Document GKRd52bgym9OJL5Nzn8zbjkdn

EMORANDUM DEPARTMENT OF HEALTH, EDUCATION, AND WELFARE PUBLIC HEALTH SERVICE _ FOOD AND DRUG ADMINISTRATION 1 ^ ; Dr. Robert M. Schaffner, Director Office of Technology (BF-400) 3M : Dr. Alfred Weissler, Acting Director Division of Color Technology (BF-430) iJECT: Summary and Comments on Prof. Levin's Analytical Results for Asbestos in Talc 1. The purposes of this memorandum are to present a summary of the analytical results for asbestos in Cosmetic talcum-type powders obtained by Prof. Seymour Z. Lewin of New York University in his role of consult ant to FEA; to compare his results with those obtained by other labora tories 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 talc, 2. I 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-recognized expert on mineralogical chemistry and because he is a member of the academic community and there fore likely to be impartial in a confrontation between industry and government. Furthermore, his competence had previously been recognized by industry (by virtue of their own use of him as a consultant) which appeared to confer a desirable immunity against possible industry attacks on the validity of the results. 3. Dr. Lewin1s findings are shown in Table X; the key to the identities of the numbered samples is given in Table TV, Please note also the ex planatory comments in Dr. Lewin's memo of July 10, 1973, which is an Attachment to Table I. No varieties of asbestos other than chrysotile (a serpentine) 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 chryso tile in an additional 18 of the samples. These results were obtained primarily by means of X-Ray diffraction, supplemented in some cases by optical microscopy and other techniques. 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 X-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. EXHIBIT WCD-26 Page 2 - Dr. Robert M. Schaffner 4. In Table II, I have compared Dr. Levin'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 means of X-Ray diffraction). This comparison, which was undertaken in order to obtain additional information on the samples, shows good semi-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 X-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 5% and 10% 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 Johnson 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 lgica! species. Moreover, with regard to the two varieties of asbestos of concern here, it is unfortunate that the one which is a clear inhala tion hazard to man, namely chrysotile, poses an intrinsically more dif ficult analytical problem than the othe^ tremolite, which has not yet been shown to present a biological hazard. This is due in part to the less prominent X-ray diffraction peaks of chrysotile and to the fact that the fibers are often too small to be seen in the optical microscope. 7. In connection with a proposed new regulation on the safety of cos metic talcum powders, we face the problem of specifying an analytical test for asbestos which must be satisfied by the powders if they are not to be considerated adulterated. On the basis of information available at present, I recommend consideration of the following procedure. The powders shall be examined first by X-ray diffraction, which has a sensi tivity of the order of 1% for chrysotile and somewhat greater sensitivity Page 3 - Dr. Robert M. Schaffner for tremolite. If either species is found, confirmation that the species is present in fiber form is to be obtained by optical microscopy and elec tron microscopy. This is necessary because tremolite is known to occur in a non-fibrous form, and the X-ray diffraction pattern of chrysotile is the same as that of antigorite, a non-fibrous form of the same min eral. The sample is considered adulterated if the presence of fibrous tremolite or chrysotile is shown by the above procedure. An alternative procedure, based solely on optical microscopy (which is a less expensive and more widely available technique) might be proposed. However, the difficulty with optical microscopy alone is that it may completely miss the presence of chrysotile if the fibers are submicros copic, which may well be the case in finely-milled talc* X-ray diffraction is not subject to this source of error. Enclosures Ph. D. FINAL X-RAY POWDER DIFFRACTION ANALYSES .OF COMMERCIAL COSMETIC fWEERS '- t fhlge= ct= Sampi Taie Chiotte Pite Quarts % 70$ 3$ 2 100$ icd0 3 99$ Hodo 4 100$ oda 5 95$ 2$ 6 80$ 2$ 7 86$ 7$ 8 95$ 2$ 9 89$ 7$ 10 93$ 3$ II 90$ 2$ 12 100$ Hodo 13 60$ nodo 14 31$ 50$ 15 100$ do 3,6 7$ nodo 1$ nodo 3$ 5$ 2$ 3$ 2$ 2$ 2$ nodo n*d0 .2 $ nda ora nodo nodo I\ode Hod nodo nodo 3$ riodo- 2$ 2$ 4$ riodo nodo 10$ riodo 17 60$ 18 90$ 19 97$ 20 35$ : 21 67$ 22 59$: 23 42$ 24 94$ 25 95$ 26 95$ 27 78$ 2 8 ea,,20$ 30$ 4$ ' 1$ 6o$ 25$ 35$ 50$ 1$ 2$ 1$ n,do 1$ 4$ 2$ 2$ 1$ 2$ 1$ 2$ 2$ 3$ 4$ 2$ Dodo nodo 2$ nodo 4$ 3$ nodo 3$ . 3$ nodo TKe d a Ho d o don & 29 ea,,94$ nodo 2$ n Qdo. 30 97$ 1 $ 2$ n o d 31 47$ 50$ 2$ 3$ 32 G0$ 7$ 3$ 2$ Dolc= Trenv= mit .ei Calcite elite t- HeGLo Hedo Hed n0do Hodo Hedo Hod Hedo Hd Hodo Hodo Hodo nodo n*do n.de n0d0 Hodo n<>d0 2$ Hado nda nod nodU nfld0 nodo Hade nodo ndo nodo nQdo 2$. Roda Hodo Hodo Hodo Hodp nodo nodo Hodo 7$ Hodo nedo nodo nodo nod `~rnT~> C5<P co 6$ 2$ nodo Hodo 3$ 5$ 3$ nod nodo Hod. 2$ Ho do 2$' nodo 8$ 8$ nodo Hodo nado ndo Hodp Hoda Hodo n 0 do B do H edo rio d o 10$ tio d o Heda H o do H e do nodo nodo Hodo nodo nodo nado n* do n'-sd Rodo ndo ndo iitdo ho da H o do n.do 6do 1 Chryso- Other tile Species Hode> Hodo Hodo Hdo nodo Hodo CaUndeeyl ? Hdo ndo n0do * nodo do nodo ZnJndeeyl riodo n0do ' C>cp Kaolin Starch ndo nodo Hodo Hode nodo nodo ? nodo ? Ho do nodo nodo ndo no do Hodo Kaolin^ Mica Kaolin ?ag 2 Fhlgo= &<= Blo> m t m M ' Tale 0hlrtt J i k . Qn&jpfcg' m ite 33 55$ 40$ 2$ nodo 3$ 34 r 7$ 4$' ' 3$ 8$ 35 78$ 5$ 2$ 10$ 5$ 36 @&<>8i$ 4$ riodo node Rada 37 38$ 50$ 38 87# 5$ 5$ node 4$ 2$ 7$ 2$ 39 94$ 3$ Hoilo 3$ Redo 40 67$ 25$ 41 33SS 8$ node 3$ 2$ . 2$ 5$ 5$ 4a 89$ 6$. nodo Rodo 3$ 43 97$ Astia n9do 3$ Hod 44 cscs <T3C=> =>= e=><=j 45 66$ 30$ nod nd. 4$ 46 48$ 40$ Roda 5$ 7$ 47 98$ Redo n*de Reda Hodo 48 88$ 4$ 2$ 2$ 4$ 49 100$ ndo nodo. Redo Hodo 50 95$ 5$ nod. Rode Hoda 51 100$ Redo riodo Rdo Rod 52 87$ 8$ 2$ 3$ Hod0 53 90$ 4$ 2$ 2$ 2$ 54 ,a87$ 3$ 4$ Redo 4$ 55 80$ 15$ zido 5$ Rado 56 90$ 7$ EUdo 3$ node 57 80$ 15$ Rodef Hodo 5$ 58 96$ nado tiedo 4$ Redo 59 cac90$ 6o oa<,60$ 61 38$ Heda 30$ 40$ tUdo Hod riedo .3$ Hod 4$ Redo 7$ 18$ 62 85$ 2$ mdo 3$ Rodo 63 87$ 2$ 2$ 4$ Redo 64 eao8o$ 5$ 65 ca<,78$ 15$ 3$ . 2$ nd0 Rode 3$ 4$ 66 84$ 5$ 3$ . 3$ 3$* 67 78$ 15$ 68 80$ 15$ 69 97$ 1$ n,,d Hodfl node Rede Hodo Hodo 5$ 5$ Rodo Trro- hrys= Calelt . o l i t e t i l Redo Ho(lei Redo Redo Redo Rod, Redo Redo Rode nd0 nd1 Red Rede Rode Redo Rede n.d Rode Rede Rado ndo Redo nodo Redo Rede Rodo Redo 2$ n&d0 Rdo Rodo n.d 009 C53 Rode OCB Rode nd0 Redo Rodo Hodo Rode 2$ node Redo Redo Rode Rode Rode nodo Rede rdo Redo Hodo Rede Rede Redo nod Redo Rod Hodo R#de Rode Rede Reds ? Rod Redb ' Hedo Redo Hodo Rod* Redo Redo Rode Redo Rede Red Rode * Rede Rode 2$ dc Rod Redo R6.de Rode 10$ Redd Hod<> Hodo 5$ Hodo Redo Redo Rodo Rde Rede . Rode Hodo Red& A2$ Redo Rode 2$ Red. Rod* >Redo 2$ Redo Redo 'thr Spasi MU 2r #Kaolin St#r@h ZnStear 2nStear0 ZnSt^afc - mm 3 aisnl Ikl Chlorife -.-Mtf TO 28$ 71 85$ 72 86$ 73 ca*80$ 74 90$ 75 75$ 76 75$ 77 9 i$ 78 85$ 79 81$ 80 &o50$ 81 <Uo80$ 82 ea<,78$ 83 a84$ 84 s a 92$ 85 sa86$ 86 85^ 87 &e30$ 88 61$ 89 68$ 90 55$ 91 ca.50$ 92 64$ 93 55$ 94 ca46$ S5 86$ 96 28$ 97 s w 98 eao40$ 60$ 10$ 5$ io$ n0d a 5$ io do Aodo 2$ 5$ 40$ 7$ 12$ 6:$ 4$ 5$ 4$ 50$ nd* ' i$ iiodo 1$ ilo dio 1$ 4$ nodo lccio 1$ n,,d9 JlCl ndo 3$ nodo n0da Hodo 5$ 4$ 1.$ 4$ nodo i :$ 2$ 5$ HoCi n0do ' 2$ Hoo l'iodo 3:$ 3$ o do Diod 4$ 3:$ n d 3$ t$ 3$ Qa&i*fcs 5$ 2$ 4$ 3$ a do Hodo 5$ 2$ 4$ Aod0 8$ 6$ 4$ riodo riodo lio do 4$ 4$ 5$ 8$ 7$ Aodo 6$ 6$ 6$ 5$ 6$ 5$ . nodo 99 ao40$ nodo 3$ siodo 5O0 a 80 ;0 63$ >02 63$ m 9353 104 91$ 10$ 8$ 2$ 3$ 3$ 4$ 3$ no d nodo %$ Aodo 7$ 3$ ilo do 2$ raifc lite 7$ na 0 ndo ilad0 n0d 2$ 5$ rudo 5$ 5$ 15$ 5$ Q$ nodo riodo nodo 3$ nodo 2$ 8$ riod0 Hodo 4$ rid0 3$ Hod 4$ n-cd0 3$ odo C$ n0do 4$ n,,do 12$ 3$ 25$ n-do io $ ildo 25$ 2$ 3$ 5$ 20$ Hodo 25$ ri0do 35$ n ado 4$ Ado 45$ nodo 35$ hodo 6$ 2$ Rado 3$. n sd0 Red Rod Had 5$ 3;$ 5$ nodo Rodo nodo Rodo n 0d ndo Rod0 Rodo EUo 4$ 5$ 3S Red 5$ 5$ 4$ 2$ 8$ 12$ lio dq 6$ 2$ 2$ nodo 4$ nodo. 15$ ndo 4$ irlodo 3$ Hoda riodo * XId 15$ 10$ Rodo Had .hffjrs fefeutz* t lM S|3i@g Rodo Rodo n>do A0ele ZnStear R0tU Roda Rodo Rodo Rodo, Rodo ? 7 t 7 ? ? ? ? 5$ 5$ y yX' 5$ * 5$ KAca 5$ ' 4$ t 3$ ' 10$ 15$ ' Addo Kaoln, Mica n qdo Rodo Kaoln, Mica ZnSfcear o do 7$ ! Rodo - rid pa^a 4 fhlg@= Be>1 -assola Tkle Ohlorit^ M E Quarts mt 05 92$ .06 91$ 07 57$ .08 8%$ 09 7L\$ 10 99$ 11 K2$ ,12 ea.060$ 3$ 3$ 5$ 10$ 1$$ n* d 0 40$ n 0do i# 1$ 2$ 2$ 3$ 1$ 2$ rudo 2$ 3$ U do 2$ 3$ nodo Ho <U 4$ 2$ 2$ 6$ 3$ 3$ ndo 15$ no do C aieit nodo Ho do nodo ndo Ho do n<,d0 n 0d s 10$ Tr&n^ t nodo Ho dg nodo 2$ 2$ ndo t$ nod 13 15$ 14 53$ 15 53$ 16 53$ 17 42$ 15 53$ 19 *9$ 20 46$ 21 87$ 22 56$ 23 51$ .24 54$ .25 55$ .26 75 .27 85# .28 60$ .29 97# 30 a088# 31 ca092 .32 95$ .33 94# 34 93$ 35 93$ 36 69$ 37 91$ 38 35# 3 9 ca <>85# 15$ 4o$ *0$ 40$ 35$ W W 40$ 8$ 35$ *0$ 40$ W 10$ rudo nodo nodo 7$ 3$ 3$ 2$ 3$ 2$ 4$ 4# .7$ rude nod n do nodo Ho do nodo n 0d o Ho do ndo 2$ Ho do n^do ide nodo 3$ n 0 dc. Ho do nodo Aedo 3$ 2$ 4$ 2$ 3$ 3$ Ilo de 3$ ilo do 3$ 3$ 3$ 3$ 15$ 3$ 6$ 8$ nodo 5$ 3$ 3$ 2$ 4$ 4$ riodo nodo 2$ n ,,de Ho do ndo n od 0 . ndo 2$ 3$ 2$ 2$ 7$ 4$ 4$ 4# 4$ 4$ 5$ 4$ 3% 4$ 4$ 3$ 3$ 8$ nodo nodo 3$ 3$ 2$ n 4do nodo 2$ 2$ 2$ 2$ 3$ ndo n odo Ho d$ nodo nd0 2$ nd Ho do n<>do n cdo nod. nodo nodo Ho do zio do rio dd zi do Hg do nodo nod9 nod He do ndo nod nodo ndo nodo Zlodg Hado Ho do nodo n<>do Ho do nodo H* do nodo nodo Rode Ho do nod R ide nod Ho d b rude Ho dg tra c e tra c e nodo n *do zud* nodo nd0 Redo Hado , J>ofi <a ,40 ea 085# n0do n o d 0 2$ 1$ H o d nodo Shrys Other til Hado n ed Ho do nodo ? nodo ned nodo nado nodo Ho do nodo Y nodo nod, ? n od 0 ? 7 7 7 nodo n 3do nodo ned trac e v np dg Ho dg Ha do Ha do Ha do Re de ned nodo ned nodo Kalin Salicylic A 0,Bric Brie Acit aUndecyl, ZsStear Mg&z> ZiiStai*o KgOT3 Sam pls T a le 'C h lo rit# 141 80# Hodo 142 79# 143 55# 144 ea70# 7# 2# IQ# 145 ca70# 3# 146 e a ,, 85# 147 ca85# 148 ca,45# 149 cao50# 150 80# 151 63# 152 oa70# 153 a080# 154 ca.70# 155 eat. 84# 156 79# 157 63# 158 78# 159 ea074# 160 60# 161 59i 162 58# 163 55# 164 92# 165 92# 166 ca*50# 167 76# 168 169 cx> 170 52# 171 70# 172 43# 173 e a .99# 174 c a 06o# lie do ru da 40# 10# 2# 25# 2# 2# 10# 10# 10# 2# 7# 10# 25# 25# 25# 2# 3# 5# 40# 10# dsXZi ^ado 10# 50# sled i# - pag 5 St? _B.it Quartz Hedc 2# 5# Hodo do 4# 3# 6# Hodo Hodo Ho-do Hodo Hodo Hodo node nod. ncdo Hod 4# node n$ dq no do Hodo 2# Hodo iiodc Hoda Hod0 2# Hodo Hedo Hodo 00 ' -- xVodo Hodo Hodo Hodo 2# 4# Rode nod 10# 5# 2# n edo Hoda 4# 4# 6# 3# 3# ftodo Hod 2# 2# 3# Rode Hodo 2# Hodo ~= 5# 5# Hodo nod. 15# - DX= mifc C a le ite 1# n<,d Trm-"' lit V nod* - 0hryso= til Rode - Other Species SnStear, MgGO^ 5# Hod, Red. Redo 25# Redo 5# 10# Hedo Hodo 5# ? ZnStear, Kaolin 3# Hod* Redo 2# SnStear Kaolin ZnO Hodo 5# Redo nod. ZnStear0 Redo 5# Rode Rode Kaolin 8# Hodo 2# Rodo 2nStaar0 12# n.do 8# ? Kaolin node 5# 10# ncdo node Hedo Rode Rode, Kaolin node Redo Redo Rode Pyrophyll It riodo n.do Rode n.do Zn0s B o r ic Acid 2# Hod. 2# Rode ZnO 2# Hod Rodo ? 3# he do 2# nod0 18# n.do .6# 8# ^ 2# 10# Hodo Hodo 4# 10# nod ? 4# 10# nod trace 4# 10# Hod0 Hade 5# 10# Redo Red 20# Rode 10# 10# k" 2# Hed. node 1# 2# Hodo n.de ? 8# Redo Redo ? 12# Hodp .2 # Xlado CP=> tfSCJ taco Gypsum BO Ica.80# pcs <acs 25# Rode Redo 8# 15# Rod Hode nde 5# Rode 2# Rode Redo Rode nod ? node Redo Redo nod. ' Kaolin, M ica pag@ 6 Phlge= Ofc= Bol<8~ Tmm- Ghrys- Otlier Saiml T&l<z hl.er'it T>t@ Ctoartg i te CaXoifce U tm t i l e ' Sb@ @s 75 ea<>86$ 3$ 176 ea>79$ 177 84$ 3$ 10$ 178 a50$ 20$ 179 97$ QoCU 180 88$ ziodo 181 cao70$ n0d<, 182 ca*40$ 25$ 183 a76$ 10$ 184 93$. 2$ 185 ca50$ 186 a50$ 8$ 5$ 18? aa85$ 5$ i 88 70$ 15$ 189 72$ 12$ 190 a082$ 12$ 191 965S 2$ 192 100$ n .d . 193 ea,93$ 2$ 194 a.94$ . 2$ 195 97$ a da n-od* .2$ 4$ 2$ n.d ndfl Hodo 15$ to dp nd0 liodo n.d. ndo 2$ n 9do 2$ ndo nodo nodo sudo n,,do 10$ 15$ 2$ 5$ 3$ nd<, ndo n 0do n edo 2$ ndc n.do 2$ 3$ 3S n.d,, nd n.d 2$ nodo ndo Hado n 0do ndo 4$ ndo i 2$ n<>do Hodo 2$ ttod Hodo ndo Qo da 4$ 2$ 3$ 2$ ndo 2$ 3$ 3$ ndo Hqdo nodo n 0do nodo n.do 10$ Xhod<> 10$ nado 25$ 25$ 5$ 5$ 5$ n 0do nodo n<d rudo 3$ nodo A9do ?' . todo t no d nodo n .d c ? Hado nodo nodo ndo nd4 rudo n*d* - ? 1$ ? 3$ rudo ndo Unde qda 7 2$ n,d 1$ t 1$ nodo rudo f ndo nodo ndo ndo nado ? 71odj ? Hade nodo Kaoln K aelin ZnO 2n0 ZnO ZnStear New York University Department of Chemistry 4 Washington Place, Room 4!0 New York, N .Y . 10003 Telephone: (212) 598-3427 ATTACHMENT TO TABLE X , 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 serve to summarize the main points of our discussion on this date of July 10, 1973 with respect to the 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 x-ray diffraction data for talc and all solid phases (whether naturally occurring, or added in the course of processing) encountered with talc in mineral, industrial, cosmetic and pharmaceutical products. . B. Elucidation of the x-ray diffraction spectrum (i.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 crystallogr; 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 talcs containing various accessory minerals, including chrysotile and- tremolite. E. Measurement of the degree of enrichment, due to air elutriation, of asbestos in the lightest fractions of the dust from commercial B3 2 P. Development of a method based on the combination of x-ray diffraction,, chemical reactivity, and microscopy for the estimation of the chrysfctile and tremolite contents of consumer products (these two being the only asbestiform minerals encountered in all the American products examined so.far, with only one possible exception), and application of the method to the analysis of about 200 standard store-purchased specimens. G. Investigation of alternative analytical methods, vis., diff erential thermal analysis and density gradient centrigugation, as alternative or supportive techniques. Our results to date support the following conclusions: 1. The chrysotile that Is found In commercial talcs Is generally, different In significant respects from the chrysotile that occurs as massive, fibrous growths In veins In serpentine rocks. That Is, the for mer has diffraction peaks that may differ from the latter by as much 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 endo- therms and exotherm are shifted relative to those of the latter (and apparently diminished). . 2. The presence of chrysotile as a minor constituent in talc may be established with reasonable certainty on the basis of (a) the presence of x-ray diffraction peaks in the vicinity of 7*23 to 7*^3 A and 3*59 to 3*65 A, (b) the pronounced weakening or complete disappear ance of these peaks upon treatment -upon -treatment- of the specimen with 1 M HC1 at 8oC 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 .5^ (these fiber bundles may be short and straight, and may be coated with a bumpy encrustation of MgC|Ch, or may be embedded In talc or other particles), and (d) the presence of fibers under the electron microscope which yield an electror diffraction pattern that corresponds In d-values to those found in the x-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 measuring the area under the x-ray diffraction peak at about 7-3 A 4- I'ntpmal standard. The best internal standard 3 is calcium oxalate monohydrate (peak at 5-83 A). 4* The quantitative results are conditioned by the fact that segregation effects in talc powders are considerablej the analytical method gives a reproducibility of 2 to 3^ average deviation in replicate determinations on the same sample, but different samples . from the same bulk container are found to vary by as much as 200^. 5. The quantitative results are further complicated by the factjzi that antigorite gives an x-ray pattern that is indistinguishable from that of chrysotile. The HCl treatment specified above does not affect ground antigorite, but it is not yet known whether antigorite, if it occurs in talc, has the same chemical reactivity as the ground material from massive antigorite, or whether (like chrysotile) its properties may be variable depending upon the rock matrix in whic^ 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 products, including tremolite, quartz, chlorite, dolomite, and others. There is no ambiguity in the identification of these latter species, but 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 talcs tested are free of any detectable amount if any of the ashestiform minerals, according to the criteria enumerated above. Thus, there appears to be an adequate supply of talc 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. -. TABLE II ' INTERLABORATORY COMPARISON OF ANALYTICAL RESULTS FOR TREMOLITE IN COSMETIC TALCUM-TYPE POWDERS SAMPLE NO. 1 2 N.Y.U. (X-RAY DIFFRACTION) RESULTS FEAa (OPTICAL MICROSCOPY) n. d. (not detected) tv.d. PFIZER k (X-RAY DIFFRACTION) 3 n. d. 4 EL. d . 5 n. d. 6 n. d. 7 n# di* 8 n. d. 9 n. d. 10 n. d. , 1 1 n. d. 12 n. d. 13 n. d. \, 14 n. d. 15 n. d. 16 c 17 n. d. 18 n. d. 19 n. d. 20 n. d. 21 n. d. 2 2 n. d. SAMPLE NO. 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 _________________ ________________________R E S U L T S _____________________________________ N. Y. U. FDA. PFIZER (X-RAY DIFFRACTION) (OPTICAL MICROSCOPY) (X-RAY DIFFRACTION) n. d. u. 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. n. d. n. d. n. d. n. d. n. d. n. d. -- n. d. n. d. n. d. n. d. N. Y.U. (X-RAY DIFFRACTION) RESULTS ' FDA (OPTICAL MICROSCOPY) PFIZER (X-RAY DIFFRACTION) n. cL n. d. 51 n; d. 52 n. d. i 53 n, d. 54 n. d, 55 n.d. 56 n, d. 57 u. d. 58 n. d. n. d. 59 n. d. 60 n. d. n. d. 61 n. d. n. d. 62 n. d. 63 570 moderate amount 64 n. d. 65 n. d. 66 n. d. 67 TL 68 n. d, 69 n.d. 70 n. d. small amount 71 3X n. d. 72 n. d. ti.d. 73 n. d. n. d. small amount N. Y.U. RAY DIFFRACTION) RESULTS FDA (OPTICAL MICROSCOPY) PFIZER (X-RAY DIFFRACTION) 75 n, d. 76 5X 77 3% small amount 78 5%. moderate amount 79 n. d. 80 n. d. n. d. 81 n. d. 82 n. d. 83 n. d. 84 n. d. 85 n. d. 86 n, d. n. d. 87 n. d. n- d. 88 4% large amount 89 5% 90 37, large amount large amount 1-67= 91 n, d. 92 57o large amount 93 57= large amount 94 47= large amount 1- 97= 95 27= ' 96 87= moderate amount 0.77= 97 127= large amount 8.17= 98 n. d. n. d. n. d. n. d. very small amount SAMPLE NO. 101 102 103 104 105 106 107 108 109 110 111 112 113 114 115 116 117 118 119 120 121 122 123 124 125 126 ____________________________ RESULTS______________________________ " N. Y.U.. F Di FFIZER ^ (X-RA.Y DIFFRACTION) (OPTICAL MICROSCOPY) (X-RAY DIFFRACTION) 15% large amount 10% large amount n. d. n. d. n, d. n. d. il-d. n. d. 2% 2% n. d. 17. 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. a. d. n. d. SAMPLE NO. 127 128 129 130 131 132 133 134 135 136 137 138 139 140 141 142 143 144 145 146 147 148 149 150 151 152 _______________________________________ R E S U L T S ____________________________________ N. Y.U. ' FIA PFIZER (X-RAY DIFFRACTION) (OPTICAL MICROSCOPY) (X-RAY DIFFRACTION) n- d. n. d. n. d. - trace trace n, d. n, d. n- d. n. d. n. d. n. d. n. d. Tl,d . n. d. n, d. n. d. 57 .57 n, d. n, d. n. d. 27 small amount 87 present n- d. n. d. n. d. n. d. 153 154 155 156 157 158 159 160 161 162 163 164 165 166 167 168 169 170 171 172 173 174 175 __________________________ ' RESULTS__________ _________________ . N.Y.U. FDA PFIZER ..... (X-RAY DIFFRACTION) (OPTICAL MICROSCOPY) (X-RAY DIFFRACTION) n, d. 27= small amount approx. 0.57, n. d. 27. 6% n, d. n. d. n. d. n. d. n. d. 107. large amount 3.87 n, d. n. d. n. d. n. d. 27. n. d. n. d. 27 n. d. n. d, n. d. n. d. n. d. n. d SAMPLE NO. 179 180 181 182 183 184 185 186 187 188 189 190 191 192 193 194 195 N.Y.U. (X-RAY DIFFRACTION') n, d. n. d. n. d. n. d. 17. 37. n- d. n- d. 27. 17. 17. n. d. n.d, n. cL n. d. n. d. n. d. RESULTS FDA (OPTICAL MICROSCOPY) PFIZER (X-FAY DIFFRACTION) , Footnotes: a. Work done by Mr. Arnold E. Schulze, Division of Microbiology, (See Appendix A) b. Pfizer, Inc, Minerals, Pigments, and Metals Division, Easton, Pa. c. The use of a dash means that the powder does not contain talc and therefore is not expected to contain tremolite or chrysotile as contaminants. No asbestos was found. SAMPLE NO. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 \-UZo TABLE III ' INTERLABORATORY COMPARISON OF ANALYTICAL RESULTS FOR CHRYSOTILE IN COSMETIC TALCUM-TYPE POWDERS N.Y.U. (X-RAY DIFF.) RESULTS FDA PFIZER2- (OPT. MICR.) (X-RAY DIFF-) n-d.(not detected) 'n. d. n -d. COLUMBIA SCIENTIFIC^ . 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. n. d. . n. d. n. d. HFBC #? * . _______________________________________ R E S U L T S ________ N. Y. U. FDA PFIZER5 (X-RAY DIFF.) (OPT. MICR. ) (X-RAY DIFF.) COLUMBIA SCIENTIFIC5 23 1 24 n. d. 25 7 26 *? 27 n. d. 28 n. d. 29 n. d. 30 n. d. 31 n. d. 32 n. d. 33 n. d. 34 xi.d. 35 n. d. 36 n. d, 37 n. d. 38 n, d. 39 n. d. 40 n. d. 41 n. d. 42 n. d. 43 n. d. 44 45 n. d. 46 n, d. 47 n. d. SAMPLE NO. 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 N.Y.U. (X-RAY DIFF.) n. d. n. d. n. d. tu d. n. d. 7 ru d. tu d. tu d. n. d. ti.d. n, d. tu d. ru d. ru d. n. d. tu d. TL n. d. tu d. n. d. n. d. ti.d. ti.d . n. d. ti.d. RESULTS FDA PFIZER3 (OPT. MICE, ) (X-RAY DIFF.) n. d. n. d. xi.d. n. d. tu d. zu dtu d. n. d. COLUMBIA SCIENTIFICb HPBC SAMPLE NO. 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 90 91 ' 92 93 94 95 96 97 N. Y.U. (X-RAY DIPT. ) n, d. n. d. n. d. n. d. n. d. ? 9 7 ? 9 7 ? 7 5% 5% 5% 5% 5% 47; 7 3% 10% 157c RESULTS FDA ?FIZERa (OPT. MICR. ) (X-RAY DIFF. ) n. d. n. d. n. d. n. d. n. d. n. d. n. d. possible, in talc grains n. d. possible, in talc grains much antigorite^ ? n. d. possible, in talc grains moderate antigorite? n. d. n. d. COLUMBIA SCIENTIFIC^ HPBC inconclus ive inconclusive inconclusive < 0 .1 % inconclusive AMPLE NO. N. Y.U. (X-RAY DIFF.) 98 ' n, d. 99 n. d. 100 ii.d. 101 n. d. 102 7% 103 n. d. 104 n. d. 105 n. d. 106 n- d. 107 n. d. 108 n.d. 109 7 110 n. d. 1 1 1 n.d. 112 n. d. 113 n. d. 114 n. d. 115 n. d. 116 n. d. 117 1 118 n. d. 119 n. d. 120 7 12 1 n. d. 122 7 RESULTS FDA PFIZERa (OPT. MICR. ) (X-RAY DIFF.) n. d. possible, in talc grains much antigorite? n. d. n. d. n. d. COLUMBIA SCIENTIFIC^" n. d. HPB 4MPLE NO, 123 124 125 126 127 128 129 130 131 132 133 134 135 136 137 138 139 140 141 142 143 144 145 146 147 148 _________________________________________R E S U L T S _________________________________ N.Y.U. FDA " PFIZER4 COLUMBIA (X-RAY DIFF.) (OPT. MICR. ) (X-RAY DIFF. ) SCIENTIFIC^ 9 1 ? n. d. n. d. n. d. n. d. Trace n. d. n. d. n. d. n. d. n. d. n. d. ix.d. n. d. n. d. n. d. n- d. IX. d. 10% 7 2% ix.d. n. d. n, d. n. d. HPBC AMP] NO. 149 150 151 152 153 154 155 156 157 158 159 160 161 162 163 164 165 166 167 168 169 170 171 172 N. Y.U. (X-RAY DIFF,) ? n. d. n. d. n. d. n. d,, n. d, . ? n. d. 8% n. d. ? trace n. d,, n. d. 10% 1% ? ? n. d. RESULTS FDA PFIZER13 ' (OPT. MICR. ) (X-RAY DIFF.) n. d. n. d. n. d- o.i%e n. d. possible, in talc grains n. d. COLUMBIA SCIENTIFIC15 n. d. inconclusive iIPBc n. d. 8% n. d. n, d. ? n. d. SAMPLE HO. 175 N.Y.U. (X-RAY DIFF.) 7 RESULTS FEA PFIZERa (OPT. MICR. ) (X-RAY Diff. ) COLUMBIA SCIENTIFIC13 HPBC 176 ? 177 n. d. 178 7 179 n. d. 180 n- d. 181 n. d. 182 ? 183 184 n- d. 185 n. d. 186 187 n. d. 188 7 189 n. d. 190 7 .. 191 n. d. 192 xid 193 7 194 7 . 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-by Drs, Pontefract and Cunningham, - Antigorite is a non-fibrous form of the same mineral as chrysotileBy transmission electron microscopy. TABLE IV KEY TO SAMPLE NUMBERS OF COSMK' TALCUM-TYPE POWDERS AMPLE NO. PRODUCT NAME FURTHER IDENTIFICATION 1 Airmens Powder, Medicated Bristol-Myers (No, IF25) 2 Amolin Deodorant Powder Norwich 3 Aquamarine Cooling Spray Bath Powder Revlon (143) 4 Bagatelle Amber Dusting Powder Corand (DCH) 5 Bourjois Bath Powder 6 Caldesene Medicated Powder Pennwalt (5274) 7 Cashmere Bouquet Body Powder Colgate-Palmolive 8 Chanel No. 5 Bath Powder 9 Countess Rocheau Cake Dusting Powder Jergens \\\ 10 Crepe De Chine Dusting Powder, Millot House of Fragrance (L1132) 11 Crepe De Chine Poudre Mist, Millot House of Fragrance 12 Cuticura Talcum Powder Purex (07170) 13 Des enex . WTS-Pharmacraft 14 Desitin Baby Powder Pfizer (1139Z) (3/29/72) 15 Desitin Baby Powder Pfizer (115A) (5/10/72) 16 Diaparene Baby Powder Breon (E1030) 17 Dorothy Gray "Secret Of The Sea" Dusting Powder 18 Emeraude Talcum Powder Coty (355-4010) 19 English Leather Mem 20 Faberge "Music" Dusting Powder (2891) 21 Friendship Garden Dusting Powder Shulton (3/27/72) 22 Friendship Garden Dusting Powder Shulton (5/9/72) 23 Friendship Garden Dusting Powder Shulton (7/13/72) PLE 0. PRODUCT NAME 4 Heaven. Sent Aerosol Bath Powder Mist 5 . Heaven Sent Bath Powder * *6 Helen Press 1 ''Little Lady" >7 Imports. Spain Mens' Talc 28 Isis Floral Talcum Powder 29 Johnson's Baby Powder 30 Johnson and Johnson Medicated Powder 31 Koscot Beauty Dust-- Oil of Mink 32 Lanvin Arpege Dusting Powder 33 Lanvin Arpege Powdered Mist 34 Lanvin Arpege Talc 35 Lewis Baby Powder 36. Loves Fresh Lemon Glossy Powder 37 Macy's Scented Borated Talcum 38 Macy's Talcum, Apple 39 Marcelle Dusting Powder, Hypo-Allergenic 40 Mary Chess Perfumed Dusting Powder 41 Mennen Baby Magic Powder 42 Mennen Quinsana Foot Powder 43 Merck Talc, Product No. 6460, Lot No. 6460) 44 Mexsana 2387-D Medicated Powder 45 Old Spice Body Talcum 46 Persian Lilac Deluxe Dusting Powder 47 Persian Lilac Spray Bath Powder 48 Pond's Perfumed Talc Body Deodorant Dream Flower 49 Prince Matchabelli Beloved Spray Powder FURTHER IDENTIFICATION Rubinstein Rubinstein (028Q) (3612) (12 88) Manley R James (2K4) (B112) (H202) (8039301) Plough Shulton April Showers (LFN) April Showers (B200B) (115B) MPLE NO- -' PRODUCT NAME 50 Quest Deodorant Powder 51 Replique Spray Bath Powder 52 Riviana Foods - Italian Stearin Talc 53 September Morn By Pond's 54 Seven Winds After Bath Talc 55 U S P Talc 56 Vaseline Intensive Care Baby Powder 57 Yves Saint Laurent Rive Gauche Spray Talc 58 Z B T Baby Powder 59 Zeasorb Super Absorbent Medicated Powder 60 Ambush*Dana ixisting Powder 61 April Showers 62 Avon Unforgettable Perfumed Talc 63 Beloved Perfumed Dusting Powder, Prince Matchabelli 64 Coty Face Powder Rachel 65 Desert Flower Spray Bath Powder 66 Emeraude Dusting Powder 67 Emeraude Spray Dusting Powder 68 Faberge" Flambeau Deodorant Spray Powder 69 Jean Nate Spray Bath Powder 70 ' Jeris Talc, Flesh 71 Jolie Madame Dusting Powder, Balmain 72 Lady Esther Face Pcwder, Rachel 73 Max Factor Face Pcwder, Rachelle 74 Medicated Comfort Powder 75 OH- de London Talc * FURTHER IDENTIFICATION Parfums Raphael (004) For Rice (19b ) DuBarry (021085) (I 209) (F1021) Stiefel (9884) Shu1ton (F 1 BKI) Coty Coty (1 AEY) (37 WBF) (1 N 247) Parke-Davis Yardley (498) r.--.v,-.-:. 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 Dusting Powder 81 Cashmere Bouquet 82 Jean Nate/Talc 83 Mermen Shave Talc 84 Shower To Shower Body Powder 85 Pure Baby Powder, Dart Drug 86 Pond's Dream Flower Perfumed Talc 87 Almay Hypo-Allergenic Face Powder 88 Constance Carroll, Bouquet Talc 89 Djer-Kiss Talcum 90 Flamingo Dusting Powder., Tussy 91 Lander Lilacs And Roses Talc 92 Mavis Talcum 93 Mavis Body Powder 94 Tangee 95 ZBT Baby Powder 96 Blanchard's Dusting Powder 97 Born Wild Dusting Powder 98 Lander Gardenia And Sweet Pea Talc 99 Lander Lilacs And Roses Deodorant Body Talc 100 Miss Dior Dusting Powder 101 Tai Winds Spray Talc . FURTHER IDENTIFICATION Tom Fields, Ltd. Revlon Corday (4908) Houbigant (11F) : (on 345) (B 81) Johnson & Johnson (5507BG) (K 11C) (0 13D) Kerkoff (L1047) Vivaudou Vivaudou Luft-Tangee (B0048) Del Labs (Avon (DCC 1272 2-14-72,HWS) PLE PRODUCT NAHE 32 Tosca Dusting Powder 03 Coty L'Aimant Talcum Powder 04 Coty Emeraude Talcum Powder 05 Coty L'Aimant Dusting Powder .06 Coty Imprvu Dusting Powder ,07~ Coty Muguet des Bois Dusting Powder .08 Revlon Intimate Perfumed Bath Powder L09 Jean Natd" Bath Powder ' 110 Jean Nate''Spray Bath Powder 111 Old Spice Body Talc 112 Dr. Scholl's Foot Powder 113 Faberge Xanadu Luxury Bath Powder Spray 114 Faberge Zizanie de Fragonard 115 Faberge Tigress Bath Powder 116 Faberge Woodhue for Men 117 Faberge Brut for Men Shower Buff All-Over Body Powder 118 Faberge Talc 119 Faberge Aphrodesia Bath Powder 120 Faberge Straw Hat Bath Powder 121 Faberge Aphrodesia for Men Shower Buff 122 Faberge Xanadu de Luxe Bath Powder 123 Faberge Woodhue Bath Powder 124 Faberge Music Dusting Powder 125 Faberge Flambeau Bath Powder FURTHER IDEMTIFICAt I0X (1JJ) (0U) (1M) (IDE) (2D0) (241) Lanvin - Charles of the Ritz (2137) Lanvin - Charles of the Ritz (2103) Shulton? Inc. (MFO) (20517) (Yl) (2132) Ref. 61159-019 Ref. 2052-003 Ref. 5027 (0252) Ref. 5400 (raw material: from France) Ref. 2052 (2172) Ref. 502 7 Ref. 1244-028 (2342) Ref. 2052-002 Ref. 0714-018 (3121) Ref. 2052 (3471) .MPLE NO. PRODUCT NAME 126 Mermen Baby Magic 127 Walgreen's Crib Age 128 Caldeaene Medicated Powder 129 Desiten 130 Vaseline Intensive Care 131 Johnson and Johnson Medicated Powder 132 Johnson Baby Powder 133 Johnson's Baby Powder 134 Johnson's Baby Powder 135 Johnson and Johnson Medicated Powder 136 Johnson and Johnson Shower to Shower Body Powder 137 Johnson and Johnson Shower to Shower Body Powder 138 Johnson and Johnson Shower to Shower Body Powder 139 Avon Brocade Sp.ray 140 Avon Bird of Paradise Spray 141 Avon Tai Winds Spray Talc 142 Mennen Bath Talc 143 Pin-Zow Talque 144 Overton's "High-Brown" Face Powder 145 . Softee Face Powder 146 Westport Face Powder 147 Hazel Bishop Pressed Powder 148 Lady Wayne Face Powder 149 Solitaire Cake Makeup 150 Dreamglo Pressed Powder FURTHER IDENTIFICATION (108T) (109T) (0452 K) (C 512Z) (0709X1) (0872K) (31602) (B1652) (4065) (A308) Perfection Beauty Products, Inc., Pearl River, N.Y. iMPLE NO- PRODUCT NAME _> L51 Early American Old Spice Talcum Powder 152 Corsage Dusting Powder 153 Ammens Powder, Medicated 154 Bismoline Medicated Powder 155 Rite Aid Pure Baby Powder 156 Warner Pure Baby Powder 157 Mavis Imported Talcum 158 Avon Brocade Perfumed Talc 159 Avon Blue Lotus Perfumed Talc 160 Avon Beauty Dust Refill - Charisma 161 Avon Elusive Beauty Dust Refill 162 Avon Rdgence Perfumed Talc 163 Pinaud Clubman Talc 164 Grand Union Baby Powder 165 Cashmere Bouquet 166 Almay Face Powder, Soft Beige 167 Tawny Tone Body Talc Prom Black Heritage 168 Colgate Tooth Powder 169 Dr, Lyon's Tooth Powder 170 nCn Bouquet Talc. 171 Tangee Dusting Powder 172 Jeris Talc 173 Corsage Dusting Powder 174 Lander Gardenia & Sweet Pea'Deodorant Body Talc FURTHER IDENTIFICATION Land er (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.) AMPLE MO. 175 176 177 178 179 180 PRODUCT NAME Lander Baby Powder Lander Lilac 4 Roses Body Talc Beloved Perfumed Dusting Powder Jean Nat^ Talc No. 60 Jean Nate'' Spray Bath Powder Tinkerbell Body Talc 181 Yardley Sigh Shadow Brush-On Eye Shadow 182 Max Factor Face Powder, Rachelle 183 Tweed Bath Powder, Lentheric 184 Yardley Next to Nature Sheer Pressed Powder 185 Yardley April Violets Dusting Powder 186 . Yardley Red Roses Dusting Powder 187 Yardley Springflowers Talc 188 Yardley White Lavender Talc 189 Yardley Red Roses Talc 1190 April Showers Deodorant Talc 191 Chantilly Houbigant Dusting Powder 192 Tihkerbell Dusting Powder 193 Tihkerbell Powder Mitt 194 Tinkerbell Dusting Powder 195 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.)