Document 3eyyekv3nQErL5XypNk3EvOG6

C olorado School of M ines R esearch P.O. Bo x 112 80401G o l d e n , C ol o r ad o I nstitute O c to b e r 27, 1972 P r o je c t C 10 704 D r . A1 G o u d ie 5 Finley Road Edison NJ 08817 D ear D r. Goudie: In com pliance with y our re q u e st I have m ade X -ra y diffraction step scans on Baby P o w d er T alc Sam ples 108T and 109T fo r the purpose of d e te r m ining if serp en tin e (possibly chrysotile) is p re se n t. It is my u n d e rsta n d ing that a contention has been m ade that these sam ples contain approxi m a t e l y 3% c h r y s o t i l e . T he r e s u lts of th e se stu d ies do not su b sta n tia te this. They do show that the sam ple contains chlorite which give sim ila r, but distinguishable X -ra y diffraction peaks. If the ch lo rite peaks w ere m istakenly assum ed to re su lt from the p re sen c e of chry sotile, then one would m istakenly assum e that the s a m p le s co n tain about 3% c h ry s o tile b a s e d on the d iffra c tio n p e a k in te n s i t y r e s u l t i n g f r o m th e a d d i t i o n of 3% c h r y s o t i l e to the s a m p l e s . A sb e sto sfo rm c h ry so tile is but one sp ecies of the m in eral serp en tin e. O ther species a re not a sb esto sfo rm . H ow ever, all species give s im ila r X -ra y diffraction p a tte rn s so that X -ra y diffraction can only indicate the p re s e n c e o r ab sen ce of se rp en tin e . If X -ra y diffraction indicates the p r e s e n c e of s e r p e n tin e , o th e r m e th o d s m u s t be u se d to d e te rm in e if it is ch ry so tile. H ow ever, according to the FDA guidelines, if a talc sam ple y ie ld s no d iffra ctio n data w hich could be a s c rib e d to serp en tin e (including ch ry so tile) then the talc is re g a rd e d as a ccep tab le relative to c h ry so tile content. The m o st effective way to a s c e rta in if a serp en tin e m in eral m ay be p r e s e n t in a s a m p le by d iffra c tio n is to f i r s t d e te rm in e if the m a te r ia l y ie ld s a d i f f r a c t i o n p e a k in th e v i c i n i t y of 7 A. T h i s i s th e m o s t i n t e n s e d i f f r a c tion peak for serp en tin e. H ow ever, this diffraction peak cannot be used in d iscrim in ately since other non-asbestos m in e ra ls have th eir m ost intense d i f f r a c t i o n p e a k s in th e s a m e r e g io n . A n a w a r e n e s s of th e g e o lo g ic a l and m in e ra lo g ic a l a sso c iatio n s of talc im m ediately suggests the chlorite m in e ra ls. They a re com m only asso ciated with talc and yield th eir m ost intense d iffractio n p eak at e sse n tially the sam e place as that of serp en tin e Minerai Industry Research C O L O R A D O S C H O O L OF MINES R E S E A R C H I N S T I T U T E D r. Al Goudie Page 2 O ctober 27, 1972 (including chrysotile). F o rtunately there is a way to distinguish betw een the serpentine m in e ra ls and chlorite m in e ra ls by X -ra y diffraction. C h lo r ite g iv e s a d if f r a c tio n p e a k at about 14 Aand s e r p e n tin e does not. T hus if a su sp e c t 7 Apeak is o b s e rv e d then the sa m p le m u st be ch eck ed f o r a 14 A p e a k . If a 14 A p e a k o c c u r s , th e 7 A p e a k r e p r e s e n t s c h l o r i t e , not serp en tin e. The X -ra y diffraction m u st be d e term in e d by a c c u m u lating counts for a few m inutes at each of sm all in crem en ts acro ss the peaks. Continuous counting or counting rates give neither adequate counting statistics nor sufficient peak discrim ination. Step scanning, of s e v e ra l sp lits of Sam ples 108T and 109T revealed the p re s e n c e of a peak in the 7 A region as shown on the accom panying c h a rts. H o w e v e r, th e y a ls o show th e p r e s e n c e of p e a k s in the 14 A re g io n w hich a re in the p ro p e r p o sitio n to show that the 7 p eak s re su lt fro m the p re s e n c e of chlorite and not serpentine. Since the contention was m ade that Sam ples 108T and 109T contain about 3% c h r y s o t i l e , th e y w e r e s p i k e d w ith 2. 7% an d 2. 8%, r e s p e c t i v e l y , of finely m illed chrysotile which was obtained from Johns-M anville. As m ay be seen from C harts 2 and 8 the chlorite and chrysotile peaks are d is t i n g u i s h a b l e a n d d i s t i n c t i v e . T h e c h l o r i t e p e a k o c c u r s at a b o u t 7. 06 A. The chrysotile peak is quite broad and shows at le a s t 2 m axim a at a p p ro x i m a t e l y 7. 32 a n d 7. 3 8 A. It w a s f i r s t th o u g h t t h a t t h is b r o a d e n i n g m a y have resulted from overgrinding, however, relatively coarse unground m a te ria l gave the sam e p atte rn . It is p o ssib le that the peak broadness r e s u lts fro m d iffe re n t v a r ie tie s of s e rp e n tin e in addition to c h ry so tile . S te p s c a n s of S a m p l e s 108T a n d 109T s p i k e d w ith 2. 7% an d 2. 8% c h r o s o tile, respectively, show that the are a under the chrysotile peak is c o m p a ra b le to the a re a u n d er the ch lo rite p eak s. If one w ere to m istakenly a s s u m e t h a t th e 7. 06 A p e a k r e s u l t e d f r o m c h r y s o t i l e i n s t e a d of c h l o r i t e , h e w ould c a lc u la te th a t the s a m p l e s c o n ta in about 3% b a se d on i n c r e a s e d diffraction in te n sitie s a fte r the addition of ch ry so tile. This would be especially tru e if step scanning w ere not used since the chlorite and serp en tin e peaks would not be resolved. It is probable that the contention th a t the two ta lc s a m p le s c o n ta in about 3% c h r y s o tile is m is ta k e n ly b a s e d on the m agnitude of the 7 A ch lo rite peak. If this is so, it could have been avoided by step scanning the p ro p e r reg io n s. Sincerely, W. T. C an e e r A ssistant M anager M ining Division W TC/psk Dr. A. J. Goudie Johnson and Johnson Research Center 501 George Street New B runsw ick, New J e r s e y 08901 EXAMINATION OF JOHNSON AND JOHNSON'S BABY POWDER Date: 27 October 1972 MA Number: 2546 Copy of 4 waiter c. me cren associates, ine, 2820 SOUTH MICHIGAN AVENUE . CHICAGO, ILLINOIS 60616 EXAMINATION OF JOHNSON AND JOHNSON'S BABY POWDER Summary Two sam ples of Johnson and Johnson's Baby Powder, batch number I 108T and 109T, which c o rre sp o n d to the sam p les examined by P r o fe s s o r Seymour ? Z, Lewin of New York U niversity on behalf of the FDA have been examined by Ix - r a y diffraction, light m ic ro s c o p y , tr a n s m is s io n e le c tro n m icroscopy and e le c - I tron diffraction to determ ine w hether they contain any asbestiform m inerals. Both samples contained an insignificant amount oftrem olite -- a few isolated crystals. Neither sample contained chrysotile. |i I Introduction l On behalf of the FDA, P r o f e s s o r Seymour Z. Lewin of New York \ j University is examining a number of com m ercial talcum powders for the presence ' of asb estifo rm m in erals. Two of the sam ples which he has examined a re sam ples j of Johnson and Johnson's Baby Pow der, batch number 108T and batch number 109T. Johnson and Johnson therefore requested Walter C. McCrone Associates to ext am ine sam ples from the sam e batches to determ ine whether they contained any \l asbestiform minerals. M aterials and Method of Conducting Tests Two sam ples w ere submitted, identified as Johnson and Johnson's Baby Powder, batch num bers 108T and 109T. For x -ra y diffraction examination, the samples w ere examined on a Phillips-N orelco verticle diffractom eter using CuKa radiation and a scanning sp eed of 1 p e r m inute. The d is p e r s io n staining technique w as used for the lig h t m icroscopical examination and the electron m icroscopy-electron diffraction ex I I 'If am in a tio n w as c a r r i e d out using p r o c e d u r e s p re v io u sly d escrib ed (MA r e p o r t 2330-1; dated 10 August 1971). waiter c. mecrone associates, inc. Results X-ray Diffraction The d iffra c to g ra m s w ere carefully examined in the vicinity of the m ajor peaks of chrysotile and trem olite. Neither m ineral was present. The p r e s e n c e of peaks in the vicinity of 12. 0-12-5 26 , the region in which one of the f j. principal lines of chrysotile may be found, was c o rre la ted with peaks in the v i cinity of 6 26 and a r e thus a ttrib u ta b le to c h lo rite s . No significant peaks w e re i o b s e rv e d in the 24 re g io n which would be re q u ire d w ere c h ry s o tile p re s e n t. Light Microscopy Using the dispersion staining technique and a liquid of refractive index 1.550, the samples were examined for chrysotile particles and fibers, but none could be found. Using a sim ilar technique with a liquid of refractive index 1.605, the samples were sim ilarly examined for the presence of trem olite and a few individual crystals were found, some rod shaped. Electron Microscopy and Electron Diffraction S everal e le c tro n m ic ro s c o p e g rid s from both sam p les w ere ex- \I. amined in their entirety and although some fibers w ere observed these were shown 5 by e le c tro n d iffractio n to be s h a r d s of talc o r ro lle d talc. No c h ry s o tile f ib e r s w ere found. Conclusion I A d e tailed ex am in atio n of two sam p les of Johnson and J o h n so n 's Baby Powder, batch num bers 108T and 109T has shown this m aterial to be sub stantially free of asb estifo rm m in e ra ls. A few trem olite rods w ere observed in both s a m p le s . No c h ry s o tile has been detected . Respectfully submitted, Ian M. Stewart Manager, Electron Optics Group waiter c, mecrone associates, inc. University College, Cardiff Postal Address: University College, Newport Road, Cardiff CF2 iT A . Telephone Cardiff 442 11 Telegrams: Coleg Cardiff From.... D.r..F.D..Pooley............. Department o f ...Mineral.Exploitation.. AIR MAIL FDP/MM 8th November, 1972, Dr. A.J. Goudie, 5, Finley, Edison, New Jersey 08817, U . S.A. Dear Dr. Goudie, We have extensively examined the sample 108/T powder for chrysotile asbestos but can find no evidence of any of the mineral at all. Both electron microscope and X-ray techniques have been employed and we have also applied a chrysotile concentrating technique which we have developed to the sample which enables us to definitely demonstrate chrysotile at the 0.10% level and nothing was found. I will be communicating a number of simple tests to you in the near future for demonstrating chrysotile at low levels. Yours sincerely, F.Dc Pooley X-ray Study of Johnson & Johnson's Baby Powder Retain 108T (4-17-72) Gordon E. Brown Princeton University Retain 108T (4-17-72) of Johnson & Johnson's Baby Powder was examined by slow, continuous scanning x-ray techniques. A Norelco vertical diffractometer with a LiF crystal monochrometer and sample spinner was used in this work. Other pertinent experimental condi tions were as follows: CuK<* radiation (40KV, 20mA) ; scan speed = 1/4 29/min.;Oscale factor = 4; time constant = 4; 1 slits; scan range = 5-BO 20; PHA (12V baseline, 12V window); amount of powder = Ocl gr. ( < 3 2 5 mesh). The diffraction tracing is attached to this report and a list of d. spacings is given in Table 1. Twenty-four of the recorded peaks have been assigned to talc using cards 19-770A and 13-558 from the ASTM powder diffraction file. Seven additional peaks were also re corded and all but one have been attributed to chlorite, magnesite, chalcopyrite and rutile. The unknown peak represents a d-value of 1.48 A No evidence of chrysotile or tremolite was found in the x-ray dataooutlined above. The two strongest chrysotile peaks (7.31 and 3.65A) as well as the three strongest tremolite peaks (8.38, 3.12 and 2.70A) were unobserved. The peak at 3.12A is attributed to talc (006,115) and cannot be a tremolite peak. Peaks due to CuK/^ were also searched for but were not found. It is concluded that retain 108T (4-17-72) from Johnson & John s o n 's Vermount talc mine is a very pure talc with less than 5% im purity due mainly to chlorite and magnesite. A careful search for chrysotile and tremolite impurities proved negative. Table 1: X-ray Data for Johnson and Johnson 1s Baby Powder Retain 108T (4-17-72) Mineral Talc hkl a (a ) 2 9 !deg -) 002 9.45 9.36 Chlorite 002 7.14 12.40 Talc 004 4.69 18.93 Talc Talc 020,111 022 4.57 4.13 19.42 21.50 Chlorite 004 3.56 25.0 Rutile (?) 3.26 27.33 Talc 006,115 3.12 28.58 Magnesite 104 2.75 32.58 Talc 130 2.64 34.00 Talc 200,132,131 2.60 34.50 Talc 133,132,117 2.49 36.08 Talc 204 2.45 36.73 Talc 008 2.34 38,46 Talc many including 134 2.28 40.50 Talc 136 2.10 43.18 Talc 136 1.94 46.80 Talc 0.0.10 1.87 48.62 Talc 242 1.73 52.93 Talc 244,138 1.69 54.34 Talc 1.65 55.90 C h a l c o p y r i t e (?) 1.58 58.37 Talc 0.0.12,317 1.56 59.21 Talc 060,332 1.53 60.52 Talc 330 1.51 61.30 Unknown 1.48 62.85 Chlorite 139,208 1.42 65.65 Talc 2.0.10 1.39 67.18 Talc 1.3.12 1.39 67.53 (K* ) Talc 0.0.14 1.34 70.38 Talc 264 1.30 72.90 .1III 14 i I i '1 G ;! 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The following mineral content was determined: Lot 108T Major: Talc Trace: Chlorite, Magnesite Lot 109T Major: Trace: Talc Chlorite, Magnesite, Dolomite The step-scanning technique was then employed for increased sensitivity in the detection of chrysotile asbestos. It had been previously demonstrated that with this procedure it was possible to detect chrysotile in talc at a level of 2-3% by weight. The results, shown in Figures 1 and 2, indicate no diffraction peak in the region corresponding to an intense chrysotile reflection (7.31A or 12.120). Therefore, the samples of JOHNSON'S Baby Powder do not contain chrysotile at the minimum detectable level which is attained by X-Ray diffraction. Differential Thermal Analysis A semi-quantitative method based on the analysis of standard samples of chrysotile in talc had been developed using the technique of differential thermal analysis (DTA). The limit of detection of this method is 1% by weight of chrysotile. Thermograms of JOHNSON'S Baby Powder, Lots 108T and 109T, showed no thermal *A Trademark of JOHNSON & JOHNSON. f t --co&u i G <GHn w H $ 0 l# X Q ^ ^<L3Nit/ 3 Q _ m < y Z ,g y g ? > _ l'J 8 /sey PooJer L ot ^'o^ T FIGURE 2 k>Wutm -=4o mx'Ycn Subject: ANALYSIS OF J O H N S O N 'S* BABY POWDER FOR TREMOLITE ASBESTOS PROJECT NO. 503 New Brunswick, N.J. November 8, 1972 The two lots of JOHNSON'S Baby Powder examined by Dr. Lewin had been previously analyzed qualitatively by X-Ray diffractometry (report of October 31, 1972). It was desired to further analyze these samples for the presence of trace quantities of amphibole asbestos minerals; such as, tremolite. An X-Ray step-scanning procedure had been developed for the detection of tremolite in Vermont talc. The limit of detection of this method is 0.1% by weight of tremolite. Figure 1 shows the peak obtained for an intense tremolite reflection (8.38A or 10.5 20) for a standard sample of 0.5% tremolite in Vermont talc. Plots of the step-scans through the same region for JOHNSON'S Baby Powder, Lots 108T and 109T, are shown in Figures 2 and 3, respectively. The results do not indicate the presence of amphibole minerals. Therefore, the samples of JOHNSON'S Baby Powder do not contain tremolite within the limit of detection of the X-Ray diffraction step-scanning technique. Since tremolite does not exhibit intense thermal transi tions distinguishable from talc, differential thermal analysis is not *applicable for the detection of this mineral in talc at low levels. ab *A Trademark of JOHNSON & JOHNSON. a s *% T r e m o l it i u Tfd SS'-ffo FIGURE 1 t % f3 f nt\ & f ,{ t*/s//va FIGURE 2 // - \ 0Pt>^T~ &>