agreement of results from dif- ferent Laboratories is much less satisfactory for chrysotile than that discussed above for tremolite For example samples 89 and 163 were found by Dr. Lewin to contain % and of chrysotile respectively but chrysotile was not found in these samples by the other laboratories Also a preliminary finding of chrysotile in a sample of Johuson and Johnson Shower to Shower Body Powder has been disputed by the company which claimed that their own analyses by several different techniques fail to show the presence of chrysotile The explanation for these differences is attributable largely to Dr. Lewin's inclusion in the term chrysotile of mineral species which show significant differences from classical chrysotile as discussed in paragraph 3 above . 6. The difficulties involved in analyzing talc and other samples for small amounts of asbestos have been pointed out by many investigators It is not surprising that the results of different laboratories disagree sometimes especially in the presence of transitional or altered minera logical species Moreover with regard to the two varieties of asbestos of concern bere it is unfortunate that the one which is a clear inhalation hazard to man namely chrysotile poses an intrinsically more difficult analytical problem than the other tremolite which has not yet been shown to present a biological hazard This is due in part to the Less prominent ray diffraction peaks of chrysotile and to the fact that the fibers are often too small to be seen in the optical microscope 1 In connection with a proposed new regulation on the safety of cosmetic talcum powders we face the problem of specifying an analytical ; test for asbestos which must be satisfied by the powders if they are pot to be considerated adulterated On the basis of information available at present I powders shall tivity of the recommend consideration of be examined first by ray order of % for chrysotile the following procedure The diffraction which has a sensi- and somewhat greater sensitivity HHS00000198 Page Page 3 Dr. M Schaffner Page that the species confirmation considered for tremolate tremolate If species is found, confirmation and elec- species species found confirmation species present in fiber either either optical optical microscopy the is present obtained fiber This form microscopy microscopy tron microscopy This is necessary because tremolite pattern of chrysotile occur in a non fibrous pattern - diffraction that antigorite the chrysotile fibrous fibrous form is is the same as sample antigorite presence fibrous eral. eral The adulterated adulterated presence tremolite chrysotile considered shown procedure procedure procedure An alternative tremolite procedure based solely shown above less expensive procedure available technique microscopy microscopy which However expensive and and more technique might be proposed proposed difficulty difficulty optical microscopy microscopy alone that completely miss the presence presence chrysocile chrysocile microscopy talc are submicroscopic submicroscopic which may finely well well be the case ro to this source error Enclosures _ : Alfred Weissler Weisser Weisser . Speer easssstot FINAL REPORT L^'vin RAY POWDER DIFFRACTION ANALYSEOSF COMMERCIAL COSMETIC POWDERS 4 PhlogoSample Tale Chlorite pite my 70 % 75 100 n.d. 3 99 100 nodo nodo nod n.d. 15 n.d. 95 % % 5 805 % 58 865 % % 95 % 3 5 89 75 % 1010 935 % % 11 11 90 20 % .12.12 100 n.d. nodo 1313 60 n.d. n.d. 14 31 50 % 15 16 . 100 eon nodo nodo oom nod 10 17 60 18 90 .19 97 * 22232 35 22232 67 22232 59 % 22232 42 22232 948 25 95 26 95 27 78- : ca.20 ca.20 30 % 1 60 25 35 50 % % % nodo .1 % % % % % % % % % 45 % n.d. . 08.94 31 97 47 32 80 do 1g 50 75 12 13 12 35 Gee Quartz n.d. Dolo mite n.d. n.d.n.d. n.d.n.d. n.d.n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d. 3000 n.d. n.d. % n.d. % n.d. % % n.da n.d. 10 nod % n.d. n.d. % n.d. 10-0 n.d. 8 n.d. 25 nodo % % | nodo % % n.d. n.d. n.di n.d. % % n.d. nod % % .% nodo n.d. n.do 20 n.d. nado n.d. % 2 % n.d. % % Trem- Calcite elite , n.d. n.d. Chryso ' tile Nodo Other Spesies n.d. n.d. n.d. nodo nod nodo n.d. n.d. nod nod n.d. nod n.d. - n.do n.d. CaUndecyl n.d. n.d. ? n.d. nodo nodo n.d. n.d. | n.d. Nodo Nodo n.d. n.do n.d. n.da n.d. nodo nodo nido nodo Nodo nod n.d. nod --y n.d. n.do n.d. ' n.d. ZnUndecyl ote oo Kaolin Staroh n.d. nodo nod nodo n.d. n.d. nodo n.d. n.d. n.d. - n^,d n.d. n.d. n.d. Iboda " nodo noda nodo nodo n.do n.d. 10 ned n.d. n.d. g nad nado nodo ? n d .n.d neda ? n.d. n.do < Kaolin Mica n.d. n.do nad = n.da =Kaolin n.d nodo n.d. n.d. n.d. n.d. nodo nod HHS00000200 Page 2 ample 33 Phlogo- Quarte o& Tale Chlorite pite Quarte 55 40 % nod 34 785 % % 35 35 780 36 3.81 37 38 % % 50 % n.d. % 10 n.d. nodo 38 87 5 %% % 39 94 % nod % 40 67 25 nodo % 41 33 % % % 42 89 % nodo = n.d. 43 97 nsdo ndo = 3 44 45 66 30 n.do d 46 48 40 n.d. % 47 98 nodo nodo nod 48 88 % 25 _ % 49 100 .ned n.d nodo 50 95 % nod nod 51 100 52 87 53 90 54.a.87 54.a.87 54.a.87 54.a.87 ... 80 nodo % % 3 15 n.d. nd 20 % 20 0 % % nod nodo % ... 90 70 Nodo % 57 80 58 96 59 oa.90 60 oa.60 oa.60 63 38 62 _ 85 63 87 64 0.80 65 ca.78 ca.78 66 84 15 nod nodo 30 40 of % % 15 5 nodo n.do ; da noda nodo 49 .3 nodo Nodo % nodo % 25 % 35 = % n.d. % nodo 3 67 78 15 68 - 80 15 69 97 15 n.d. n.d. Nodo nd n n.d. -- -- ---- Trom- mite Calcite olite 3 n.d. nod ~ Chryse tile n.d. Other Species % n.d. nodo n.d. % n.d. n.d. n.d. nodo nodo n.d. n.d. n.d. Mioa % nodo nod n.d. | % nodo n.d. Nodo nod % % nod n.d. nodo nodo n.d. n^,d^, nod n.d. n.d. % noda n.d. nodo n.do n.d. nodo PP . . . Kaolin - % nodo n.d. nodo nodo nado n.d. n.d. nodo 20 nedo nod % n.d. n.d. n.do- nodo nodo n.d. n.d. n.d. n.d. 25 45 n.d. n.d. , nod nodo nodo da nid nado node n.d. n.d. * n.d. n.d. nod ? nud x nido nodo ' n.d. n.d. % n.d. n.d. nodo n.a. nid nod nodo n.d. Nodo .n.d nodo % 18 nodo nodo 30 40 30 nod 20 - nodo 10 nido nod nod nod nado nod n.d. n~ |d nodo nada nod % nad nado n.d. nado | nodo nod A. 12 - Starch ZnStear a ZnStear = ZnStear % % n.d. a " % -- -- ---- n.d. Nodo n.d. 20 nodo n.do HHS00000201 page 3 Phlogo- ample Tale Chlorite Chlorite pite Quarta 70 28 60 n.d. 50 73 85 20 n.d. % 72 860 % 3. % 73 02.80 10 n.d. % 74 90 n.d. n.d. n.d. 75 76 77 78 079 60 81 : 82 75 75 92| 85 % ca.50 ca. 02.78 % n.do -- -- ---- 20 % 40 % 12 -- od % % % % nado % % nodo % % % nod % % % 83 02.84 02.84 _ % 84 ca.92 % 85 oa.86 % . 86 ; 87 85 2.30 .406 50 88 61 n.do 89 68% % 90 55000 n.d. _ .91 .91 92 ca.50' % 64 n.d. 93 55 94 82.46 82.46 28. % .95 86 nodo 96 28 nodo 97 31 % 98 ca.40 ca.40 Nodo % nod nodo % n.do Nodo % % n.d. n.d. 400 3d Nodo % % % n.d. n.d. n.d. % % % %| % n.d. % % % % 6 5. n.d. ca.40 ca.40 nodo % n.do n.do ea.80 63 630 93 91 . 10 % % % 3 % % nodo nod nod % n.d. | 7 % nodo 20 Dola mite % n.d. n.d. % % 15 10 nodo nodo % % nodo % 3 % 3 07 07 % 12 25 10 25 % 20 25 35 % 45 35 % % % % 15 45 % Calcite * Trem- Chryse- olite tilo Other Species nodo n.d. % n.d. 53 % Nodo Nodo nod -- -- ---- 85 ' n.d. n.d. noda nod n.d. nodo nodo nod % Nodo n.d. % nodo n.d. n.d. n^,d n.d. h.d. % nod % nad n.d. nod nod % 3 % nod nod ned nodo n.d. n.d. n.d. n.d. n.d % % % nodo % % % %. % 12 n.d. n.d. n.d. nodo nodo n.d. n.d. nodo n.d. 15 10 n.d. nodo Bodo Modlo n.d n.d * ZnStear nod n.d. Reds n.d. noda nodo| i ? WD ? ? n.d. n.d. Kaolin Mica Kaolin Mica ZnStear n.d. % wa a : Fa n.do n.d. HHS00000202 4 page _ _ ample Phlege Tale Chlorite pite Quartz Dolo- mite 05 92 38 .06 917 % .07 87 % .08 .09 .10 68100 74 . 15 99 n.do. 31 425 = 40 .12 ca.60 n.d. 1% 16 2% 2% 35 12 % n.do % 35 nodo 20 35 n.d. nod % % % % 38 3,5 nod 15 nodo nodo Calcito nod nod n.d. nodo n.d. nodo nodo ModMaoda 10 - .23 14 15 .16 37 18 19 20 .21 22 23 .24 : 25 ; .26 : .27 . .28 + .29 30 31 .32 33 .34 .35 36 .37 .36 .39 75 53 53 15 40 40 n.d. n.d. n.d. n.d. | 53 40 nodo 42 35 nodo 53 49 = 40 40 n.d. n.d. 46 87 40 %- Bo o 20 56 51 54 55 75 85 35 40 nodo nodo 40 nodo 40 = n.d. 10 % nodo nodo 60 - nod Nodo 97 - nodo noda ca. 8a.92 75 = n.d. 3 % 95 % % 94 200 % 93 93 | 89 91 388 % 400 ' % 20 % nid 85 -.7 % oa.85 n.d. noda % % % % 15 % % 7000 458 % * % % % nodo nodo nodo n.d. 2000 nod nodo % n.d. % % % % % % 4 % % % nod nodo noda nado nodo nodo % 856 nodo 40 n.d. nodo n.d. . n.d. % noda 3 % n.d. nodo nod n.d. % nod nodo n.d. n.d. nod n.d. = nodo n.d. % Modo nodo % 3 % nod % nodo 20 Nodo % 35 n.d. 20 nodo nado .40 2.85 nodo nod 20 14% n.d. Trem olite n.d. nod nodo % % nod % Nodo Chrys tilo n.d. n.d. nodo nodo nodo ? Nodo nod nodo n.do nod nodo n.d n.d. nodo nodo nodo ns^o n.do nod nodo D n.d. nodo ? nado n.d. nodo 54 n.d. ? n 1 -- -- -- n.d nadi 7 n.d. n.do. nodo n.d. nodo trace n.d. ' trace trace n.d. nods n.d. n.d. n.d. ned nado nodo nodo nodo nado nodo n.d. n.d. Modo n.d. Nodo Nodo . nodo nodo nodo Nado Nado Nodo Other Specira Kaelin - Salicylic A. , Boric Boric Aci CaUndecyl ZnStear MgCO3 ZnStear MgCO3 HHS00000203 Sample 141 Phlogo- ta Tale Chiorite pite Quartz 80 n.d. n.d. 233 142 79 % 50 400 243 55 % nod % oa.70 144 oa.70 10 noda 60 . D010- Tram- Chryso- Other mite Calcite olite tile Species % = n.d. n.d. n.d. ZnStear 55 25 Nodo nado nod % MECO3 = n.d. 7 10 ~~. nada nod % Lo . ? - ZnStear - Kaolin 145 : ca.70 ca.70 . % Nodo nod 30 nod n.do 20 ZnStear Kaolin - ZnO 146 147 148 149 150 151 152 ca.85 ca.05 45 ca.50 . 80 63 08.70 n.d. n.d. 8 40 10 20 25 20 noda n.d. noda n.d. nodo n.d. asdo 4 n.d. nodo 10 % % n.d. n.d. % nodo % % so n.d. 12 . n.d. nod % 10 nodo nodo n.d. n.d. nado n.do 2000 % n.d. n.d. noda n.d. Nodo Mada ? n.d ... nodo n.d. Zn tear Kaolin ZnStear Kaolin Kaolin Pyrophyll 153 ca.80 ca.80 154 ca.70 155 ^a.04 156 157 158 79 63 78 159 160 161 ea.74 60 59 162 50 163 164 - 92 165 92 166 ca.50 167 76 168 SEXXXXXX 169 ox 170 52 .171 70 % 10 10 10 % % 10 x 255 25 = 25 % % % 40 10 == fi fi fl p.d. 10 nodo 48 nodo nodo nodo n.d. 20 n.d n.d. n.d. n.d. % nodo n.d. n.d. = 0503 n.d. n.d. noda 48 % % % % Nodo n.d. 20 % % n n.d. % . ,, .d. Se oo % % nod n.d. % .nodo % nod n.d. nod % -- -- -- nodo ? Zno Boric Zno %~ 18 20 % indo n.d. t 10 10 % % n.d. node nodo 800 n.do 7 4 we % 10 nodo trace % 10 % 10 nodo nodi node . n.d. 20 % = n.d. n.d. 10 - . 10 nod % 25 80 12 = nod n.d. n.d. 00 aoe eo ca.80 25 n.d. n.d. nodo % ... oo nodo ? n.d. ae 00 80 Gypsum 15 n.d n.d. nod 172 173 174 43 oa.99 ca. 50 n.d. % nodo n.d. 200 nodo n.d. 15 % n.d. n.d. = nodo n.d n.d. 256 n.d. nad nod ? n.d. - KaMoicla in HHS00000204 Sample Tale 175 176 ca. 86 ca.79 177 84 178 02.50 179 975 180 88 181 ca.70 182 ca.40 183 ca.76 184 185 186 187 ca.50 ca. ca. 188 705 189 72 190 ca.825 191 192 100 193 .ca.93 194 c8.947 195 97 Page 6 Chlorite % % = 10 20 nodo Phlogo- pite nod 28 % 20 n.d. de Quartz 10 15 20 % % D0100 mite n.d. n.d. n.d. % nodo nodo n.d. n.d. n.do n.d. Ila . 12 nod 25 10 20 15 noda n.d. noda nod % n.d. 20 n.di % nodo % n.d. .% n.d. = 15 12 12 200 nod % n.d. = n.d. . 25 nodo n.d. .% n.d. n^do n.d. n.da nodo n.d. 38 40 % 20 n.d. _ % nodo nado =% nodo 2 % n.d. % nodo n.d. nodo % _ Trem- Calcite olite n.d. n.d~ n.d. * Nodo n.d. nado n.d. n.do n.d. n.d. n.d. 10 n.d. nodo n.d. n.d. - node - =10 n.d. % % | 25 25 % n.do n.d. % 58 % n.d. % % nod = n.d. n.d. n.d. n.d. nod % nodo nada nod~ nodo Chrysotile ? , nodo n.d. nado n.d. 50 ~ n.d. n.d. 1 n.d 2 n.d 1 nod n.do ? 2 nod Other Species , Kaolin . Kaolin ZnO ZnO ZnO ZnStear HHS00000205 New York University Department of Chemistry 4 Washington Place Room 410 New York N.Y. 10003 Telephone 212 598-3427 ATTACHMENT TO TABLE I Memorandum to Dr. George Thompson Food and Drug Administration From S. Z. Lewin Chemistry Department New York University Re Determination of Asbestos Contents of Commercial Talcum Powders This will servteo summarize the main points on this date of July 10 1973 with respect to the of our discussion factors involved in the detection and estimation of asbestos in talc and the status of the tabulation of results of the analyses of commercially avail- able consumer products containing talcum powder My research group has been engaged in studies of talc and its accessory minerals continuously since July 1971 and we are continuing to work in this field We have undertaken to investigate the follow- ing problems A. Tabulation of the ray diffraction data for talc and all solid phases whether naturally occurring or added in the course of processing encountered with talc in mineral and pharmaceutical products industrial : cosmetic B. Elucidation of the ray diffraction spectrum 1.e. precise locations and relative intensities of peaks and variability thereof of chrysotile Assignment of the diffraction peaks to the crystal planes responsible for them and interpretation in terms of crystallogra phy of the effects of grinding orientation and sample preparation C. Investigation of the chemical properties of chrysotile antigorite chlorite tremolite and talc specifically measurement of the rates of hydrolytic and ion replacement reactions D. Microscopy both optical and electron of chrysotile and of tales containing various accessory minerals including chrysotile and tremolite E. Measurement of the degree of enrichment due to air elutria- tion of asbestos in the lightest fractions of the dust from commercial HHS00000206 F. Development of a method based on the combinatioon f ray diffraction chemical reactivity and microscopy for the estimation of the chrysbtile and tremolite contents of consumer products . these two being the only asbestiform minerals encountered all the American products examined far with only one possible exception and application of the method to the analysis of about 200 standard purchased specimens G. Investigation of alternative erential thermal analysis and density analytical methods viz diff- gradient centrifugation as alternative or supportive techniques Our results to date support the following conclusions 1. The different in chrysotile that is found in commercial talcs is generally_ significant respects from the chrysotile that occurs as . massive fibrous growths in veins in serpentine rocks That mer has diffraction peaks that may differ from the latter by is the much for- _ as 0.2 A at 7.3 A it is more reactive toward dilute acids it shows a different appearance under the microscope and its DTA endotherms and exotherm are shifted relative to those of the latter and apparently diminished 2. The presence of chrysotile as a minor constituent in tale be established with reasonable certaintoyn the basis of a the may presence of ray diffraction peaks in the vicinity of 7.23 to 7.43 A and 3.59 to 3.65 A b the pronounced weakening or complete disappear- ance of these peaks upon treatment treatment of the specimen with 1 M HCl at 80 for 1 hour c the presence of fiber bundles of visible size under 250x or higher magnification in the optical micro- scope which show a refractive index of about 1.54 these fiber bundles may be short and straight and may be coated with a bumpy encrustation of M C03M C03 or may be embedded in talc presence of fibers under the electron or other particles and d the microscope which yield an electror diffraction pattern that corresponds in values to those found in the ray diffraction pattern these fibers typically do not have a hollow central capillary running through them 3 The concentration of chrysotile in a talc may be estimated by the area measuring L- Lunde under the ray diffraction on internal standard The peak best at about internal 7.3 A standard HHS00000207 is calcium oxalate monohydrate peak at 5.83 A 4. The quantitative results are conditioned by the fact that segregation effects in tale powders are considerable the analytical method gives a reproducibility of 2 to % average deviation in replicate determinations on the same sample but different samples from the same bulk container are found to vary by as much 200 5. The quantitative results are further complicated by the fact that antigorite gives an ray pattern that is indistinguishable from that of chrysotile The HC1 treatment specified above does not affect ground antigorate if it occurs in talc has but the it is not yet same chemical known whether reactivity as antigorite ~ the ground material from massive antigorite or whether like chrysotile its _ properties may be variable depending upon the rock matrix in which . it is found 6. Subject to the qualifications inherent in the above we have obtained quantitative estimates of the chrysotile contents of about 200 commercial talcum powder specimens We have also determined the contents of the other minerals in these quartz chlorite dolomite and others products There is including tremolite no ambiguity in the identification of these latter species the quantitative results for these are also affected by the segregation problem which is most serious for those constituents present in the smallest amounts 7. Most of the commercial tales tested are free of any detectable amount of any of the asbestiform minerals according to the criter^,a enumerated above Thus there appears to be an adequate supply of tale for which there is no ambiguity about the absence of chrysotile or tremolite In about 10 of the samples tested there appear to be definitely detectable amounts of either chrysotile or tremolite present HHS00000208 F.620 ~ TABLE II INTERLABORATORY COMPARISON OF ANALYTICAL RESULTS FOR TREMOLITE IN COSMETIC TALCUM POWDERS SAMPLE NO N. U. RAY DIFFRACTION RESULTS FDA OPTICAL MICROSCOPY PFIZER RAY DIFFRACTION 1 d not detected 2 n.d. 3 d 4 nd 5 d 6 d 7 d 00 n : 9 n 10 n.d. 11 n.d. 12 ; . n.d. 13 n.d. . 14 d 15 d 16 C 17 n.d. .18 . 19 d - d 20 n ; 21 d 22 n.d. x HHS00000209 SAMPLE NO 23 24 25 26 27 28 29 30 31 22 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 N. RAY DIFFRACTION n.d. n nd n.d. n.d. d d n.d. n.d. d d A. d d n.d. d d n.d. d n.d. n.d. ~~ d n.d. n.d. n.d. RESULTS FDA OPTICAL MICROSCOPY PFIZER RAY DIFFRACTION . . : . . . HHS00000210 SAMPLE NO 49 50 51 52 53 54 55 56 -57 58 59 60 61 62 63 2015 65 167 167 68 69 70 722 72 73 ; 74 N. U. RAY DIFFRACTION d n.d. nd d o. d d d d n.d. B. d n.d. n n % n.d. ; n.d. d % d d n % d d d RESULTS += FDA MICROSCOPY OPTICAL MICROSCOPY PFIZER RAY DIFFRACTION . d d n moderate amount small amount d d small amount = cane iin meereaen, pour ab bo sree UREN EE a IR TNA at > . SAMPLE NO 75 76 77 78 79 80 81 82 83 . 84 85 86 87 88 89 90 91 20 93 94 95 96 97 98 99 100 . _ U. RAY DIFFRACTION d % % % n.d. n.d. n.d d n d d d d 4 % % n.d. % % % % % 12 d n.d. n.d. RESULTS FDA OPTICAL MICROSCOPY PFIZER RAY DIFFRACTION . small amount moderate amount . d n.d. d large amount large amount large amount large amount large amount large amount moderate amount large amount , d very small amount : 1.6 1.9 | 0.7 8.1 etter, wrem n are es SAMPLE NO 101 N. RAY DIFFRACTION 15 102 103 104 10 d n.d. 105 d 106 107 n.d. n.d. 108 % 109 110 % n 111 112 113 114 ' 115 17 n.d. d d " d 116 . d 117 , n.d. 118 119 n.d. . n.d. 120 n.d. 121 n.d. 122 123 124 125 126 n.d. d , d d d - RESULTS FIA v4 OPTICAL MICROSCOPY large amount ; large amount PFIZER RAY DIFFRACTION 10 to 15 n . : . ; - HHS00000213 - SAMPLE NO ; 127 128 129 130 131 N. U. RAY DIFFRACTION n.d. d n.d. trace trace RESULTS FDA - OPTICAL MICROSCOPY 132 133 d - d 134 135 136 137 d n.d. d 1. ot 138 n.d. 139 140 141 142 143 144 d n.d. n.d. n.d. % .5 145 146 . 1. , D. 147 148 149 150 d % , % . n.d. small amount present 151 152 n.d. . n.d. n.d. PFIZER RAY DIFFRACTION . HHS00000214 * SAMPLE NO 153 154 155 | 156 157 158 159 160 161 162 .163 164 165 166 167 168 169 170 171 172 173 174 175 176 177 178 N. RAY DIFFRACTION d % d 10 d n.d. d % d % d d RESULTS - FDA OPTICAL MICROSCOPY / PFIZER RAY DIFFRACTION small amount approx 0.5 large amount d 3.8 HHS00000215 SAMPLE NO 179 .180 .180 181 182 183 184 185 186 187 188 189 190 191 192 193 194 195 Y. X RAY DIFFRACTION DIFFRACTION n.d. d n.d. n., . % % d n.d. % % 17 n.d. n.d. n.d d n.d. n.d. RESULTS FDA > OPTICAL MICROSCOPY PFIZER RAY DIFFRACTION , Footnotes * a b C. Work done by Mr. Arnold E. Schulze Division of Microbiology See Appendix A Pfizer Inc .; Minerals The use of a dash means Pigments and Metals Division Easton Pa that the powder does not contain talc and therefore is not expected to contain tremolite or chrysotile as contaminants No asbestos was found HHS00000216 SAMPLE NO 1 2 3 4 5 6 7 .8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 ~ TABLE III INTERLABORATORY COMPARISON OF ANALYTICAL RESULTS IN COSMETIC TALCUM POWDERS FOR CHRYSOTILE N. RAY DIFF FDA OPT MICR RESULTS PFIZER RAY DIFF .n.d .n.d not detected d COLUMBIA SCIENTIFIC a n.d. d d ? R. d . , . n d n.d. n.d. d n oe n.d. n d n , d n.d. HPBC HHS00000217 AMPLE NO 23 sON. Y. RAY ) DIFF ? 24 25 n.d. ? 26 ? 27 d 28 d 29 d 30 d 31 n.d. 32 n.d. 33 d 34 n.d. 35 d 36 * d 37 n.d. 38 . d 39 n.d. 40 d 41 n 42 d 43 n 44 oe 45 d 46 n.d. 47 n.d 48 n.d. . FDA OPT ) MICR RESULTS PFIZER RAY DIFF ; , . ' COLUMBIA SCIENTIFIC HPBC , . . . HHS00000218 SAMPLE NO 49 50 51 52 53 54 55 56 57 58 59 60 61 83 63 ee vee 64 eae A 65 66 67 , 89 69 70 71 72 73 74 N. . RAY DIFF) n.d. FDA OPT MICR) RESULTS PFIZER RAY DIFF) n n.d. n.d. d ? D.d. n.d. d d d d d d n.d. n.d. , d 1. d n n.d. . mid % d n n.d. n.d. d d d d d 1. d d d d COLUMBIA SCIENTIFIC : HPBC . . , . eer wane se HHS00000219 SAMPLE NO 75 76 77 78 79 80 81 880 83 84 85 86 87 88 89 . 90 N. RAY DIFF) d n.d. d d d ? ? ? ? ? . ? ? ? 5 % % 91 22 93 94 % % 4 ? 95 % 96 10 97 15 FDA OPT MICR RESULTS PFIZERA RAY DIFF) n.d. n.d. d ) d n d d possible in talc grains n.d. possible in talc grains much n antigorite ? possible in talc grains moderate antigorite d n COLUMBIA SCIENTIFIC -- -- -- -- inconclusive inconclusive inconclusive 0.1 inconclusive HHS00000220 AMPLE NO 98 99 100 N. Y. RAY DIFF n.d. n.d. Did 101 n 102 103 104 105 106 107 108 109 110 111 112 113 114 115 116 117 118 119 120 121 122 7 d n.d. n.d. n.d. n.d. n.d. ? d n.d. n.d. n.d. n.d. .n.d d ? d d 3 n.d. ? _ RESULTS FDA OPT MICR PFIZER RAY DIFF d possible in talc grains much . antigorite d d d . : COLUMBICOLUAMBIA SCIENTIFICh MPBC d Be TAN BEE AI ERT HHS00000221 AMPLE NO Y.U. _ RAY DIFF 123 124 . ? I 125 ? 126 d 127 d 128 d 129 n.d. 130 131 132 133 Trace n.d. n n.d. 134 d 135 n.d. 136 d 137 d ; 138 d 139 n.d. 140 n.d. 141 d 142 d 143 | 144 10 ? 145 "% 146 d 147 n.d. 148 d for FDA OPT MICR ) RESULTS PKIZER RAY DIFF) . : ; d COLUMIBA SCIENTIFICb HPBC ; HHS00000222 AMPLE NO 149 150 N. RAY DIFF - | ? d FDA OPT MICR RESULTS PFIZER .DIFF n.d. COLUMBIA SCIENTIFIC HPBC 151 152 n d n.d. 153 154 d d . d ; 0.1 d 155 2 156 n.d. 157 % ., 158 d 159 ? . 160 trace 161 n 162 163 164 165 n.d. 10 % ? a possible in talc grains d . inconclusive = d 166 167 168 169 170 171 ? n.d. =: -- % d | oo , 172 D. - 173 2 174 n REE EP SST ONS TEE Hsp as: eee ae SP erS eh aT T Ee, HHS00000223 SAMPLE NO 175 N. U. RAY DIFF ? FIA OFT MICR RESULTS PFIZER" RAY DIFE) COLUMBIA SCIENTIFICb HPBC 176 ? 177 d 178 179 180 181 ? n.d. d n.d. 182 ? 183 ? 184 n.d. 185 n.d. 186 ? 187 n.d. 188 ? 189 d 190 ? 191 d 192 n 193 ? 194 ? 195 n.d. : ootnotes : Pfizer Inc. Minerals Pigments and Metals Division Easton Pa Columbia Scientific Industries Austin Texas using Differential Thermal Analysis Health Protection Branch of Canadian Government Ottawa by electron microscopy oral communication Drs Pontefract and Cunningham Antigorite is a fibrous form of the same mineral as chrysotile By transmission electron microscopy HHS00000224 620 TABLE IV KEY TO SAMPLE NUMBERS OF COSMETIC TALCUM POWDERS AMPLE NO : PRODUCT NAME 1 Ammens Powder Medicated 2 Amolin Deodorant Powder 3 Aquamarine Cooling Spray Bath Powder 4 Bagatelle Amber Dusting Powder 5 Bourjois Bath Powder FURTHER IDENTIFICATION Bristol No. IF25 Norwich Revlon 143 Corand DCH 6 Caldesene Medicated Powder . 7 Cashmere Bouquet Body Powder 8 Chanel No. 5 Bath Powder Pennwalt 5274 Palmolive . 9 10 11 .12 13 14 15 16 '17 18 19 Countess Rocheau Cake Dusting Powder Crepe De Chine Dusting Powder Millot Crepe De Chine Poudre Mist Millot Cuticura Talcum Powder Desenex . Desitin Baby Powder Desitin Baby Powder : Diaperene Baby Powder Dorothy Gray Secret Of The Sea Dusting Powder Emeraude Talcum Powder . ~ English Leather Jergens House of Fragrance L1132 \ House of Fragrance Purex 07170 Phermacraft Pfizer 1139Z 3/29/72 Pfizer 115A 5/10/72 Breon E1030 Coty 355-4010 Mem 20 Faberge Music Dusting Powder 21 Friendship Garden Dusting Powder 22 Friendship Garden Dusting Powder 23 Friendship Garden Dusting Powder mL 2891 Shulton 3/27/72 : Shulton 5/9/72 Shulton 7/13/72 HHS00000225 28 29 30 31 32 33 34 35 36 37 38 39 40 41 43 44 45 46 47 48 49 PRODUCT NAME Heaven Sent Aerosol Bath Powder Mist Heaven Sent Bath Powder . Helen Pressl Little Lady Importa Spain Mens Talc Isis Floral Talcum Powder Johnson's Baby Powder Johnson and Johnson Medicated Powder Koscot Beauty Dust of Mink Lanvin Arpege Dusting Powder Lanvin Arpege Powdered Mist Lanvin Arpege Talc Lewis Baby Powder Loves Fresh Lemon Glossy Powder Macy's Scented Borated Talcum Macy's Talcum Apple Marcelle Dusting Powder Allergenic Mary Chess Perfumed Dusting Powder Mennen Baby Magic Powder Mennen Quinsana Foot Powder Merck Talc Product No. 6460 Lot No. 6460 Mexsana 2387 Medicated Powder Old Spice Body Talcum Persian Lilac Deluxe Dusting Powder Persian Lilac Spray Bath Powder Pond's Perfumed Talc Body Deodorant Dream Flower Prince Matchabelli Beloved Spray Powder FURTHER IDENTIFICATION Rubinstein Kubinstein 028Q 3612 1288 Manley & James 2K4 B112 H202 8039301 Plough Shulton April Showers LFN April Showers B200B 115B Ste RE ATES ETS HHS00000226 53 54 55 56 57 58 60 19 63 64 65 66 67 68 69 70 72 73 74 75 PRODUCT NAME Quest Deodorant Powder Replique Spray Bath Powder Riviana Foods - Italian Stearin Talc September Morn By Pond's Seven Winds After Bath Tala U P Talc Vaseline Intensive Care Baby Powder Yves Saint Laurent Rive Gauche Spray Talc BT Baby Powder Zeasorb Super Absorbent Medicated Powder Ambush Dusting Powder April Showers . Avon Unforgettable Perfumed Talc Beloved Perfumed Dusting Powder Prince Matchabelli Coty Face Powder Rachel Desert Flower Spray Bath Powder Emeraude Dusting Powder Emeraude Spray Dusting Powder Faberg^'Flambeau Deodorant Spray Powder Jean Nat^'Spray Bath Powder Jeris Talc Flesh Jolie Madame Dusting Powder Balmain Lady Esther Face Powder Rachel Max Factor Face Powder Rachelle Medicated Comfort Powder OH de London Talc . FURTHER IDENTIFICATION Parfums Raphael 004 For Rice 19B DuBarry 021085 I 209 F1021 Stiefel 9884 ShulFt1oBKnI Coty Coty 1 AEY 37 WBF 1 247 Parke Yardley 498 ete PPUDSe ASAT HHS00000227  a tt ttt erenc ente ree er MPLE NO PRODUCT NAME 76 To Know Me is To Love Me - Tinkerbell 77 Touch And Glow Face Powder Creamy Peach 78 Toujours Moi Bath Powder 79 Yardley April Violets 80 Chantilly Disting Powder 81 Cashmere Bouquet 82 Jean Nate Tale 83 Mennen Shave Talc 84 Shower To Shower Body Powder 85 Pure Baby Powder Dart Drug 86 Pond's Dream Flower Perfumed Talc 87 Almay Allergenic Face Powder 88 Constance Carroll Bouquet Talc 89 Kiss Talcum 90 Flamingo Dusting Powder Tussy 91 Lander Lilacs And Roses Talc Mavis Talcum Mavis Body Powder Tangee ZBT Baby Powder 97 98 99 Blanchard's Dusting Powder Born Wild Dusting Powder Lander Gardenia And Sweet Pea Talc Lander Lilacs And Roses Deodorant Body Talc 100 Miss Dior Dusting Powder 101 Tai Winds Spray Tale FURTHER IDENTIFICATION . Tom Fields Ltd. Revlon Corday 4908 Houbigant 11F on 345 B 81 Johnson & Johnson 5507BG K 11C 013D 013D Kerkoff L1047 Vivaudou Vivaudou Tangee B0048 Del Labs Avon DCC 1272 2-14-72 HWS a ALD SSTMIO EET 735: .08 109 110 FRODUCT NAME Tosca Dusting Powder Coty L'Aimant Talcum Powder Coty Emeraude Talcum Powder Coty L'Aimant Dusting Powder Coty Impr^'vu Dusting Powder Coty Muguet des Bois Dusting Powder Revlon Intimate Perfumed Bath Powder Jean Nate Bath . Powder : Jean Nate Spray Bath Powder 118 119 120 121 122 123 124 125 Old Spice Body Talc Dr. Scholl's Foot Powder Paberge Xanadu Luxury Bath Powder Spray Faberge Zizanie de Fragonard Faberge Tigress Bath Powder Faberge Woodhue for Men Faberge Brut for Men Shower Buff Over Body Powder Faberge Talc Faberge Aphrodesia Bath Powder Faberge Straw Hat Bath Powder Faberge Aphrodesia for Men Shower Buff Faberge Xanadu de Luxe Bath Powder Faberge Woodhue Bath Powder Faberge Music Dusting Powder Faberge Flambeau Bath Powder FURTHER IDENTIFICATION 1JJ 01A 1M IDE 200 241 Lanvin ~- Charles of the Ritz 2137 Lanvin - Charles of the Ritz 2103 Shulton Inc. MFO 20517 Y1 2132 Ref 61159-019 Ref 2052-003 Ref 5027 0252 Ref 5400 raw material from France Ref 2052 2172 2 patmess Ref 5027 Ref 1244-028 2342 Ref 2052-002 Ref 0714-018 3121 Ref 2052 3471 2Ss TGA et HHS00000229 Sa IMPLE NO PRODUCT NAME 126 127 128 Mennen Baby Magic Walgreen's Crib Age Caldesene Medicated Powder ' 129 Desiten Vaseline Intensive Care 131 Johnson and Johnson Medicated Powder 132 133 134 136 137 139 140 141 142 Johnson Baby Powder Johnson's Baby Powder Johnson's Baby Powder Johnson and Johnson Medicated Powder Johnson and Johnson Shower to Shower Body Powder Johnson and Johnson Shower to Shower Body Powder Johnson and Johnson Shower to Shower Body Powder Avon Brocade Spray Avon Bird of Paradise Spray Avon Tai Winds Spray Talc Mennen Bath Tale 143 Pin Talque 144 145 146 147 148 149 150 Overton's Brown Face Powder Softee Face Powder Westport Face Powder Hazel Bishop Pressed Powder Lady Wayne Face Powder Solitaire Cake Makeup Dreamglo Pressed Powder FURTHER IDENTIFICATION 108T 109T 0452K C 5122 0709x1 0872K 31602 B1652 4065 . A308 Perfection Beauty Products Inc., Pearl River N. HHS00000230 MPLE NO PRODUCT NAME 151 152 153 154 Early American Old Spice Talcum Powder Corsage Dusting Powder Ammens Powder Medicated Bismoline Medicated Powder 155 156 157 158 159 160 161 162 163 Rite Aid Pure Baby Powder Warner Pure Baby Powder Mavis Imported Talcum _ Avon Brocade Perfumed Talc Avon Blue Lotus Perfumed Talc Avon Beauty Dust Refill - Charisma Avon Elusive Beauty Dust Refill Avon Regence Perfumed Talc Pinaud Clubman Talc 164 165 166 Grand Union Baby Powder Cashmere Bouquet Almay Face Powder Soft Beige 167 Tawny Tone Body Talc From Black Heritage 168 169 170 Colgate Tooth Powder Dr. Lyon's Tooth Powdar C Bouquet T^lc 171 172 173 174 Tangee Dusting Powder Jeris Talc Corsage Dusting Powder Lander Gardenia & Sweet Pea Deodorant Body T^tc FURTHER IDENTIFICATION Lander 101672 4212DX Supplied by Mfgr List No. 719 Lot 201 Supplied by Mfgr Beauty Mustus Inc. Greenwich Conn . Winarick Inc. Distr by F. W. Woolworth 2662 George W. Luft Co. 2762 Winarick 2732 Lander Co. ) ents sates vee HHS00000231 AMPLE NO 175 176 177 178 179 180 PRODUCT NAME Lander Baby Powder Lander Lilac & Roses Body Talc Beloved Perfumed Dusting Powder Jean Nat^'Talc No. 60 Jean Nate Spray Bath Powder Tinkerbell Body Talc 181 182 183 184 185 186 187 188 189 0190 191 192 193 194 195 Yardley Sigh Shadow Brush Eye Shadow Max Factor Face Powder Rachelle Tweed Bath Powder Lentheric Yardley Next to Nature Sheer Pressed Powder Yardley April Violets Dusting Powder Yardley Red Roses Dusting Powder Yardley Springflowers Talc Yardley White Lavender Talc Yardley Red Roses Talc April Showers Deodorant Talc Chantilly Houbigant Dusting Powder Tinkerbell Desting Powder Tinkerbell Powder Mitt Tinkerbell Dusting Powder Tinkerbell Body Talc FURTHER IDENTIFICATION Prince Matchabelli 235A 2264 2101 Tom Fields Ltd. Div of MEM Ref No. 721 Supplied by Mfgr) Yardley 44 A2 162 165 260 271 214 Ref No. 9882 2JBB Tom Fields Ltd. Tom Fields Ltd. Tom Fields Ltd. Tom Fields Ltd. HHS00000232