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*PB84190651* P B 8 4 1 90651 NTZS One Source. One Search. One Solution. ANALYSIS OF TALC BY X-RAY DIFFRACTION AND POLARIZED LIGHT MICROSCOPY MCCRONE (WALTER C.) ASSOCIATES, INC. CHICAGO, IL MAY 1977 PLAINTIFF'S EXHIBIT WCD-12 U.S. Department of Commerce National Technical Information Service QE-CPC00003968 One Source. One Search. One Solution. Providing Perm anent, Easy A c ce ss to U.S. Governm ent Information The National Technical Information Service is the Nation's largest repository and disseminator of government-initiated scientific, technical, engineering, and related business information. The NTIS collection includes almost 3 million information products in a variety of formats: electronic download, online access, DVD, CD-ROM, magnetic tape, diskette, multimedia, microfiche and paper. Search the NTIS Database from 1990 forward More than 600,000 government research information products have been added to the NTIS collection since 1990. All bibliographic entries for those products are searchable on the NTIS Web site at www.ntis.gov. Download Publications (1997 - Present) NTIS provides the full text of many reports received since 1997 as downloadable PDF files. When an agency stops maintaining a report on its Web site, NTIS still offers a downloadable version. There is a fee for each download of most publications. For more information visit our website: www.ntis.gov U.S. DEPARTMENT OF COMMERCE Technology Administration National Technical Information Service Springfield, VA 22161 QE-CPC00003969 A nalysis o f T alc by X-ray D i f f r a c t i o n and Polarized Light Microscopy McCrone (W alter C.) A s s o c i a t e s , I n c . Chicago, il Prepared for National In st, for Occupational S a f e t y and H e a l t h , C i n c i n n a t i , OH May 77 PB84-190651 QE-CPC00003970 ANALYSIS OF TALC BY X-RAY VIFFRACTJON AND POLARIZED LIGHT MICROSCOPY RfPBOOliCfD 8> NATIONAL TECHNICAL INFORMATION SERVICE US OrPARTMFNi Of C0MMf#C( SPRINCIlfiD VA U .S.. DEPARTMENT OF HEALTH, EDUCATION AND WELFARE Public Health Service Center for D isease Control National Institute for Occupational Safety and Health Q E -C P C 00003971 BIBLIOGRAPHIC DATA 1. PtportL'o. SHEET 2. 4. Title and Subt itle ANALYSIS OF TALC BY X -nA Y LILFRACTION AND POLARIZED LIGHT MIC:r o s c o p y 7. Author(s) Lucy B. N[cCrone 9. Performing Oti ;anization Name and Address W alter C. McCrone A ssociates, Inc. 2820 S. MI chigan Ave. Chicago, I L 60616 12. Sponsoring 0 -ganization Name ai>d Address National In stitu te fo r O ccupational Safety and H ealth 4676 Colun ibia Parkway C incinnati, OH 45226 IS. Supplementary Notes 3. Recipient's A ccessio n No. 1 906.5 1.. S. Report Date May 1977 6. 8. Performing Organization Repc. No. 10. Projeet/Task/Work Unit No. 11. Contract/Grant No. CDC-210-75-0063 13. Type of Report Sc Period Covered Final: May '75 - May '77 14. 16. Abstracts One hundred talc sam ples have been analyzed by polarized light m icroscopy, d is persion staining, x -ray diffraction and, when n ecessary, by transm ission electron m icroscopy and electron m icroprobe. The analytical methods were refined in scope, sensitivity and accuracy a s a p a rt of the p ro je c t. The sam p les ranged from 1 to 99% talc with an a v erag e of 63%. T w en ty -th ree o th er m in e ra ls w ere identified including the serp en tin e s: an tig o rite , lizardite and chrysotile; the amphiboles: antkophyllite, trem clite and actinolite; the carbonates: calcite, dolomite, ankerite and magnesite; the talc-like m ineral chlorite as well as quartz, m ica, feldspars, m agnetite, coal, graphite, hydroxygaptite, clays, hydrous iron oxides and ru tile . C h rysotile was found in only one sam p le which, how ever, contained only 1-2% ta lc . M ore than one-third of the sam ples contained trem olite o r actinolite often in m ajor amounts and usually partly fibrous. This rep o rt was subm itted in fulfillm ent of C ontract No. CDC-210- 75-0063 by] W alter C. M cCrone A sso ciates, Inc. under the sp o n so rsh ip of the N ational Institute fq r Occupational Safety and Health. 17. Key *ords aid Document Analysis. 17o, Descriptors x -ray diffi action d o lom ite . m icroscopy m agnesite ' polarized lectrom agnetic radiation quartz . talc asbestos amphiboles ) serpentine 3 calcite 17b. Idem ifiers/( )pen-Eoded Terms chlorite m inerals dispersion staining x -ray step scanning 17. COSATI F ii Id Group 18. Availability Statement FORMNtlS-St (Rltv. io.?) ENDORSED BY ANSI AND UNESCO. k 19. Security C lass (This Report) UNCLASSIFIED 20. Security Class (This Page _____ UNCLASSIFIED_____ THIS FORM MAY BE REPRODUCED 21. No. of Pages 76~ 22. Pure uscomm-oc sass-Pra QE-CPC00003972 ANALYSIS OF TALC BY X-RAY DIFFRACTION AND POLARIZED LIGHT MICROSCOPY Lucy B. McCrone W alter C. McCrone A ssociates, Inc. Chicago, Illinois 60616 C ontract No. CDC 210-75-0063 U. S. DEPARTMENT OF HEALTH, EDUCATION AND WELFARE Public Health Service C enter for D isease Control National Institute frr Occupational Safety and Health Cincinnati, Ohio 45226 May 1977 U QE-CPC00003973 ABSTRACT T here has been considerable controversy during the past few y ears over the com posidon of talc as used in cosm etic talc products. At one tim e m ost of these products w ere re p o rte d to contain c h ry so tile . Although th e se data w ere shown to be erroneous it seem ed desirable to examine a large num ber of raw m aterial talcs from various m ines to determ ine p recisely what m inerals a re p re sen t. One hundred talc sam ples have been analyzed by polarized light m icroscopy, dispersion staining, x -ray diffraction and, when necessary, by transm ission electron m icroscopy and electron m icroprobe. The analytical methods w ere refined in scope, sensitivity and accuracy as a p a rt of the project. The sam ples ranged from 1 to 99% talc with an av erag e of 63%. T w en ty -th ree other m in e ra 's w ere identified including the serp en tin es: an tig o rite, liz a rd ite and chrysotile, the amphiboles: anthophyllite, trem olite aad actinolite; the carbonates: calcite, dolom ite, ankerite and m agnesite; the ta lc -lik e m in eral chlorite as well as quartz, m ica, feldspars, m agnetite, coal, graphite, hydrox yapatite , clays, hydrous iron oxides and ru tile. C hrysotile was found in only one sam ple which, how ever, contained only 1-2% ta lc . M ore than o n e -th ird of :he sam ples contained tre m o lite o r actin o lite often in m a jo r am ounts and usually partly fibrous. This rep o rt was subm itted in fulfillm ent of C ontract No. CDC210-75-0063 by W alter C. M cCrone A ssociates, Inc. under the sponsorship of ihe National Institute for Occupational Safety and Health. ili QE-CPC00003974 CONTENTS A b s t r a c t ........................................................................ iii A cknowledgm ents ....................................................... vi in tr o d u c tio n ......................................................... . . . 1 M ethods of a n a l y s i s .................................................. 1 X -ra y d if f ra c tio n .............................................. 1 P o la riz e d light m ic ro s c o p y .......................... 15 S ta n d a r d s ...................................................................... 21 L is t of m i n e r a l s ................................................ 21 C alib ratio n c u r v e s ............................................ 23 Sam ple c o m m e n ta ry ................... .............................. 34 A p p en d ices: A. D ata s u m m a r y ............................................ 35 B. X -ra y line scans ofs ta n d a r d s ................ 41 C. A nalytical d isp ersio n staining c h a rt . . . 55 v QE-CPC00003975 INTRODUCTION Using the techniques of x -ray diffraction and polarized light m icroscopy we have analyzed 100 sam p les of ta lc pow der supplied by NTOSH. When n e c e s sa ry electro n m icroscopy and electron m icroprobe analysis have been used to supplem ent the data developed by the other techniques. The purpose of the work was to furnish MOSH with the analytical resu lts which a re tabulated in the attached Data Summ ary, (Appendix A. ) While so doing we have tried to refine the m icroscopical and x -ray methods used as they apply to the analysis of talc. METHODS OF ANALYSIS Each sam ple was analyzed by x -ray diffraction and m icroscopy. The x -ray work was done using a Philips x -ray generator and diffractom eter. Each sam ple was fir s t scanned continuously to reco rd a diffraction pattern representing the whole sam ple. The m inerals identified w ere listed and any questionable peak assign ments were noted, for confirmation or resolution by polarized light m icroscopy including dispersion staining. Quantities of each component were estim ated whenever possible, both by polarized light m icroscopy 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 ord er to determ ine any quantities of these present in the talc. R esults of these three types of analysis w ere reconciled with each other and then combined and presented in individual reports for each sam ple. X-RAY DIFFRACTION Sample preparation To insure the b est x-vay powder diffraction results the contract specifies that sam ples in which the a v erag e p a rtic le s iz e exceeds 10 /u n m u st be ground fin er before undertaking x-ray diffraction analysis. Judgment of whether size reduction was n ecessary was m ade by determ ining the p article size distribution m ic ro scopically. The sam ple was used as received if the average particle diam eter was below 10 pm . If the av erag e p a rtic le was la rg e r than 10 p m , o r if the sam ple was not homogeneous because it cartained lumps o r huge p articles, a 2-gram portion was m illed in isopropanol fo r about 10 m inutes in a M cCrone M icron!zing M ill and d ried by slow evaporation to a fre e flowing pow der. 1 QE-CPC00003976 Initially this powder was packed into aluminum cups which rotate in a m otordriven sam ple holder of our design in the Philips diffractom eter. Satisfactory line scans w ere obtained with this sam ple mounting technique but step scanning results w ere not a t all reproducible. After experim enting with various methods of mounting the sam ple, including the use of stationary as well as rotating sam ple holders, we concluded that the m ost reproducible resu lts w ere achieved when the powder was p ressed into a pellet and rotated in the sam ple holder. We therefore prepared the sam ples by p ressin g them in a mold with a die, using a hydraulic p re s s . The half-inch diam eter briquettes o r pellets thus produced had sm ooth surfaces which gave very much b etter reproducibility in step scanning. The aluminum cup was replaced by a flat aluminum disc to which the pellet was attached w ith a h im uf (high vacuum) g re a se . By restin g It lightly on the g rease the pellet can be leveled eithex' in a leveling p re ss o r in the sam ple holder of tbe diffractom eter, pushing with a flat such as a m icroscope slide. All crystalline m a te ria ls used in the sam ple holder assem bly on the su rfa ce exposed to the x -ray beam w ere found to contribute peaks to the line scan. B ra ss , aluminum and Teflon all caused a certain amount of difficulty In this way. Finally we elim inated a ll in te rfe re n c e except an am orphous band n e a r 16 29 by using K E L -F , a stiff fluorocarbon polym er, for all p arts of the surface exposed to the x -ray beam. This sam ple holder is illustrated in the sketch below. specimen holder o f P hilips goniometer ' ^ \ / \ 1 o f 4 braea screws holding Kel-F platform to , / brass support ^ Kel-F holder fo r / y i --^ Z -F platform f 8anpU briquette -brass support a o t _ l yp j- eet screw A j --r o ta tin g Kel-F re c e p ta c le fo r sample fo r bi'ass y j b lo ck, to ;!y * r o ta tin g s h a ft, hollow , Kel-F holder control ' height o f sample holder ---- p in through m etal u n iv e rsa l j o i n t ----- u n iv e r sa l j o i n t w " -----r o ta tin g s h a ft, m etal 1y to 20 rpm motor F igure 1. R otating sam ple h o ld e r for x -ra y d iffra c to m e te r 2 QE-CPC00003977 The chief difficulty encountered with p re sse d pellets was that they w ere hard to m ake with parallel surfaces which, hi turn, m ade them hard to level perfectly in the Sample holder. F or this reason we have som etim es had to co rrect the angles In the tab les in Sam ple D ata R eports listin g ste p scanning data - Wb did this only when we w ere certain from o th er data of the tru e identity of the peak in question, The problem of making good pellets has been largely solved by fabricating a new, very well hardened steel mold and die. B riquetting is thought to have the disadvantage of increasing the p referred orientations of platy m inerals such as talc, chlorite and m ica. Although a few of the sam ples w ere run both as pressed pellets and packed powder it is not possible to determ ine from the data at hand w hether enhancement occurred as a resu lt of briquetting because too many other variables a re involved. Briquetting has the advantage that pellets can be used over and over again, as is necessary for the calibration standards of which the appropriate ones should be reru n every day that step scanning is done. The calibration standards were p re pared by weighing out requisite amounts of the standard and of Verm ont talc which had been m icronized fo r 60 m inutes, m ixing in isopropanol e ith e r in a W aring B len d er o r In the m icronizing m ill, drying and b riq u ettin g . Sample and stan d ard pellets a re conveniently kept in sm all glassine envelopes. L ire scanning All x -ray work was done using nickel filtered copper radiation. A fine-focus P hilips tube pow ered a t 42 kV and 25 m a was used fo r about 80^ of the w ork. The la s t 20% was done using a stan d a rd focus P h ilip s tube a t 40 kV and 18 m a. (The step scanning calibration curves were redeterm ined every tim e the generator o r sam ple form was changed in any w ay.) Line scanning fo r each sam ple was done from 4 a to 70 26. A fter considerable experim entation we concluded that because the sam ples usually are m ixtures of sev eral m inerals it is b est to scan at the m ost sensitive possible diffractom eter settings to bring out sm all peaks which a re due to m inor constituents of the sam ple. This m eans that the strongest peaks a re usually off-scale on the chart. We th ere fore m easu re these peak m axim a by line scanning a t lower sensitivity or by step scanning and the resulting peak intensity data on the line scanning chart. X -ray line scans recorded in this way provide a good starting point for identifying the com ponents in a talc sam p le. Beginning at 4* 20 the peaks encountered and th e ir assignm ents a re as follows In T able 1. 3 QE-CPC00003978 Table 1. X -ray diffraction peak assignm ents 20 d, k CuKu Intensity Comments or crite IA i Peak assigned to A ltern ativ es fo r choice 6.3 14.0 80 8.75 10.1 8.88 9.95 100 95 9.45 9.35 100 9 .5 9 -9.69 9 .6 6 -9.79 9.21-9.12 9 .1 5 -9.03 50 20-80 1C. 52 8.40 100 10.55 8.38 100 10.61 8.33 100 10.61- 8.33-10.70 -8.26 70-55 12.01 7.36 12.05 7.34 100 100 12.20 7.25 100 chlorite Vermiculite chlorltes have strong peaks at 1 2 .4 4 -1 2 .5 5 and 25 .1 3 ; Vermiculite has much weaker peaks at 12.39 and 24.99*. biotite m ica muscovite m ica m uscovite, phlogopite, biotite, phlogopite biotite has a strong peak at 26.42, muscovite at 26.83, phlogopites from 26.49 to 26.60 talc grunerite (am osite) cum m ingtonite (m ontasite) dimming - tonite grunerite n e ith e r am phibole found in any talc sample analyzed riebeckite (crocidolite) trem oliteactinolite grunerite (am osite) anthophyllite trem oliteactinolite riebeckite (crocidolite)i crocidolite not found in any talc sam ple; distinguish by m icroscopy-crocidolite is the only asbestos with negative elongation cummingtoni anthophyllite has a (montasite) fairly strong peak at anthophyllite 27.59; am osite and grunerite (am osite), , m ontasite not found in any talc sam ple analyzed cum m ingtonite (m ontasite) chrysotile lizardi te antigorite lizardite chrysotile, antigorite lizardite b est distinguished by polarized light m icro s copy with dispersion staining 4 continued QE-CPC00003979 *20 d, A CuKc. Intensity V l. 1 Peak assigned to A lte rn a tiv is Comments or criteria for choice 12.44- 7.1112.55 -7.05 13.04 6.44 17.38 5.10 100 60 50 c h lo ri1-* orthoclase fo rste rite antigorite, chrysotlle, lizardite - chlorites have a strong p ea'; n e a r 6.3* - -- 17.48 5.07 16 tre m o li te forsterite look for strong trem olite peak at 10.55 17.83 4.97 18.62 4.76 30 20 m uscovite trem olite -' chlorite - look for strong trem olite peak at 10.55 18.78 4.72 18.99 4.67 18.99 4.67 80 66 20 chlorite talc anthophyilite -- anthophyilite i talc peak of intensity 8 enhanced by orientation; talc \ look for anthophyilite peaks at 10.70* and 27.59 19.32 4.59 19.32 4.59 19.32 4.50 30 50 20 19.32 4.59 45 antigorite llz ardite biotite talc lizardite, talc antigorite, talc talc, lizardite, antigorite lizardite, antigorite distinguish serpentines from talc and from each other by m icroscopy; look foi biotite peak at 10.1 5 continued QE-CPC00003980 26 d, A CuKa Intensity I /! i Peak assigned to A lternatives Comments or criteria for choice 19.45 19.49 4.56 4.55 25 40 19.58 4.53 19.67 4.51 19.75 4.49 20.49 4.33 20.83 4.26 -0.93 4.24 12 20 35 6 35 30 21.03 4.22 21.13 4.20 45 35 21.55 4.12 22.04 4.03 22.09 4.02 6 * 90 talc chrysotile talc trem olite ai. -tophyllite talc quartz antigorite mio roc line trem olite talc dolom ite orthoclase chrysotile talc look for chrysotile peak at 12.01 chrysotile peak is broad and poorly defined - talc peak seldom observed anthophyllite look for unthophyllite peak at 27.?9 trem olite - seldom observed - quartz look for m ajor peaks or use microscopy trem olite m icrocline look for strong m icrocline peak at 27.50, trem olite at 10.55 and use m icroscopy - seldom observed orthoclase J dolomite l assignable to orthoclase unless a m a jo r am ount of dolomite present 22. 90 3.88 22.90 3. 88 22.90 3.88 30 30 70 22. 96 3.87 16 li/ardite orthoclase forate rite o rthoclase, look for m ajo r lizard itc forsterite peaks at 12.05' and fo rsto rite, 36. 03; look fcr strong lizurdlte 1 orthoclase peak at 28.04' , orthoclase, or use microscopy llzardite trem olite 6 orthoclase, etc; calcite continued look for m ajor trem olite peak at 10.55 QE-CPC00003981 1 9Oe d, Intensity Feak assigned tc Comments or c rite ria A ltern ativ es fo r choice *: f 1 23. 02 3.86 12 calcite trem olite look fo r calcite peak j a t 29.40 and u se m icroscopy 23. 39 3.80 23. 84 3.73 24. 10 3.S9 80 18 5 '" 'th o c la s e m u sco v ite d olom ite -- - - observed only when muci dolomite present 24. 36 3.65 24. 50 3.63 24. 62 3.62 25. 13 3.54 60 60 60 80 chrysotile lizardite antigorite chlorite lizardite chrysotile, antigorite lizardite use polarized light m icroscopy with d ispersion staining serpentines look fo r chlorite peak at 6.3 25. 90 3.43 1 2 6 . 38 3.376 40 talc trem olite biotite nearly always present look for trem olite peak at 10.55 26. 42 3.37 100 biotite trem olite look for biotite peak at 8.75 26, 64 3.343 100 quartz m icas look fo r quartz peak at 20.83 26L 66 3.34 25 m uscovite quartz look for m uscovite peak at 26.83 26 83 3.32 100 m u sco v ite - - 27 ,08 ?.. 29 50 m icrocline 7 continued QE-CPC00003982 "28 d, CuKa Intensity Comments o r c rite ria I/!i P eak assigned to A lternatives for choice 27.26 3.268 75 27.33 3.26 80 27 50 3.24 100 27.59 3.23 50 trem olite g ru n e ri te (am osite) m icrocline anthophyllite 27.94 28.03 28.58 3.19 3,18 3.12 30 100 55 28.58 3.12 100 m uscovite orthoclase riebeckite (crocidolite) tale * 28.59 28.68 3.121 100 3.11 100 trem olite actinolite grunerite (am osite) use m icroscopy; grunerite has higher re fra stive indices trem olite anthophyllite 1 look for anthophyllite m icrocline ( peak at 10.70 and m icro - cline peak at 27. use microscopy oOcO orthoclase m uscovite look for m uscovite peaks: 8.88 and 26.83 tale trem olite use microscopy; crocidolite has negative elongation trem olite actinolite, riebeckite enhanced by orientation; look for talc peak at 9.45 tale 1 talc J look for trem oliteactinolite peak at 10.55 and talc peak at 9.45 29.17 3.06 100 29.17 3.06 90 29.40 3.035 100 anthophyllite g ru n e ri te (am osite) calcite calcite, grunerite anthophyllite anthophyllite look for anthophyllite peaks a t 10.70 and 27.59 use m icroscopy-grunerite has oblique extinction look for calcite peak at 23.02 ; use m icroscopy 8 continued QE-CPC00003983 2 0 Intensity Comments o r criteria Cu:Kd d, A l / l l Peak assigned to Alternatives for choice 00 29 ,90 2.987 30 ,40 2.938 30 .96 2.886 31 .26 2.859 31 .47 2.84 31 .88 2.805 32 2.754 35 40 100 25 50 45 70 32 .63 2.742 100 32 .,78 2.726 40 33 .09 2.705 33 .53 2.670 90 10 33 .66 34 .42 34 .58 2.66 2.603 2.592 80 80 30 34.94 2.566 55 35 .15 2.558 70 35 .46 2.529 40 35 .559 2.52 90 35 .( ;o 2.52 40 35 1 2.512 35 A >4 2.503 70 18 m uscovite trem olite d olom ite m uscovite chlorite trem olite grunerite (amosite) m agnesite riebeokite (crocidolite) -- -- -- -- -- -- m agnesite grunerite m agnesite trem olite dolomite -- biotite biotite chlorite trem olite -- -- chlorite m uscovite chlorite chlorite m uscoriie trem olite artigorite antigorite, biotite biotite biotite antigorite forsterite m agnesite -- calcite 9 continued look for am osite peak at 10.61" confirm m agnesite by m icroscopy look for crocidolite peak at 10.52 o r use m icroscopy seen if much dolomite present; use microscopy look fo r trem o lite peak at 10.55" look for m uscovite peaks at 8.88" and 26.83" look for chlorite peak at 6.3" look for trem o lite peak at 10.55" look for antigorite peak at 12.20" look for biotlte peak at 8.75" look for m agnesite peak at 32.63" QE-CPC00003984 20 o Intensity CuKa d, l/l-y Peak assigned to Alternatives Comments or criteria for choice 35.96 2.495 14 36.03 2.49 100 36.25 2.476 36.52 2.458 65 80 36.52 2 .458 100 36.52 2.458 12 36.65 2.45 40 36.65 2.45 80 37.36 2.405 37.70 2.334 10 25 37.76 2.380 30 38.48 2.337 16 38.52 38.76 39.31 2.335 2.321 2.285 30 40 18 39.45 2.282 12 40.28 2.237 41.14 2.192 41.38 2.18 41.72 2.163 6 30 80 35 calcite lizardite talc chlorite forsterite quartz chrysotile biotite dolom ite m uscovite trem olite talc trem olite trem olite calcite quartz quartz dolom ite biotite trem olite m agnesite, lizardite calcite -- fo rste rite , quartz chlorite, quartz chlorite, forsterite biotite chrysotile -- trem olite m uscovite trem olite talc -- quartz calcite -- -- -- antigorite look for calcite peak at 29.40 look for lizardite peak at 12.05 look for chlorite peak at 26.64, forsterite peaks at 17.38 and 22.90 look for chrysotile peak at 12.01 look for biotite peak at 8.75 look for m uscovite peaks at 8.88 and 26.83' look for trem olite peak at 10.55 peak enhanced by orienta tion; look for talc peak at 9.45' look for calcite peak at 29.40; use microscopy look for quartz peak at 26.64 look for trem olite peak at 10.55 10 continued QE-CPC00003985 '2 a Intensity Comments or criteria Cu|Ka d, l/l Peak assigned to Alternatives for choice 41.78 2.16 40 41.78 2.161 30 41.99 2.15 42.25 2.13 42.44 2.128 60 46 9 42.99 43.14 43.25 2.102 2.095 2.09 45 18 10 44.95 2.015 15 44.95 2.015 45 45.30 2.000 45.30 2.000 60 80 45.47 1.993 45.79 1.980 80 6 46.81 48.04 48.50 1.939 1.892 1.875 12 50 17 48.64 1.870 40 50.08 1.817 17 50.55 1.804 20 51.17 11.786 30 i l . 781 51.62 1.769 4 53.88 1.700 35 antigorite m icrocline m icrocline antigorite lizardite talc quartz -- -- -- m agnesite calcite chrysotile -- -- calcite d olom ite trem olite trem oli te d o lom ite chlorite biotite biotite chlorite m uscovite quartz -- -- m agnesite trem olite calcite -- -- talc talc calcite quartz d olom ite dolomite -- m agnesite m agnesite 11 continued look for antigorite peak a t 12.20 look for m icrocline peaks at 27.08 and 27.50";use microscopy seen only when much quartz present not seen in line scan of standard look for dolomite peak at 30.96" look for trem olile peak at 10.55 look for chlorite peak at 6.3 look for biotite peak at 8.75 seen when much quartz present look for calcite peak at 29.40 o r use m icroscopy look for talc peak .'t 9.45 QE-CPC00003986 20 CuKa d , Intensity / l l Peak assigned to A lternatives Comments or criteria for choice 55.03 1.672 55.70 1.649 57.40 1.604 58.89 1.567 59.09 1.562 7 40 8 8 40 59.60 1.550 59.80 1.545 59.98 1.541 70 10 15 60.02 1 .5 4 80 60.20 1.536 40 60.24 1.535 60 60.41 1.531 70 60.50 60.58 61.80 1.529 1.527 1.500 55 40 60 61.80 1.500 25 62.35 1.488 65.38 1.426 67.09 1.394 67.36 1.389 67.74 1.382 68.14 1.375 6 4 20 15 7 11 quartz trem olite calcite dolom ite antigorite chlorite dolom ite quartz biotite antigorite chrysotile lizardite talc talc lizardite anthophyllite m agnesite m agnesite talc dolom ite quartz quartz -- -- -- -- -- -- -- biotite quartz -- antigorite talc -- -- anthophyllite lizardite -- -- -- -- -- -- doublet with peak at 60.20 look for quartz peaks at 26.64 and 20.83 look for biotite peak at 8.75 doublet with peak at 59.09 chrysotile has single peak, anti qorite has doublst (59.09 and 60.20) doublet with peak at 61.80 doublet with peak at 60.41 look for anthophyllite peaks at 10.70" and 27.59 12 continued QE-CPC00003987 20 Intensity Comments or criteria CviKa d, l / l i Peak assigned to Alternatives for choice 68.30 1.372 68.36 1.371 9 4 69.00 1.36 60 69.34 1.354 8 quartz m agnesite biotite m agnesite -- quartz -- -- look for m agnesite peak at 32.63, o r use m icroscopy 13 QE-CPC00003988 Step scanning Samples w ere analyzed for trem olite, anthophyllite, chrysotile and quartz by step scanning. Because the sam ples a re m ixtures, som etim es very complex, it is b e tte r to step scan the stro n g est peak of each m ineral that is reasonably in terferen cefree than to use too weak a peak, e .g ., the 1.54A line of quartz, even though it is b e tte r resolved from in terferin g substances. The regions chosen on this basis for step scanning are as follows: Line Region a alinolite - trem olite (26 - 1 0 .5 5 , 8.38A ): 10.30 - 10.70 29 anthophyllite (20 . 10.7 0 , 8.26A ): 10.00 = 10.90 20 o r (29 . 27 59, 3.23A ): 27.50 - 27.80 20 ch:.ysotile (20 = 1 2 .0 1 , 7. 36A): 11.90 - 12.40 20 quartz (20 = 2 6 .6 5 , 3.343A): 26.55 - 26.75 20 Counting tim es of 100 seconds and steps of 0.01 20 w ere found b e st. Some peaks ' w ere scanned using sh o rter counts, especially when m icroscopy had indicated the absence of the m in eral being sought. In no case, however, was the sh o rter count e v e r le s s than 30 seconds and usually we used 50 onds. In te rfe re n c e with the 10.55 20 tre m o lite -a c tin o lite peak was esse n tially nil but the tail of this peak overlaps the anthophyllite peak at 10.70, making a weak anthophyllite peak difficult to distinguish. As an alternative the anthophyllite peak at 27.59 ':an be used except when an in terferin g m in eral such as m ic ro cline is present, as in Sample 076. C hrysotile was detected in only one sam ple, No. 048, by light m icroscopy with no detect! on by step scanning. The c h ry so tile peak a t 12. 01, the liz a rd ite peak at 12.05 and the antlgorite peak a t 12.20" may not always be distinguishable from one another. Since other serpentine peaks in the line scan do net always stand out we have relied m ore upon m icroscopy to confirm which polymorphs arc present, than upon the c rite ria for x -ray peak assignm ents given by Mumpton*, although the latter are useful when the serpentine concentration is great enough. * Mumpton, F red erick A. C haracterization of C hrysotile A sbestos and Other M em bers of the Serpentine Group of M in erals, Siemens Review XLI (1974), Seventh Special Issue, X -ray and E lectron M icroscopy News. 14 QE-CPC00003989 The quartz peak at 26.65 is three tim es the intensity of the next strongest, a t 20.83, and is p re fe rre d except when m uscovite m ica is p re sen t. The 26.65 quartz peak is usually distinguishable by step scanning from the m uscovite peak a t 26.85 and the b io tite m ic a peak a t 2 6 .4 2 " , but not from the 25% in ten sity m uscovite peak at 26.66. When m uch m uscovite is p resen t, as in Sample 125, the 20.83 peak is p re fe ra b le . Minimum levels of detection by step scanning found for standards in talc using the peaks discussed above are: trem olite - 0.5%, anthophyllite - 2.5%, c h ry so tile - 3% and q u artz - 0.2%. O ur tre m o lite stan d ard is predom inantly nonfibrous; others have reported that fibrous trem olite gives about 1/4 to 1/3 the response at 8.38A obtained from nonfibrous trem olite in talc*. M ost of the sam ples in which we found trem o lite contain a preponderance of the nonfibrous habit. POLARIZED LIGHT MICROSCOPY We have applied two kinds of m icroscopical analysis in identifying components of talc sam ples. F irs t, petrographic observations in plane p o larize! light (mainly morphology and refractive indices) and between crossed polars (morphology, birefringence, type of extinction, extinction angle and som etim es interference figures). Second, the use of dispersion staining to identify m in erals. Appendix C, the analytical dispersion staining chart, is specifically designed for talc sam ples. M ost of the above o bservations a re m ade a t 200X m agnification using the 1QX dispersion staining objective with a 20X ocular. High power objectives a re som e tim es used to exam ine the sm allest p a rtic le s and fib ers o r fo r in terferen ce figures. Our usual procedure Is as follows. Procedure 1. Analyze the x -ra y line scan to identify the m ajo r components and define any questions to be answ ered by m icroscopy. 2. Mount representative sam ples, about 0.1 mg each, of the unmilled m aterial in the C argille re fra c tiv e index liquids specified below. O bserve cen tral stop d isp ersio n staining c o lo rs in each liquid and re la te them to the curves in Appendix 3. Check birefringence and extinction between crossed polars,. and refractive indices relativ e to the mounting m edium . Look for fibers by d isp ersio n staining and between crossed polars and check whether particles a re really fibers or plates on edge by making them tumble in the liquid to exhibit all views - tapping on the coverslip with a needle will m ake the particles tumble into a succession of random orientations. Table 2 gives the refractive indices of m ost m inerals of In terest in talc samples. J . Schelz, private communicato i 15 QE-CPC00003990 Table 2. R efractive indices of m inerals sought in talc sam ples M ineral chrysotile quartz lizardite antigorite talc chlorite trem olite anthophyllite actinolite forsterite calcite grunerite (amosiie) dolom ite m agnesite riebeckite (crocidolite) R efractiv e In d ices, n2^5 C a or w (3 v or c 1.544 1.544 1.545 1.545 1.546 1.5GG 1.599 1.603 1.633 1.S43 1.653 1.669 1.677 1.694 1.698 1.552 1.557 1.588 1.5G7 1.610 1.617 1.641 1.663 1.681 1.703 1.555 1.553 1.558 1.560 1.589 1.596 1.621 1.628 1.647 1.682 1.486 1.697 1.500 1.509 1.708 IS QE-CPC00003991 M inerals, especially silicates but also the isom orphous series of carbonates (calcite, dolomite, m agnesite e tc .) vary in refractive index. Table 2 and Appendix C show average indices for the m inerals which m ight be found in talc. G enerally, the dispersion staining curves fo r these m inerals move p arallel to th em selv es as the com position changes. T he b ire frin g en c e values ( v - 3, (3--a and - us) w ill g e n erally re m a in n e arly constant fo r a given m in e ra l although the indices them selves may vary considerably. Bo h morphology and optics a re noted in o rd er to identify the asbestiform m b ie ra ls . To be a sb e stifo rm re q u ire s th at they be fib e rs , (as defined by NIOSH) m e a su rin g ,< 5 /m in d ia m e te r, <200 pm in length and have a length to width ra tio of at le ast 3:1. 25 C argille high dispersion liquid np 1.550: A representative sam ple mounted in this liquid will show ch aracteristic colors for any of the following: talc, quartz, chrysotile, lizard ite, antigorite and many fibers (paper, silk, viscose rayon and human hair, etc.). The crystallographic data in Appendix C and m orphological observations should ensure identification of m ost cf these substances or allow the conclusion that any other substance showing colors in this liquid is not one of those listed (Figure 2). C haracterization of this extraneous substance will often be possible by re ferrin g to the P article A tlas. * ng C argille high dispersion liquid n ^ = 1.585 This liquid is useful for distinguishing talc from chlorite. Edge views of chlorite a re m agenta for the index perpendicular to the plate. Talc is magenta for the index p arallel to the plate. 25 C argille high dispersion liquid n ^ = 1.605: C hrysotile and all other substances giving dispersion staining colors in liquid 1.550 will be white or pale blue in 1.605 (Figure 3). Talc is the only substance in this group that shows a \ q close to the visible (ca 700 tun). All talc plates show both n 's (P &V ) close to 1.605 in the red hence the c e n tra l stop shows a pale blue in all directions lying in the talc plate and white corresponding to the a d irectio n . O ther m in e ra ls showing co lo rs in nj> = 1.605 include tre m o lite , chlorite and actinolite (Figure 4). * M cCrone, W .C. a n d J.G . Delly. 1973. The P article A tlas, Edition Two. Ann A rb o r Science P u b lish e rs, Ann A rb o r, M ichigan 17 QE-CPC00003992 Talc: Q u artz: concholdal flakes, all show XQ ca 680 no corresponding Co u on rotation of the stage; 90* froa Che u orirnca- tlon either c (X * 590 nm) or any c' (590 <Aq <680). . a > r v ----white yellow white-blue (>700) Chrvsntile- a A blue (6G0) Paper fibers : lrrei.u ar rounded fibers ycl low-white % X 7 v pale blue Lizard Itc : aggregates of very fine plates, n's slight > chrysotile, t i y in plane of plates 1^ -- 600 nn tie magenta). Antlgorltc: .a golden yellow ('.70) (c.i 400) F igure 2 C entral stop d isp ersio n staining c o lo rs in C arg ille liquid ri25- 1.550 (HD s e rie s ). 18 QE-CPC00003993 C a r c l l l c L iq u id t>D- 1 . 6 0 5 : Talc : Trenollte: vhltc (700) Acclnolitc: Anthophylllte: j<* b l u v i o l e t (615) yallow (00) Ift or-nue yellow (670) L yellow (600) f Figure 3. C entral stop dispersion staining colors in C argille liquid nQ = 1.605 (HD s e rie s ). 19 QE-CPC00003994 C arglllc Liquid ActlnolIte: - 1.G60: P pale b lue (>700) rr4 pale M u ; (ca 700) Forrterite: blue-grc:n (640) yellow (460) a | v. pale blue (>700) *' ! 1* bluc-grc-tn (640) Dolonite: pale yellow ( c a 4.1C' a j pale blue (>700) / '**' mn f . c n t n ( 5 4 0 ) P i bluc-grccn (640) r1 y *__ r-- blue runs enta (570) r C u r . - i i n e,; o n l t < : a t M u e -g re e n (660) a / e l l e . , -.in) ____ _______ w h ite (<<4CC) Apat Ite : .w <> r \ r r e in (730) bluc-gccen (>700) a 1u c - g r e r n ( 7 0 0 ) b l u r - g r r r i t ( 7 r,0) F igure 4. C entral stop d isp ersio n staining c o lo rs in C argille liquid (RF series). 1. 6(50 20 QE-CPC00003995 Anlhophyilite often shows colors sim ila r to tremoLite but exhibits p arallel ex tinction on all views. T rem olite shows p arallel extinction for one view but oblique extinction of 10 to 21 fo r the a - Y view. Cargille Liquid n ^ = (RF series) N on-talc m in erals showing disp ersio n staining co lo rs in n ^ = l . 660 include actinolite, fo rsterite, hornblende, calcite, cummingtonite and dolomite (Figure 5). C arg ille Liquid n ^ = 1.700 (M s e rie s ) M inerals to look for in n ^ = 1.700 include cummingtonite, grunerite, crocidolite and m agnesite. STANDARDS LIST OF MINER aI.S The following m inerai standards were used for m icroscopy and quantitative x -ray diffraction: Verm ont talc (kindly supplied by W indsor M inerals) anthophyllite, Haddam, Connecticut chrysoliie, Victory Mine, Globe, Gila County, Arizona trem o lite, Fow ler, New York a -quartz, synthetic single crystal . In addition, the m inerals listed below w ere used fo r m icroscopy and qualitative x -ray diffraction: lizardite, Kennack Cove, Cornwall, England chlorite, C alaveras County, California prochlorite, C hester, Vermont anthophyllite, Guffey, Colorado anthophyllite, C ashiers, North Carolina actinolite, Lake W enatchee, Washington trem olite, fibrous, Dahl Creek, Alaska X -r ay line scnns of all of the above a re attached as Appendix B. 21 QE-CPC00003996 C a rg llle Liquid nD " 1.700: CunCTlngConltc: / v. pale > P v. pale b y '~-- --^ v. pale * Crocido!ite : Crunerlte: O y pale blue (700) yellow g490) P I blue (590) ' V }--> (620) Magnesite: (660) yellow (490) 1naeenta (530) white (>>>700) blue (690) F igure 5. C en tral stop d isp ersio n staining co lo rs in C arg ille liquid n25= 1.700 (M s e rie s ). D* 22 QE-CPC00003997 A ppropriate sam ples of these rrin erals appear on the analytical dispersion staining ch art, Appendix C, which also includes antigorite, calcite, dolom ite, fo rsterite, grunerite (amosite), m agnesite and riebeckite (crocidolite). CALIBRATION CURVES The firs t five m ineral standards listed w ere used to p rep are the briquettes for step scanning calibration as described on page 3 of this re p o rt. Using these briquettes calibration data were determ ined for quartz, chrysotlle, trem olite and anthophyllite m ixed with V erm ont talc. The calibration curves follow as F igures 6 through 15. In each figure a t le a s t two curves a re plotted, one based on integrated intensity and one on maximum peak height. In m ost regions both curves have slopes sim ila r enough so that either could be used analytically. When this was not the case the integrated intensity curve was used. Curves w ere redeterm ined completely for the last 20 sam ples which, because of generator breakdown had to be run using the standard focus tube at lower power. Curves w ere checked a t least after every tenth sam ple, as specified in the co n tract, but it was found b e tte r to check c alib ratio n ev ery day thp.t step scanning was dene, i. e . , a fte r ev ery one to th re e sam p le. T h re e m ethods of determ ining the integrated intensity w ere compared: totalling the heights of uniform steps under the peak, finding the area under the plotted peak by p lan im etry o r sq ure-countin g (F ig u re 9) and cutting out and weighing the plotted peak (Figure 11). Since we found that all three methods gave equivalent resu lts we made the g re a te st use of the firs t because it required le ss curve plotting. 23 QE-CPC00003998 to ta l of 0.01 step heights under curve, net counts per second peak height at 26.65 20, net counts per second ^ 2 5 0 0 -1 0 12 34 percent quartz in talc ~ 150 ' 140 * 130 - 120 110 100 - 90 - 80 70 - 60 - 50 - 40 - 30 - 20 - 10 F igure 6. C alibration c u rv e s, 0.25 - 3% q u artz in ta lc , 3. 343 A peak, n ic k e l-filte re d copper radiation at 4 2 kv and 25 m a. 24 QE-CPC00003999 n e l c o n n L r \ peak height at 26.65 29, net cpa o percent quartz in talc F igure 7. C alibration curves (coincident), 1-3% quartz in talc, 3.343 A peak, n ic k e l-filte re d co p p er radiation at 40 kv and 18 m a. 25 QE-CPC00004000 total of 0.01 step heights under curve, net counts per second, thousands peak heights at 26.65 20. net counts per second 0 50 percent quartz in ta lc 100 '9 F ig u re 8 C alibration c u rv e s, 3 - 100% q u a rtz in ta lc , 3.343 A peak, n ic k e l-filte re d copper rad iatio n at 4 2 kv and 25 m a. 26 QE-CPC00004001 area under curve peak height at 12,01 20, net counts per second 20 1 f *c0 o Naoa> +(-0 S ou 4> c 15 - CM c 10 - 50 o F igure 9. C alibration c u rv e s, 3 - 25% ch ry so tile in talc, 7.36 A peak, n ic k e l-filte re d copper rad iatio n at 42 kv and 25 ma. 27 QE-CPC00004002 total of 0.01 step heights under curve, net counts per second peak height at 10.55 29, net counts per second F igure 10. C alibration c u rv e s, 1 - 45% tre m o lite in ta lc , 8.38 A peak, nickel-filtered copper radiation at 42kv and 25ma. 28 QE-CPC00004003 milligrams, weight of curve plotted on paper and cut out A peak heights at 10,55, net counts per second o 70 0- percent tremolite in talc gure 11. C alibration c u rv e s, tre m o lite (17- 98%) in ta lc , 8.38 A peak, n ic k e l-filte re d copper rad iatio n at 40 kv and 18 m a. 29 QE-CPC00004004 Figure 12. C alibration cu rv es, 0 .5 - 1.0% trem o lite in talc, 8.38 A peak, n ic k e l-filte re d copper radiation at 42 kv and 25 m a, old d e tec to r. 30 QE-CPC00004005 t o t a l of 0.01 step heights under curve, net counts/second peak height a t 10.70 26, net counts per second 31 QE-CPC00004006 total of 0.01 step heights under curve, net counts per second peak heights at 27.59 28. net counts per second O 800-, 700- r 50 600500- 400 300- 200- 100- 0 + ~i------- 1------- j------- 1------- 1------- 1------- -------- 1------- 1------- f-0 0 5 10 percent anthophylllte in talc F igure 14. C alibration c u rv e s, 3 - 12% anthophyllite in ta lc , 3.23 A peak, n ic k e l-filte re d copoer rad iatio n at 42 kv and 25 m a. 32 QE-CPC00004007 total of 0.01 step heights, net counts per second peak heights at 10.70 29, net counts per second 800 ,, 700 . 600 500 400 300 200 100 - L 60 - 30 percent ant.lophylli:e in talc Figure 15. C alibration c u rv e s, 3 - 12% anthophyllite in talc, 8.26 A peak, n ic k el-filte re d copper rad iatio n at 40 kv and 18 m a. 33 QE-CPC00004008 SAMPLE COMMENTARY The purpose of this section is to put down som e random observations concerning certain sam ples or the se t of sam ples as a whole. 1. No am osite (grunerite) o r crocidolite (riebeckite) asbestos was detected in any sam ple. I 2. C hrysotile was found only in one sam ple, No. 048. This is not really a talc sam ple about 70% of It c o n sists of the olivine, fo r s te rite , and only one o r two p ercen t of talc. The amount of ch ry so tile was estim ated at 4-5% by m icroscopy and a sim ila r amount of antigorite was also detected by x -ra y diffraction. 3. Two o th er sam p les, 062. and 063, contained m odest am ounts of f o is te r ite (5%) but no c h ry so tile o r a n tig o rite , though a little liz a rd ite v'as noted in Sample 062. One p ercen t o r less of m agnetite, Fe^O^, was common to the th ree fo rsterite-co n tain in g sam ples. 4. T rid y m ite was found in one sam ple only, No. 090, a t a level of 30%. This sam ple contained 22% q u a rtz and 25% clay but only 5-10% talc. 5. Small amounts of m agnetite, Fe O^, w ere found in many sam ples but one sam p le, No. 077, contained 15%. No o th e r sam ple contained n e arly this much. 6. A nthophyllite was net detected unless a t le a st 8% of tre m o b 'te -ac tin o lite was also p re s e n t. It was found in all sam ples containing 13% o r m o re tre rro lite . 7. T rem o lite a n d /o r actin o lite w ere found in la rg e q u an tities, up to n e a rly 60%, in many sam ples. Em phasis on the G ouverneur talc3 partly exDlains why so many w ere found. 8. Q uartz was p re s e n t in all but nine of the 100 sam p les. The m axim um q uartz contents of 21%: and 22% o c cu rred in two sam p les, 055 and 090, which ap p ear to be re la te d only by th e ir low ta lc content o th erw ise. 9. T h ere w ere ten very pure talc sam ples: 009, 057, 067, 068, 069, 071, 072, 109 and 111. The p u re st of them is 057. Im p u ritie s, Wiiich differed in each sam p le, w ere chlorite, dolomite, quartz, m agnesite and m ica. 10. Seven sam ples contained m o re than 50% of ch lo rite: 053, 076, 098, 099, 102, 118 and 125. R utile, TIO^, was identified in two of th ese sam p les. 11. Eight sam ples had high m agnesite contents, from 3J to 50 p e rc en t, and fo u r teen sam ples w ere high in dolom ite, 10 - 20%. High c alc ite content was uncommon; one sam p le, No. 105, contained up to 15% and four o thers w ere in the 8 to 10 p e rc e n t ra n g e . One sam p le, 0 7 3 ,contained 9C% of dolom ite. 34 QE-CPC00004009 APPENDIX A Data Summary Appendix A is a five page table which sum m arizes the analytical re su lts for each of the 100 sam p les. F o u r m ethods of quantitation w ere used and a re coded as fo llo w s: method code x -ray diffraction step scanning S x -ray diffraction line scanning L polarized light m icroscopy M difference D The method usually used in finding the quantity of a given m in e ra l is noted after the % sign in the column heading for that m in e ra l. When a method different from that noted in the heading was used the le tte r code for that method follows the percentage listed in the table for the p articular sam ple. In the case of tre m o lite -a c tin o lite "% fib e rs " m eans the p ercen tag e of the total trem olite and/or actinolite that is fibrous, as contrasted with m assive p articles. This w as, of course, always determ ined by polarized light microscopy with the use of dispersion staining. 35 QE-CPC00004010 SI ta* 5: m Sgif il 5^*5g | f I I ?ta <J t ta`-4 ^*4 ^- ta ta tn 5; ? $ * s * .^ . t *- * * U S _ 3 t_____________________ 1 S K fr 8 f Vv y V v s H s ^ S 1 . 4 1 > O "ta ta ! i l ^ *T> : 5> ??? <\***S>`WhJC3LTi . S & v - * E , J . & V E J tal s i y> ta i JJ 5 5 5 - ^ T7 5 N S J v> <3 <3 <3 <S <5 Vv v V V >< N S vv ^ *"N -- N Ste' >**i i~K*5 i 34 v v 'V S S S S Q S ' t a TN Oi , il 1 gs !f> * ta M ^557^ APPENDIX I Pa g e 36 1- S *- ^V?f * --v -s sfi ** v-- v *? * * ta tat a w $ - ^ - ? o *44 0 ., t Hy , V N> ' , ~ * * tv> a ,*>_ 5: n\n v ^ > 5i ** V - ^^ , Ooo frj JC vl -- v- 3 i** ta n ^i ! * i *0 V> ? it i i S N N !T) ^ *?5v`"j3s5 ^ VV ^v _v ~ ta ^ ^ VJ j< a SJ ta Vtn w ta ta S _ *> v CO ^ *>v. _ ^ W 'o <o U *k CKl jk $ 5 5 ? 5 i ? 5 5 s 5 s n ta SSH 5 .2 ? n s ! n H a U h H Q E -C P C 00004011 QE-CPC00004012 QE-CPC00004013 Ho.'l /** *4 S6S Oil 3.V 066 6.71 m in 010 M Oil U t 072 SSt O l i. 3 074 S14 OTS 1.3 t-Z 0% i i s o n Ik 6 078 i i S o n S.6 080 S. 9 08l k it m- )$9 *4 - 4 WUIIU^iyili WUIWI1* ui/unit uiruxr ooiorrnit ttusf>ar iizardiri ministri mica. - <jflr* NU -------- =j <11 2-5 1-2 30-50 2-3 0.5 rate errmonre- opa<t -cfnoliit partalis 4 3 - k7L 9k-Id /-2 < a z ti 02 97-98 <0$ftfkik -/ / <1M 5 f7 </ 1.5 97 i S 90- 9Z (p.Synpkte. 2-3 M 2-3 Al 0.5 9k-98 a7 95-97 QShlMtitL *9017 *10 Ai 5- 3 -5 2-3 /-2totltc S k 72-80 5/#A#0 ttmttititi hZ hl < !U ~S 56 -5 0 10-20 V S-6 5-/0 *1 M 24mandi/* 6 At 1-Z /-3 S-O *1 1-4 bifltik t-2 04 1-7 23 1Z 70-62 40Otf i n ) 'ItUjM'ft 27-35 S ltf ib n ) tsmtjmiti. 41 -56 54-70 (fi ft Mjhitiii t ckuf s - ic 2.4 85-95 - 5 !-Z 5 *1 2.2 7-76 2-3 <1 1-2 is-zo <1 2.5 5-80 iz /2 o-tz - . *5 2.S 70-85 4 78-83 3.7 75-80 10 i CONTIHUtlD 3.1 75-87 r^ wO APPENDIX A Page 39 QE-CPC00004014 AHPtiWlX A Page 40 APPENDIX B Appendix B consists of 13 x -ra y line scans of known m in erals, as listed below. Figure B -l Figure B-2 Figure B-3 Figure B-4 Figure B-5 F ig u ri e B-6 Figure B-7 Figure B-3 Figure B-9 Figure B-10 Figure B -ll Figure B-12 Figui-e B-13 X -ray line scan of V erm ont talc, full scale = 2000 counts/second X -ray line scan of Vermont talc, full scale = 500 counts/second X -ra y line scan of anthophyllite, C a s h ie rs , NC X -ra y line scan of anthophyllite, Guffey, CO X -ray line scan of anthophyllite, Haddam, CT X -ray line scan of chrysotile, V ictory Mine, Globe, G ila County, AZ X -ray line scan of lizardite, Kennack Cove, Cornwall, England X -ray line scan of a -q u artz, synthetic X -ra y line scan of fibrous tre m o lite , Dahl C reek , AK X -ra y line scan of tre m o lite , F o w ler, NY X -ra y line scan of actin o lite, Lake W enatchee, WA X -ra y line scan of c h lo rite , C alav eras County, CA X -ray line scan of p ro ch lo rite, C h ester, VT 41 QE-CPC00004016 * iO QE-CPC00004017 Figure 0-1. X -ray line scan of Vermont talc, full scale 2000 counls/secoml Reproduced from best available copy i/s*?cond I { h QE-CPC00004018 QE-CPC00004019 Filtro H X - r a y Hm* '''a n of V e r m o n t talc , full s c a l e 500 counts, se c o n d R e p r o d u c e d .` rom best available opy, fccr-i: QE-CPC00004020 QE-CPC00004021 Kl/jm * H - l . X - r n lin** sonn nf inthoph llUo, C a s h t o r s , NC Reproduced from best available copy. QE-CPC00004022 3 i 1 QE-CPC00004023 r vm Reproduced rom best available copy. o o QE-CPCOOOi QE-CPC00004025 F ig u re R -5 . X - r a y lino son n of anthophyllito, Hndriam C T i QE-CPC00004026 re Of- .ow i QE-CPC00004027 QE-CPC00004028 Reproduced from _ ^sf available copy. o Filfaro U - 7 . X - r a y lino s c a n of li/.',- ilo. Xonnaok Covo, C o rn w a ll, Knulaml QE-CPC00004029 > QE-CPC00004030 Reproduced from best available copy. ^r rJ QE-CPC00004031 W Reproduced from uesl available copy. C7 QE-CPC00004032  F i n i r n~f>. X - r a y line i?i*nn of fihrms tre m o lilo , Dahl ( ' r o c k A K QE-CPC00004033 TC t QE-CPC00004034 )ahl Creek, A K Reproduced from best available copy. 1 QE-CPC00004035 AN Mii|Oiu.>o JO ut.i s .>UI] i' u j - x - ,, I - H .lirici co rom ? copy. QE-CPC00004036 rvv.V I QE-CPC00004037 i QE-CPC00004038 <U e c X CT < QE-CPC00004039 QE-CPCOi C: ooo w7 o j Reproduced from I best avaifable copy, y F m ir c l-l.'i, X - r a y lino s r r m of [iiochlnritc;, C h e s t e r , VT QE-CPC00004041 QE-CPC00004042 *v * J | Reproduced from | best available copy CO . JkJ. QE-CPC00004043 i ! t m "oO oooo o iu . QE-CPC00004045 Reproduced National Technical Information Service Springfield, VA 22161 This report was printed sp e cifica lly for your order from nearly 3 m illion titles available in our collection. For economy and efficiency, NTIS does not maintain stock of its vast collection of technical reports. Rather, most documents are custom reproduced for each order. 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