Document LpprQgn7JXLgm2mLNOd6Ny4V3

ANALYSIS OF TALC BY X-RAY DIFFRACTION AND POLARIZED LIGHT MICROSCOPY Lacy B. McCroue W alter C. McCrone Associate, Inc. Chicago, Illinois 40616 Contract No. CDC 210-75-0063 3 d epa r tm en t o f h e a l t h , education and w elfa r e * Public Health Service Center for Disease Control National Institute for Occupr*inal Safety end Health Cincinnati, Ohio 45226 asetisasssm c oaia i. * *. IMICT 2. ViiU tdbfiiU ANALYSIS o r TALC BY X-RAY DIFFRACTION AND POLARIZED UGHT MICROSCOPY 7.AmM i I Lucy B. McCrone t. P*lMit| X*m* m4 A Walter C. McCrone Associate, Inc. 2920 9. Michigan Ave. Chicago, lT. 60616 12. Spni.iii| O'gaaixan Saa* aa4 A24 ii - National institute for Occupational Safety and H ealth 4676 Columbia Parkway Cincinnati, OH 45225 1J. SuffltMuirr N on J. tc ActM.,., s . 1. kga Uaia May 1977 4. ' a. Na. 1U'(M.iai Ra< 10. Praiaci.'Tamk taik Ua>i Sa. M. Caatraci. Uraa* Na. CDC-210-75-006 3 IJ. 7ff* * r A J'tf r *- * * u. On hundred talc samples have bn analyzed by polarized light m icroscopy, dia per loo ftatnixif, x -ray diffraction and, when necessary, by .xansmlaston electro n m icroscopy and electron nucroprooe. The analytical method were refined In scope, sen sitiv ity and accuracy as a p a rt of the project. The sample ranged from l to 99% talc w ith an average of 63%. Twenty-three other mineral were identified including the terpentines: anti go rite , lizardite and chryaotlle; the amphibc-lee: antbophyUlte, trem olite and actin o lltc; the carbonates: calclte, dolomite, aakerlts and magnesite; the talc-Uke m ineral chlorite as well as q u artz, mica, feldspar, magnetite, coal, graphite, hydroxygaptite, claya, hydrous iron oxides and rutile. Chryaotlle was found In only one sam ple which, however, contained only i-2Hf talc. More then one-third of the ample contained trem olite o r actlnoUte often In m ajo r am ounts and usually partly fibrous. This report was submitted in fulfillment of C o n tract No. CD C-210- 75-006 3 by W alter C. McCrone Associates, Inc. under the sponsorship of the National Institute for Occupational Safety and Heslth._______________________________________________ If. tT t4 U UmumH Aaalyaia. 17. OlHtipim x* ray diffraction dolomite microscopy magnesite polarized electromagnetic radiation quartz talc asbestos amphlboles serpentines calclte U k Tra chlorite minerals dispersion staining x-ray step scanning ' 17. COSATt f iml4 G rr. I I . A*ilakil<f *V**a iixOOMZD ST AHit A*0 UNtJCO. li. Stomtr CUit ___HtatNp afnLIAxr-firu n W w ur v. a .. <1* < PmVwCLA5.vriP r x u roau hat sc ai:faoh.c.f.i> GO i:. p, 57 OC let- i ABSTRACT Thar* lias been considerable controversy during the p u t fair years over the com position of tala as used In cosmetic talc products. At one time m ost of these products w ere reported to contain curysotile. Although these data were shown to be erroneous it seemed desirable to examine a large number of raw m aterial talcs from various mines to determine precisely what m inerals a re present. One hundred talc samples have been analysed by polarised light microscopy, dispersion staining, x -ray diffraction and, when necessary, by transm ission electron microscopy end electron microprobe. The analytical methods w ere refined in scope, sensitivity and accuracy aa a p art of die project. The sam ples ranged from 1 to 99% talc with an average of 63%. Twenty-three other m inerals were Identified Including fits serpentines: antlgorlte, llzardite and chrysotllei the amphlbolsst anthophylilts, trsm ollte and actlnolltet the carbonates: calcite, dolomite, anksrlte and magnesite; the talc-like mineral chlorite an well aa quartz, mica, feldspars, m agnetite, coal, graphite, hydrox yapatite , clays, hydrous Iron oxides and ru tile. Chrysotills was found In only one sam ple which, however, contained only 1-2% talc. M ore than one-third of the sam ples contained tram olite o r actlnollte often in m ajor amounts and usually partly fibrous. This report was submitted in fulfillment of Contract No. CDC210-79-0063 by W alter C. McCrone Associates, too. under the sponsorship of the National Institute' for Occupational Safety and Health. 111 58 INTRODUCTION Using toe techniques of x-ray diffractloo ind poU rized light microscopy we have analyzed 100 sam ples of talc powder supplied by NIOSH. When accessary electron m icroscopy and electron m icroprobe analysis have been used to supplement the data developed by the other techniques. Tbs purpose of die work was to furnish NIOSH with die analytical resu lts which a re tabulated In the attached Data Summary, (Appendix A.) While so doing we have tried to refine die m icroscopical and x -ray methods used as they apply to the analysis of talc. METHODS OF ANALYSIS Each sample was analyzed by x-ray diffraction and microscopy. The x-ray work was dons using a Philips x-ray generator and diffractom eter. Each sample was f ir s t scanned continuously to record a diffraction pattern representing the whole sam ple. The m inerals Identified were listed and any questionable peak assign ments were noted, for confirmation or resolution by polarized light microscopy including dispersion staining. Quantities of each comp, aent were estimated whenever possible, both by polarized light microscopy and from the continuous scan. X -ray step scanning was done, preferably after m icroscopy, for amphibole and serpentine m inerals and for quartz, in order to determ ine any quantities of these present in the tale. Results of these tores types of analysis were reconciled with each other and then combined and presented in individual reports for each aam pte. X-RAY DIFFRACTION Sample preparation To insure the best x-ray powder diffraction results the contract specifies that sam ples In which toe average particle size exceeds 10 pm must be ground finer before undertaking x-ray diffraction analysis. Judgment of w hether size reduction was necessary was mads by determining toe p article size d istribution m ic ro scopically. The sample was used as received If the average particle diam eter was below 10 pm . If the average particle was la rg e r than 10 pm , o r if the sam p le was not homogeneous because It ctatalned lumps o r huge particles, a 2-gram portion was m illed in Isopropanol for about 10 m inutes in a McCrone M lcronizing Mill and dried by slow evaporation to a ire s flowing powder. r APPENDIX A Data Summary Appendix A la a five page table which sum m arizes die analytical re su lts for each of die 100 sam ples. Four methods of quantitation w ere used and a re coded as follows: method code x-ray diffraction step scanning S x-ray diffraction line scanning L polarized light microscopy M difference D The method usually used in finding the quantity of a given m ineral is noted a fte r the % sign in the column heading for that m in e ra l. When a method different v- fro m that noted in the heading was used die le tte r code fo r that method follows the percentage listed in the table for the particular sam ple. hi the case of trem olite-actinolite ,T<J fib e rs" m eans the percentage of the total trem olite and/or actinolite that is fibrous, as contrasted with m assive particles. T h is w as, of course, always determ ined fay polarized light microscopy with the use of dispersion staining. 35 PRODUCT TALC SAMPLES FOR LABORATORY ANALYSIS DSHEFS Sample # Company and Sample D esignacin . Gouverneur T a lc Company (NY) 001 N y tal 300 Gouverneur T a lc Company (NY) 002 N y tal 400 Gouverneur T a lc Company (NY) 003 5X Gouverneur T a lc Company (NY) 004 325 Gouverneur T alc Company (NY) 005 X Gouverneur T a lc Company (NY) 006 FT Gouverneur T a lc Company (NY) 007 3X Source of i Sample 1 S u p p lie r Supplier 1 S u p p lie r Supplier i Supplier < 1 Supplier S u p p lie r Johnson & Johnson,.Verm ont 009 Product T alc (98Z Pure) Company H itch co ck T a lc Company 034 Murphy, N .C ., P ro d u ct T alc Harvard Windsor M in erals, G assets "37" 035 J u ly 29, 1975 (Vermont) Harvard Windsor M in erals, West Windsor 036 M ineral Ray G rind C om posite, Vermor S a rv a rd Windsor M in erals, Ludlow "36" 037 J u ly 29-30, 1975 (Vermont) *' Harvard Windsor M in erals, "G a ssc tts" 038 36, Ju ly 28-30, 1975 (Vermont) Harvard Vermont T alc Co- Bagging Bulk 039 Sample, 7 /1 6 /7 5 , 2nd s h i f t , VT Harvard I PRODUCT TALC SAMPLES FOR LABORATORY ANALYSIS DSHEFS Sample B 040 041 042 043 044 045 Company and Sample Source D esignation Of Sample Vermont T a lc Company - Bagging Bulk Sample, v e r t a l XXXD 1 9/17/75 1 st s h i f t (Vermont) Harvard Southern T alc Co. (C ohutta M ill) C hatsw orth, Ga. P roduct (Powder) Sample Mine I.D . 04-00493 MESA Packer S tatio n #3, V anderbilt T alc, M ill 91 G ouvem eur, N.Y. NI0SH 1 st s h i f t 11/4/75 (FT) * Survey Packer S tatio n 2, V anderbilt M ill 91 G ouverneur, N.Y. T a lc , NI0SH (Nytal 100), 1 st s h if t 11/4/75 Survey C e ra m ita lc HOT, V a n d e rb ilt T a lc Co. 1 s t s h i f t 1 1 /4 /7 5 (NY) NI0SH Survey ; , Bagging S ta tio n #3, V an d erb ilt T alc C o ., M ill #1, G ouverneur, N.Y. NI0SH 11/4/75 (N ytal 200) Survey 046 047 048 049 050 051 052 053 j 054 H itchcock Corp. 95 Mine MESA ID# 3100222 (NC) H itchcock C o rp ., #3 Mine ID#3100683 (NC) MESA Wray Mine & M ill, I$ c . M inerals and chem icals ID# 31--0008 (Vermont) MESA Bagging S ta tio n , V anderviit Talc Co. 2nd s h i f t . M ill #1 NI0SH G ouverneur, N.Y. (N y tal 300) 1 1 /3 /7 Survey Bagging S ta tio n , V a n d e rb ilt, 2nd s h i f t , 11/3/75 (N ytal 200) M ill #1, G ouverneur, N.Y. NI0SH Survey southern Talc Co., Southern M ill P ro d u ct T a lc sam ple, C hatsw orth, Ga Rock C l i f f Mine, ID# 0900492, 9 /3 /7 MESA Southern Talc Co., Southern M ill, C hatsw orth, Ga. ID# 09-00492 ore from Rock G-llff MESA Southern Talc Co., Southern M ill Ore from Judge Hole Mine ID# 09-00492 - MEAS J in c e rb o ro Mine & M ill. American Talc Co-. 'line. Ore A lpine, Ala. from (M ont), h'i 1lowcrcek. ID` 01-00433 iMESA . f PRODUCT TALC SAMPLES FOR LABORATORY ANALYSIS DSHEFS Sample # Company and Sample D esignation S o u r c e " "! of Sample Thompson-Weinman C o ., C a r t e r s v l l l e , MESA 055 Plane, C a r t e r s v l l l e , Ga. , Ore from Brady K iue, ID#09-00224 9/5/74 Cohutta M ill, Southern Talc Co. C hatsw orth, Ga. 9 /3 /7 4 , Ore from 056 E rnest Mine ID#09-00493 MESA American T alc d o ., A lpine, Ga. V interboro Mine & M ill, 9 /5 /7 5 . 057 001-00433, F in a l Prod.O re from Mont MESA n o near T a lc Co, G arren P i t P ro d . 06, A llam ora, Hudspeth C o., Texas 058 ID# 41-00869 MESA P io n eer T alc Co. I n c . , Apache P it Product, #4, Texas 059 ID# 41-00869 MESA P ioneer T a lc Co. I n c . , #4 Texola P it P roduct, Texas 060 ID# 41-00869 MESA Southern Clay P ro d u cts, #2, Bottom P ro d u ct, A llam ora, Rud*P*ch 061 C o ., Texas #18 MESA i l l v h i t e Co. I n c . , Van Horn, Cumberson Co, Texas ID#41-01527 062 Ground C alcin ed P ro d u c t MESA M ilw hite Co. I n c . , #11, Van H orn, Culberson Co. T exas,,E agle Hat 063 P it Crude ID#41-01527 MESA Pioneer T alc C o., A llam ora, Uudspetl . Co, T exas, #8 G arren Ceramic 064 ID# 41-00869 MESA M ilu h ite Co. I n c . , Van Horn, Texas 065 #14 Tumble Down P ic P ro d u c t, ID# 41-01527 MESA Emtal 42, E a stern Magnesia T alc 1 066 Co. Vermont 8 /2 8 /7 5 HARVARD 067 P fiz e r (B a rre tts M ill) Montana minus 12 m icron * NIOSH Survey \ P fiz e r (B a r r e tts M ill) Montana 068 minus 325 mesh NIOSH Survey P fiz e r ( B a r r e tts M ill) Moncana 069 minus 20 m icrons NIOSH Survey i PRODUCT TALC SAMPLES FOR LABORATORY ANALYSIS DSHEFS Sample 9 070 071 072 073 07A 075 076 Company and Sample D esignation Cyprus (Three Forks M ill) Montana minus 325 mesh - Cyprus (Three Forks M ill) Montana M istron Vapor (minus 10 m icron) Cyprus (Three Forks M ill) Montana Floor Sweepings (Bagging A re a ). Cyprus (Y ellow stone Mine) Montana D rill Hole Southern t a l c (S o u th ern M ill) Ga. 98Z p a ss in g 200 mesh Southern T aic (S o u th ern M ill) Ga. 99Z p a ttin g 325 mesh (#1767) Southern T alc (C ohutta M ill) Ga. 95Z p a ssin g 325 mesh Source o f 1 Sample NIOSH Survey NI0SH Survey NIOSH Survey NIOSH Survey NIOSH Survey NI0SH Survey NIOSH Survey S outhern T a lc (C o h u tta M ill) Ga. NIOSH 077 25Z p a ssin g 200 mesh Survey M ilv h ite T alc Co. In c . (T ex.) 078 F in ish e d CMA p ro d u c t ^ NIOSH Survey Westex T a lc Co. (TDM) 079 Dark -(M ilw h lte In c .) NIOSH Tex. Survey j M ilv h ite T alc Co. (Tex) 080 K arshel mix - 92-200 mesh NIOSH Survey Westex T alc Co. (M ilv h ite In c .)(T e x NIOSH 081 White mine 93-200 mesh Survey Southern Clay Products - Tex. NIOSH 082 Garren Mine #2 n Survey Texas T a lc Co. - TP1 (T e x .) 083 yline (Texas P a c if ic ) SIQSH Survey Texas T alc Co. Tex. OSA 3avid Mine NIOSH Survey PRODUCT TALC SAMPLES FOR LABORATORY ANALYSIS DSHEFS Salop1* 9 085 Company and Sample D esignation Texas T alc Co. (Tex.> TP2 Mine Cyprus In d u s tria l M inerals Co. 086 Loyce Fine Mine (T ex.) P ioneer Talc Co. In c . (T ex .) 087 Texola Mine ' P io n e e r T alc Co. In c . (T e x .) 088 Dees Mine M ilw hite Co. In c . B ryant 089 Soapstone Mine A rkansas Source of Sample NIOSH Survey NIOSH Survey NIOSH Survey NIOSH Survey NIOSH Survey Laws M ill ( C a l i f .) 090 Clay sam ple, k a o lin + IX g lu e NIOSH Survey Laws M ill Micro t a l c from 091 trtiite Eagle Mine ( C a lif ) Standard In d u stria l M inerals NIOSH Survey Laws M ill (C a lif) Desert Talc 092 Standard In d u s tr ia l M in erals NIOSH Survey Laws M ill ( C a lif) * 093 . io 11day Talc Scandara T ndtiStrial M inerals K eeler T-076 (Cyprus) (C a lif) 094 Tecopa Mine (100Z P a n a a in t) NIOSH Survey NIOSH Survey K eeler HGQ-55 Blend (C y p ru s)(C al) NIOSH 095 4 Panamint, 3 O asis, 3 W hite Eagle survey K eeler S ie r r a Cloud B lend (Cyprus) NIOSH 096 ^C aff# fi n t ` 1 White Ea8 l survey K e e le r, MSC M istron (C y p ru s )(C a lif ilo sn 097 Panamint + 0.5Z s t e a r i t e " Survey K eeler S i e r r a l i t e (C y p ru s)(C a lif 7U<33H 098 T alc City (F risco ) . Survey K e ele r G la c ie r 200 (C y p ru s )(C a lif , NIOSH 399 T alc C ity (T a ilin g s ) Survey PRODUCT TALC SAMPLES FOR LABORATORY ANALYSIS DSHEFS Sample Cccpar.y and Saspl D esignation Source of Sample K eeler USP ( C yprus )( C a lif) NIOSH 100 O asis Mine (100Z) Survey K eeler (C alif) (Cyprus) 101 W hite E agle S c re e n in g s NIOSH Survey K eeler (C alif) (Cyprus) NIOSH 102 Suggar Mine - Survey P f i z e r (C al) T a lc ro n CP 44-31 NIOSH 103 E c lip s e , B onnie, M ongolian Survey P f iz e r (C al) C ercron CF 96-38 NIOSH 104 E c lip s e , Acme, M ongolian Survey P f i z e r c e rc ro n CF 96 -3 6 ( C a lif ) NIOSH 105 W hite E a g le , M ongolian, Apex Survey Cyprus (LA) Furnace C reek ( C a lif ) NIOSH 106 Tecopa (100Z Panam int) Survey Cyprus (LA) V a n d e rb ilt c ru d e 107 S o ft LB (C a lif) NIOSH Survey American T alc (A la b in a ) 84 C olor ilOSH Dark 200 Mesh o re from Willow Survey 108 Creek Mine in Mont. 1 American T alc (Alabama) 92 C olor ilOSH : 99% 400 Mesh o re from W illo r Creek 109 'Mine in Mont Survey Ludlow G a sse tts M ill (Vermont) 110 W indsor M in erals Product 111 112 i 113 114 West Windsor M ill (Vermont) Uindsor M inerals Product West Windsor M ill (Vermont) Hammondsville Mine Windsor M inerals Vermont T alc Company (Vermont) C hescer M ill - V e r ta l 77 Vermont Composite Sample M oretovn, Vermont - D r.Froines I PRODUCT TALC SAMPLES FOR LABORATORY ANALYSIS DSKEFS SAMPLE * 11S COMPANY AND SAMPLE DESIGNATION R.T. V a n d e rb ilt (NY) Mouldene -' . 116 R esu b m ittal o f *071 SOURCE OF SAMPLE Company 117 R esu b m ittal o f *089 118 R esu b m itta l o f *098 119 120 121 122 123 124 R.T. V a n d e rb ilt (NY) F ibertal 1 Company R.T. V a n d e rb ilt (NY) F ibertal 6 Company R.T. V a n d e rb ilt (NY) F ib e r t a l 12 Company C a l if o r n ia Mine no lo n g e r in operation MESA Western T alc (C a lifo rn ia) (R.T. V a n d e rb ilt) MESA ID *0401138 MESA American T alc Co. A lpine, A la. W interboro Mine & M ill Prim ary C ru sh er, Sample 9 /5 /7 4 . ID*01-0O43. Ore From Willow Creek Mine in A lder, Montana MESA [ 12S G eorgia Mine no lo n g e r in o p e ra tio r MESA MTEJBIX A Pmc37 u U 8 lU il il'n S 9 jlil8 - ' ' ? ; ? f ; i d T* * ii APPUOIX \ W^ ^ ^ ^ M*^ *N** ^ r- _ --^ s. .* rx TT ** T* y < g a * < *r* <9 t < . T * T S. ** P*- .; H y S NN N^ S 5 5 il 5 <> w # ^ ^ r* 3 XS i 2 a *X l ! * ` . . . - Tyi' *t *t T\* --- -- * : * I*- ln l* -i Si i - - X 5 1 .................................... " *_ I t 1pt*- *! ?r t'j'j; s ; - " S ia -g " i* 5T- * 5 * " 5 ? S H j B 1* S 8 3 j S s K s: - n t> ^ A <*l ------ -- a m^ N- N-** II Pri *. : **^ * IX rk itti IH E*| -. 4 * ................................. I K i -- 8 ! ATTENDU A PAM39 ;I JtfVUDIX A Pm c 40 %L ti chlorltt tK %L %UM . i. litftr lllMttttt NJKSlU (CA- %i piarti ST TT ;s i I ts I ti ! : ; .15 : 1> / 1j 3-4 1 l-i * 1 * -2 5-6 1iii 1 (S ; 05:t i :; ;< ; 1t .i !*11 j!1iii ;Jl1 1ii li!o1t ;i i :; 1; !- j i-i * ; ji !* II I I -dotai :h m 75-66 !I I h! 'm s , Bt-64 ! j 43-18 i . : 4S a t* 453 <f tm l 1I.I:! rt ! I30 *I !; hi ij :t 15-20 I TI `/rJ ! I ff 1 ; 45% I 46-SI W ; 66-37 s s ; 27-71 (Imfdtk tool Saofmti^eoot CMS 1 KIM/ 44 '* \ a* 4044 5 jk t* tO-fS ! i !i ''1 10-1S s s 55-76 -fmmk <ats 1-3 L i 11 n ; !i ; 1 . !1 - i ; i 11 i i ; n hi ! i 1 1 :*+ , , 7573 31 31-63 i ; ' 5 5 j 3t-6t ij fbtt iats 4043 f/XS !S7 1 .45 I t (Mm. o t it HfUffik 06 ' 43-15 M it* * ! vi to SS&JL .i! \i!i ! i ii i i ; r \ 11-95 2j _ -rl.k.