Document 93B3LOJ7O5grJxEqgYLDyoVyq

v- 1' . *%.. * <CS c x u ' x x t -iAra m v a n / uvao r* w a lte r a m " o n e a s s o c ia te s , In c . ( 4U10iJa224tJ ; 1 U / i 1 CONSULTINQ; ULTRAMICROANALYSW MICROSCOPY - SMALL PARTICLE PROBLEMS 8OU0-STATE CHEMISTRY 22 D ecem ber 1975 M r. M artin A bell . Room 206 ' 1014 Broadw ay C in cin n ati, Ohio 45202 . " D ear M arty: E n clo sed a re tw o copies o f o u r f i r s t sam ple d ata rep o rt.- Six m o re a re nearly finished, but cannot b e m ailed u n til a fte r the fir s t of the y e a r. I w ill re tu rn to th e office on January 5 . ~ W ith b e st w ishes, & .h S incerely. _ LBM ife e n c lo s u re re ft 4800 , Buoy B . M oCrone \. / \ S en io r R e se a rc h S c ie n tist ^ / / C O O x liW ^ M . C u v /e & i / - i e(a^ \ n e \ C sJiJi'C L a^ L ~r4r t d lu 'U 'i o iftA t / ^ 3 ) 'f/jo*.'/ f k e~ Y ^ /* / * I ,w '' '. ./ 2020 s o u t h Mic h ig a n a v e n u e Ch ic a g o ; Il l in o is easts 3 i2 /M 2 -7 to o - c a b le : c h e m ic r o n e PLAINTIFFS EXHIBIT CAM-231 CAMC-Logiudice-002699 AU A l * ? r *<<fnu V I11VWI1 r ntJU ' IU U U A IU f * J.X/ CAMC-Logiudice-002700 xu x i a i i uitm i '* a n ti/oii / i ifoo^ NIOSH C o n tract N o. 210-75-0003 Sam ple D ata R ep o rt, Sam ple 83755 <001) iU`ic ia^o;ffi2/2i P a rtic le s iz e d istrib u tio n . T he p a rtic le siz e Retribution wan determ ined by lig h t m icro sco p y w ith a m anual count baaed on M a rtin 's d ia m e te r. R esults a re p lo tted In F ig u re 1. Since the av erag e p a rtic le siz e is 2 .97 pm grinding the sam ple is unnecessary fo r x -ra y diffraction. D ata sum m ary. The f ir s t te n m in e ra ls follow ing ta lc in the d ata sum m ary a re th o se specified fo r an aly sis in C ontract N o. 210-75-0063. (T hese w ill be tab u lated in th a t o rd e r In a ll subsequent Sam ple D ata R ep o rts). Since no ' c h ry so tile o r c h lo rite could b e fo o n ^ m lcroB croplcally^0 explain th e peak a t 12.1 < on fiie x -ra y lin e sc a n w e exam ined th e sam ple fo r th e tw o se rp e n tin e s, antlgorite and lisard ite. T a lc . The w eight p e rc e n t o f ta lc w as calcu lated by d ifferen ce to b e betw een 30 and 45%. Som e fib ro u s ta le i s p re s e n t a s ro lle d up s h e e ts . In C axgille high A sp e rsio n liq u id 1 .5 5 0 th ey show ta lc c o lo rs by d isp e rsio n sta in in g w ith h 0 H430 c to 440 run andx. j / 610-620 urn. 0t ... A nthopbyllite. A n aly sis f o r afo o p h y llite i s som ew hat h a m p ered b ecau se we have .*. n o t y e t found a com pletely sa tisfa c to ry sta n d a rd to u s e in p re p a rin g calib ratio n V '4 cu rv es fo r x -ra y t& ffractian an d A sp e rsio n stain in g . In g e n e ra l, th e dispersion stain in g c o lo rs o f anthophyH ites a r e c lo se to th o se o f tre m o lite a an d th e two a re A stfnguiB hable only by th e extinction p o sitio n s of th e a - y view : trem o litea show oblique extinction of fro m about 10 to about 21*, w hile anthophyllites show p a ra lle l extinction. W e found a v e ry few p a rtic le s in th e sam p le w hich ap p eared to have p a ra lle l extinction on th e a view b u t com plete confidence is lacking because th e re w ere too few p a rtic le s to b e s u re . T he th re e p rin cip al x -ra y d iffractio n lin es fo r the ' ;**;> - 2 - wofter a m ccrone associates, Inc. y x. ' `v . v */ .*.fc***:V;*'U*%vi'i*".*.>;'V*.,t!'.*"''.s-! CAMC-Logiudice-002701 j.u xi x v i *xuAn v j . _ --------------------- m v tjii / i nour* `HJ`KK>aZ`*0iJFiJ/ 22 w _________ m o s t re lia b le anthophyllite p a tte rn in th e ASTM file (16*401) o c c u r a t 10.61** 27.69* an d 2 9 .1 6 * . A n other p a tte rn in the ASTM file (9-455) gives th e sam e lb xo. 70*, 27.50* and 29.26" . 1 3 UICC sta n d a rd sam p le co n tain s a p ro p o rtio n o f anthophylUte* confirm ed o p tically * a s w ell a s v ario u s im p u ritie s . A lin e sc a n o f th e a pp ro p ria te reg io n s gives th e th re e anthophyllite lin e s a t 1 0 .8 5 * , 27.70* and 2 9 .4 5 * . Ignoring p o ssib le in stru m e n ta l e rro rs of our own w e m u st assum e th a t peaks w ithin the ran g es 10 .6 1 "-10.85* * 27.50* -2 7 .7 0 " and 2 8 .1 8 * -2 9 .4 6 * . could b e due to anthophyllite. T rem o lite o v erlap s in th e reg io n s around 10.55* and p o ssib ly 2 7 .2 5 * . C alcita overlaps a t 29.40*. . Step sca n s o f th e se reg io n s a re given in F igure 2 . A nthophyllite peak cen ters bp ; m a rk e d in re d , tre m o lite In g re e n . W e narraot sa y th a t th e se a r e in fe e t anthophyllite peaks but th ey could be* especially sin ce a peak ap p ears In each :& r o f th e th re e re g io n s. W ithout c a lib ra tio n cu rv es w e only su g g e st th e quantity re p re se n te d b y t i e peaks a s le s s than 3%. The o p tical re s u lts su g g est a low er I i value. *. S erp en tin es.- The peak a t 12.1" in the lin e scan . F ig u re 5 , is n o t due to ehxysotile b u t to the nonfibrous serp en tin e, U zard ite. No eh ry so tile fib e rs w ere found by d isp ersio n stain in g in sam p les m ounted in C arg ille high d isp ersio n liquid 1.650* p a r tic le s show ing X0fs o f 540 and 610 am w e re id e n tifie d a s U zardite r a th e r tfr o n tig o rite , w hich show s 500 and 520 nan u n d e r th e sa m e conditions. H q u an tity o f U zard ite w as e stim a te d to b e 10-16% fro m th e x -ra y lin e scan . The d ispersion staining co lo rs fo r q u artz and U zardite a re different by only 10 to 40 urn in th e high d isp e rsio n C arg ille liq u id o f ch o ice, 1 .5 5 0 , thus they a r e **1* to rfgigHwgnish o p tic a lly , sin c e they have s im ila r m orphology. They can b e so distinguished b u t th e procedure Is slow . M.t* **' K* - 3 - waiter c. me crone associates, inc r:*T `A. . * . , s iw.K Lr' CAMC-Logiudice-002702 j- dMr . . .>ri"v:,,*' J.U-H- i , t i z a m rcioan / man-* cr\ 4U46382248?#14/22 The .tro n g e s tjt-ra y diffraction peak, a tie .M - . la relativ ely tre e of in te rfe re n c e s. Step ucanning, aiv ea.th e am tam t o f q u a rt* , about 2 * (eee g o re a ,. ' T rem oiltes - C A .V C U A ^o 7 * So m uch tre m o lite is p re se n t, 40-50% by w eight estim ated fro m flte x -ra y lin e sca n (F ig u re 5 ), th at ste p scanning w as u n n ecessary . Step- so sn sed tre m o lite peaks a t 10.55- and 27.26" a re show n, how ever, in F igure 1 . U sing A sp ersio n stain in g th e proportion of fib ro u s trem o lite w as estim ated a t 0% o f th e to ta l tre m o lite . B ecau se o f ti g r e e t d ifferen ces in w eight betw een th e m assiv e p a rtic le s and the fib e rs th e p ercen tag e could not b e derived from fib e r counts. I t w as obtained by estim ating a re a s occluded by fib er and by . m a ssiv e p a rti le s , th en converting to volum e (w eight) p e rc en t by dividing th e percent fib ers by four. , `F to ten exam ined a t 200X the averaged p e rc e n t o f the tre m o lite p re se n t a s fib e rs b y a r e a w as 13.6% , w h lch w o u ld b e ab out 3% b y volum e. - i n a r a k . A few p a rtic le s of calotte w ere id en tified optically by th e ir flffptnrfrm S taining co lo re and re fra c tiv e index re la tiv e to th e m ounting m ed ia In C arg llle liquids 1 .6 0 5 , 1.650 and 1.670. T he p rin cip al calcita x -ra y peak a t 29.40" is b u rie d in th e presum ed anthophytlite peak (lig a re 2). N ot enough Wa s o b serv ed o p tic a lly to; account alo n e f o r th is p eak. A few par*'**" o f d o lo m ite b u t no m a g n esite w e re d e tec te d in C a rg llle liq u id 1.670 by d isp ersio n stain in g . X -ray lln - T he to tal sam ple is rep re se n te d by F igure 5, the x -ra y line sca n fro m 2 0 of 5" to 7 0 ". C onditions w e re : C u rad iatio n w ith Ni filte r , a t 42 kV 25 m- S cale fa c to r w as 1000, tim e c o n stan t w as 2 , m u ltip lie r 2 , p ~t. sp eed 1" p e r m in u te , c h a rt sp eed 1 /2 in c h p e r m in u te, s lits 1 " , 0.0 2 4 " , 1* . L . . . w aiter c. m =crone associates, inc. V :*J.**,'/ .S** CAMC-Logiudice-002703 v> I%.5 ;*'C xu~ii- x 7 /'cum i m v o n / m ao- 4 u a a z a 4 o ;iP is/^ ii * (am p le was ro ta te d in an alum inum b o ld er wMoh co n tributes a larg e peak a t 38.5* and a s m a lle r one a t about 4 4 .5 * . A lignm ent of the goniom eter is cheeked d aily u sin g a q u a rts stan d ard . A slo w er scan of die reg io n betw een 0* mw< 12* w as a lso ru n fo r b e tte r re so lu tio n . T h is scan F ig u re 4 , w as m a d e a t th e sam e o p e ra tin g conditions e x ce p t th a t th e sc a n sp e e d w as 1/2* p e r m inute. . * R esp ectfu lly subm itted, Lucy B . M cC rone ~ R esearch S cientist LBM tfe refs 4800 1 . <*5 w aiter c m ccrone associates, inc. `%* **r\t . *. ! . ^ * <* CAMC-Logiudice-002704 '.v-'i ''b-b. b iV_ *"VW <st t t V*V*. * CAMC-Logiudice-002705 xu Xa X > * S' V**S" FICBBJE 2A. X-ray step scans at snthophyllite lines In the regions of 10O and 29 20. 1 CAMC-Logiudice-002706 7 * li. . i i.,.i i i- : :i : i ' r ' " \ i \ ` i P is 0*7ST. I ' . . . I S o strofi tbx/ . ..i: ; :[ ir . : ' . . J!#.. Instrumental conditions! 50 c o u n t /se c ., & second tim a i. . . am atane 10 20 o r 50 second i Mi com ics, 0.010 20 s te p s , l/8 ', /m in 'c h a r t speed, 0.024" s i l t . C 1 i lI 8-7fS2T -7**" C S e& ti& so iic e ttd ., yoVs*; ii i cJI ... Ii ctI c i CAMC-Logiudice-002707 1U - 1Y - 1 ; /JOZAM ! N I O S H / 1WSB-* . xxne or quartz \ o.oaw z w ) i. . i \ 4046392248;#19/2i Standard: 12 quartz in talc > v W Sample 83755 (001) ; 22 quartz, approximately Instrumental conditions; 500 counts/sec., 8 second time constant, 50 second counts, steps Of 0.01 29, 1/8" / min. chart speed, 0.024" slit. FICORK 3. : ( t CAMC-Logiudice-002708 ! ( 1: CAMC-Logiudice-002709 t-rji - . . ,.i ' i i-Z?! !' I t. . : , :I 1. , vvi i ; : j -- . * A: 1-j *4 > I li.! : V::: / `.Ti -ir~:--1" . . s . ! ,;*FT - r . ..I 4-.:-- r * p . <* (I t fM * ..... H ............. I " ! **! : : .... i . ` J ::: Z O F "' .... I_ . . r_ . . . -*....... :-4 ; : rz ::: o :/- T _ . . .... 4- i z i o , I j_: X-RAY DIFFRACTION DATA. . f Sambia No? .1 Material; ......... ' Project No.' I I A /c Radiation S rf5*.-.sai.-Pw ifer - .v. IM M M 1~.i~; . Scale Factor ,,/.O ff ^ [ Multiplier,l..J..Z ~....L ...Z nr i. Constant &{ ScarvSpeed lf/.IHhh...,. Ch irt Speed &k>/`j*rJh Slit U S ^ A u i ' l z i l ....... i - : r ~ r Remarks M IH M Ik N a iM M II i *** **** ' i Date, '././tiy^r.ZST Operato^ *9*9/n*yjitn'9>9/iiv\nr