EXHIBIT JNJ-447 J o D l o0 1 o0 1 1 J J ] J ]J JJ J J J J INVESTIGATION OF POSSIBLE ASBESTOS CONTAMINATIONS IN TALC SAMPLES SCANNING ELECTRON MICROSCOPE EXAMINATION Specimens of powdered talc were received from Johnson & Johnson Co. and from McCrone Associates. Analysis of these samples using the scanning electron microscope was requested in order to determine the possible content of fibrous crysotile asbestos contained in the talc samples. The first lot of material examined was labeled by McCroneAssociates Lewin. The samples were mounted on one half inch aluminum electron microscope stuBs stuDs with silverprint glue. The glue was first placed on the aluminum stub and the sample was then pressed to the surface of the wet silver print. used to remove excess talc from the surface. A jet of pure Freon was The specimens were then shadowed with a thin layer of carbon and gold providing a conductive path to the specimen stub. The stubs thus prepared were placed in the scanning electron microscope which was operated at 20 kilovolts electron beam energy and were examined at magnifications between 20 and 25,000 times. The initial effort was directed toward detection of the presence of fibrous morphologies in the basically sheet structured talc bodies. To this end acysotile ~otile asbestos specimens were prepared as outlined above and observed in the S.E.M. as illustrated in Figure 1. l. To be noted, of course, is the highly fibrous structure as opposed to the layered structure of the talc bodies. The asbestos fiber can be seen to shred both at the ends and on occasion at the center of a fiber bundle giving an appearance not unlike rope but on a much magnified scale. Having established the general appearance of asbestos) suitable samples were selected for examination in a scanning electron microscope. A magnification of 1,000 times seems quite adequate to pick up any appreciable fibrous morphology present within the talc sample. In order to make the survey as quantitative as possible, a grid of pictures was mapped on the surface consisting of five pictures on each side of JOJO-MA2546-01283 2 l l l l oD a square covering thus 25 squares at 1,000 times magnification. structures were observed during this examination of both the original Lewin material and the Shower to Shower material supplied by Johnson & Johnson. micrographs are shown in the following figures. Examples of these Figure 2 shows one such fibrous material which is in fact split on the end and is generally within the limits of possilile diameter of an asbestos fiber. The general character of the split at the end, however, rather than being shredded, gives a somewhat more solid appearance indicative of an organic fiber such as wood. Figure 3 shows an area at the center which may possibly indicate an asbestos structure. however, exist. oD Numerous fibrous Slight differences in character, Although the rough appearance of this body is shredded, careful examination indicates that it is more than likely an edge on view of a talc structure. Figure 4 shows another such structure. In addition, however, at the center of the micrograph indicated by the arrow, is a small broken fiber which is too small to ]l identify for certain as either talc or asbestos. Figures 5 and 6. _j l] J short length. Other such examples are seen in These may probably be discounted on the basis of their very One such fiber which is sufficiently long to be suspect is seen in Figure 7, taken at 500 times magnification. Figure 8 and 9 show higher magnification 10,000 times respectively. These are, however, seldom encountered. pictures of such fibers taken at 5,000 and These cannot be entirely discounted although the net vobme involved, even if they are asbestos fibers, is extremely small. Figure 11 shows an example in the lower right hand corner of a fiber which is almost ] certainly wood. Asbestos cannot possible take such a small radius of curvature with- out being entirely shredded. gation gat ion is shown in Figure 12. most curious end structure. One rather curious fiber found during this investiIt is roughly the proper size and length but shows a This is more than likely a talc body which has encoun- tered an on endcollision end collision and become shredded during its processing. microstructure No evidence of indicative of asbestos was found. JOJO-MA2546-01284 3 l l l CHEMICAL EXAMINATION OF FIBERS Considering that little could be categorically determined to be asbestos in the material based solely upon morphology, efforts were made to use microchemical analyses of such fibers in the scanning electron microscope. the use of a non-dispersive X-ray detector, which analyzes the X-rays energy resulting from electron beam impingment. suIting Areas as small as a 1,000 Angstrom fiber can be analyzed under suitable conditions. l These efforts involve Figure 15 and 16 show traces of an oscilloscope picture in which the energy of X-rays is displayed along the horizontal scale and the number of X-rays arriving at the counting detector is displayed J] on the vertical scale. In Figure 15 an asbestos fiber was used as an object for X-ray analysis by reducing the electron scan image to a line which was aligned along the asbestos fiber. 1 The asbestos fiber was imbedded in the talc matrix and was in fact part of the doped specimen. trace. A number of elements can be identified from this The ones which are certain to be part of the specimen itself rather than artifacts of the instrument aremagnesium and silicon. J] J] J J] J] J] J] 'I 'l This pattern was used as a standard and compared to other counts taken from suspect fibers in other fields of view. dard. Efforts were made to maintain the geometry the same as that in the stan- An example of such an effort is seen in Figure 16. No strong similarities could, however, be shown in any fiber sample. TRANSMISSION ELECTRON MICROSCOPY Considering the lack of success in obtaining definitive results by scanning electron microscopy transmiss transmission ion e lec lee tron microscopy was tried. Specimens were mounted by standard techniques of swirl dispersion on electron microscope grids covered with a formvar film. A large number of grids were examined and numerous examples of fibrous material were seen. Of the large number of grids examined, three ex- amples offibers of fibers which upon examination by electron diffraction could be classified as likely candidates for crysotile crysoti1e asbestos in the shower to shower material and one example was found in the Lewin material. These are shown in Figure 16, 17, 18 JOJO-MA2546-01285 4 D JJ and 19. In Figures 17a and 18a, electron micrographs of the transmission type show the typical stranded appearance of crysotile crysoti1e asbestos. through 19, the diffraction pattern is closely similar to that indexed for crysotile crysoti1e asbestos. l '--• In each case, Figures 16 Figure 18a is a double exposure of the diffraction pattern and the bright field micrograph. In order to avoid confusion as to the area used in diffraction, the bright spot at the center of the micrograph is a delineation of the area used in diffraction. o0 J] o D l ] ~ The diffraction pattern, however, is rotated by roughly 40° from the axis of the specimen. It is felt therefore that crysotile crysoti1e asbestos does exist in the specimens of shower to shower and Lewin supplied to this laboratory. It is, however, further concluded that, on the basis of samples supplied to us, transmission electron microscopy can only find a total material by volume of less than 1/100 of 1 percent crysotile crysoti1e asbestos in the shower to shower material and less in the Lewin material. CONCLUSIONS The extensive investigation reported here must conclude that the scanning electron microscope by itself is unable to make distinctions between asbestos fibers within samples of talc and other such fibers of wood, wool, and talc fibers. Only the shredded appearance (not found in any specimen examined other than that purposely doped with asbestos) is the sole basis for assuming the existence of asbestos in the specimens. J Efforts to use non-dispersive X-ray detection yielded a negative result, and could not be used as well. Transmission electron microscopy shows less than 1/100th 1/lOOth of 1 percent asbestos in the material given to us. JJ Neither scanning microscopy alone or in conjunction with microchemical analysis can be reasonably expected to prove the existence of crysotile asbestos in talc. l J - J JOJO-MA2546-01286 Wmm- - i FEE RX 12:" Jami mart EE- 3 C?umf I I f- X-RAY XRAY DIFFRACTION PATTERN SAMPLE NO. 137. .. , .. , .I ---i-, , , .. -.. oo 110 oo 'oo I -f .. ' 1- ..... .., oo ,. .. 1,.. - · ~1- Be Below: low: I 110 0 -.. - I TALC 89% 89%;; CHLORITE 4% 4%;; CHRYSOTILE 2% oo ----. ,. .... ! - ~ iO '" !• -... I I - -... I I II )(y l(y .. . .. 13 ~- j ... "-1-' - Analytical Results: 7/ 71'.. h/' :J76~ j707 ,. I II , ~ --...t , 1 I a-QUARTZ aQUARTZ 3%; 1- I DOLOMITE 2%; PHOTOMICROGRAPHS OF DRY POWDER NO. 137 JOJO-MA2546-00138 . •,. ~ 0 $! "" 0 '. . ~, ~ <, ~ ~ ~ ~ ~ :;:; '> c 6<> v ~ -;:s9 .. <.::CJ • ', c ~ •·o '", ~ ~ d '" ,~ 'Q e j. 4· --- • . Q IJ . • .. .. - -./1:\ ~ 0 ~' 0 t:l ']f t:J ...' "'I ~ > ~ ;. ....,_, <::> .. ~DRY POWDER, SAMPLE ~ 0 ~~ c; . 0- • c 0 ~ ~ "'" - 0 T . 0 1 MM • J, """ ~d SOTILE OTlLE ~ ~~ ..... • () OF ALTERI NG SOTILE ...... • SAMPLE NO . 137 IN IMMERS ION LIQUID OF n = 1. 580 ~----~~ ~~;-;:O~TlLE FIBERS OBJECTIVE DOWN FROM BEST FOCUS UP JOJO-MA2546-00139 FROM BEST FOCUS • SAMPLE NO . 137 IN IMMERSION LIQ LIQUID UID OF n = 1.580 DDED ~~~~~t"~)~DDED PARTICLE =1 -=i 1 MM. -_ 0 .o.1 t IN ~~:'.' Jtl;.L}\'L OBJECTIVE DOWN FROM FRO M BEST FOCUS TALCS OBJECTIVE UP JOJO-MA2546-00140 FROM BEST FOCUS X- RAY DI FFRACTION PATTERN DIFFRACTION SAMPLE NO . 136. eo '0 eo .0 eo (r I ." 00 •o '0 .0 eo eo , 70 eo " ' e~, ~~- ,. 70 eo 00 eo 00 eo 50 .0 ~0 .0 .0 •o 30 50 .0 30 ....:1 _ ~ \\ eo 00 eo .. .0 ... I j. _L I I " n. 30 ~ - I .10 1 J 87%j CHLORITE 4% TALC 87%; 4%;j PHLOGOPITE 3% 3%;j aa-QUARTZ - QUARTZ 2% 2%;j DOLOMITE 2% 2%;j CHRYSOTILE 2% ytical Results: Anal yt ical Resu lts: PHOTOMI PHOTOMICROGRAPHS CROGRAPHS OF DRY POWDER NO . 136 ' f:, .. •• 'i . ~ .c:: ..- ~ • "'"i ~ .. • .. "". of ~ -j 1 b t < ~o ~,,~ • ..... _ . ___ • ,. p C> > ,~ "'" ~ ; ~. 0 . 1 mm mm.• -. • ~I>~ V • 4i; ..:> ~ -:P . ~~ ~ ~ .£ ,,~ ~ JOJO-MA2546-00141 .. . ..s.;.· .. . .- - POWDER, SAMPLE NO . 136, 136 .- Pg ~~ ~ ~ G ~ ~ .' G? ' j ·. 0 \ ~ . ~ l .. ~ ~~ t- ... a· .... . 3 -:-- a. .. u a ~t/511I>tftIJ!f- ~, •. 0" .n :if -'k ~ -4 ., ~s ... = fi t) ~ ;:) '• ~ f ~ ~ () '.~ -~~ • ., ' Q tJt ~ . \\>t::c tr ' ~ (} ~ ~~ ~ pf ' ... ~ C9 J)t 1)0 ~~ . 1:I, G ·~ .;> 0 1 . 580 IN I MMERSION LIQUID OF n = 1. OBJECTIVE DOWN FROM BEST FOCUS • BEST FOCUS OBJECTIVE UP FROM BEST FOCUS JOJO-MA2546-00142 DO~ FROM BEST FOCUS BEST FOCUS UP FROM BEST FOCUS CHRYSOTILE CHRYSOTlLE FIBERS FI BERS W WITHIN ITHIN TALC PARTICLES , ORGANIC ORGANI C FIBER JOJO-MA2546-00143 _ _ _l-dycms ~~:: -... 1h ,... "'?It. ~... " . ~cfJl.~~ ~,. , . .(~..-:; , 'I ~ , .. a:.~ .. · ~ ~ ",~., ~t:"/ .........:-....) .': . ". 'j~' ~., '~~CP- ~~ ~ "" ,~,~, ~ · 0'· . ~ " '. -. .. • · ... .~ · .~ • (. ',. i "'~ ~ 0.4 .. ~)J,." o..R..• ~~ ~~. \.' "~ .....~~ ," " d "" '. .' £! Q , ..... ': ~~V~:,lJ.. 'p.. -;. ...., . 0 ' ,J •. - ,;I ~:'W 'J ;, q" .. -. : .1 .. .' .Do .~<::". ' . t· ~ '... " ~' v~~·~ . . ~ \~;."" ~.'; ~.~ .... c... '~"~ .... '~.,,~.~--y\. ~e~" ...,:, · ,\..:.Iv iP.• . •~•''''. ~ . a51n:' ~ .' "'0' b • -_,t'. ••.. ' • • • ' Z"'.-J,. ~~. ~. ~dt._ W', • U' , 'f:>ri _ • ~ »·rJ..-'4 , I -:~t.::~~7~\~.':ld~·.'O;.~~:'."':~.)'~.; :pI ' /'/ ..~.~·~~.~6,\~. " '.- ' . / ) ' . - · .:•. .' "-:,.,, .~, .~. ,9. .\' . . ~~, .~ :i·'i'.' ' • ~ '~t\.i ':;'" Y: 'I. • ~', ~ . '~'".~;,,~ '11' .. ~ ." .• ~'Q'. '~~-;~ '- ''''.. '. ,''''' . .. tJ·I'~'. ~ .c:P:'lA . ..~,p,~.:. ~-"L.~,~ ',:~~iJt~~ ,•"/'1·~.:~~~ = (;o~' ~~~Jj. -. .!~ ~~I~ ..~.. .....' ~ ,.~ 1 . ~~,':!~ i.:J !,. ,. .;.~ .. ' ~ ...,,' " ~ <. ":b~" ~~~~..~~. '~! .11. !'" o . " ·~ltll··-·", ; • '\~. '~'''' ,. '. p..,' .. 'J:' to .:'.~. o.5J'~: il\,~, ...., ~.;;."Zl(!.,\. .. .,. :'b~'''''u..~. ~ '- ~'."'" l":' t 0 40 , G v. a-.;. ~ '" . ~ .:,",~ .. .... .: rl-;) - \I "., ,0 ~· , '. •. " :.' \. " '_ ~ •• .~ • ••• , ~ .-"';...c2. - 0 4 .:. • " . '"<''' ~ •.c:.. ,.,' :'.. '" J ~ '., D ' ~ ~ t'" • .' U l J . • ~. .. ~A.~,p.,~ '• . :"-""-I .Vj.<;,Q)" , ,0.,...... .: • • ", .J~ ~.~ ~ i· • .• ... t'lW Cl', '1-.". ~~ 'to: 1>. .~ . " 'tA' . ~~'l', It_·.~, P 0 .'. • ., . ! . '..... 6 . U'. " ..:.". .~?!.. ~ .. ~.~. . " . ~ . ~.r." '-~'. ~ ()~ • Ii- . ' v"(> .••••• ,C7.-.,'j ~ (I0 .,. • _ ..... ' ~... .\ "'. D.. .lih.. . ~.,.. ", • 0fJ Plate 5 Talc Ore, Heavy Fraction; x 100; n = 1.503 This photo shows the general character of the typical heavy mineral fraction. Small amounts .of talc are invisible in the background. Carbonate is the dominant mineral. Opaque grains are chromite, and actinolite is labelled Ac. Protected Document--Subject to Protective Order JNJNL61_000029427 • • Plate 6 Talc'Ore, Heavy Fraction; x 400; n = 1.503 This view shows mostly carbonate, some chromite (opaque) and an actinolite grain of typical morphology at the center. Protected Document--Subject to Protective Order JNJNL61_000029428 • .' • ! 'I I I I Plate 7 Talc Ore, Acid insoluble Heavy Fraction: x 100: n = 1.503 Actinolite, talc, chromite, and a large anthophyllite fiber. Note that much of the talc is of poor morphology and/or is inclusion-filled. Protected Document--Subject to Protective Order JNJNL61_000029429 • " • • Plate 8 Talc Ore, Acid Insoluble Heavy Fraction; x 400; n = 1.503 Inclusion-filled talc, actinolite and anthophyllite. Protected Document--Subject to Protective Order JNJNL61_000029430 • • v " .. ·~r . .. ' ,:. ' Plate 9 Talc Ore, Acid Insoluble Heavy Fraction; x 400; n = 1.503 Platy talc and actinolite. Note that the small equant grains of actinolite could be easily mistaken for carbonate. Protected Document--Subject to Protective Order JNJNL61_000029431 • • . ' . ' ..... l~ ... r' ~. _e • .• Plate 10 Talc Ore, Acid Insoluble Heavy Fraction: x 400: n = 1.503 Inclusion-filled talc with partial fibrous morphology, platy talc, and characteristic grains of actinolite. Protected Document--Subject to Protective Order JNJNL61_000029432 , ' • • " Plate 11 Talc Product, Bulk: x 100: n = 1.503 Platy talc with a few carbonate grains (high relief). Protected Document--Subject to Protective Order JNJNL61_000029433 • • Plate 12 Talc Product, Bulk; x 400; n = 1.503 Typical platy talc of good morpho1ogyo Protected Document--Subject to Protective Order JNJNL61_000029434 • • Plate 13 Talc Product, Bulk; x 400; n Platy talc and carbonate. Protected Document--Subject to Protective Order = 1.503 JNJNL61_000029435 • • "j , '. ., ... .' /' .".. .' : . -:<~ . .. 'j ~. Plate 14 Talc Product, Bulk; x 400; n = 1.503 Platy talc and one actinolite grain. Protected Document--Subject to Protective Order JNJNL61_000029436 • • Plate 15 Talc Product, Heavy Fraction; x 400; n = 1.503 Typical field showing carbonate, talc, actinolite, and chromite. Protected Document--Subject to Protective Order JNJNL61_000029437 • • .. ~ ':"' "''t ••.: •••• •• ..i ,. ". 'u' To'.' - .1(", • • -~ -..L'''.,' . w;., ," -. .... ':.... .• "0 •• . . . ., ,,/,.''t. "" ::••• , .".-.,_. .,:-*. 1'~i>..·'''' ." '~,. '1.<' • • '. ~- ~ _. r.:" . (! __, ' " ~'.b-. ~'. . . ' ·I"'l"."•. ,,.·'l~ :...•. -r. ~ .•• ~ . .' :.~. ~"" r.~.: '. •~ »'~.~ "":".' •.• J••.• ~ t"P ...... ' .~.~ .~ ',. - ., -t~.,. . . -. ..,' <~:t .~- e,' ':~t>"" • - • • ~: .'.~ '. • • • ,." , • "''i01. " . .'.. ".'t·. ' ". ... ..: . '. -'t'.. '., "~"".:"" • • ~ • .' • " \ \ •••.• I '.. .. . . •• ", ,. : Q. •• ~. ~ •• t!. ·~.··~..;.~<~!~f.;.:,'·-.,,~~::s. ,:-·:,.·.:·;::~~···t·~,L;i.~~':t:"~:" ~~~i.:·"-C:~·"~l"';~"~\'···"· \",~, ':"~';.''Ii •.•.;~ •!... '. .,.,. ..:t: •. • ' l.'.· .".... ""!' • ",... .;_ . • ." ~. ~:.. ...~.., I: .. r ' •. . , . • . .. ,,':" . . i .. ~.;. - . ..•• . . '.'''.. ' .~:' e':" ~ ':~'. ~i !;J~.. ••.. ~ .. :\ "~'.~"".' ""~ •. "~"''''.'''''''': '.' ;,f/'Q., ..... ' •• ~. -, .•. ~ .•_-.. ~ .. ;,~r-j.,'~·.~.~ . . r'''.~''''''i: . . .':l: .·•.f· .... r- C .. _'~:o:'!'o'.~" .,.'. ••.. ~"'·<:r, .-.k.--.···· ," .'e·~·_, e • • :n . ,e ' ~.\\.j, ':-'. ~jiJ.., " "L._ ~'• •. ..~,. ~~, -~." .,,.,. . ~. '.'- ",-", ". .,:~.l~., f:"l4t ~. ',& • ,. ~ .J ~ . . ~ . . • • . ,."'-.. ....., '.•. ·t·~_ .. \·~ ' . - / . . J• ''':.-a:" (. ~ ••-=.~'" .~. . .a..·~· .. ' ·A-a··· 'st' : ';:-""',':-. . Jlor. -~i·~~~.~~ ~ ,,~~,~'" f·. ,., ..-.. • • . . . • . .. 47' - ~-. \ ."~~ '~""."~"-.~<.~~: ....: .'., •........ 'i'.• :;~~1:~ .." .- ~., .......:~.'~ .~~~ ·UJ, .. ' .• ~ ".~ ~ ~.•• :""tV':?: ,~~' . . ~< ~.I '! ~~\ ••.. ~.~ ~ ...: . •:~;'.~.,!.~ !.~~~~::.~ .. ~.,~/.. ; ~_" .' :L~··. _,.< :~.'-";~~G~ 7':•. ..J.:...:_ ' •• ' . ' :--;..... -., , ~ 10:-' ; .:.... ~ .. !'~ r ~ ·0 • • -:-:. . •••.;··~'·~'· P;' ,.- ~,.!1 ",", -' "'.:; ''- , i 1 ~.' .~. \ t . ." t' . , ' ":- ~:.. IT' if . :., .. -". .4' . ".0 • • .. ._.;;,t.~~.~:':~.l».•, '.. . ,~ " ~~.~ ')"'f."" ..:'. , - ••.••. r.., .....-.: ~ ' ... . '- . , .. o . . • ~ '.l/:. •.. ~ . ..... ;..• ' '; ....." •1 .'"">' •. ,_. '~'.1Il'~ ·t.,,· ~•.. - ""1:' ""~'.' • ..r-;· .. · ~ ' . A'. ",,' '•• ~.i .....i-'\~ t ... :-.i/l.....:...: . ,.~.: - .r;.. .~ ~ ••~.. ,.1t ~.~.:~ ~ ~ .~. r .;' ·.-t.'. :, .,':.' ,.,.. ~;t~:'~~ .. " . ~ ~~ " <,.)" -:,. •.. ....' J .. '. '. -. . ~"I·'-~·~ '.-.-. ~ K .'. .... ', . • •- ";..1' •J • . -.... .~ ...,. i . . ,.,1 .. •\. . . ~..., ~ ~'--.~ • . 1~ y ,~~ --- J'.,.. .. .. r .. - J I * . • .. fl•• ' I'.:.. ,_.'. • . *' .~:'" V... . ,; . ~~.,_." .•.. ~ • •- , . '-...... r. ....... a ,~~", .• _ '. ~. !"" •• ,-'. .' ;p ; .• •.• . _... ".'~ . •. , ./ .••. -, ' ,~ ~'!t.~;. "..L.., ...~~ :'···f·~· ~~'.I . "'.If. ~. .. . . f' 'I.'"':..1 •. ." . . .;" .. ~ \ •• .• ' •.-;'.... . ,'" ~-./ . . '.';" .I~r .. _ .. " . . . . • ,_"~~."".' . . : ... ' •• .,..•• c:!' " ~ Plate 16 Talc Product, Acid Insoluble Heavy Fraction; x 100; n = 1.571 Talc is invisible cecause of high index oil used. Visible grains consist of chrornite '(opaque) and actinolite. Note the large variation in .aspect ratio of the actinolite. Protected Document••Subject to Protective Order JNJNL61_000029438 • • . ' Plate 17 Talc Product, Acid Insoluble Heavy Fraction; x 400; n = 1.571 Chromite and actinolite of varying morphology. The cha~acteristic striations are clearly visible in the actinolite grains. Protected Document--Subject to Protective Order JNJNL61_000029439 co' • • • •• • I ~. I Plate 18 Talc Product, Acid. Insoluble Heavy Fraction; x 400; n = 1.571 Large actinolite grain with irregular shape. Protected Document--Subject to Protective Order JNJNL61_000029440 • • 4, • Plate 19 Talc Product, Acid Insoluble Heavy Fraction; x 400; n = 1.571 Typical actinolite, fibrous talc, chromite and epidote. Protected Document--Subject to Protective Order JNJNL61_000029441 .I • • • Plate 20 Talc Product, Acid Insoluble Heavy Fraction: = 1.503 Note the large compound grain (platy talc and actinolite) at bottom center. Other minerals are platy talc (very low relief) actinolite, and chromite. x 400; n Protected Document--Subject to Protective Order JNJNL61_000029442 •n • • I • • ... ---~. .. -- .... _.... - . - -_... . Plate 21 Talc Product, Acid Insoluble Heavy Fraction: = 1.503 Small talc fibers, platy talc, and inclusion-filled talc plus chromite and actinolite. It is the presence of grains such as the inclusion-filled talc that makes grain counting analysis difficult. x 400: n Protected Document--Subject to Protective Order JNJNL61_000029443 walter c. me crone associates, inc. CONSULTING: ULTRAMICAOANALYSIS· MICROSCOPY' SMALL PARTICLE PROBLEMS' SOLID-STATE CHEMISTRY 5 November 1975 Mr. Vernon Zeitz Windsor Minerals Company P. O. Box 680 Windsor, Vermont 05089 Dear Mr. Zeitz: This letter will supplement our report of 1 July 1975 on a series of talc ore samples which we have analyzed for you. Table 1 shows the actual fiber counts and the approximate equivalent concentration in parts per million of the amphibole particles which we found in these samples. Some of them seemed rather high. one had 10 and one had 9 amphiboles. Most of these come in bundles of 1. 2 or 3 fibers with anywhere from 2-5 amphiboles tn a bundle. The examination of the fines suspension seems to be much more sensitive to the presence of amphibole than looking at the sediments. In several occasions we found amphibole particles in the flnes which we did not find in the sediment. Since most of these amphibole particles are rather small they would stay suspended in our ultrasoneration procedures, whereas the larger, blocky, amphiboles or chunks of amphiboles generally are not fibrous and are obscured by the large talc particles which are in the sediment. I would suggest that when we analyze these we should concentrate primarily on examining the fine fraction of the ultrasoneration suspension. Thank you for consulting McCrone Associates and if there are any further questions concerning this report, please feel free to contact me. e. ~Griege Yours sincerely, ~~::~esearCh l/'~ P ysicist GRG:fe attach. ref: 4055 2B:?O SOUTH WC~IIG';'I; ,iVEtWE· ell'CAGO, ILLINOIS GOG1G" 312/8.12·7100 • CABLE: CHEMlcnON[ Plaintiff's Exhibit J&J 341 J&J-0123238 JNJNL61_000079334 Protected Document--Subject to Protective Order -r " -- - Table 1 ~ SEDIME.NT Sample Number D-HC D-GI F-HC H-WI I-WI P-GI Q-HC U-HC U-Gl V-WI V-HC V-GI W-HC W-GI X-HC Y-HC Y-GI Z-HC Z-GI AI-HC BI-HC BI-WI BI-GI CI-HC CI-GI DI-HC Dl-WI DI-GI E1-HC EI-WI E1-GI F1-HC F1-WI Fibers of Asbestos Date 7/22/74 7/15 9/13 9/16 9/23 10/28 11/4 - 12/2 - 12/2 12/9 12/9 12/9 12/16 12/16 12/26 12/30 12/30 1/6/75 1/6 - - - Number of Fibers 7/26/74 7/29 9/7 9/23 2 0 0 0 . 4 amph. 9/28 11/1 11/8 12/6 12/6 12/20 12/13 12/16 12/20 12/20 12/28 1/3/75 1/6/75 1/10/75 0 0 0 2 amph. 0 0 2 amph. 0 0 9 amph. 0.0 0.0 0.0 0.3 0.0 0.0 0.2 0.0 0.0 2.0 1/13 0 0.0 0 5 amph. 0 0 0.0 1/13 1/17 2/24 2/28 2/24 2/24 3/3 3/3 3/10 3/10 3/10 3/17 3/14 3/24 3/24 3/7 3/3 3/7 3/10 3/14 3/14 3/17 3/21 3/21 3/24 3/29 3/29 GI-HC GI-WI HI-HC HI-WI 3/31 3/31 4/4 4/4 4/7 4/11 4/7 4/11 D -WI 7/15 H -GI 9/16 3/17 Fines PPM PPM 0.2 0.0 0.0 0.0 0.4 0 0 0 0.0 0.0 0.0 0 0.0 0.0 0.0 0.0 0.0 0 0 0 0 4 amph. 0 0.4 0.0 1.5 0 0.0 0.0 0.0 0.0 0 0.0 0 0.0 0 0.0 2 amph. 1 amph. 0.2 0.1 0 0.0 0 0.0 0 0.0 8/2 0 0.0 9/23 0 0.0 0 6 amph. 0 0 1.5 0.0 0.0 0 0.0 2 amph. 0.2 0 0.0 0 0.0 10 amph. 2.0 1 amph. 0.1 1 antigoriteO. 1 0 0.0 1 amph. 0.1 0 0 0.0 0.0 Walter C. McCrone Associates, Inc. J&J-0123239 Protected Document--Subject to Protective Order JNJNL61_000079335 ~. - '"""-.... -~ ' . -~~~~ . . . ~ walter c. mccrone associates, inc. ~i CONSULTING: ULTAAMICROANAI..Y$1$ • MICROSCOPY • SMALL PARTlCLE PROBlEMS • SOLI[)..$TATE CHEMISTRY 02 November 1984 Mr. Roger Miller Wiixlsor Minerals :P .a. Box 680. Route 44 Windsor, Vermont 85089 Dear Mr. Hiller: We haw CXJDpleted Q.Jr -analyses for asbestos in the four air filter samples which )101 submitted. The analyses were performed by transmission electron microscopy in accordance with EPA method 600/2-77/178. Results of the analyses in terms of asbestos fibers per filter are as follows: Fibers*/filter ~ 2 8 9 2.1 X <6.6 X 1~ 6.0 x llr 6.6 x 11 * chrysotile lo3 ~oJ asbestos Fiber size information for each sample is given in the attached tables. Thank you for consulting McCrone Associates. If you have any questions please feel free to call me. Sincerely, Hark E. Paleni.k Senior Research Microscopist HEP:fe F.ncl. Ref: 4055 ~XHI81t 21120 SOUfH MICHIGAN AVENUE • CHICAGO, ILliNOIS -18 o 312/e-2•1100 o CABLE CHEIIIICRONE Plaintiff's Exhibit L-5BB Protected Document--subject to Protective order 1 of 1 ~~,\ J&J-0044521 JNJ 000063266 Pltf_JNJ_00006449 Plaintiffs' Exhibit J&J 342 mccrone environlllental services, inc, 200 OAKBROOK BUSINESS CENTER 5500 OAKBROOK PARKWAY NORCROSS. GA 30093 • 404·449·846 t 22 August 1985 t , Windso [ rUne ralf:), Inc. } , . :=., .' .' P.O. Rox 680 \'iindsor, Vermont 05089 Attention: Hr - .. --..-----.-.. /:;i\r;~:~--~. LaP ierre ,'~) S(fet y , p.ealth_...~~~~~~.-Director SUBJECT: Analysi8-of-S~ven Talc Samples for Asbest6s Mineral Content by Transmission Electron Microscopy McCrone Project NO. ME-1862 Re: Dear Mr. LaPierre: HcCrone Environnlental has completed received the from analyses your office Services, of on tIle Inc. seven 25 July, Norcross, of talc 1985. samples The Georgia, that samples we were labelled as follows: HHI 85-25 (l) l'U'1I 85-26 * (2 ) l'lN I 85-27 (3 ) 1'i~II 85-28 ( 4) 1'iNI 85-29 (5) WMI 85-30 (6 ) l'lMI 85-31 (7 ) .,. McCrone 'l'EH Lab Number 'l'he samples were prepared following our- usual technique for TEN sample bulk analysis. Small (about 10 mg.) representative portions of each sample were weighed and suspended in 10 mI. of nanopure water microliters) of and ultrasonicated the a SUbsidiary oJ suspended for samples 5 minutes. were placed Drops on (6.5 electron walter c. mccrone associates, inc. 2R<'0 SOUTH MICHIGAtl AVENUE • CHiCllGO. ILLINOIS 60016 • J 12·6~2·1700 J&J-0034630 Protected Document--Subject to Protective Order JNJMX68_000013019 ... ~ ... ~. mic [escepe gr ids and allowed to dry. were analyzed sample verified were at 20,OOOx analyzed. by selected The prepared sample grids magnification. The area presence electron of Ten grid asbestos diffraction squares per minerals was (SAED), energy dispersive X-ray analysis (EDX) and by morphology. Chrysotile asbestos was detected only in the samples labelled WMI 85-28 and WHI ·U5-30. Because only a few fibers were detected in the portion of each sample analyzed, no accurate value of the weight percent of chrysotile asbestos could be calculated with statistical certainty. each sample analysis suggest that the amount of chrysotile asbestos in the samples 0.0001 labelled WlH The 85-28 data and obtained ViM! 85-30 from is less than percent by weigbt. Thank yOll for consulting NcCrone Environmental Services, Inc. If you have any questions concerning these results, please contact our office. Sincerely, ~D~1 ~~~:1I Thomas J. Gore III aboratory Microscopist ~",,--",,-).~Q~ es R. Millette, Ph.D. a ager, Electron Optics Group TJG/JRM/arwp cc: 1) Windsor fline rals, Inc. Windsor VT Mr. Arthur J. LaPierre, Safety, Health and Training Director Windsor Minerals, Inc. Windsor V'r mccrone environmental selVices, inc. J&J-0034631 Protected Document--Subject to Protective Order JNJMX68_000013020 1~~~ mccrone environmental services, inc. ~ ~ rfA fA ~D 200 OAKBROOK BUSINESS CENTER 5500 OAKBROOK PARKWAY NORCROSS, GA 30093 • 404·449-8461 F\ECEIVFD M.4Y 2 29 April 1986 1986 W. M.l. Windsor Minerals, Inc. P. O. Box 688 Windsor, Vermont 95909 Mr. Roger N. Miller, President Attention: McCrone Project No. ME-2275 Re: Dear Mr. Miller: Under your Purchase Order WS-05B3 we received three (3) talc samples for WMI85-53, asbestos WMI8S-55, analysis. The samples were and WMI85-57. identified as Examinations by transmission electron microscopy resulted in the detection of trace amounts of chrysotile asbestos in the samples. The results are tabulated below. Amount Chrysotile Detected Nt. % Sample No. HMI8S-53 WMIBS-5S WMI8S-57 9.frHHl3 9.""15 9.9955 If there are any questions regarding these results, please do not hesitate to contact our office. Sincerely, ~ ~ Thomas Kremer Electron Microscopist ~........ R..~Q:LtG...es R. Millette, Ph.D. ager, Laboratory Services TR/JRM/mts cc: Windsor Minerals, 'l1 Windsor VT Inc. 1) Mr. Roger N. Miller, President a subsidiary of walter c. mccrone associates, inc. 2820 SOUTH MICHIGAN AVENUE· CHICAGO. ILUNOIS 60616 • 312-842-7100 Plaintiffs' Exhibit J&J 361 J&J-0004375 Protected Document--Subject to Protective Order JNJNL61_000078566 ~. ' L ",ii INTEROlfFICE COJ,mESPONDENCE LOS ANGELES TO SEE DISTRIBUTION DATE ATTENTION FROM March 25, 1992 L.A. FILE R. C. MUNRO YOUR FILE SUBJECT COPIES TO. I I CYPRUS ORE RESERVES - ARSENIC & TREMOLITE Excerpts from Cyprus Talc Reserve Report by. R. c; Munro Geology & Environment There are some important environmental issues related to the geology and mineralogy of the Cyprus talc depos_its, particularly in Vermont. Arsenic Arsenic iron sulphides (arsenopyrite) are, with their alteration products, present in many of the talc-carbonate schist ore zones in the Vermont area. Total arsenic, as . analyzed in the Ludlow Rainbow deposit, averages generally less than 100 ppm but with some .small zones in excess of 1000 ppm. No apparent major effort is underway to regularly monitor or completely .assess the total arsenic content of ores, tailing sofids and wastes although the distribution of sulphides and arsenates in the talc ore system .is generally understood. In near surface we-athering zones, crushed. rock, stock pile.s ~nd mine working areas., the arsenic sulphides (above) co.nvert in part to the more solub_le arsenates, . for example, the hydrous nickel arsenate, an11abergite (38% AS 20 5 ). Soluble -arsenic is measured in cores, ore samples, mill feed, product and tailings. Soluble arsenic content is monitored and governed under EPA/OSHA regulations. High (e.g.+ 6 ppm As) soluble arsenic contents of mill feed at the West .windsor mill contribute to reduced recoveries and milling rates. At West Windsor, part of the mill recovery problem at least .is being ascribed to a high fines content in the feed and to low. pH of the process water, both of which contribute to increased soluble As. The probJem has been Onder study at West Windsor since 1987 by Mill Manager, Jeff Scott, who indicated that if the arsenic content is above + 6 ppm soluble As and the talc content falls below 62% talc production rates and _recoveries can fall by 50%. The product specs are -3 ppm As or less at West -Windsor and current material in the silos is measured at 9. 73 ppm to 2.33 ppri, soluble As.. , Protected Document - Subject to Protective Order IMERYS 219720 1 of 3 Pltf_lMERYS_00057875 i --" . To me, there also seems to be- the overall risk of continuing conversion of As in sulphide to-more soluble arsenates:in some stockpiles, waste, and solid tailings as acid, wate_r, air _and time work on them. Trem.olite The other serious mineralogical contaminant in the talc ores of Vermont is the. fibrous variety of the amphibole minerals, tremolite and actinolite (hydrous calcium iron-magnesium. silicates) which have been classified. as- asbestiform minerals by OSHA-and-EPA-...OS.HA-was expected.to de-classify:non.:fibrous.(blocky) tremolite . on Febru~ry. 29, but has not as yet announced their decision. As a result, all tremolite, the fibrous varieties of.all ampbiboles and chrysotile , asbestos in talc. ores. are a s'c>urce of great concern. to all talc producers and especially to marketers o.f cosmetic products. . Cyprus claims that there are .no fibres in their cosmetic talc products and they work rigorously to ensure this. However~ a recent paper published by Rutgers University worker, Alice Blount, suggests the presence of fibre in several cosmetic talcs, some of which might have been from Cyprus West Windsor material, which is a source. of great concern to Cyprus manag.ement and potentially to their principal customer, Johnson~ John~on. Talc de. Luzenac personnel are well aware of the situation and Phillip.e Moreau is currently .quietly working to identify the reality and the magnitude _of_ the problem. . . Vermont 'talcs are derived from .altered serpentine - a natural host for asbestiform minerals. There. is certainly visible tremolite and actinolite in specific zones _of the Vermont deposits - fibrous tremolite was identified by the writer in exposures and cores at the East Argonaut and Black Bear. mines. Cyprus. staff report past tremolite from the Hammondsvile and Clifton deposi~s. . . Tremolite in thes.e deposits. is e.ncountered in the contact zones between the talc and the: surrounding schist; 'in "grey talcs" in. the vicinity of the contacts; and associated with the chlorite/amphibole waste zones Within the talc ores that are locally termed "cinders". Cyprus maintains a selective mining program in Vermont that is directed toward exclusion of all of these potentially fibre-bearing zones from the ores sent to the mills, and those suspect tonnages, including the associated talc, are left in. the pit walls. or _sent to waste piles. Minor occ.urrences of amph_iboles a_nd a.sbe~tiform minerals are also. attributed to confined areas of the Montana dep_osits~ Tremolite (blocky) was encountered in a dike zone at Antler. A chlorite zorie at intersecting faults at Yellowstone S40 contained some minor tremolite, and stockpiles of'Beaverhead open pit_fines, slated -2- Protected Document - Subject to Protective Order IMERYS 219721 2 of 3 Pltf_lMERYS_00057875 ... . ,_ :., I for buriali have been measured .at 0.33% to 0. 70% tremolite by Three Forks and Alpine Mill Labs. ' . No fibrous mater-ial showed up in samples taken by-the writer at the Western .source Red Hiil mine in Califor.nia, but min.or tremolite is possibly present in the contact zone where it should be avoidable by selective mining. . . Arsenic content-(fotal and soluble) and the 'presence of fibrous minerals in exposed stockp_iles and waste need to be checked at Alpine, .Alabama- and the: now closed California-_proper:ties,.operated, by. Cypri.Js:o.ir,: the.,,past.;: . -/flwvt /eji . R. J.. Kerstetter G. L. Toll G. B. Lawson - .BCL J. Paulsen. P. Moreau -:- Talc de Luzenac -3 - Protected Document - Subject to Protective Order IMERYS 219722 3 of 3 Pltf_lMERYS_00057875 TEM ASBESTOS ANALYSIS OF ARGONAUT PRODUCT COMPOSITES Summary Report 312/2018 CONFIDENTIAL Table 1. Result Summary cHRY?'sonLe Sam le Number of Fiber . Number of Sample Description Map Structures Concentration Structures Coliseptre?on 25 <5 pm pug-n 25 pm <5 run .gepm? Ludlow Coarse March 2004 0 BBL 0 1 339%. Ludlow Flne February 2004 Aorrler 1 . 111,- .. Ludlow Coarse February 2004 AO4115-2 .891, 1; Ludlow Fine January 2004 Acme-l eoL . 1 $3er Ludlow Coarse January 2004 Aurore-2 0 0 0 Ludlow Fine December 2003 Amror 0 0 ?qu 0 1 ?ng, .3-2 Ludlow Coarse December2003 warm 0 .. 3.6L 0 1 {1130.1- Ludlow Flne November 2003 A03640-1 0 1 0 ?l 1:313; "var ?for; Ludlow Coarse Novemberzooa Aosaro-z 0 0 0 391% Ludlow Fine October2003 Atlases-r 0 0 ?13391; 0 0 Ludlow Coarse Odober2003 A03596-2 0 0 -7 Pp}; 1 0 1 Grade 95 Quarter 2003 Aomw 0 0 . 0 1 3: were? '1 cure -: Ludlow Fine September 2003 Aossaa-l 1er . BQL W151 Ludlow Coarse September 2003 Acme1190;. Float Feed September 2003 Aaasro-a 0 0 .1 12011.Ludlow Fine Augu'stzooa A03464-1 1 not! 3 11034542 0 . - - Ludlow Coarse August 2003 0 ?1 .1331. 1 0 0 . 15211, .7131?" .ke. 'r'T Float Feed August zoos Aaaerez a -. - Zegg .4 - LudlowFlne July 2003 ?3438-1 0 0 0 0 . Ludlow Coarse July-2003 A03438-2 0 ?9917 0 0 LBDL, . 1 ?Hf?3' Float Feed July 2003 Adam-r egg 23g.- Grade 96 Quarter 2003 1?0-3572? 0 0 5m; 0 1 EPI- BDL Below detection limit as de?ned by ASTM 6620-00. ND Not detected as de?ned by Johnson Johnson internal test method TM7025. Page 8 of 13 Protected Document - Subject to Protective Order 462269-008 TEM ASBESTOS ANALYSIS OF ARGONAUT PRODUCT COMPOSHES Summary Report 31212018 Table 1. Result Summary AMPHIBOLE Sample Number of 5 5' A Number of fabeslg? ample Description No. Structures Structures go ca ragga; 25m <5um 25pm mm Ludlow Coarse May 2002 A02358-2 0 0 I 0 Float. Feed May 2002 A02359-2 0 0 Ludlow Flne April 2002 Aosreer 0 Ludlow coarse April 2002 Aozsres 0 0 Float Feed April 2002 A02359-1 0 0 Grade 96 1?t Quarter 2002 0 Ludlow Flne March 2002 Aozaros 0 0 Ludlow Coarse Maroh 2002 A023-lo-6 0 0 Float Feed March 2002 A02216-3 0 Ludlow Flne February 2002 11023103 0 0 Ludlow Coarse February 2002 A02310-4 0 0 Float Feed Febnlary 2002 Aozzrez 0 Ludlow Flne January 2002 #023101 0 0 Ludlow Coarse January 2002 warm 0 0 Float Feed. January 2002 A022161 0 0 Grade 66 Quarter 2001 A02008-1 0 Grade 66 Si") 42%:3mber Aozooer 0 0 Float. Feed December 2001 A02052-2 0 0 Float Feed November 2001 A02052-1 0 0 Float Feed Gambler 2001 A01621-3 0 0 Grade 66 3'd Quarter 2001 A01571-1 0 0 Float Feed September 2001 A01521-2 0 BDL Below detection as de?ned by ASTM 6620-00. N0 Not detected as de?ned by Johnson Johnson internal test method Protected Decument - Subject to Protective Order IMERYS 462269-011 Page11of13 (I) TEM ASBESTOS ANALYSIS OF ARGONAUT PRODUCT COMPOSITES Summary Report CONFIDENTIAL Table 1. Result Summary KMPHIBOLE Sample Number of Number of ?@193, Sam le Descri tion No. ?c ?r95 . . Structures E?c?g?agm if" epp?m: . Ludlow Fine June 2003 A03379-1 0 0 0 0 . Pefa Li?? :3 ram-Lax: ask; a .32 Ludlow Coarse June 2003 #4033792 0 0 0 0 -r aim? Float Feed June zoos 0 agem?m'. "a Ludlow Flne May 2003 21033231 0 lH??Mit??wd Ludlow Coarse May 2003 A03323-2 0 0 1 Haunt": I .F?mui'r. - Float Feed May 2003 0 0 0. Ludlow Flne Apnl 2003 A03275r 0 0 J. Ludlow Coarse April 2003 A03275-2 0 0 0 0 Lgmaob m? urn, - ?fatten?r Float Feed Apnl 2003 A03414-1 0 0 0 0 . Grade 96 1" Quarter 2003 .V?r ?Tr??P-E??ssai?Ludlow Flne March 2003 A03200-1 0 0 0 0 ?9801:5511. Ludlow Coarse March 2003 Aoazoo-z Float Feed March 2003 A031953 0 0 Ludlow Fine February 2003 A03146-1 0 0 Ludlow Coarse February 2003 A03146-2 0 0 Float Feed February 2003 A03195-2 0 0 Ludlow Fine January 2003 A03063-1 0 0 Ludlow Coarse January 2003 A03063-2 0 0 Float Feed January 2003 A031951 0 0 Grade 96 Quarter 2002 moose-1 0 0 Ludlow Flne December 2002 A03003-1 0 0 Ludlow Coarse December 2002 0 0 BDL Below detection limit as de?ned by 6620-00. ND Not detected as de?ned by.Johnson Johnson intramal test method TM7025. Protected Document - Subject to Protective Order Pagerfla 1M ERYS 462269-009