450 NEW 8RUNSWIC~ ~ ~ October 17. 1972 R. Schaffner, Ph.D. Director, Office of Product Technology Bureau of Foods Food and Drug Administration Department of Health, Education, and Welfare 200 "C'' Street Washington. D. C. 20204 Subject: SHOWER-TO-SHOWER Brand Body Powder Dear Dr. Schaffner: As a result of a finding by Professor S. Lewin that a SHOWER-TO-SHOWER Brand Body Powder sample contained 5o/o chrysotile asbestos, we have carried out extensive studies on the sample in question obtained from Prof. Lewin as well as representative samples from production of SHOWER-TOSHOWER Body Powder. As you requested in our meeting of September Zl 1 l 972. we are providing our data as follows: 1. Italian Talc Mine: Reports by: (a) (b} (c) (d) 2. Prof. F. D. Pooley (University College. Cardiff, U. K.) Atomic Energy Research Establishment (A.E. R. E •• Harwell) Mining Institute. Torino, Italy Prof. S. Lewin (New York University) Investigation of SHOWER-TO-SHOWER Body Powder: Reports by: (a) (b) (c) (d) (e) (!) (g) (h) Prof. M. J. Buerger, · (M. I. T.) Prof. G. E. Brown (Princeton University) McCrone Associates (Dr. I. Stewart) (Dr. W. Mccrone) Colorado School of Mines Research Institute Prof. F. D. Pooley (University College, Cardiff, U.K.} Prof. S. S. Pollack (Carnegie-Mellon University} Mr. J. Sch':!lz. (Johnson & Johnson) Dr. J. M. Wehrung (Sperry-Rand) DEFENDANT'S EXHIBIT D-8372 r- . J&J-0130530 JNJAZ55_000017552 D-8372 Page 1 of 247 - 2 - R. Schaffner, Ph.D. October 1 7, l 9724 5j A review of the data shows that: 1. Italian Fontana mine does not contain chrysotile asbestos deposits. 2. The Italian talc powder from the Fontana mine used in SHOWER-TOSHOWER Body Powder has been shown to be free of chrysotile asbestos by both Prof. Pooley and Prof. Lewin . 3. Investigations by all available methods carried out by experts failed to establish any chrysotile asbestos in SHOWER-TO-SHOWER Body Powder. The investigations included transmission electron microscopy and electron diffraction, x-ray scan, step scan, Guinier camera, d ifferential thermal analysis (DTA), petrographic techniques including optical staining techniques, and scanning electron microscopy. A review of the data by the various experts clearly shows that Prof. Lewin' s finding is wrong and has no basis in fact. We would like to point out that a release of such untrue information will create a great deal of unwarranted alarm among the public and will cause serious damage to our reputation and business. In view of the nature of the enclosed material and the comments regarding Professor Lewin's work, we request that this material be held in strict confidence by the employees of the Food and Drug Administration interested in this subject, unless we consent to other use of it. On behalf of myself and my colleagues, I wish to thank you for gtvmg us the opportunity to fully review our data on this subject on September 21. Very truly yours. JOHNSON &- JOHNSON \0 - Ni.--r'"'-~ W. Na shed, Ph.D . Director of Science Information WN/cw Attach. bee: Dr. Mr . Mr. Dr. Dr. Dr. R. D. H. A. R. G. A. Fuller R. Clare Stalzer Goudie Mr. S. C. Smoy~r Dr. T. H. Shelley Mr. W. Steinberg Mr. R. c. · Stites Mr. E. G. Vimond Rolle Hil dick-Smith J&J-0130531 JNJAZ55_000017553 D-8372 Page 2 of 247 D-8372 Page 3 of 247 '3 '5 '3'on 30534 7554 453 DR. FRED POOLEY Born: London, England Education: B.Sc. 1962 University of Wales (Cardiff) l'{. Sc. University of Wales (Cardiff) Minerai Separation 1963 Ph.D. University of Wales (Cardiff) 1965 Mineral Engineeri.ng Employment: British Medical Research Council Fellow 1965-1967 University of Wales Lecturer Mineral Separation 1967. Unive~sity of Wales J&J-0130535 JNJAZ55_000017555 D-8372 Page 4 of 247 ✓ University College, Cardiff 454 Postal Address: University College, P.O. Box 78, Cardiff CF1 1XL. T dephone Cardiff 442 11 Telegrams : Coleg Cardiff From ...........................R.~.!':.....:f..t.. D..,.... J?..o.o.l.e_y,........_ __ Department of.. .........Mine:t:al ....Ex.p.lo.itation ............ FOP/MM 28th September, 1972. Dear Dr. Shelly, The mineralogical X-ray and morphological examination of the Italian mine samples has been in progress for over a year. The samples were all collected under·my supervision at the Fontana mLne, which is the same mine from which the 'Shower to Shower' sample was obtained. The report of the examination contains a brief outline of the results obtained. No chrysotile was found at the mine or in the samples taken, some tremolite was located, but was not asbestiform in character and has not been detected in 00000 talc imported into Great Britain for the past year, nor in shipments dating back to 1949. I hope that it is of some interest to you. Yours sincere; _ 7-P i!J4. F.D. Pooley. J&J-0130536 JNJAZ55_000017556 Protected Document--Subject to Protective Order D-8372 Page 5 of 247 455 . • . \L~~ ~ - .. ~ -~ .. . _, / DEPARTMENT OF MINERAL EXPLOITATION UNIVERSITY COLLEGE CARDIFF J&J-013O537 JNJAZ55_000017557 D-8372 Page 6 of 247 456 AN EXAMINATION OF ITALIAN MINE SAMPLES AND RELEWWT POWDERS This document represents the completion report of the Italian mine samples and other powders supplied by Johnson and Johnson, Cosham, Portsmouth, to the Department of Mineral Exploitation. The persons involved in the examination of the material reported here were: Mr. J. Lightfoot Mr. G.A. Ringston Dr. F.D. Pooley Received: 8th September 1972 J&J-0130538 I JNJAZ55_000017558 I Protected Document--Subject to Protective Order D-8372 Page 7 of 247 REPORT OF INVESTIGATION OF ITALIAN MINE SAMPLES AND' RELATEO POWDERS 457 Introduction Talc is hydrated magnesium silicate (Mg 3 Si~0 14 (0B) 2 ) whicn can occur in a number of forms. In its compact form it is known as stealite or soapstone. The form normally employed for toilet purposes is soft and very friable in character.. It is mined in many parts of the world including the U.S.A., Canada, France, Italy, Norway and India, as well as several other countries. It occurs in both a flaky and lath like form and the chief deposits occur in altered magnesia-rich calcareous rocks such as dolomite, marble, and magnesian limestone. The purest talc deposits occur in association with dolomite and marble. Talc also occurs in altered basic rocks such as serpentines and again as thin beds in mica schists. Commercial talcs contain a nwnber of related mineral impurities. They may include antigorite {hydrated magnesiwn silicate} magnesite or members of the magnesite-ch.alybite series of carbonates, dolomite (calciwn magnesiwn carbonate}, tremolite and actinolite (calcium, iron magnesiwu silicates}, chlorites (Jnagnesium aluminium iron s ·i li.catesl and other minor minerals such as the sulphides and spinels. The hand specimens examined in this report were collected at the Italian mine and do not represent an average collection 0£ specimens of material being produced at the mine. The specimens were collected wi.th the intention of sampling those areas with obvious non talc mineral inclusions. Specimens were retained which showed differences in physical appearance, i.e. fibrous, flakey, massive and powdery in texture. Specimens of ore in which colour variation was observed were also collected. In general the colour of the talc ore varied from grey through white to a light green colour. Obvious inclusions in the talc ore itself were retained and a careful search at the various sample locations in the talc seam was performed for fibrous arnphibole minerals. Specimens of the hanging and footwall were also collected to assess their mineral content as these were likely sources of ore contamination, although the method of mining which consisted of hand filling methods precluded any gross contamination of the ore. The hand spec:Lrnens have been, where possible, prepared for examination by the optical microscope and both polished blocks and thin sections of material have been employed. Representative fractions of all hand specimens have been reduced to powder form and subjected to powder X-ray diffraction examination. Th.e representative powdered samples also form the samples for morphological examinati:on by the electron microscope. J&J-0130539 Protected Document--Subject to Protective Order JNJAZ55_000017559 D-8372 Page 8 of 247 2. The list of samples obtained from the Italian mine are· given in Tables land 2 and throughout this report the samples are referred to by thP preceding code number for each specimen. 458 The objective of the examination has been mainly to establish the major minerals which occur in association with talc at the rtalian mine. In particular to look at the association of these minerals wit~ the talc and especially those minerals wh.ich are of the same family as the commercial asbestos minerals, i.e. the amphiboles and serpentines. The objective of the optical examination has been to establish textural and mineral relationship and not to quantify the phases occurring in each hand specimen. X-ray work has been aimed at establishing the minerals observed by optical means and to produce reference patterns for future investigation together with computed data from pattern measurement. Electron microscope work has been selective in nature and performed on the finer fraction of the powdered specimens. Its aim has been to describe the morphology of the particles produced by comminution of the hand specimens and to investigate any obvious structural information which might be of use in identification of individual mineral particles. Representative data obtained from the various examinations are included in the following report. J&J-0130540 JNJAZ55_000017560 Protected Document--Subject to Protective Order D-8372 Page 9 of 247 3 459 TABLE 1 LIST OP- ITALIAN MINE SAMPLES Code No. Description I. l. Talc from -footwall contact I.2. Sorting pieces (with obvious colour differences} I.3. Coloured talc _(green) I.4. Face 10 sample with obvious amphibole inclusion. I.5. General ore I.6. Suspected Quartz sample I.7. Mica schist specimen I.8. Massive talc I.9. Grey talc 1st face I.10. Granular talc sample I.11. Carbonate and talc I.12. Footwall sample? I.13. Amph.ibolite Inclusion showing passage into talc bottom transit. I.14. Inclusion in talc seam face 4, middle of seam. I.15. Talc footwall contact I.16. Inclusion from face 1. I.17. Footwall rock sample I.18. Face 3 carbonate/talc sampla I.19,; Tremolite/quartz/talc sample I.20. Amphibole sample from Gi.anna I.21. Inclusion from face 2. I.22 •. Carbonate/talc sample ·I.23. Black gneiss 2 ft below talc seam :r.24. Talc next to carbonate face 2. :I.25. Footwall limestone I.26. Talc inclusions 1°,•"'1 1.212 J&J-0130541 Protected Document--Subject to Protective Order JNJAZ55_000017561 D-8372 Page 10 of 247 4 460 Table 1 Continued Description Code No. I.28. I.29. Quartz/talc sampie . Sample 6 footwall I.30. Quartz/Carbonate/talc sample I.31. Black inclusion face 1 I.32. Face 2 inclusion from base of talc 1.33. Talc from lower left end of working I.34. Marble/tunnel wall I.35. Massive carbonate from rear end of working I. 36. Grey talc specimen I.37. Carbonate in talc inclusion I.38. Pyrite/talc specimen I.39. 5" - I.40. Platey talc I. 41. Face 2, . good specimen I.42. Face 1, coloured green (talcl I. 43. Face 10, fibrous sample I..44. Face l, pure. talc? I..45. Face 1, good speci..men J:.46. Face 3, coloured specimen O pieces from crush.er --· J&J-0130542 JNJAZ55_000017562 0 Protected Document--Subject to Protective Order D-8372 Page 11 of 247 - J TABLE 2 46 l · OTHER SPECIMENS EXAMINED Code No. Description Bl Pure talc 1st face B2 Greenish talc 1st face B3 Talc 6 inches above footwall B4 Talc from above .inclusion BS Inclusion in talc B6 Talc 2 ft above inclusion B7 Section 2 ft above inclusion B8 Pure talc 1st· face B9 Gre~ talc 1st face Also examined l.) Batch shipments of f6{2!n~ talc 2) Old samples of British powders. J&J-013O543 JNJAZ55_000017563 Protected Document--Subject to Protective Order D-8372 Page 12 of 247 462 OPTICAL EXAMINATION OF SPECIMENS Il - I46 Thin and poli~hed sections were ~repared of the specimens of wallrock and, 'where possible, the talc ore. The minerals which formed a major constituent in at least one of the secti.ons were ·g u·a ·rtz, muscovite, talc, chlorite, (var sheridanite), calcite, garn·et, and tremolite; the latter only occurred as a major constituent in section Il9. Phases which were always minor or accessory were microcline, plagioclase, biotite, pennine, epidote, clinozois~~, hornblende, actinolite (section 17), rutile, and opaque constituents pyrite, pyrrhotite, and chalcopyrite. The identification of the minerals in the sections of these specimens was based on the optical characteristics of the minerals in transmitted and reflected light, both under plane polarised light (PPL} and crossed nicols (XN}, combined with the results of the X-ray diffraction study of the crushed hand specimens. In some cases material was extracted from the sections and examined in R.I. liquids as in determining that the most common chlorite mineral in these specimens is a variety called sheridanite having a R.I. w equivalent of 1.590 t o.oos and a birefringence of 0.012 - 0.014. Similarly much of the muscovite was nearly uniaxial with a R.I. of 1.600 corresponding to the variety phengite, an abnormally siiiceous muscovite. In the case of talc its confident determination optically is difficult since its optLcal properties are identical to muscovite. However, it was found that the common "feathery" form of the talc combined with the invariable occurrence of minute transparent inclusions (suspected to be silica) in the talc producing a •dusty• appearance in thin section and a greenish colour in hand specimen, enab1ed talc to be distinguished from muscovite. Talc a1so exhibited slightly higher order interference colours in general. Where talc was only an accessory mineral to muscovite, as in some of the wallrock samples, then i t could not be distinguished with certaintly. In the following pages (no. 7 to 48 ) the Italian specimens are systematically described as regards their mineral composition and mode of intergrowth. Numerous photomicrographs taken under PPL and XN are provided with the description to mainly illustrate the rock textures which, it is hoped, will provide information useful in the comminution of particularly the talc ore samples, and also displays the non occurrence of asbestiform amphiboles in the talc ore. J&J-0130544 JNJAZ55_000017564 Protected Document--Subject to Protective Order D-8372 Page 13 of 247 7 463 Spe:cime:11 ·11 Specimen Il consisted of several pieces of wallrock with one piece displaying the talc/footwall contact. One polished section was made of the talc/footwall contact and one thin section of the wa1lrock alone. The wallrock. is a sch.ist which in thin section displayed a segregation of the main minerals into th.in lenticular bands composed, as in Figure l, of lon~ tabular aggregates of intermixed muscovite (var. phengite) and chlorite (var sheridanite), and granular quartz exhibiting a polygona~ grain boundary structure. Accessory rutile occurs as orientated inclusions in the ch.lorite and muscovite, and a1so opaque constituents which in polished section were identified as dominantly pyrite metacrysts wit~ minor pyrrhot•i ·te. Some subhedral porphyroblasts of plagioclase also occur .. Fig. 1. Photomicrograph, X 40, of thin sect:1_on of wal.lrock Il under crossed nicols. A sch:ist of quartz (granular white-black) , muscovite Uaillellar yellow-blue}, and ch.lorite (lamellar white-blueisn grey}. Specimen I3: 'coloured talc' The minerals composing tlti.s specimen are major ta·lc and chlori•te (var sheridanite) with the talc content much greater than chlorLte, together with accessory garnet, rutile, and an unidentifiable finely dispersed phase occurring as minute transparant inclusions along the cleavage planes and grain boundaries of the talc and imparting a dusty brown appearance to the talc in thin section and a greenish colour in hand specimen. The talc occurs as rnediwn.grained feathery aggregates wh.ich are in places 'dusty' and grade into 1 clean 1 transparant aggregates which are free of any inclusions. It aooears that some retroqrade metamorphic process has caused J&J-0130545 JNJAZ55_000017565 Protected Document--Subject to Protective Order D-8372 Page 14 of 247 8 minor chlorite is dispersed in the talc matrix as small lenticular and globular. fibrous aggregates. Rare garnet, possibly a member ~f th.e ugrandite series because of its anisotropy, occurs as sul:>hedral porphyroblasts. . • .\ · ' • 464 ' . .-:1 '· T f ·j .l ·., j ..··~.. · , . ·I j .. .·.........,.,.~. . •· '~-J Fig. 2. Photomicrograph, X 24, of thin section of 'coloured talc' specimen 13 under crossed nicols. Dominantly talc (yellow-blue interference colours) showing murky brownish black patches due to presence of fine unidentifiable inclusions. Specimen IS: general ore A coarse aggregate of curving foliaceous and feathery crystals of ta·lc displaying evidence of shearing and translation twinning. As in specimen I3, dusty inclusions of a transparant mineral witn a general prismatic habit occurs dispersed in the talc. As before, but to a lesser extent, the talc is cleansed of these inclusions along zones associated with deformation and translation twinning, and it appears that the inclus~ons have either been converted to talc (as in the conversion of tremolite to talc by low temperature CO 2 metasomatism) or incorporated into the talc structure as a result of retrograde deformation metamorphism. Rare small subhedral garnet pqrphyroblasts also occur. J&J-013O546 JNJAZ55_000017566 Protected Document--Subject to Protective Order D-8372 Page 15 of 247 465 9 Fi.g. 3. Photomicrograph, x 24, of th.in section of 'general ore• specimen I5 m1der crossed nicols showing the texture of the talc, and the 'murky' inclusion-rich talc compared to the clear inclusion-free talc. Specimen I6 Specimen I6 consists of a very coarse aggregate of interlocking anhedral magnesite grains which·exhibit strongly irregular and angular penetrating grain boundaries. The magnesite is characterised in thin section, Fig. 3a, by its marked change in relief and perfect rhombohedral cleavage in plane polarised light, and very high order interference colours, Fig. Jb, Wlder crossed nicols. Intergranular pockets of fine grained foliaceous and radiating prismat~c crystals of talc together witn rare ch.lorite {var. sher~danite} occur. In places the prismatic clusters of talc appear to have formed at the expense of the magnesite, perhaps as a result of a retrograde thermal metamorphism with its formation being ascribed to a reaction between the magnesite and silica. One subhedral porphyroblast of plagioclase felspar occurs in the thin section. J&J-0130547 JNJAZ55_000017567 Protected Document--Subject to Protective Order D-8372 Page 16 of 247 IO 466 Photomicr~raph.., x 24, of th.in sect~on of specimen 16 under plane polarised ligh..t,. consisti.ng dominantly of magnesite with minor talc and rare ch..lorite. ~·--. . ~ ' I . - , .··\ Photomicrograph of thin section of specimen I6, mag x 24, under. crossed nicols showing the occurr- ence of small equigranular and prismatic crystals of talc penetrating and interstitial to coarse &nhedral magnesi.te. J&J-0130548 JNJAZ55_000017568 Protected Document--Subject to Protective Order D-8372 Page 17 of 247 467 11 Specimen ·r7 This specimen of wallrock is a quartz-muscovite-garnet schist (Figs. 4a, 4b, and 4c) containing some accessory actino•lite, brown hornblende, ~ and rare biotite. The muscovite (var. phengite) forms long lenticular bands showing a preferred orientation in a matrix of interlocked equigranular quartz grains dispYaying strongly irregular grain boundaries. Large euhedral porphyroblasts of garnet, forming one o f t ~ major phases, are dispersed throughout tne rock. Accessory subhedral tabular and rhombic sections of actinolite (colourless to bluish green pleochroism) occur orientated parallel ~o the schlstosity. The actinolite also occurs as rims to euhedral grains of rhombic and tabular outline whi.ch may have . originally been brown hornblende but now are pseudomorphed by what appears to be a mixture of talc, chlorite and residual hornblende . Some talc is present as small pockets within the muscovite layers but this identification is based on the form, the lower refractive index and the occurrence of dusty inclusions. The colour, birefringence etc. of the talc is otherwise the same as muscovite. In polished section the main opaque accessory mineral is pyrrhotJ.te occurring as subhedral laths lying parallel to the scl).istoslty. Traces of chalcopyrite also occur, and some rutile rods mainly as inclusions in the garnet porphyroblasts • .... . .. ., . r-- "9!:rr-'';- -•-- :•·· "''~ f ·_,,. . ! . - .... II'- .. - , :, .· ---···--, '"•O:-<. . ,. ... . '• .I. ' ..· \,, , ' . . '. ,.-.:·~.:.\)'.\:--:·• ' • r- "',. r.': f :_;~~~::,·; :., . , .. , '· . ' . • -\ ~ ... ::) / t . •, ..,., . ., ·, . ·£', . . '. . .• "!.r, 't).,, ,.____ - - ~ ~1,, ·· ; : "I •~ \ ;'. , l, • \, ... . .;\. .. ,..._~ -~.,..,. .. . -· '\ \ . ';\ .. -;._ ",i-· .. --~- ] ) . ·,,1 T •- , ··, .. . ', . ...' . . . ·' .,... ..,,. , ..... .,.,,, ·~ Fig. 6b. - tu,'...,; \., , ~.. ' Photomicrograph, x 40 mag., of thin section r 9 under crossed nicols showing garnet (black) in a coarse matrix of foliaceous talc (bright interference colours) and chlorite (white to blue-qrey interference colours). J&J-013O553 JNJAZ55_000017573 Protected Document--Subject to Protective Order D-8372 Page 22 of 247 472 16 'granular talc' Specimen: ·I10 and IroA: Both I1o and I10A consist of an intergrowth of medium grained and randomly orientated major talc with minor chlorite (var. sheridanite) (Fig. 7). Some small porphyrohlasts of garnet also occur scattered in the talc/chlorite ground mass. In this specimen the talc ~snot crowded with inclusions as is th.e case ~n most of the othe~ samples • . , ,~ 11'T~ ,. : ,... ~ -;•.-·•·:•1•··•• . i• ' . .,..J, ;;· ·11,, . ,•. ( . • ,, ,J. . \ •; J. • ·, •, ' •J , ~• ., •·.r j!, ~t~~t'{~i!. '<,~~:?;?;~i/t~!~\;~~t':,\j Fig. 7. Photomicrograph, x 40 mag., of t.hin section 1 10 , unde.r crossed nicols,• consisting of talc (blue and yellow interference colours), chloriteCwhite and greys), and garn·et (black). Specimen I11: 'carbonate and talc' Specimen I11 consists dominantly of a mosaic of coarse to fine grained anhedral interlocking magnesite grains with :Lnte.rstitial pockets of coarse to medium grained foliaceous aggregates of talc (Fig~. 8a and 8b). The talc is crowded with near sub-microscopic inclusions of a transparant phase together with a brown amorphous material which causes the talc to appear dusty or turbid in thin section. Some fibrous chlorite (var. sheridanite) occurs as small pockets intergrown with the talc. Traces of rutile and pyrite occur. J&J-0130554 JNJAZ55_000017574 Protected Document--Subject to Protective Order D-8372 Page 23 of 247 17 473 Fig.· -8 a. Photomicrograp~, x 24 mag., of thin section 111 under plane polarised light showing a subhedral pyri.te metacryst O,lack·l in. a matrix of compact .granurar magnesite with interstitial foliaceous talc (top centre} • Fig. Sb. Photomicrograph, x 24 mag., of thin section 111 undor croaeed n.tcole showing a pyrite mr.t.1.1cr.yF1t (blndt.) 1n n 'Jr,.,11ul1:1r 1ftn•.11w11 lt:o matrix, wlt.h " f6liaceoua interstitial aggregate of talc (top centre). J&J-0130555 JNJAZ55_000017575 Protected Document--Subject to Protective Order D-8372 Page 24 of 247 18 474 Specimen I1i An aggregate . of anhedral quartz as the main constituent with minor interstitial muscovite and green chlorite (var. pennine) Fig. 9. The long muscovite laths show a preferred orientation. Chlorite occurs in interstitial pockets as randomly orientated platy grains. some epidote is present and a trace of magnesite. The chlorite displays a pleochroism from light green to brownish-cream, and anomalous blue interference colours in some cases. However, most of the chlorite grains display lower second order to upper first order interference colours. Thus a range of ch.lorite composition is probably represented in the section. Fig. 9. Photomicrograph., x 40 mag., of thin section I12 under crossed nicols. Specimen I:13 This specimen consists of an aggregate of mainly medium grained platy to fibrous ·chlori.te (var. sheridanite) and equigranular quartz. These two enclose ragged replacement residuals of ca1c•ite and subhedral metacrysts of pyrite with rare· chalcopvrite. J&J-0130556 JNJAZ55_000017576 Protected Document--Subject to Protective Order D-8372 Page 25 of 247 475 19 .)I: . • . - .\ . . ~ ·•:.". .,,,._ ~ ~ .... . I -1 . 'f~~- I• :,• : •. -~ ·"· Fi.g. -10a Photornicrograp~ x 40 mag., of thin section I13 under PPL showing subhedral pyrite metacrysts (black} in a matrix of dominantly chlorite and quartz with minor calcite. ,,J . ~j i1t' 1/t.i-h- -.i' '\r.'"'1-:•1,:. i_{ . .t: a_ _.- -...,:. y . ,., '. "'~ · '• • -" ,; <: :• •~- - a·• '' -, - . - •,, ..• •,/ ;i:.,:~1---i,J -l ,. -... :,/'~": .. ·-;_ i';' .f''!1 ,iJ'.. .·~- ~ . ...'I\ ·:,l •-« ._..,;___? ~.. •._,. ·. 4 ,, .... ,,.. \ . ~ • I ' •(\ . . --~ • . . . . .- . :~ ···- "'~ ,i:•v'~·\ (i"·_~ \· ' , ·.,':I'/ ' ~-.. ...-"t,) \.• ' ...~- • . . . 'l'1'' .t ' • . IV I I """•,. -. \' ~ . u '7'-- _,,. ' '"' .• '"' Ji',. ~-::- rt-'i' .. •,_. ,: ~- ' , ' ls\. 1. lt'l",...,' -. . ~ 'VI,,---.. '~,~· .,- - .,~.- ~ • ';,ff" 11.m-P- ·'" Ill' ..,. I --~f.i•.;;Vt .. jj, ~ l '>; ...... ~.'- ·-1.~$ •.., . ·(. ~4$;.e•. _,. _., -~ ; . : ·1·1 ·p··// .~-;-:-,;i.- , • ..._.~ .- , · \j. "t· J 1,'IAJ/1!/_r 1 :.. JI , ' I'',.. lo.I ,~• .. • • · \ • l/ ,.,•, • ', ~a. .· "l 1 :1\ ·: ;\ Jj;:i {! l:c~ - ~-·J ·.·•/ ~-1 --r; . ,•• ' ~ .·1~ ~'.:, , ,1 _fl~~" fi .(-- ' .. _,..,.~ ..... ) :•;~ ' , ... ·- • I I : k ~ ': -~, ,, ~~ . • ! ' .\ . ·:..-· • ... J, ·' .· . ,.~ . . .,. .q I\ . '}·-\~. •t·.--_,:1, ,,·1 ' (hJ ' '""' ,. • . . ~t ·.., • f'·.-.'t::r,, ",. hJ~..,. ~ -~~ ,, ~..., II It.~ '.•?·- ; .'''lt; ,~1. . - 'f' . •_,. ;· t.t :· ( • ~ r. ).v·\ I,•;.,,. t.'{ . , ~' .~ l:;-J. ,, ~i 'f . . . f ' . :\ .,"'4';;.1!-\J;, : " ~-r; · · · Fig.: '10b • • ..,._J . , .; ' '·w '• . • • \ .... l ... ' • I,. t ~ 't, -~ _. .,. I •, ,, 'I ·1,t ', . '. • ~•• .,, ' .. • ..._ , ~ -• •• ' ..:'.>'~.'.II \ { '/ • .~)f -,; . ~:~~ ~~ .;•,.,1./... ,. *-:it ·~r ~··").,} t..,,.,~ ., : ~ ,•. , '. \. f, ' ~ i · \'ii;,/"" \, • ~•-r.,.t, ·· • ~~~•I~\ \ .. .. • • ' ',\I\ ,,. -~} ,4. J ·, ' . ., r '~:,-i. \ l t . • .. ,~ £•.fl , \ _., • • , \ . ~-.-. / -~i~·-., . ~.,\ I f ,-- , ~ I f I•~ 1 ' I ~ • 1 ') •ii • ..."(. .v~ ,\ . 1 '·' -J •!It ..: l I\ /J. r '- _·•:\ •'&, :Jt•. Jk.i i • U,;--; ,. . 1 • • .1 •. · ~&-~i,:,,),:1,.. .--;·,_., , 1J : . • • ' "•"' • \ ,. • Photomicrograph, x 40 mag., of thin section I13 under XN showing chlorite (fibrous white and greenish-grey) and calcite (col.our.eel) enclosing subhctlral lackl. Muscovite (dominantly purple interference colours). Quartz (white and greys). J&J-0130560 JNJAZ55_000017580 Protected Document--Subject to Protective Order D-8372 Page 29 of 247 23 479 Specimen I 1 5 This specimen is dominantly composed of ch.l·orite (var. sheridani.te} and guar-t z: as orientated aggregates producing a schi.stosity. . very mi.nor amounts of ma·gn·e s-ite and ·talc occur. Tb.e talc occurs as thin laths intergrown witnthe ch.lori.te (Fig. 13b) • FJ.:q.· ·l·Ja· · Photomicrograph, x40 mag., ·of thin section I15 under PPL showmg the irregular but preferred elongation of granular tvartz; s~gregations in a matrix of fibrous ch.lor~te var. sheridan~te). Fi.g. llb Photomicrograph, x 40 mag., of thin section I15 under XN, composed of chl·or i te (fibrous white, greenish grey, blacklr quartz (granu1ar wh~te-grey-black), and talc (blue, red, and yellow interference colours). J&J-013O561 JNJAZ55_000017581 0 Protected Document--Subject to Protective Order D-8372 Page 30 of 247 24 Specimen I1G: 'first face inclusion' 480 This specimen is composed of ·a rnediwn grained aggregate of dominantly ch.lorite {var. sheridanite) and quartz, with minor magn·e s•ite,· clin·oz·oi's·ite, · talc, and muscovite, and displaying a poor schistosity. Scattered euhedral to sub_hedral pyrite metacrysts occur as well as medium grained crystal aggregates of rut~le associated with clinozoisite forming 'stringers' parallel to the general schistosity of the rock. In 'the photomicrograph of figure 14a the brownish speck.led· ·areas are dominantly chlorite although in Figure 14b talc and muscovite are more apparent because of their interference colours. Figure 14a~ Photomicrograph, x 40 mag., of thin section I16 under PPL. J&J-0130562 Protected Document--Subject to Protective Order JNJAZ55_000017582 D-8372 Page 31 of 247 25 481 "Fi:g.. · :14b • Photomicrograph., x 40 rnag~, of thi.n section I:16 under crossed nicols. A chlorite - quartz rock with minor talc and muscovite, and accessory magnesite, clinozoisite, rutile and pyrite. J&J-0130563 JNJAZ55_000017583 Protected Document--Subject to Protective Order D-8372 Page 32 of 247 48 26 1 footwall' This speci.Jnen of footwall rock is a rnuscoyite~uartzgarnet schist c~nsisting of long lenticular anhedra quartz aggregates. Both are enclosing fractured and altered euhedral porphyroblasts of garnet. Accessory sphene also occurs as well as serpentine-quartz pseudomorpha a ftcr il mJ rn.!l"al d l uplayi.ng rhombic and tabular scL:t :I onB. Fig. · 15a Photomicrograph, x 24 mag., · of thin section I17 · under PPL showing garnet euhedra in a matrix of segregated quartz and muscovite. Fig. 15b Photomicrograph, x 24 mag., of thin eect~on 117 under XN. Garnet (black), quartz (white to grey), and muscovite (le.rnellar · and coloured). J&J-0130564 JNJAZ55_000017584 Protected Document--Subject to Protective Order D-8372 Page 33 of 247 483 27 speetmen· 1 1-8 : • Face 3, carbonate/talc• A coarse to medium grained aggregate of subhedral interl<;>cking grains of· magn·e si·t e with. minor ·ta·lc occurring as scattered small interstitial clusters associated with rare chlori te (var • . sheridanitc) <1nd Pi.g. 16a nlllSCOVi te (Pig a. l6c.1, 16b) • Photomicrograpn, x 24 mag., of thLn section I1a under PPL of granular magnesite with _scattered tabular crystals and clusters of talc. Fig. 16b Photomicrograph, x 24 mag., of thi.n sect~on I1e under XN of granular ma9nesita (h.1.gh order 1.nterference colours, and scattered tabular crystals and clusters of talc (top _r ight, .coloured) and rare chlorite (white to blue-grey colours}. J&J-0130565 JNJAZ55_000017585 Protected Document--Subject to Protective Order D-8372 Page 34 of 247 28 Specimen: I1g: 484 This specimen consists of an aggregate of coarse grained anhedral magnesite intergrown with solitary bladed crystals and crystal aggregates of tremolite associated with minor amounts of fine fibrous talc and rare anhedral grains of quartz (Figs. 17a, 1 7 b ) . - Fig. 1·1a Photomicrograph., x 24 mag., .of thin_ section ot r 19 under PPL, showing coarse bladed tremolite intergrown with very coarse grained magnesite. Fl:g. 17b Photomicrograph, x 24 mag., of thin section I1g under crossed nicols showing coarse bladed tremolite and· anhedral coarse-grained magnes~te with minor small fibrous aggregates of talc (top left} .. J&J-0130566 JNJAZ55_000017586 Protected Document--Subject to Protective Order D-8372 Page 35 of 247 29 48~ •In~luaion, face 2 1 • Specimen I21 is composed of a fine grained interlocking aggregate of ~ r a l magnesite, as the major constituent, associated witli scattered laths and interstitial fine-grained fibrous aggregates of very minor !2.!.£ (Figs. 18n ;mu 1.81..>). F.ig. 18a Photomicrograph, x 24 mag., of thin section 121 under PPL. Magnesite with rare talc. Fig. 1'8b Photomicrograph, x 24 mag., of thin section I21 under crossed nicols. Magnesite with rare talc. J&J-0130567 JNJAZ55_000017587 Protected Document--Subject to Protective Order D-8372 Page 36 of 247 30 486 Specimen I22 This specimen is dominantly composed of coarse subhedral to euhedral interlocking grains of maqn·e s·i te associated with intergranular fibrous clusters of· talc which often enclose smaller euhedral magnesite grains (Fig. 19). · Fi:9 2 19 · Photomicrograph, x i4 magnification, of thin section 122 under plane polarised light. Magnesite and intersti.t~al a _g gregates of talc. J&J-0130568 Protected Document--Subject to Protective Order JNJAZ55_000017588 D-8372 Page 37 of 247 31 Spe·c ilnetf I ·2·3 i ·' Black Gneiss 2 • below talc vein• 487 Specimen I2J consLsts dominantly of medium grained anhedral interlocking~~ as orientated bands enclosing large microcline anhedra and anhedral ·aggregates. Scattered platy aggregates of m~scovite occur orientated parallel to the general direction of the quartz banding. Minor ep1.c'!ot~ iind ,~11 lni- 1 -~~~~ also occur [Figs. 20a and 20b). Fig. 20a Photomtcrograpll, x 24 mag., of thln section I23 under PPL·. Quartz-muscovite-microcline gneiss. Fig. 20b Photomicrograph, x 24 mag., of thin section I23 under XN. Qu~xtz-m~scovite-microcline gneiss. J&J-013O569 JNJAZ55_000017589 Protected Document--Subject to Protective Order D-8372 Page 38 of 247 32 488 '· Face 2 , Talc _next to carbonate• This speciJnen of talc ore consists dominantly of coarse fibrous talc with minor chlorite (var. sheridan.lte) occurring as small lenticular fibrous aggregates within the main mass of talc {_Figs. 21a and 21b). A few· small subhedra of garnet are present. As in previous specimens there are two forms of talc present: (1) a talc that in thin section appears brown {Fig.2la) under plane polarised light due to finely dispersed _dusty inclusions of a transparant mineral and a brown amorphous material, (2} a clear transpar..int talc free of incluolons which .1ppo,1ru to have· been formed at the expen:.H! o f the other by sumo mctauomait:Lc 'cle~nsing• process. Talc crystals in optical continuity can bu seen to chcmge sharply from 1 dust:.y • brown talc to tho cluar talo. Fig.• ~ - · Photomicrograph; x 24 mag., of t!un section I24 under PPL. 'Dusty• and clear talc enclosing small lenticular aggregates of chlorite. F:lg.2lb Photomicrograph, x24 mag., of thin section I24 under XN • . coarse talc with lenticular aggregates of chlorite. J&J-0130570 JNJAZ55_000017590 Protected Document--Subject to Protective Order D-8372 Page 39 of 247 JJ 489 This specimen of footwall rock ~onsists of an interlocking aggregate of mediwn grained anhedral quartz enclosing occasional large anhedra of microc·11ne feldspar (Figs. 22a,22b). Minor magnesite occurs as pockets interstitial to the quartz, and also scattered laths' of muscovite. Green chlorite (pt~nnine) and epidote occur in trace amounts. I I Fig. 22a Ph.otomicrograph, x 24 mag.,· of thin .section I2s under PPL, dominantly a quartz-microcline rock witn minor muscovite and rare pennine and epidote. Pi.9. · 2'2b Photomicrograph, x 24 mag., of thin section I25 under XN. J&J-0130571 i ! I ; JNJAZ55_000017591 ·Protected Document--Subject to Protective Order D-8372 Page 40 of 247 34 49( Specimen. I26 !. This specimen contains• ·chlor·1·te,· talc, ma·g n·e:a:1=te and· r ·ut-1.le~ One part of the . thi.n section consistede>fa massive coarse fibro~s and feathery aggregate of talc enclosing pockets of coarse magnesLte. This texture graded into one which was dominantly fine grained ·c hlorite (var. sheridanite) intimately intergrown vit~ minor quantities of fibrous and platy talc (Fig. 23) as well as scattered small equigranular and rod-shaped rutile crystals. Ph.otondcrograph., x 40 mag., of thi.n section r26 under crossed nicols showing minor· talc (coloured) intimately intergrown with major chlorite. · J&J-0130572 JNJAZ55_000017592 Protected Document--Subject to Protective Order D-8372 Page 41 of 247 35 49 Specimen I.27 Specimen I27 is dominantly compo~ed of quartz, chlorite (var. sheridanite) and talc (Figs. 24a anhotomicrog:raph, x 40 mag., of thin.soction lJl under PPLJ muscovite-quartz schist. Photomicrograph, x 40 mag., of thin section I31 under XNJ muscovite-quartz schist. J&J-0130575 JNJAZ55_000017595 Protected Document--Subject to Protective Order D-8372 Page 44 of 247 38 494 Specimen 132 Th.is specimen consists of coarse feathery lenticular aggregates of dominantly chl·or-J.:te (var. sh.eridanite) intimately intergrown w~tn minor amounts· of ta1c (Figs. 27a and 27b). Small inclusions of rut1·1 e occur along the bowidaries (shear planes) between the chl.orite aggregates and also along ch.lorite cleavage planes. Finely dispersed submicroscopic dusty inclusions of an unidentified phase similar to that found J.n talc occur in the ch.lorite. Fig. 27a Photomicrograph, x 24 mag., of thin section I32 unqer XN. Feathery aggregates of sheared chlorite (white to greenish grey· to black) with m.tnor talc (coloured). Fig. ·27b Photomicrograph, x 24 mag., of thin section !32 under XN. Finer grained chlorite-tala mixture. J&J-0130576 JNJAZ55_000017596 Protected Document--Subject to Protective Order D-8372 Page 45 of 247 39 495 Spect.men I-33 This spec1Jnen of talc ore consists of a mediUlll to fine grained . randomly orientated intergrowth. of dominantly- t ·a lc with. minor· ch..1:or·ite (var. sh.eridanite) ~ The chlorite--rsintimately mixed with the talc (Fig. 28).. Some pockets of coarse interlocking anhedral magnesi•t e grains occur enclosed by the talc-ch.1.orite matrix. Fiq. 28 Photomicrograph, x 24 mag., of thin section I33 under XN. J&J-0130577 JNJAZ55_000017597 Protected Document--Subject to Protective Order D-8372 Page 46 of 247 4U Specimen I-35 496 This specimen consists dominantly of magnesite as a very . coarse to medium grained interlocking aggregate of euhedral to subhedral grains·. Minor· ·tr·e rnol·i ·t e occurs as long prismatic crystals forming interstitial clusters, and as solitary crystals penetrating the magnesite and along tha grain boundaries of the magnesite. Minor· chlorite -(var. sheridanite) and rare ·t ·a ·lc occur associated w:ith the tremolite segregations. ·(Figs~a, 29b). Fi.g. 2'9a Photomicrograph, x 24 mag., of thin section I35 W1der PPL. Magnesite-tremolite-chlorite-talc rock. : Fig.· '29b .... . ~· Photomicrograph, x 24 mag., of thin eoction Ils under XN. Priemat~c tremolite 1n magneaLte 1n the extLnction poaitlon. J&J-0130578 Protected Document--Subject to Protective Order JNJAZ55_000017598 D-8372 Page 47 of 247 41 497 Specimen I37 ·This spe~imen consists dominantly of magnesite with minor talc. The magnesite occurs as an aggregate of very large iiiagnes1te anhedra enclosed by finer grained subhedral magnesite which. is .intergrown with feathery intergranular clusters ·of ta·~c (Fig. 30) • ,; , Fi.g. 30 Photomicrograph of thin eect~on 137,_ x 24 mag., under XN showing the finer intergranular magnesite associated with small laths of talc (fibrous and coloured). J&J-0130579 JNJAZ55_000017599 Protected Document--Subject to Protective Order D-8372 Page 48 of 247 42 498 Specimen· I39 This specimen is dominantly composed of talc forming coarse feathery aggregat~s intimately intergrown with minor finer grained chlorite {var. sheridanite) and containing fine disseminated inclusions of ruti•le. Occasional £ine grained quartz. as well as larger oval-shaped augen o~ quartz and rare garnet occur scattered throughout the talc matrix. The talc ~s for the most part crowded with. inclusions, as in previous sections, but elongate areas of 'clean• talc occur as 1n Fig. 31a • • !,!_g .. ·Jla· Photomicrograph, x 24 mag., of thin section I39 under PPL. Fi.g. l!!?. Pnotomiorogrnph, x 24 mag., of th.in section 139, under XN J&J-0130580 JNJAZ55_000017600 Protected Document--Subject to Protective Order D-8372 Page 49 of 247 43 499 Specimen I,41 rhls specimen of talc ore consists of a coarse aggr~ate of feathery ~ intimately intergrown with minor· ·c h:lor-i "te · (var. sheridanite), and enclos~ng rare large porphyrobla5ts of subhedra1· garnet which occasionally contain long prismatic inclusions of ~ l L t e (Fig.32a). ,. ; I ~ .; \1 I· '• ,; ·, I: i 1· Fig. _. 32a I Photomicrograpn, x 24 mag., of thJ..n sect~on I41 under XN. Feathery aggregate of talc ·with. garnet porphyroblast {bottom right, . black). ·I i J&J-0130581 JNJAZ55_000017601 Protected Document--Subject to Protective Order D-8372 Page 50 of 247 44 Specimen• I42; 500 'No.l Face, green coloured' Specimen 142 consists dominantly of an aggregate of fine grained fibro~s' chlo~ (var. sheridanite) intimately inter- · grown with minor very fine grained talc as in Fig. 33. .,\ \ i ,- .. :·, I • ,: I '· L I Fi.g. 33 Photomicrograph, x 24· mag., of thin section I42 under crossed nicols of chlorite (white, greenish _ grey, black}, and fine grained talc (yellow). J&J-0130582 JNJAZ55_000017602 Protected Document--Subject to Protective Order D-8372 Page 51 of 247 45 specimen !J.3: 501 'Face 10 fibrous sample' Specimen 143 consists dominantly of· £!!!.<.?E:lli .(var::. sheridanite), occ~ring in the form of a coarse ~h.eared fibrous aggregate .intimately intergrown with very minor talc as in Figure· 3 4 • F1.g. 34 Photomicrograph, >< 40 mag., of thin sect.ion I43 unde crossed nicols showing deformed fibrous chlorite (white-greenish grey-black) intergrown with platy and prismatic crystals of talc (coloured). · Specimen I4,jA As for'I43 the specimen consisted dominantly of chlorite (var. sher~danite) with very minor talc. The 'cross fibre•typs texture found 1.n I43 and produ~by she~ring at righ.t angles tp the schi.stosity was absent in specimen I43A• J&J-0130583 I JNJAZ55_000017603 I Protected Document--Subject to Protective Order D-8372 Page 52 of 247 46 Specimen I441 502 'First face pure talctt A coarse.~ggr~gate of lamellar talc showing a preferred orientation and enclosing augen of w~appears to be an intimate .intergrowth of ·q uar·tz and· serpentine (Fig. • 35). Both talc crowded wi.tn fine unidentified inclusions and 'clear• talc are present. See also description for I45. Piq. ·35 Photomicrograph, x 24 mag., .of sectio~ I44 wider crossed nicols showing coarse lamellar·talc enclosing rare anhedral segregations of probable serpentine-quartz composition. J&J-0130584 JNJAZ55_000017604 Protected Document--Subject to Protective Order D-8372 Page 53 of 247 ,: 47 I 503 'No.1 good specimen• ~ Th.1,s specimen of 'talc ore' consists nearly wholly of talc occurring in the form of a randomly orientated 'ma~ted• aggregate of fibrous talc enclosing minor guartz·-serpentine augen. As in previous sections the talc is rendered murky or dusty by fine inclusions of a brown amorphous material and .an unidentified transparant phase. In places the talc has ·been cleansed of these inclusions along zones which · appear to be independent of any intergrowth or c~~stallographl.o features of ~he talc (Fig. 36). \ .. I .i ,; I Fi.g. ·36 Photom~crograph, x 24 mag., of th.in spec;unen I45 under crossed nicols showj.ng the form. of aggregation of the talc and the difference between th.e 'murky' talc and the linear transgressive zone of 'clear' talc. J&J-0130585 JNJAZ55_000017605 ·Protected Document--Subject to Protective Order D-8372 Page 54 of 247 48 specimen I46: 'No.3 face, coloured• Thi.s specilnen cons~sts of very coarso lenticular aggregates of long fibrous and feathery' ·ta'lc crystalsenclosing rare anhedral porpnyroblasts ofgarnet. J&J-0130586 JNJAZ55_000017606 Protected Document--Subject to Protective Order D-8372 Page 55 of 247 505 49 DIGESTIVE TESTS To confirm the presence of acLd soluble carbonate material and also to help identify the type of carbonate present in the rock specimens collected,each powder specimen was subjected to a digestive test. Half gram quantities of each of the powders were treated with normal hydrochloric acid for several hours at approximately 10°c. The residues were reweighed and ths filtrates were analysed for their calcium and magnesium content using the EEL. 240 Atomic Absorption Spectrophotometer. The aim of tb.e digestion was not to estimate the total acid soluble fraction only to help establisn th.e carbonate. minerals present and to estimate roughly their quantity to help 1.nterpret the X-ra~ powder photographs obtained from the samples. 1 The results are present under thl:ee headi.ngs, namely Rock Types', 'Carbonate Specimens•, and 'Talc Specimens•. It can he seen that only small quantities of carbonate material are present in the talc specimen group, similarly in the rock specimens with the exception of the marble specimen which is practically 100% calcite. The carbonate group of speciJllens appear to be mixtures of calcium and magnesium carbonate with a number of specimens being possil>ie dolomites. J&J-0130587 JNJAZ55_000017607 ·Protected Document--Subject to Protective Order D-8372 Page 56 of 247 !>U ROCK TYPES Specimen % Weight No. Loss Il I7 Il2 <0.2% 3.0% <0.2% Il3 4.2% IlS I16 117 I20 I23 I25 I27 I29 I31 I34 6.0% 4.8% 6.0% 11.2% 1. 4% 22.4% 9.0% 3.6% 9.6% 92.2% ' Calcium <0.2% <0.2% <0.2% 1.0% <0.2% 2.0% <0.2% <0.2% <0.2% <0.2% <0.21 <0.21 <0.2% >20.0% ' Magnesium . <0.21 <0.2% <0.2% 0.4% 0.4% 0.4% <0.2% <0.2% <0.2% <0.2% <0.2% <0.2% <0.2% <0.2% CARBONATE SPECIMENS Speci.men % Weight % % No. Loss Calcium Magnesi.um I4 I6 Ill Il4 Il8 119 I21 I22 IJO 135 I37 22.8% 48.01 21.6% 44. 2% 75.2% 37.8% 61.8% 91.2% 15.0% 50.8% 51.0% 3.0% 6.0% 3.0% 7.0% 14.0% 5.0% 8.4% 16.0% 1.9% 6.6% 4.4% 1.1% 1.151 6.4% 5.0% 24.0% 4.0% 8.0% 15.2% 1.6% 13.4% 24.0% TALC SPEC::IMENS Specimen No. 12 13 IS I8 I9 IlO I24 I26 128 I32 133 136 Wei.gh..t ' Loss 3.6% 1.61 5.4% 6.0% <0.21 4.2% 8.0% ,c;0.2% 12.6% 1.2% 5.6% 4.6% ' Calcium -,).21 <0.2% <0.2% <0.2% <0.2% <0.2% ,<0.2% <0.2% <0-2% <0.2% 0~341 <0.2% I Magnesium 0.41 <0.21 <0-2% <0.2% <0.2% <0.2% . ... 0.2, ,<0. 2% <0.2% 0.4% <0.21 <0.2% · /Continued •••• J&J-0130588 JNJAZ55_000017608 Protected Document--Subject to Protective Order D-8372 Page 57 of 247 507 51 TALC SPECIMENS (Continued) Specimen No. ' Weight Loss 138 1.0% 139 <0.2% 7.0% <0.2% 0.8% 6.2% -<0.2% 8.0% 140 I41 I42 143 144 145 % % Calcium Magnesium <0.2% <0.2% <0.2% <0.2% <0.2% <0.2% <0.2% <0.2% <0.2% <0.2% <0.2% <0.21 <0.2% <0.21 ,<0.2% <0.2% J&J-0130589 JNJAZ55_000017609 Protected Document--Subject to Protective Order D-8372 Page 58 of 247 52 Electron Microscope Examination of ltalian Mine Samples and Imported Batch Shipments of Italian Powder 508 The main purpose of the electron microscope examination of mine samples and also representative fractions of the Italian powder has been to establish whether or not any particles corresponding to the commercial forms of asbestos were present. The electron microscope is an instrument which is most usefully employed in the examination of particles less than ten microns in size. It has been used in this investigation therefore to examine only the finer particulate portion of the Italian samples. It may be argued that only a small fraction of each of the powdered samples was examined and that this was not representative of the total sample. However, we can assume that the fraction examined was representative of the dust formed from each sample and that it is this finer fraction which is the most important from a biological standpoint. Also as the size of the biologically active commercial asbestos particles fall entirely within the particle size range examined we can consider the main aim of the examination to be entirely satisfied by only looking at the finer fractions from each of the Italian samples. ; I I To acquaint ourselves with the type of particles formed by the commercial asbestos minerals, Figs. A-D have been included. They represent samples of Amosite, crocidolite. Anthophyllite and Chrysotile asbestos. Also Figs. E-F have been inserted to demonstrate typical single particle electron diffraction patterns which can be obtained from the four asbestos types for comparison with patterns obtained from the Italian samples. Sample Preparation Small portions of the powdered rock samples and imported powder specimens were placed in 15cc centrifuge tubes to which distilled water was added. The powders were then dispersed first by hand shaking and then with the aid of a small ultrasonic bath. The concentration of suspended material in the tubes was adjusted by eye using dilutions of distilled water. The tubes containing suspended solids were then allowed to stand for 20 minutes to allow the larger particles of mineral to sediment to the bottom of the tubes. Electron microscope grids coated with carbon films were prepared and small drops of the particulate material from each of the specimen tubes were mounted on specimen grids and allowed to dry. The specimens were inserted into an A.E.I. E.M.6. electron microscope and examined for particles resembling commercial asbestos fibres. Where suitable particles were observed, selected area electron diffraction patterns were taken and compared with those produced by the commercial asbestos minerals. In all cases photomicrographs representative of the type of particles found in each sample were taken while interesting diffraction patterns were also recorded. J&J-0130590 JNJAZ55_000017610 Protected Document--Subject to Protective Order D-8372 Page 59 of 247 509 53 Particle Morphology The carbonate rich materials were found to produce ~ompact particles which were very electron dense. On the whole.they were finer particles than those obtained after crushing talc rich specimens. No fibrous material whatsoever was found when carbonate material only was comminuted. The morphology of particles produced from the footwall rocks i.e. limestone, marble, gneiss and the amphibolites were also very compact, although in the gneiss specimen platey particles were present probably representing the muscovite content of the specimen. Again in the footwall rock specimens fibrous particles were very scarce. Those lath like particles detected resembled the amphibole minerals rather than chrysotile. Selected area diffraction patterns which were obtained from the lath like particles in no way resembled the typical amphibole fibre diffraction pattern. They were generally very distorted patterns containing streaks rather than spots indicating a rather stressed and deformed material. The specimens which were composed of talc together with other mineral associations, presented a very different picture. as far as particle shape was concerned. In the main particles were flat and plate-like, some being very thin and translucent in the electron beam. Particle sizes varied from very small to quite large plates some with very sharp discrete edges, others with rather ragged outlines. Comparing particles from those samples of talc which varied in bulk morphology in hand specimens, no observable difference could be drawn between them. Similarly, a comparison of particles produced from talc specimens of varying colour revealed no differences in the overall particle shape. Similarly those specimens rich in chlorite did not form particles with any distinctive features. There were, however, observable differences in particle morphology between individual powder specimens. In the main most produced good plate like particles, however, one or two specimens were found to contain considerable numbers of lath like particles, these being very thin in character. These particles resembled the arnphibole asbestos type particle being less regular and also very much larger in projected diameter. Diffraction patterns from these particles matched those obtained from the platy particles with which they were associated and in no way resembled th~ typical amphibole diffraction pattern obtained from single amphibole asbestos fibres. Other fibrous particles were observed in the mainly talc specimens which_ to some extent resembled chrysotile asbestos fibres rather than amphibole minerals. They often had a somewhat textile appearance but were, however, crystalline. Diffraction patterns from these fibres were very distorted and in no way matched typical chrysotile or amphibole patterns. J&J-0130591 JNJAZ55_000017611 Protected Document--Subject to Protective Order D-8372 Page 60 of 247 54 510 The only group of specimens in which amphi.bole fibres we.re confirmed were in those specimens wi.th known amphibole composition. However, even the fibres found in these specimens barely resembled the fibre·s formed by the commercial amph.ibole asbes~os minerals. To assess the particles produced from the pure 'amph.il>ole mineral (.Tremolite),found in three of the specimens, small crystals of the mineral were taken from the hand specimens and crushed separately. An examination of the finer particles produced revealed stubby electron dense fibres associated with. irregular lumps of the ·same mineral. Diffraction patterns from these fibres were similar to those obtained from the commercial arnph..ibole minerals, although they were more difficult to obtain because of the greater thickness of these particles. Other specimens in the group, which. did not contain talc but were composed of sheet silicate minerals mainly muscovite, were also practically free of fibrous particles. Th.ere appeared to be no general tendency for these other mine~als to form fine fibrous particles. A number of very fi.ne short fibres were observed on grids prepared from several of the talc specimens, th.ese were, however, chance small pieces torn from the edges of talc plates. They appeared in those samples which. had a tendency to form copiua nwnbers of very fine particles when subjected to comminution. The specimens examined can be grouped into four categories on the basis of particle morphology and they are as follows: (a) Talc specimens with impurities of carbonate and chlorite. O>l Rock type specimens, i.e. footwall limestone etc. Those speci.Jnens composed mainly of carbonates. Amphihole specimens with carbonate and talc. (.c) (dl The talc specimens were characterised by the large number of plate 11.ke particles often translucent in the electron beam. Rock specimens varied from specimens which were composed mainly of compact electron dense particles to those w~th some sheet silicate content 1.n whi.ch plate like particles become apparent. Those specimens composed mainly of carbonate material produced compact rounded particles, often very small and grouped together in aggregates. Finally the specimens containing amph.1. bole were character~sed by the compact nature of the particles with. evenly distributed fibres and very few translucent plates. The groups of particles described are illustrated by the following micr~graphs which illustrate the various forms. Selected area electron diffraction patterns obtained from si.ngle particles of the amph.ibole mi.neral are also presented showing the si.m.i.larity of these patterns to those obtai.nea from commercial asbestos fibres. Also included are single crystals patterns and polycrystalline patterns. from talc, chlorLte and muscovLte rich. specimens. It can be seen that they axe very different in character to those obtained from the amphibole mineral. However, patterns- from the sheet sLlicate minerals mentioned above are all very similar and it is i.Jnpossible to identify each. of these minerals from their J&J..0130592 JNJAZ55_000017612 Protected Document--Subject to Protective Order D-8372 Page 61 of 247 55 I ! I 511 electron diffraction patterns or to tell them apart without applying a more sophisticated approach to the diffraction procedure. With specimen tilt facilities enabling the particle to be rotated through more than 450 discrimination is possi.ble between certain of . these minerals. As mentioned earlier, patterns obtained from lath like particles found in the talc specimens were identical to those observed from general plate like forms. Those fibres with a text~le like appearance often only gave very streaked patterns but in one or two cases these also resembled very closely the ·normal talc pattern. J&J-0130593 JNJAZ55_000017613 Protected Document--Subject to Protective Order D-8372 Page 62 of 247 56. Examples of Commercial Amph.ibole'and Chrysotile asbestos particles together witn typical selected area elec~ron 51 di~fraction patterns. Chrysotile asbestos particles x 3000 · , .. L • , Anthophyllite asbestoe particles x 3000 -· J&J-0130594 JNJAZ55_000017614 Protected Document--Subject to Protective Order D-8372 Page 63 of 247 57 5L Amosite asbestos particles x 3000 • Crocidolite asbestos particles x 3000 J&J-0130595 JNJAZ55_000017615 Protected Document--Subject to Protective Order D-8372 Page 64 of 247 58 51 ~ AJUphibole asbestos selec·ted area electron diffraction pattern • .. Chrysotile asbestos selected area electron diffraction pattern .. · J&J-0130596 Protected Document--Subject to Protective Order JNJAZ55_000017616 D-8372 Page 65 of 247 59 51 r Electron mi.crograpb.s. of particles produced: from specimens wh.1.ch have been clastd.fi.ed as rock · types. J&J-0130597 JNJAZ55_000017617 Protected Document--Subject to Protective Order D-8372 Page 66 of 247 60 516 Fig. l. Specimen Il3 s~am ·1nclusion showing passage into talc x 3000. The parti.cles are mai.nly compact and electron dense. A few flakes, no fibres present. Fi.g. 2. Specimen I15. Talc footwall contact.· x 3000. Compact part~cles with a few small flakes. No fibres present. J&J-0130598 JNJAZ55_000017618 Protected Document--Subject to Protective Order D-8372 Page 67 of 247 61 FLg. 3. .S l Specimen I16. Lithological inclusion from Face l. x 3000. Compact electron dense pcirticles. No fi.bres present.- "V" . . P. . .... . Att,'· ., • .: .... •t.t t . Fi.g. 4. .. • Specimen I17. . ·•··~,. -• •·' •- Footwall rock sample, .x 3000. Mal.nly compact particles produced with a few plate like forms. J&J-0130599 JNJAZ55_000017619 Protected Document--Subject to Protective Order D-8372 Page 68 of 247 62 518 ~ 'ii,,11 ... • • . ,,• ·• FLg. 5. Specimen 123. Black gneiss, 2ft below talo 3000. Compact electron dense ·p"artt.cles produced. · seam. la x •. -~ Fig. 6. Specimen I25. Footwall limestone. Comp~ct electron dense particles. · x 3000. J&J-0130600 JNJAZ55_000017620 Protected Document--Subject to Protective Order D-8372 Page 69 of 247 63 519 Fig. 7.- Specimen I27. L.ithological .incl.us.ion face 1. x 3000. Platey electron dense part~cles. No fibres. Fig. 8. Specimen 129. sample 6 Footwall. x 3000 compact electron dense particles w~th a few plate-l~ke forms. J&J-0130601 JNJAZ55_000017621 Protected Document--Subject to Protective Order D-8372 Page 70 of 247 64 52( }; ~. ~ ... Fi.g • . 9.- Specimen I31. Black inclusion face 1. x · 3000 A mi.xture of plate-like and compact forms mai.nly electron dense in character. Fig. 10 •. Specimen 134. Marble from tunnel wall. x 3000 Mainly ~ompact electron dense particles with a few plate-like forms. J&J-0130602 JNJAZ55_000017622 Protected Document--Subject to Protective Order D-8372 Page 71 of 247 65 Electron mi.crographa of part~cles. produced from those specimens mainly composed of carbonate minerals. J&J-0130603 JNJAZ55_000017623 Protected Document--Subject to Protective Order D-8372 Page 72 of 247 66 Fig. 1. Fi.g. 2. 522 Specimen Ill• Carbonate inclusion with some talc. x 3000. Particles consist of a mixture of compact and plate-like forms. Specimen I14• Inclusion in talc seam Face 4, middle of seam. x 3000. Granular . particles with plate-like types and lath-like forms. J&J-0130604 JNJAZ55_000017624 Protected Document--Subject to Protective Order D-8372 Page 73 of 247 67 52 Fi.g. · 3. Specimen I1a- Carbonate/talc sample, x 3000. Particles compact and electron dense. A few plate-like forms • • ,.. Fig. 4 • - Specimen I21Inclusion from Face 2. x 3000. This specimen produced plate-like and compact particles with some lath-like forma. J&J-0130605 Protected Document--Subject to Protective Order JNJAZ55_000017625 D-8372 Page 74 of 247 68 ... ,- ,. JL •_1 .•. · .~,~t~~~ flf_·· . -;,,, . . ~,,, ~ .. Fig. S. Massive Specimen 135. end of working, x 3000. carbonate from rear Compact electron dense particles with some plate-11.lte talc particles. Fig. ·6. 'specimen 137. Carbonate in talc inclusion x 3000. Compact particles together with some plate-like forms and rolled talc sheets. J&J-0130606 JNJAZ55_000017626 Protected Document--Subject to Protective Order D-8372 Page 75 of 247 69 JL 5 r ..... Electron Micrographa of spec·iJnens of talc 1dth. carbonate and other mineral inclusions. J&J-0130607 JNJAZ55_000017627 Protected Document--Subject to Protective Order D-8372 Page 76 of 247 /\J 526 Fig. 1. Specimen I3. Coloured talc (Green) x · 3000. Particles plate-11.ke. Few fibres, rolled sheets and shords. Fig. 2. Specimen I5. General ore, x 3000. Plate-like particles together with short lath-like particles, also a typical example of textile type fibre. J&J..0130608 i JNJAZ55_000017628 Protected Document--Subject to Protective Order D-8372 Page 77 of 247 ,l 527 Fig. · J. Specimen Ia. Massive talc, x · 3000. Plate- like particles with a few lath- . forms also typLcal text~le type long f~bre. ··a· ,..... • l'i f' ' ' • -. • ;.: •"f,:,i.. . ~ -( ,. ti. ·•1 . a .· · . , .~. h Specimen 19. Grey talc First Face, x 3000. Pract~c ally all plate-like with a ·fev lath forms. J&J-0130609 JNJAZ55_000017629 Protected Document--Subject to Protective Order D-8372 Page 78 of 247 i.i. • • Fig. 5. 52l " Specimen IlO• Granular talc, x 3000. All plate-like particles. • G ' . Fig. 6. Specimen I24. Talc next to carbonate inclusion, x 3000. This specimen was found to contain a large number of lath-like particles, as can be seen from the micrograpn above. No diffraction pattern corresponding with an amphibole fibre was obtained from a sele~tion of the elongated particles. J&J-013O610 JNJAZ55_000017630 1 Protected Document--Subject to Protective Order D-8372 Page 79 of 247 J 52~ Fi.g • . 7. Specimen I26- Coloured talc inclusions, x 3000. The particles produced from the various coloured inclusions in the talc were found to be mainly plate-like w~th a few lath forms • •• Fig. 8. Specimen 128• Talc/Quartz specimen, x 3000. Particles from this specimen were ma1.nly platelik~ but accompanied by more compact opaque particles. A few textile type fibr~s were observed. J&J-0130611 ; i ·Protected Document--Subject to Protective Order JNJAZ55_000017631 D-8372 Page 80 of 247 74 •· ......... ,·tt •·. ,. . •ir~ -~-- 530 • ~J ;.·i ... Fiq. 9 • Specimen IJ2· Face 2 inclusion from base of talc seam, x 3000. The specimen produced a mixture of irregular particles varying from compact to plate-like in form w~th a few. lath like particles. Fig.lo. Specimen I33. Talc from lower left- end of working ¥ 3000. Part~cles mainly plate-l~ke w~th some lath. forms. J&J-0130612 JNJAZ55_000017632 Protected Document--Subject to Protective Order D-8372 Page 81 of 247 7S 531 Fi.q. 11. Specimen I3a. Pyrite/Talc specimen, x 3000. Plate-like particles with some rolled tubes of talc. ..... ~ - .· ' -'~ ' • Fi·g :. '1 2. Specimen 139. 5" - O coloured pieces from the crusher, x 3000. These various coloured talc p~eces produced only plate-l~ke particles. J&J-0130613 JNJAZ55_000017633 Protected Document--Subject to Protective Order D-8372 Page 82 of 247 76 532- ;: I Fig. 13 .... ... ..._ ~ " ~. A.. Specimen I41- Face 2, good talc specimen x 3000. Plate-like particles together with rolled talc sheets lath forms and textile type fibres. Fiq. 14. Specimen I42• Face 1, green coloured talc, x 3000. Thi.s coloured specimen produced plate-iike part~cles wh.i.ch were rather more electron dense. J&J-0130614 Protected Document--Subject to Protective Order JNJAZ55_000017634 D-8372 Page 83 of 247 ,. 77 532 ,.! • • ·' . F.1g. 15. Fi.q. 16. -· ,. Specimen I43. Face 10. Fibrous looking hand specimen, x 3000. Th.is sample waf;l found to be pract~cally all plate-like 1n form. Specimen 144. Face l. Pure talc sample, x3000. Plate-l~ke particles with some lath-like forms. J&J-0130615 JNJAZ55_000017635 'Protected Document--Subject to Protective Order D-8372 Page 84 of 247 534 78 · Fig. · 17. Specimen I4S. Face l. Good talc specimen, x 3000. A mixture of plate-like particles and f.1.brous forms, including rol1ed tubes and texti.le type fil>res. · -~'•A ·.-. ~- .~....,. " • . .~ - . ~ .... Fig. 18.- Specimen 146• Face · J. Coloured specimen · x 3000. Plate-like particles with shards and latn like forms, together with a typical textile form, whi.ch can be seen to have a sheet-like form. J&J-0130616 JNJAZ55_000017636 Protected Document--Subject to Protective Order D-8372 Page 85 of 247 79 535 Electron Micrographs of partLcles produced from those specimens containing amphibole mineral and also from the amphibole mineral itself. J&J-0130617 JNJAZ55_000017637 Protected Document--Subject to Protective Order D-8372 Page 86 of 247 80 5 7_ib• -~ ~ • , !•· • -- . • Fi.g. l. Specimen 119. sample x 3000. Tremolite/carbonate talc Compact partlcles,a few lath forms present. .. . , •• t · Fi:g. 2 •· Amphl.bole sample from Guiana Specimen 120. level 1212. x Jooo. numerous lath forms. Compact partLeles w~th J&J-0130618 JNJAZ55_000017638 Protected Document--Subject to Protective Order D-8372 Page 87 of 247 Bl 537 . I - • -• ~• ,.. •t • & • •· • .- . ~ • All#. -- Fi.gs. · 3 and 4 Particles produced from single crystals of tremolite extracted from specimens Ilg and I20• x 3000. Very few fibrous particles were produced when th~s specimen was crushed. Those that were fibrous :ln nature were thlclt and stubby in character, less than 501 of the particles were elongated ~n shape. J&J-0130619 JNJAZ55_000017639 Protected Document--Subject to Protective Order D-8372 Page 88 of 247 82 53i , '. -!'., ,.:. _- •• . .i •·.1..,, ·:·_,.·.·.·.::_:;.~'.~._ .· '/·;,t ·. " ~-'.ii''_ ".{,. .: j. :: · :·,. · r,.-. ., t .. , :. , , Fi9a. 5 and 6 Selected area electron aiffract~on patterns obtained from amphibole pu-ticles found in specimens 119 and I20• J&J-0130620 JNJAZ55_00001764 'Protected Document--Subject to Protective Order D-8372 Page 89 of 247 83 539 Fi.g • . 7 •· Typical selected area diffraction pattern obtained from talc plates. Fi9. 8. Selected area diffraction pattern obtained from a typica1 textile type f~bre showing features of a rotated or coiled structure. J&J-0130621 JNJAZ55_000017641 Protected Document--Subject to Protective Order D-8372 Page 90 of 247 54 X-RAY ANALYSIS OF ITALIAN MINE SAMPLES Introduction This report concerns the X-ray powder analysis of the The samples were class1.f1.ed into three categories accordi.ng to their chemical and physical Ita1i.an mine samples. _properties a (J.l (ii) 'Rock' Type 'Talc' Type (iii) 'Carbonate• Type All the samples were prepared by similar means and the procedure for obtaining the X-ray powder patterns was standardised. From these powder photographs, several were chosen which clearly showed disti.nct mineral phases. These were used as standards for this group of samples. Th.ese standard patterns were compared against the ASTM index and th1.s comparison illustrates the need to prepare standards for a particular locality from specimens at that locality. Tne samples were compared with. these standards by computer methods and. visually and the results and d1.screpanciea between the methods of compar1.son noted. LIST OF SAMPLES See Table 1 _I SAMPLE PREPARATION The samples were received mainly as large rocks and were labelled according to their appearance and location in the mi.re. .I i With the larger samples a section waa cut from the middle to be a representative aample, for the smaller samples as many pieces as possible were crushed to form the representati.ve sample. a These samples were then roughly broken up and placed in 'Tema 1 disc mill and ground for 5 mins. until all the sample was belo'91' ·a pprox. 100 mesh. These powders were stored 1.n clean plastic bags. The samples, when requ.ired for X-ray analysis, were further ground {to less than 300 meshl 1.n a small agate ball mill and then sieved throug~ a 350 mesh screen and stored in plastic bags. The grinding milis and other apparatus used were thorough- ly cleaned between samples and during the grinding care was · taken to obtaui a good representative sample. J&J-0130622 JNJAZ55_000017642 Protected Document--Subject to Protective Order D-8372 Page 91 of 247 X-RAY ANALYSIS . • 541 All the samples were analysed using a Debye-Scherrer camera mounted on a Raymax RX 3-D X-ray generator. A copper X-ray tube was used with nickel filters (0.02 nun thick} and the power rating of the tube set at 36 kV and 22mA. I The apparatus was carefully aligned and checked before All the samples had the same exposure ' mount~g a sample. time of 8 hrs. • I The samples were loaded into o.s mm diameter Lindemann glass tubes to be mounted in the Debye-Scherrer cameras. In the cameras Ilford Industrial 'G' X-ray film was used. The film was processed using Kodak DX-80 developer and Ilford Hypain fixer. The films were developed for 5 minutes using a 1:4 dilution for the developer and fixed for 2 minutes. The films were then washed in running water for 30 minutes and allowed to dry naturally. The X-ray films were then measured. Using an illuminated screen and the line-spacings I 1 ! calculated, taking into accoW1t film shrinkage, from these line spacings the bragg angle and 'd' spacings can be calcu• lated. I I : f • STANDARD PATTERNS I When all the samples X-ray phOtOCJraph.s had been measured and the 'd' spacings calculated, they were visually inspected to find the fi.lm showing samples with pure m.ineral phases. Th.ese patterns were then taken as standards. · The samples were then broken up and the different mineral phases were sorted by hand to attempt to find a purer standard. These samples were then crushed in a simJ.lar way to the samples crushed beforehand. · For X-ray analysis they were placed 1n 0.2 mm diameter tubes and given a 12 hr exposure. This method was used to give finer lines on the X-ray photograph and the larger exposure wa3 to try and detect as many impurities as possible. I . ' I ' ., I i The 'd' spacings of the standards were compared wt.th the They were compared w~th themselves to check that all the Talc and Ch.lorite standards matched each other and were similar in intensity. A.S.T.M. index and also with. themselves. .! •• I Several standards were prepared containing the same mineral. This was because the 'd 1 spacings of the mineral varied slightly from sample to sample and especially wJ.th chlorite, · depending on its composition the major reflections varied between 13·. 5% and 15. 0%. This was mainly due to varying iron content and this can easily be seen on the X-ray films as it causes fluorescence with copper radiation and blackens the X-ray film generally. J&J-0130623 JNJAZ55_000017643 Protected Document--Subject to Protective Order D-8372 Page 92 of 247 86 542 RESULTS For the analysis of the results the samples have been divided into ftve sections: (i) (ii} standard patterns sample patterns (rock type) (ii.1) sample patterns (carbonate type) (iv) sample patterns (talc typel batch sample patterns (.includes old powders and C.vl shipments}. Two methods were used to find the mineral present in the sample. One method uses a computer program to detect the mineral. In thi.s method th.e b:r:agg a·n gles of samples were compared with the bragg angles of the standard and the number of lines fitted printed out. A print out was also obtained of all the standards whicn fitted a particular line to find all the possible minerals present and to see which l~nes were common to several standards. As thJ.s procedure is quite long, the lines in the sample were fi.rst sorted into order of decreasing intensity and then the three most intense lines of the sample compared with the standards. If all three lines failed to match it was considered that that standard was not present and so the program deleted that standard from the comparison. At the end of the program the list of the standards was prLnted with the percent~ge of lines fitted to the sample noted. The obvious disadvantage of this comparison was that the program could take no account of the. relative i.ntensiti.ea of the. lines and so a visual method was used to fJ.nd which was the major mineral phase. The computer program usually found the m:l.neral phases present in the samples but could not place them in the correct order. J&J-0130624 Protected Document--Subject to Protective Order JNJAZ55_000017644 D-8372 Page 93 of 247 543 87 Patterns used as standards from the Italian mine samples and their comparison w~th A.S.T.M. data and against themselves. '· J&J-0130625 JNJAZ55_000017 Protected Document--Subject to Protective Order D-8372 Page 94 of 247 '-'U · SAMPLE SIP l ; •· TALC .',i'•:'ff •. :q._ "•~ 0 Compari:son against A.S.T.M. ; •index: · •l line unmatched, 1.1145 A Patterns not included: 6-263 Muscovite -2Ml, 7-25 Muscovite (IM), 7-32 Muscovite (2Ml), 7-76 Ripidolite (Chlorite), 7-78 ·Thuringite (Chlorite), 7-166 Bavalite lChlorite), 10-183 Peninnite Chlorite, 11-78 Dolomite, B and T Quartz •. Most probable minerals present: Talc Muscovite Calcite Comparison against Italian Standards Patterns not incruded: Chlorite (142), Chlorite (I4), Muscovite (I35), Magnesite (16), Tremolite (Il9/I20)~ Dolomite • . Most probable ~inerals present: Visual comparison Talc, Calcite ,. SAMPLE SIP 2 Talc Minerals detected I ~ . Calcite TALC i, ;; I j, "j1 I Comparison against A.S.T.M. index: 0 2 lines unmatched, 1.1159A l.1353)( Patterns not included: 7-76 Ripodolite (Chlorite), 7-78 Thuringite (Chlorite}, 7-166 Bavalite (Chlorite). Most probable minerals present: !!..!,£, Muscovite, Calcite · Comparison against Italian Standards Patterns not .included: Chlorite (142), Chlorite (14), Tremolite (Il9/I20). Most probable minerals present:!!!!£, Muscov~te, Magneatte. Visual Comparison Talc, Chlorite, Magnesite Minerals Detected Ta·lc, Chlor~te, Magnestte J&J-0130626 JNJAZ55_000017646 Protected Document--Subject to Protective Order D-8372 Page 95 of 247 SAMPtE SIP 3 CBLPRITE Comparison against A.S.T.M. index: 2 lJ.nes unmatched, l.l739R, 0 1.29A Patterns not included: 6-263 Muscovite -2Ml, 7-25 Muscovite (IM) 7-32 Muscovite (2Ml), 7-79 Forsterite (Olivine), 8-479 Magnesite Most probable minerals presant: Chlorite, Talc Compari:son against Italian Standards Patterns not in.e luded: Muscovite (I35), Tremolite (Il9 and I20) Most probable minerals present: Chlorite, Talc. Visua·1· Cornpari:son · Minera·l s Present Ch.lorite, · Talc Chlorite, Talc SAMPLE SIP 4 CHLORITE Comparison against A.S.T.M. index: 3 lines unmatched l.174~, l.13iai, 1.098.oi. Patterns not 1.ncluded: 6-263 Muscovite -2Ml, 7-32 Muscovite {2Ml], 8-479 Magnesite, 11-78 Dolomite, 13-437 Boric Acid • . Most probable minerals present:, Chlorite, Talc Compaiison aqainst Italian Standards Patterns not included: Calcite (134), Magnesite '( 137), Muscovite (135), Tremol1te (Il9/I20}, Dolomite. Most probable mineral present: Chlortte, Talc Visual Comparison Minerals Present Chlori.'te, Talc Chlorite, Talc J&J-0130627 JNJAZ55_000017647 Protected Document--Subject to Protective Order D-8372 Page 96 of 247 46 . ; .! ' tJ ) ; • ,._.____..._.....,,,......__._.. .,.,.,.4J'.i1·iilii-~:....Willii/,,;..w;i..,;j,______...,.. Comparison agai·n ·s't' ~.:s.T.M. indexs Patterns not included: 5-586 Calcite, 7-25 Muscovite (IM), 7-77 Sheridanite (Chlorite), 7-79 Forsterite · (Olivine), 7-166 Bavalite (Chlorite). Most probable minerals present: !!]£, Muscovite, Chlor1te Comparison against Italian Standards Patterns not included: Chlorite (142), Chlorite (I4), Magnes1te(I6), Tremolite (Il9/I20). Most probable minerals present: ~ Vi.sual ·comparis·o n Mi.nerals Present !.!,!£, Chlorite Talc, Chlorite SAMPLE SIP 6 MUSCOVITE Comparison against A.S.T.M. indexs J lines unmatched, l.7999R, l.372~, 1.2741.R. Patterns not included: 3-881 Talc, 7-79 Forsterite (Olivine), 7-166 BavalLte (Chlorite), 7-183 Penninite (CHlorite), 8-479 Magnesite, 11-78 Dolomite, 19-770 Talc. Most.probable minerals present: Muscovite, Chlor1te ~omparison against Ital.ian· Standards Patterns not included: Magnesite (I37), Tremolite (Il9 and I20), Dolomite Most probable minerals present: Visual Comparison Muscovite, Calcite Muscovite, Talc Mineral Present Muscovite, Calc~te - J&J-0130628 JNJAZ55_000017648 Protected Document--Subject to Protective Order D-8372 Page 97 of 247 Sl\MPLE SIP 7 MAGNESITE Comparison against A.S.T.M. Index: Patterns not ,included: l line unmatched 0 1,1092A 5-586 Calcite, 6-263 Muscovite -2Ml, 7-25 Muscovite (IMl, 7-32 Muscovite (2Ml), 7-160 Chlorite (Kotshubeite), 7-76 Ripodolite (Chlorite), 7-78 Thuringite (Chloritel, 7-166 Bavali.te (Chlorite), 10-183 Penninite Chlorite, 13-437 Tremolite. Most probable minerals present: Magnesite, Dolomite, Talc Comparison against Italian Standards Calcite (134), Chlorite (I4) Muscovite (IJS), Tremolite (Il9/I20). Most probable minerals present: Magnesite, Dolomite, Talc Patterns not included: Visual Comparison Minerals Present Talc, Magnesite. Magnes~te, Talc Comparison aga~st A.S.T.M. Indext Patterns not included: 1 line unmatched 0 1.1118A 6-263 Muscovite -2Ml, 7-25 Muscovite (IM), 7-32 Muscovi.te (2Ml), 7-42 Muscovite (3T) , · 7-79 Forster- 1.te (Olivi.ne). Most probable minerals present: Tremolite, Talc, Calcite ·comparison against Italian Standards Patterns not included: Magnesite (137), Chlorite (14), Muscovite (I35). Most probable minerals present: Tremolite, Talc, Calcite Visual Comparison Minerals Pr·e sent Tremolite, Talc Tremolite, Talc J&J-0130629 JNJAZ55_000017649 Protected Document--Subject to Protective Order D-8372 Page 98 of 247 SAMPLE 8 Comparison against A.S.T.M. Index, l line wunatched Patterns not included: 3-881 Talc, 6-263 Muscovite -2Ml, 7-25 Muscovite (IM), 7-32 Muscovite (2Ml), 19-814 Muscovite 2Ml (Vanadian), 7-160 Chlorite (Kotschubeite), 7-79 Forsterite (Olivine), 13-437 Trernolit~, 19-770 Talc. Most probable minerals present: Dolomite, Muscovite Comparison against Italian Standards Patterns not included: Magnesite (I37), Chlorite (I4) Tremolite (Il9/I20). Most probable minerals present: Dolomite, Talc Visual C~mparison Minerals Present Dolom~te, Muscovite, Calci.te Dolomite, Muscovite, Calcite Comparison against A.S.T.M. Index: 3 unmatched lines 0 O . 0 1.2095A, 1.1098A, 1.0926A I. Patterns not included: · 7-160 Chlorite (Rotschubeite), 7-79 Forsterite . (Oliv.ine), 13-437 Tremolite. Most probable minerls present: Calcite, Muscov~te Comparison against Italian Standards Pat.terns not included: Magnesite (16) , Tremol•ite Ul9-I20) • Most probable minerals present: Calcite, Muscovite Visual Comparison Minerals Present Calc.i:te Calcite, Muscovite J&J-0130630 JNJAZ55_000017650 Protected Document--Subject to Protective Order D-8372 Page 99 of 247 549 93 SAMPLE SIP 11 MAGNESITE ·:-.; ,, ~~-, .:.,:-~ :~~:·. Comparison against A.S.T.M. Index: l unmatched line 0 1.1085A Pattern·s · not included: 5-586 Calci.te, 7-25 Muscovi.te (IM), 7-160 Ch.lorite (Kotschubeite), 7-76 Ripidolite {Chl.orite), 7-78 Thuri.ngite (Chlorite), 7-166 Bavalite (Chlorite), 10-183 Penninite Chlorite, B & T Quartz. Most probable minerals present: Magnesite, . Dolomite, Talc . comparison against the Italian Standards Patterns not J.ncluded: Calci.te (I34), Chlorite (I4), Muscovi.te C.Il5}. Most probable minerals present, Magnesite, Dolomite, Talc Visual Comparison Minerals Present Magnesite, Dolomi.te, Talc Magnesite, Talc, Dolomite J&J-0130631 JNJAZ55_000017651 Protected Document--Subject to Protective Order D-8372 Page 100 of 247 94 • 550 I I ' I Examples of Patterns Obtained from Rock Type specimens and Their Major Mineral Content from X-Ray Comparison. J&J-0130632 JNJAZ55_000017652 Protected Document--Subject to Protective Order D-8372 Page 101 of 247 l. SAMPLE ·r1: · -T ALC· FROM FOO'l'WALL' CONTACT 55 -1 I Compari•s on I I l Patterns not included: Magnesite {137), Tremolite (Il9/I20). Most probable minerals present: Chlorite,. Muscovite, Talc, oolomite. • Vi.sual Comparison: .!s.!£. Chlorite. Minerals Present: ~ Calcite Chlorite, Calcite. I SAMPLE 17 MICA SCHIST Comparison Patterns not 1n·c luded: I ··. Magnesite (I37), Talc (146), Tremolite (Il9/I20). Most probable minerals present: Visual Comp·a rison: Muscovite, Talc, Quartz Muscovite, Talc,Ouartz · Mineral·s Present: SAMPLE 112 · Comparison: FOOTWALL SAMPLE? AMPHIBOLITE 3 l.ines unmatched. Patterns n·o t included: 1.2819x 1.22sK Calcite (I34), Magnesi.te (~·3 7), Talc (I46}, Talc (IS), Tremolite (Il9/I20}. Most probable minerals present: Vi.sua1· c ·o mpar1son: 6.4653~ Muscov:1te, Dolomite, owirtz.: Muscovite, Chlor1.te, Quartz · Minera:1·s Present: J&J-0130633 Protected Document--Subject to Protective Order JNJAZ55_000017653 D-8372 Page 102 of 247 SAMPLE Il3 Comparison, INCLUSION SHOWING PASSAGE INTO TALC BOTTOM TRANS'IT 0 1 unmatched line Patterns not included: 1.1541A Magnes~te (137), Muscovite (135), Tremolite (Il9/I20), Dolomite Most probable minex:als present: Chlorite, Talc, Quartz Visual Comparison: Chlorite, Muscovite, Quartz Minerals Present: Chlorite, Muscovite, quartz SAMPLE 115 TALC-FOOTWALL CONTACT Compari.son: Patterns not includeda Magnes~te (I37), Tremolite (Il9/I20). Most probable mi.nerals present: Chlorite, Talc~· Muscovite, Quartz; Visual Comparison: Chlorite, Talc, Minerals Present: Chlorite, Talc, Quartz <,, Quartz J&J-0130634 JNJAZ55_000017654 Protected Document--Subject to Protective Order D-8372 Page 103 of 247 97 SAMPLE Il6 FACE l 553 INCLUSION BELOW SEAM Comparison Patterns· not included: Talc lI45), TrernoU.te {Il9/I20) Dolomite Most probable minerals present: Visual Compar1s·o n: . Minera·1·S' Pre:sent: SAMPLE ·117 Comparison: Muscovite, Chlorite, Calcite, Quartz Chlorite, Muscovite, Calcite, Quartz Chlorite, Muscovite, Calci.te, Quart2 FOOTWALL ROCK SAMPLE 2 unmatched lines 0 6.6957A, 0 1.6305A Patterns not included: Talc (I4i), Chlorite {142), Muscovite {135), Magnesite (I6), Tremolite (119/120), Dolomite. Most probable minerals present: Calcite, Talc,. Quartz Visual Comparison: Calcite, Talc, Quartz Mi.nerals Present: Calcite, Talc, Quartz ·. J&J-013O635 Protected Document--Subject to Protective Order JNJAZ55_000017655 D-8372 Page 104 of 247 rr •)· SAMPLE 120 Comparison: AMPHIBOLE SAMPLE FROM GUIANA LEVEL 1212 1 unmatched line Patterns not included: 0 1.6309A Chlorite (142), Chlorite (I4), Mu~covite lI35), Magnesite (I6), Dolomite. Most probable minerals present: Talc, Tremolite, Calcite, Magnesite. Visual· Compar~sona Talc, Tremolite, Ch.lorite Minera'l's Pr·e ·s ent: !.!]£, Chlorite, Tremoli.te Comparison, 5 unmatched lines 0 0 0 6.3586A, 1.449A, 1.2278A, 1.212&, 1.1s20R. Patt·e rn:s· not included: Calcite (I34) , Tremolite (Il9/I20) Most probable minerals present: Muscovite, Talc, Magnesite, Quartz Visual Comparison: Muscovite, Magnesite, Quartz Mulerals Presents Muscovite, Magnesite, Quart~ J&J-0130636 JNJAZ55_000017656 Protected Document--Subject to Protective Order D-8372 Page 105 of 247 99 SAMPLE I25 LIMESTONE FOOTWALL 555 Comparison Patterns not included: Calcite (I34), Tremolite (Il9/I20). Most probable minerals presents !!!£, Chlorite, Quartz Visual Comparison: ~ . Magnesite, Quartz._ Minerals Present: ~ , Magnesite, Quartz · SAMPLE -r27 LITHOLOGICAL INCLUSION c ·o mparison Patterns not included: Chlor1.te (I42), Chlorite (I4), Tremolite (119/120), Magnes~te (16), Dolomite Most probable minera.1s present: .!!!,£, Calcite, Quartz Visual Comparison: !!.!£, Minerals Present: Talc, Calcite, Quartz . SAMPLE I29 Comparison: Calcite, Quar~z SAMPLE 6 FOOTWALL 2 unmatched lines Patterns not included: 0 1.1526A, 0 6~3031A Calci.te (134), Magnesite (.137)-, Chlorite (Ii}, Talc (IS}. Most· probable miner·a ls present: . Muscovite, Quartz,. Dolom1.te, Talc Visual c·omparison: Minerals Presents Muscovite, · Muscovi.te, Quartz · Quartz J&J-0130637 JNJAZ55_000017657 Protected Document--Subject to Protective Order D-8372 Page 106 of 247 55t 100 SAMPLE I31 BI.ACK INCLUSION 1 unmatched line Patterns not included: Magnesite (137), Talc 115) ,Dolomite · Most· probabl·e m1.n·e ra1s· pre·s ent: Vi:sual.. Comparison I Mu·s covite, Calcite, Talc Mu·scovJ.te, Calcite Muscovite, Calcite . Mi:r1erai-s· ·P resent: SAMPLE I34 0 1.2145A TUNNEL WALL - MARBLE Comparison Patterns not included: 'l're.molite (Il9/I20), Magnesite (16) Most probable minerals present: V1.sual Comparison, Calcite Minerals Present CalcLte Calcite, Musdovite, Talc J&J-0130638 Protected Document--Subject to Protective Order JNJAZ55_000017658 D-8372 Page 107 of 247 101 557 Examples of Patterns Obtained from the Carbonate Specimens and their Major M1.neral Compo- sition Obtained from Comparison with Standards. J&J-0130639 JNJAZ55_000017659 Protected Document--Subject to Protective Order D-8372 Page 108 of 247 102 SAMPLE I4 FACE 10 558 AMPHl.BOLE --~·Comparison: 3 unmatched lines Patterns not included: 0 0 Chlorite (I42), Chlorite (Y4) Dolomite Most probable minerals present: Tremolite, Talc, Magnesite Visual Comparison; !,ili_, Tremolite, Magnesite M:1.ne:ra.1s· Present, ~ , Tremolite, Magnesite SAMPLE I6 0. 1.2586A, 1.0823A, 1.074A QUARTZ Comparison Patterns not included: Calcite {134), Chlorite (I4) Tremolite (Il9/I20) Most· probable m:inerals present: Magnesite, Dolomite, Talc v~sual Comparison, MAGNESITE, Talc Mineral·s Present, Magnesite, 'l'alc J&J-0130640 JNJAZ55_0000176 Protected Document--Subject to Protective Order D-8372 Page 109 of 247 559 103 SAMPLE Ill CARBONATE - TALC INCLUSION .- Comparison: ;· ,. 1 unmatched line Patterns not included: Chlorite (I42), Chlorite (14) Most probable minerals present: Magnesi•te, Dolomite, Talc Visual Comparison: Talc, Magi:iesite,,_Calcite Minerals Present: ~ . Magnesite, Calcite SAMPLE 114 INCLUSION IN TALC SEAM 4 Comparison Patterns not included: Magnesite (I37), Chlorite (14), Muscovite (X35), Tremolite(Il9/I20) Most probable minerals present: Visua·l Comparison: · Mlllerals Present: SAMPLE Il8 FACE 3 !!!£, Dolomite, Talc Dolomite !!,!£, Dolomite MAGNESITE AND TALC Comparison: Patterns not 1.ncluded: Talc (IS),. Tremolite (Il9/I20) · Most probable minerals present: Dolomite, Magnesite, Chlorite Visual comparisons Dolomite, Talc Chlorite Minerals Present: Dolomite, Talc, Chlorite. J&J-0130641 JNJAZ55_000017661 Protected Document--Subject to Protective Order D-8372 Page 110 of 247 104 56( SAMPLE I 19 IMPURITY IN TALC- AND QUARTZ r. .., ..., .. ~ ~ ..... --· .. Compari.son: Patterns· n·o t included: Magnesite (I·3 7) Most probable minerals present: Tremolite, Dolomite, Muscovite, Talc Visual· Comparison, '.!!!.!£, Tremolite, M1nera:1s Presents. !!!£_, Tremolite, Magnesite SAMPLE I2l Magnesite. FACE 2 OCCLUSION (MAGNESITE) c ·o ~par i:5on : Patterns not 1.ncluded: Calcite (134), Chlorite (I4), Muscov1.te (I35), Treinlite (Il9/I20) Most probable minerals present: Dolomite, Magnesite, Talc Visual Cornparisont ~ , Magnesite, Dolomite Minerals Presentz !!!,£, Magnesite, Dolomite J&J-0130642 JNJAZ55_000017662 Protected Document--Subject to Protective Order D-8372 Page 111 of 247 561 105 SAMPLE I22 MAGNESITE« DOLOMITE, TALC Comparison: Patterns not included: Calcite (I34), Talc {145), Talc (I46) Muscovite (135}, Tremolite (Il9/I20), Mos:t probable minerals present: 1 Dol omite, Magnesite, Chlori.te, Talc. Vi:sua1· Co:mparison s .'.!.!!1£, Minerals Present: Talc, Dolomite SAMPLE I:30 Oolomi te. TALC ANO OTHERS Comp·ar:1s·o n: Patt~ns not· includ·ed: Magne:site (137), Talc (15), Tremolite (Il9/I20). Most probabl·e minerals present: Dolomite, Ch.lori.te, Muscovite, Talc. Visuai Comparisons Talc, Chlorite Minerals Presents Talc, Chlorite J&J-013O643 JNJAZ55_000017663 Protected Document--Subject to Protective Order D-8372 Page 112 of 247 106 SAMPLE I35 MASSIVE CARBONATE. END OF WORKING Comparison: Patterns not included: Tremolite (Il9/I20) MO"st· probable minerals present: Muscovite, Magnesite, Ch.lorite Visual Comparison c Magnesi:te, Talc, Chlorite Mutera-1s· Presents Magnes 1 te, Talc , Chlor i te SAMPLE 137 CARBONATE AND TALC Compar t:son Patterns not included: Calcite (I34), Chlor~te (14), Muscovite (135). Most probable minerals present: Magnes~te, Dolomite, Talc Visual Comparison: Magnesite, Talc Miner .-11s Present: Magnesite, Talc J&J-0130644 JNJAZ55_000017664 Protected Document--Subject to Protective Order D-8372 Page 113 of 247 107 563 Examples of Patterns and Major Mi.neral Content of Those Specimens Classified as Talc Typea Of>tabled by · Comparison. J&J-0130645 JNJAZ55_000017665 Protected Document--Subject to Protective Order D-8372 Page 114 of 247 108 SAMPLE I2 SORTING PIECES . Comparison Patterns not included: Tremolite (Il9/I20), Most probable minerals present: Chlor1--t e, Magnesite, Ta1c · W£. Visual Comparison: Chlorite, Minerals Present: Chlorite, Talc SAMPLE 1:3 COLOURED TALC Comparison, Patterns not included: Chlorite (142), Chlorite (14), Muscovite (IJS), Magnesite (I6), Tremolite (Il9/I20), Dolomite. Most probable minerals present: Visual Comparison: Minerals present: J&J-0130646 JNJAZ55_000017666 Protected Document--Subject to Protective Order D-8372 Page 115 of 247 56 109 SAMPLE IS Compari.son: GENERAL ORE 2 unmatched lines Patterns not included: 18.11572 0 7 .0073A Chlorite (I42), Chlorite (14), Muscovite {I35), Do~omite. Most probable minerals present: !21£., ~gnesi.te Visual Comparisons Minerals presents SAMPLE I8 MASSIVE TALC Comparison Patterns not included: MagnesLte (16), Tremolite (Il9/I20). Most probable minerals present: !.!!,£, Chlorite VLsual Comparison; Talc, Chlorite Minerals Present: !!,!£, Chlorite J&J-0130647 ; JNJAZ55_000017667 I 'Protected Document--Subject to Protective Order D-8372 Page 116 of 247 566 110 SAMPLE 19 FACE 1 GREY TALC Comparison Patterns not included: Calcite (I34.), Magnesite (I37), Muscovi.te (I35), Magnesite {16), Tremolite (Il9/I20);. Most probable minerals present: ~ , , Chlori.te Visible -comparison: ~ , Chlorite Minerals Present: !!!!.£_, Chlorite SAMPLE IlO GRANULAR TALC Comparison Patterns not i.ncluded: Calcite {134), Magnesite (I37), Ch.J,.orite (142) Chlorite {I4), Muscovite (135}, Magnesite {I6) Tremolite (Il9/I20) Most probable mi.nerals present: Talc, Dolomite v1·s ible compari.sont !!!£,, Dol~ite Minerals Present, E,!£, Dolomite J&J--0130648 JNJAZ55_000017668 Protected Document--Subject to Protective Order D-8372 Page 117 of 247 567 111 SAMPLE I24 TALC ·FACE 2 l Comparison: Patterns not 1.ncluded: Muscovite (I35), Magnesite (16). Most probable minerals present: Tremolite (119/120) Talc, Chlorite, Dolomite, Mag-nesi.te Visual Comparison: ·oolornite, Magnesite, Talc MLnerals Present: . Dolomite, Magnesite, Talc SAMPLE 126 TALC INCLUSIONS Compar J.son Patterns not included: Calcite (134), Tremolite (119/120) Most probable minerals present: Talc 1 Chlo~ite, Dolomite Visual Comparison: !!.!£,,' Ch.lorite Minerals Present: Talc, Cnlorite J&J-0130649 JNJAZ55_000017669 Protected Document--Subject to Protective Order D-8372 Page 118 of 247 568 112 Comparison Patterns not included: Muscovite (IJS), Tremolite (Il9/I20) Magnesite (I6), Dolomite Most probable mLnerals presents Chlorite, Talc, Quartz V~sual Comparisons Chlorite, Talc,Quartz Minerals Present: Chlorite, Talc, Quartz SAMPLE 132 OCCLUSION FACE 2 ·· .. 'f-.J.' . 1 , . ...1 '1 ~ r·~ -.. ~~ .- . · ,,. , I Compari.son Patterns not included: Muscovite (I35), Dolomite Most probable minerals present: TremoU.te (119/120) Chlorite, Talc, Magnesite VLsual Comparison: Chlorite, Talc Mi.nerals Present: Chlorite, Talc J&J-0130650 JNJAZ55_000017670 Protected Document--Subject to Protective Order D-8372 Page 119 of 247 569 113 SAMPLE 133 TALC END OF WORKING Comparison: Patterns not included: Muscovite {I 35), Tremoli.te Most probable minerals present: Talc, Chlorite, Magnesite Dolomite . Visual· Comparison: Talc, Chlorite, MagnesJ.te Miner'a ls Present, Talc, Ch.1orite, Magnes~te SAMPLE I36· Comparison: GREY TALC comparison: M.ine:rals Presents Comparison: 0 1.1517A Calcite (134),. Talc (I46) Tremolite (Il9/I20). Most probable minerals present: SAMPLE I38 0 1.2204AJ 2 unmatched lines Patterns not included: Visual (Il9/J:20) Cnlorite,- Muscovite, Talc Chlorite, Talc Chlorite, Talc TALC AND PYRITE 0 1.041A 1 unmatched line Patterns not included: Chlorite (I42), Chlorite (I4),Muscovite (I35), Tremolite (119/120) Most probable minerals present: Talc, Calcite V:lsual Compari.sonz Talc, Calcite Minerals Present: Talc, Calci.te J&J-013O651 JNJAZ55_000017671 Protected Document--Subject to Protective Order D-8372 Page 120 of 247 114 SAMPLE I39 sro S-'O' FROM CRUSHER Cornpar ison Patterns n·o t included: Muscovite, (IJS), Tremoli.te (119/:120). Magnesite (16). Most probable minerals present: · ~ Chlori.te VLs ual c-ompar·1·son: Talc, Ch.lorite, Calcite Mineral:s · P-r esent :. Talc, Chlorite, Calci.te _SAMPLE I40 PLATEY TALC Comparison: Patterns not i.ncluded: Tremolite (rl9/I20) Most probable minerals· present: Visual· Compa•r ison: Ta·lc, Magnesite, Chl.orite Talc, Chlorite,,Magnesite Talc, Chlorite,. Magnesite SAMPLE I41 · GOOD SPECIMEN No.2. Compar:ison: Patterns not .included: Calcite {I341 ·, Muscovite {135), Tremolite (119/120), Magnesite (16), Dolomite Most probable minerals present: !!!£, V:isual Comparison: Talc, Chlorite Mi.ner-a1s Present: Talc, Cb.lorite Chlorite J&J-0130652 Protected Document--Subject to Protective Order JNJAZ55_000017672 D-8372 Page 121 of 247 571 115 SAMPLE r4·2 COLOURED. TALC No. l. Comparison Patterns not included: Magnesite (I37), Talc (146), Muscov1.te (135), Dolomite. Ch.lorite, Talc . Most probable- minerals present: Visual Comparison: Chlorite, Talc Mi.nerals Present• Chlorite, 'l'alc . SAMPLE I43 - FIBROUS TALC FACE 10 -~:'\I',' ~"ii'\,,"""'I"..... .,. , '-:l\ )~\\\i} \, i. ,! •' . '. • 0 Comparison, 2 unmatched lines Patterns no·t 1n·c 1uded: '. . ' • . ·I J.>, ;. ·: · : . · .i:... .,, } t I 1:;1,.0.l I , 1.. : ,: f j ': . I i :: f,$., , : : I l !1 'j :1 J /·I . .. .J It fl •..: " : , , i;fa O 4.8928A, 4.4431A Calcite (134), Magnesite (137), Muscovite (135), Tremolite (Il9/I20) Most probable minerals Present: Chlori•t e, Talc Visual Compari·s on 1 Chlori•t e, • Talc Minerals Presents - Chlorite, Talc: J&J-0130653 Protected Document--Subject to Protective Order JNJAZ55_000017673 D-8372 Page 122 of 247 116 SAMPLE 144 FACE 1 PURE TALC Comparison: ,- 72 J, l unmatched line Patterns not includ·e d: 1.0798 Magnesite (137), Talc (I42)-, Muscovite (135), Tremlite (119/120) Most probable minerals present: Chlorite, Talc, Dolomite Visual Compari.sons Talc, Magnesite, Chlorite Minerals Present: Talc, Magnesite, Chlorite SAMPLE ·I45· GOOD SPECIMEN FACE 1 ;: -· J ... - J -. ~ • ii ·,_ 0 Comparison: 0 1.0882A, ·l.OSOSA 2 unmatched lines Patterns· not· ·1·n cluded: Calcite (134), Chlorite (r42), Chlorite (I4) Muscovite {I35}, Magnesite (I6), Tremolite (Il9/I20), Dolomite. Most probabh~ minerals present: V.isual· Comp·a r:isons Talc M.inerals Present: Talc SAMPLE ·x46· COLOURED TALC ~ , ' Magnes.ite FACE 3 ® ,. Compa:r :ison: Patterns not inc1udedt Chlorite (142), Chlorite (14), Musco~J.te (I35), Tremolite {Il9/I20). Most probable minerale present: '.!!!.!£, V~sual Comparison: Talc, Magnesite M:l.nerals Present: Talc, Magnesite Magnesite J&J-0130654 JNJAZ55_000017674 Protected Document--Subject to Protective Order D-8372 Page 123 of 247 117 573 Spec:tmeri Patterns and Coinpari:.son· Data for· samp1es of Old Powders and HJ~ Shipments I -1 J&J-013O655 JNJAZ55_000017675 Protected Document--Subject to Protective Order D-8372 Page 124 of 247 574 118 I • SAMPLE POWDER Fl BATCH 6 PW.J. 035 1 unmatched li.ne Comparison: 8.197~ Muscovite (135), Patterns not included: Most probable m1n·er·a ,1s present: Tremolite {Il9/l20) Talc. Magnesite, 'Chlorite Visual· Compar is·o n; Talc, Chlorite, Magnesite Mineral·s: Present: Talc, Chl.orite, Magnesite SAMPLE BATCH 8 POWDER {S and G} PW.J. 035 Compar1.son Magnesite (16), _Tremol~te lI19/I20} Patterns not included: Most probable· minerals pr·e sent: · !!!!£_, Magnes:l.te, Boric Acid · Visual=Compar·:1:s·o nr Mine.r·a i:s Pres·e nti Talc, Chlorite, Boric Aci.d Talc, Chlor1te, Bori.c Ac.ld SAMPLE BATCH 9 . POWDER T4 Comparison: P.W.J. 035 1 unmatched line Patterns not included: 0 l. 2587A Tremolite (119/120) Most probable minerals present: Talc, Chlorite, muscovite, Magnesite, Boric Acid Visual Comparison: Talc, Chlorite, Boric Acld Minerals Pr·e sent 1 Talc, Chlorite, Bor~c Ac~d J&J-0130656 JNJAZ55_000017676 'Protected Document--Subject to Protective Order D-8372 Page 125 of 247 119 SAMPLE BATCH 10 57: POWDER SKlBP PW.J. 035 Compari.son Patterns not included: Calcite (134), Muscovite (I35), Tremolite tI19/I20}, Dolomite Most probable minerals present: Talc, Chlorite, Magnesite, Boric Acid. V1.sua:i .compar 1·s on i Talc, Chlori te, Boric Acid Minera·ls p:r e:sentr Talc, Chlorite, Boric Acid SAMPLE BATCH 11 Comparison: POWDER LD18P 1 unmatched line Patterns not included: SAMPLE ·BATCH 12 Comparison, 8.1363.R Magnesite (16), Tremolite (Il9/I20) Dolomite Most probable minerals present: Visual· Comparison: Minerals Presenti PW.J. 035 Ta·1c', Chlorite, Boric Acid Talc, Chlorite, Boric-Aci.d, Magnesite Talc, 'Chlorite, Boric: Acid, Magnesite TALC 1960 PW.J. 025 1 unmatched line Patt·e rns n·e >t -included: · 8.12 0 A Tremolite {119/120) Visual Comparisoni Ta·1c, muscovite, chlor 1.te, Boric Acid. Talc, Chlorite, Boric Acid, Magnesite Minera·ls Present: Talc, Chlorite, Boric Acid, Magnesi.te Most prob°a'b l'e minera·ls present: J&J-0130657 JNJAZ55_000017677 Protected Document--Subject to Protective Order D-8372 Page 126 of 247 576 120 SAMPLE BATCH 13 TALC 1961 PW.J. 026 Comparison Pattern·s not included: Calcite {134), Muscovi.te U35) Tremolite (Il9/I20} · Most: probable roi:n:erals present: . Talc, Chlorite, Magnesite Boric Acid Visual Comparisons Talc, Chlorite, Magpesite, Bori.c Acid MJ..:nerals· Present: Talc, Chlorite, Magnesite, Bori.c Acid SAMPLE BATCH 19 S.S. CATHERINA W. 02/05/72 Comparison Patterns r1ot 1.ncluded: Tremolite (119/120) Most probable minerals present: Talc, Chlorite, Magnesite Visua:1. compar1.·son1 Talc, Cnlorite, Magnesite Minerals Present: Talc,. Chlorite, Magnesite SAMPLE BATCH 2 TALC S.S. EDNA 'B' 14/02/72 Comparison Patterns not i.ncluded: · Talc (.I45), Tremolite (:Il9/J:20) Most probable mi:nerals present: ·. ~ , Visua:1: Comparison: ~ , Chlor:Lte M~nerale Present: Talc, Chlorite Chlorite J&J-0130658 JNJAZ55_000017678 Protected Document--Subject to Protective Order D-8372 Page 127 of 247 121 577 CONCLUSIONS The optic~l examination has shown that there are a large number minerals associated with the rock types found both in the talc seam and in the associated rocks. The footwall rocks in contact with the talc are mainly composed of the minerals quartz, muscovite, chlorite, garnet, and some carbonate material both calcite and magnesite. Minor minerals in the footwall contact rocks include epidote, microcline, tremolite and actinolLte, sphene, rutile, hornblende, rare talc, biotite, pyrite, pyrrhotite and chalcopyrite. Rock type inclusions into the talc have similar compositions to the footwall rocks but with higher muscovite and chlorite contents. The muscovite was generally an iron rich variety (phengite}, whi.le two forms of chlorite were observed narnely sneridanite and penninite. Other talc inclusions consist mainly of carbonate minerals, calcite and magnesite in varying quantities. It is wi.tn these nodules that some tremolite is found. The rocks £urther away from the ta1c seams, namely th.e gnei.ss, become richer i.n quartz .. and mi.crocline and below these marble occurs. of .I The carbonate specimens examined by optical means showed that the carbonate minerals, calcite and magnesite, were accompanied by talc, chl.or~te, tremolite, muscovite, rutile and pyrite, all in minor amounts. In general the carbonate inclusions were large and · very discrete in the talc seam itself. The specimens examined, whi.ch can be classified as talc samples, were found to be in the main composed of talc with chlorite as the major contaminant. Some specimens, however, were predominantly composed of chlori.te with minor talc i.nclusions. Other minerals found in association wit~ the talc specimens included garnet, rutile and magnesite with rare tremolite and· a quartz or serpentine inclusion. some differences were observed i.n the talc itself, some of the talc appearing to be a little murky in texture. X-ray pictures of the clear and murky material showed no differences however. . ' I The powder X-ray examination confirmed the major minerals occurring in the hand specimens and a classification was possible into the three groups already mentioned, i.e. rock types, carbonate samples and talc specimens. The only asbestos type mineral to be detected in the hand samples was tremolite, which was found in three of the specimens. The tremolite was associated with carbonate minerals, namely magnesite and calcite, no tremolite was detected in the talc type specimens. Ch.lorite was, however, very common m the talc types, some of the specimens being very neariy pure chlorite in compos1.tion. There appeared to be some association of the ch.lor1.te with coloured talc specimens, especially those with a greyish colour. Other colour. var~atLons due to rutLle were not detected by x-rayce-umin~tion • J&J-0130659 Protected Document--Subject to Protective Order JNJAZ55_000017679 D-8372 Page 128 of 247 578 122 The examination of consecutive samples at face 1 in the mine showed that the chlorite content can vary very drastically over a 6ft thick section of the talc seam. Patterns obtained from several shipments of~~~~ talc showed that chlorite, together with carbonate material, were the major contaminant minerals. This was also true of powder samples ranging back to 1949 in which the only observable difference was the presence of boric acid. The electron microscope examination of the powdered samples showed that a difference could be drawn between particles produced from the various samples. The carbonates and rock types on the whole produced compact fibre free particles. The talc specimens were, however, platelike in appearance with varying quantities of lath. like particles coupled with fibres which were textile in appearance. Both lath and textile types of particles were not composed of minerals associated witn the commercial asbestos industry. Particles formed from the amphibole mineral found at tha mine we.re hardly fibrous in character, the majority of the tremolite breaking to _give compact particles. Those fibres formed were short and had a very large diameter when compared wi:.tl'l:. the commercial varieties of asbestos. No amphtbole or chrysotile mineral was detected in any . of the numerous powders exam:l.ned. The Italian talc~¢~¢~ contains observable quantities of chlorite and carbonate minerals and could contain any one of the following m1.nerals in very minor amounts: muscovite, quartz; tremolite, garnet and rutile. :rf small pieces of footwall rock were to contaminate the ore during production, several of the other listed minerals found in the rock type specimens could appear in the shipped product. It is. unlikely that they would be present in detectable amounts.• F.D. POOLEY Project Supervisor J&J-013O660 ! 0 Protected Document--Subject to Protective Order JNJAZ55_000017680 D-8372 Page 129 of 247 ·) ' J&J-0130661 JNJAZ55_000017681 Protected Document--Subject to Protective Order D-8372 Page 130 of 247 ~111 confidence J&J-0130662 JNJAZ55_000017682 I Protected Document--Subject to Protective Order D-8372 Page 131 of 247 .AERE-G63 COM;,IBRCIAL IN· CONFIDENCE The Morpholoey and Characterization of Talc B. W. Mott Solid State Instruments Croup, Materials Development Division_ Buildif18 393,. _ . A.E.R.E., Harwell. . . · ~ August, i-972 J&J-0130663 JNJAZ55_000017683 Protected Document--Subject to Protective Order D-8372 Page 132 of 247 581 Synopsis Samples of. ta.le submitted by Johnson and Johnson Ltd. have be~n examined by a number of phy.sical techniques to cha..ra.cteri ze the powder and i dentify any · impurities. Examination in both the scanning electron micro scope and the transmission electron microscope ·suggested the possible presence Qf a few rod-shaped particles as well as the normal platelets but non-dispersive analysis of the X-ray spectra and- electron diffraction failed to differentiate bet?reen the particles. X-ray powder. diffraction data .suggested the presence of a material other than talc in amounts l~sa than · 1%. - The extra diffraction peaks ·could not be accounted for completely by published data in. the Powqer Diffraction File and the most satisfactQry oonclusion was_ that the bulk: .of the . impurities were present as Bavalite. -s·~~//4.s··: ~jf-~-:-1 /ti- /1 . E .R . P- - .1---J~- J&J-013O664 JNJAZ55_000017684 Protected Document--Subject to Protective Order D-8372 Page 133 of 247 582 Contents 1• · Introduction 2. Optical . microscop_y 3. Scar.ning ~_lectron microscopy 4. 5. o·f 3.1 Preparation 3.2 Topographical examination . sample 3.3 Chemical analysis using non-dis_persive techniques Trw1Smission electron microscopy 4.1 Prepe.ra·tion of. sample 4. 2 Morphology 4.3 Electron.· di.ffraction X-ray diffraction 5.1 5.2 Er.perim~nt~l Attempts to identify add.i tional ·r eflections 6• . Electro~ microp~be analysis 7. Discussion 8. · Conclusfons 9. ·Acknowledgements Table I X-r~y powder Diffraction data . ·Figure 1· Scanning: ~lectron mi:crogr~ph X 500 Figure 2 S_cannif18 electron micrograph X 500 Figure 3 Scanning -electron micrograph X 10.,000 Figure 4 Transmission electron micrograph x 10 1 000 . Figure 5 Electron m.icro·probe· scan for calcium Figure 6. Electron microprobe scan for a.1..uminium in same area as f'or Figure 5 J&J-0130665 JNJAZ55_000017685 Protected Document--Subject to Protective Order D-8372 Page 134 of 247 583 1• . Introduction Samples of comm~~ially processed -talc (magnesium silicate) from their Italian source were received· fro _m Johnson and Johnson Ltd • .for a thorough characterization together Ni.th identification ot' any natural impurities. After prelir:1inary X-ray ·diffraction .studies had s:ugge.sted that material other than talc wo.s present e.t.the · sub-1%level, samples of: chlorite bedrock and magnesite inclusfons taken from the Italian min~- _w ere · supplied as aids to identification. . The various physic.al methods of ~xamination used were optical microscopy, scan_ning _elec_tron .microscopy incl~ding non.:..dispersive·· analy:lis., transmission elec~ron. microscopy, electron _diffraction, X-ray powder ·di.ffraction techniques and electron .nic.r oprobe . analysis._. 2. Optical Microscopy A sample: o_t: the p_mvder was lightly dusted on to ·a glass .s:J:.ide and. examined under low power . binoculars and in a .metallurgical microscope. As expected, the majority of the p~·rticles were plat~--l ike _but a :few. were observed in the form of rods or ·needles. . . . In contrast to the majority of the particles which had a wh:itish lustre, a few were observed witn a light green tinge. However, the . particle size was too small for adequate l,"esolution optically and it was clearly necessary to resort to electron microscopy to characterize the· particles satisfactorily. Scanning Electron Microscopy 3.1 Preparation ot' Sample Some powder was dusted on to a specimen stub that had been coated with a colloid~l suspension of' graphite in alcohol. This gave _a thin layer particles without the formation of large aggl.ommerates. or A conducting layer of carbon was subsequently deposited by evaporation on the particles. 3.2 Topographical exacdnation Examination in the Stereoscan at magnifications up to about x 10,000 generally confirmed_the results of the optical work. Platelets were predominantly present in various orientations and some needle-lilce · conf'iguratio.ns were cl_early accounted f.'or_ by plates which were vie1!'ed in an 'edge-on' positi?n and this was con:firrned by taldng stereographic photographs. _ Typ~cal· structures obtained are illustrated in Figures 1, 2 and 3. 3.3 Chemical. · analysi-s . using Non-Disoersive Techniques ~on-disp~rsi~e X-ray ·anslysis was carried out on a number of particles using a lithi~m drifted silicon - solid .state detector. • No significant - 1 J&J-0130666 JNJAZ55_000017686 Protected Document--Subject to Protective Order D-8372 Page 135 of 247 r - . .. Ju,. variation was found in relative i~tensi.ty of the ~ilicon and magnesiun . . ~haracteristic ~~ission5 suggesting that they· w_e re all of similar relative composition. This_ does not, however, prove 'that all the particles analysed were talc for the following reasons: - i) there.· is no .guarantee that all the X-ray emission measured was from an individua.i. platelet and ii) it does not exclude the presence of an impurity of similar magnesium/aluminium ratio to that of talc. The X-ray spectra obta~ned did not show significant emissions of other metallic elements indicating the absence of- any major impurity. 4. Transmission electron microscopy 4.1 Prenaration of sample An equal 'volume of talc powder and a solution or 15% nitrocellulose in weyl acetate was rubbed on to · a glass plate with a. spatula. This aliquot was then diluted \vith acetone and spread over a clean microscope slide The dried film ,vas sc_o red into . )IMl ,: iquare sections which were to dry. floated off the slide grid. on to water and picked up with an electron microscope Af'ter drying off on a filter paper, a supporting film was then This yielded a nitro·cellu1ose film in which evaporated over the :iurface. the talc platelets were encap:iulated with their p1anes lyine; generally in that of the film to preclude 'edge-on' effects. 4.2 Morphology The platelets in the film were examined in an 'EM300 transmission microscope at magnifications of up to x 80,000. This revealed that the rod-shaped ~articles which were about 250 x ·di~eter and varie~ in le~gth . up to . o.15mµ, coUld have been platelets which had folded or roiled up, but this was not positively conf'irmed (see fiBure 4) ·• . 4.3 Electron diffraction Electron diffraction patterns were obtained in situ in the microscope from a . number of particles with both types of appearance but no real evidence was obtained of a . ·s tructural difference bet.ween the plates and "rods". Two d.i_f fraotion patterns showed evidence 01' preferred orientation but this was to l expected f'rom their nature and was not considered to be indicative of.' any chemical difference between the two particles. · It must be noted, however, . . :· that al thougl') the method _o:f _preparing the sample for examination had been -chosen to separate t _h e particl~.s as much as possible, there wa_s '. difficulty in guaranteeing that completely isolated particles had been selected for diffraction •. .. . J&J-0130667 JNJAZ55_000017687 Protected Document--Subject to Protective Order D-8372 Page 136 of 247 585 • I I I 5·. X-ray diffraction 5.1 Experimenh.l· Some .of the powder was packed in silica. capillary tubes for both X-ray ·,e!r dif'fraction patterns a.nd dif'fractometer- traces. The results showed · nee of preferred orientation and this was probably due to the platelets .;ning ther.iselves in the silica tube whe_n tapped in the usual way to concentrate them in the bottom portion. Patterns were obtained f'rom two completely . different batches of talo sup_plied by the firm and also frora tw? mineral samples said to be Magnesite and Chlorite, although the latt"er was subseque~tly discovered to _· .b e Muscavite, a. micaceous mineral. The same reflections were obtained from both talc samples but some . . . differences ·,yere observed in the relatl.\Te int'ensities of some reflections. Since some preferred orientation was evident in both patterns, these intensity differences were most like~y due to . slight variations in the type · · and/or degree of preferred orientatio~ o·-r the platelets in the two ·samples. The overall conclusion was that the iwo talc samples were identical. in nature and that a.ny impurity was due_ to· the same coinpound or compounds. The first sixty six reflections from the p·atterns were selected f'or . . . identification and the calculated d-spacings are li~ted in Table I. Of these, all but 27 were satisfactoriiy accounted for by the available data on talc published in the Powder Diffraction File. This strongly suggested that an impurity ,vas present to an extent judged to be below the 1% level. The strongest 'reflections from the samples of r.fagne site and Muscavi te were absent in our talc patterns so that neither cou1d· reasonably account for the impurity reflections. A check was ma.de of the possibility . that 'the im~urity was Tremolite but none of the extra reflections agreed ·wi.th the published data for this mineral. There are a wide range o:r minerals in the Chlorite group which is a distinct possibility as an impurity since their crystal st_r ucture is related to that o~ talc and brucite. X-ray diffraction data have been_ published on five varieties and these ·were checked with the talc · patters. In the case of' Bavalite (a variety of Daphnite), it was found that. 24 of our 66 reflections could be accounted for by this :fonn of Chlori te, al though 16 of these were also included in the published da.ta . t'or ta.le. Bavalite can contain traces o~ alkaline earths, copper, ·titanium or ·manganese but the· sample from which the X-ray data were obtained was re~e>;t,e d_:t~ be (Mg0 ~4 Fe 4 _2.Al.1 ~ )(s1 2 • 6Al 1 _1.) 5 01 o.2(oH)7.a• - ._ ~ J&J-0130668 JNJAZ55_000017688 Protected Document--Subject to Protective Order D-8372 Page 137 of 247 586 5.2 Attempts to identify additional reflections In attem~t~ to prove or disprove that the extra 27 refl~ctions • were all accounted for oy a small percentage of impurity, approaches were investigated. a number of A thorough ·computer search of the Powder Diffraction File was made to list possible compounds i-rhich could account for t~a unidentified reflections. Of a whole variety · of possibilities .. including both inorganic and· organic compounds·, the only .three which appeared at all possible were Be.valite, potassium dizirconate K zr o 2 2 5 · and calcium aluminium oxide hydrate, ca.A1 o .10H o. In the case of' 2 2 4 the dizirconate, the talc patterns account for only two low angle lines of mediwu · ~ntensity" a.nd other stronger li.nes are not present. The two strongest lines o-f' the calcium compound ._could be accounted for by two low angle lines in ou~ patterns plus . two others at higher angles {where talc reflections also occur) but · that: wo_uld still leave eleven lines unidentified. _ On . the basis of published ,X-ray data therefore, Bavalite appeared to be the most likely impurity~ Since both the talc patterns were consistent with some preferred .·orientation being present in the powder samples, _i t was considered that some ~ . . of the extra reflections might have been due to enhancement of very weak reflections from t 'a.lc which would . not be observed i.n the standard pattern from -a perfectly random sampie. .. . - A computer calculati.o n was made of all possible reflections from talc assuming that the published -crystal structure was correct and c_:>n i"~is basi~, a further. 16_ of the 27 unknown reflections in the tal.c r>atterns could be . satisfactorily . indexed. 6. Electron Microprobe Analysis · -As the X-ray diffraction dat_a strongl,r suggested. the presence of an impurity which could not be . identi:fied unambiguou~ly as Baval_i te, a limited amount of elect"ron microprobe analysis was considered worthwhile. this . instrument fo~ det~cting impurity eleme~ts is The sensitivity of significantly better than that of' ·the scanning . electron microscope a.~d these · could have been missed in the work described in · Section J.3.- The seven elements selected a.s being most representative ·or the likely :impurity materials aluminium, .iron and chz:omium. varieties or· Ghlorite ·were were· fluorine, potassium, calcium, nickel, - The last four of these might be expected if some present, calcium -f'or Tremolite, calcium and iron for Actinolite and calciuui, fluorine · and potassium_for Apophyllite. The presence of iron and aluminium would substantiate ~he possibility of Bava.lite. - 4- J&J-0130669 JNJAZ55_000017689 Protected Document--Subject to Protective Order D-8372 Page 138 of 247 587 A sample of the talc was sprinkled on a ba.keli te di$C to give as even a. layer as possible and a search was made for each of the seven elements listed. Although the level of· t"he characteristic X-rays for iron wo.:1 very olo.se to that of the background~ there wa5 a possibility that iron was present in a very low concentration throu_ghout the sample. A few discrete areas were found in which calcium and aluminium were detected together a.s shown in Figures 5 and 6 but the ?rigin of the characteristic X-rays from these t\'IO elements could not be ·traced to individua1 ·: pe.rticles as the lateral and depth resolution of the e ·l ectro.n beam was muc·h greater than the average ·particle :iize. None of the • elements· f'luorine.,_ potassi~, nickel and chromium were present at the level of sensitivity which was about _100 ppm • . The results were therefore inconclusive al though riot inc orisi ~tent with . the pos si bili ty that Bavali te ,,as the major impurity. 7. Discussion The main avidence t'or the presence ot' an impurity· in the talc samples comes -from the X-ray dif'fracti.on data which st:io~s some 27 reflections in addition to those. inch~ded ..in -.t~e published ini'ormation. Just over half ot' these extra reflections .can be accou~ted ·t'or by assuming that some weak ref'lections, not normall . . ot: signif'i.c ance £o·r a : randomly oriented sample, · a.~ enhanced due to preferential type of pa~ldng the flakes in the· silica tube. . . T~s still leaves some ref'lections ' completely unaccoun~ed t'or by_ . talc, the strongest ~r which agreed with the ·published: data for Bavalite. This minerai° is said to occur in the .form · of' sheets and to be greenish in ·colour which would b·e consistent with the observations in the optical mic-~ scope-. . Since neither the transmission or scanning electron microscopy was able to distinguish between the rod like particles and the platelets, it 5ee~s probable that th~se were folded platelets as postulated. The limited electron microprobe anal.ysis carried out indicated that calcium and aluminium occurred together also present. at th~ impurity·level ·in the powder and that traces of iron were This ~ould also be consistent with the presence or a small concentration of Ba.valite -if some of the magnesium were replaced by calcium as is known to occu-~ in · s·ome varieties. Other pos_si ble _explanations of the extra reflections in our X..;.ra.y powder diffractio~- data .are (a) .that the published data on _m ineral ' talc is _incomplete or (b) that smal·l concentrations of impurities such as calcium and alumin:i~ are present in·tbe talc and gfve rise to the additional lines by slightly modifying the crystal s.tructure •. . . Neither: explanation . seems acceptable and the possibility of ' B_a val.ite · being present in a.n amount less than 1%· appears more likely . and to fi _t all the observations. - 5J&J-0130670 JNJAZ55_000017690 Protected Document--Subject to Protective Order D-8372 Page 139 of 247 .. 8. 588 . Conclusions The· two ·· sampies -of talc examin_ed are essen~ially the same and contain a common impurity _present in an· amount less than 1%. The extra reflections in the X-ray ·powder pattern not accounted for by talc are consistent with the impurity being one fox:m of Chlorite known as Bavalite. 9. Ackn0\7le dgeme nt s · The woz:k: repQ~ted was carried out by various members of the Solid State Instruments Group whose suggestions and comr.1ents are greatly appreciated. Ci rculation Messrs. Johnson arid Johnson Ltd. Commercial Office A.E.R.E. Library Mr. B~ . W. Mott (5 · copies) J&J-0130671 JNJAZ55_000017691 Protected Document--Subject to Protective Order D-8372 Page 140 of 247 Table I c· ... •• .,,. •• 0-0 •• .. • • 0 • • • • •• • • • 5o) .' .X-Ray Powder Diffraction Data Data from Diffractometer Data from Powder Diffra~tion 'i'ra.oe File P.D.F. 19-770 P.D.F. 7-166 d spacings . ~observedl Intensity ~ of stronsest 13.9846 13" 9~3585 100 8.6130 . 8.1539 7.4367 31 7 7.0418 44 . 1 d ~ 9.35 Ba.valite I d I 1 i...o 60 100 2· · 6.5298 . 4.6756 . 7.08 84 . 4-5428 . /» 3218 11 8 4.67 4.56 4-. 33 25 · 30 _ 6 4.2462 1 4.1235 3 4.12 · 6 3..8750 1 3.67 2 3.5366 49 J.52 < 2 3.4386 . 3.3337_. · 3.2867 3.2456 3-1921 3.11 25 2.8883 2.8330 2.7993 2.7279 2.6254 2.5887 2.5321 2.4747 ' 3 .36 ,:_· · 3.12 40 L . 3. 4.681- 8 100 .. . 3.523 50 2.821 10 2.6-\9 ._ 30 • 4. 20 . 89 ·_37 18 . . 1 4 2 : 2.4200 2.3394 2.2769 2.2116 2.1910 2.0987 2.0668 ·, :'. :51 10 . 2 . 36 . 2.627 . ?.589 2~479 8 .. 14 30 · . 2.337 · 2.289 2.219 2.188 " 2 . 1 2.086 2 1 2.011 2 1 3 3 2 6 _2.574 . 20 2.469 10 2 .405 · 20 2.279 10 2 J&J-0130672 JNJAZ55_000017692 Protected Document--Subject to Protective Order D-8372 Page 141 of 247 C • • • • • •• •• •• •• Data from Diffraotometer Traoe d spacings Intensity tobserved} ~ of stron~est 2.0281 17 . 1.9997 1.9786 1 1.9179 · 1.8697 1 1 Data from Powder Diffraction File: P.D.F. 7-166 P.D.F. 19-770 ·. d ~ 1..967 1.921 ·1.870 71. ,. Bavalite d I I 2.011,. 2Q 1 .893 5 2 2 4- 1.·0173 1 ~7857 1.7338 1 .6879 1 1.828 ·5 1 1.765 .5 1. 722 5 1 •.6715 1.6529 1.5777 1 .5573 1.5418 · 1.5268 1.4764 1.1+650 1 ·~4473 8 2 · · 1 .684 7-. ·1.668 ·1.654 4 1. 10 6 6 ) 2 ) 1.666 2 1 .558 . 1.540 -< 2 1_.529 •· 55 1. 4 5 (: .. .56 ~ ~1\.560 1.523 1 ;483 · 1 20 10 , ,5 . 2 2 1.4338 1.4145 1·.3958 1. 731 590 1.427 5 4 1 .4.11 . 1.386 4 1.)93 5 5 :-· 1.376 -· 2 · . · 1 • .339 5 1.228 5 5 : 12 1.3858 12' ~3354 1.3179 48 1 -:294-5 1.?500 · 1.2411 2 1 1· .·2383 1.2230 1.1828 1.1688 ·· 1.411 . 7 .1 -1 •.n6 . 2 _. .1.318 . ·a · 1.295 10· 1 1.255 2 2 1.243 . 1~233 · ·2 .·6 1 ·10 ,• . .2 .2 1 .219 · < 2 ,._ .1 .187 . . -., ~_169· 2 • Accountable on .ooinpu:ter-cal.culated pattern for TALC •• Unaccountabl.e on basis of TALC N.B. Ca1culated TA,LC pattern did not erlend bel.o• d c ·1 .600 - 2 - J&J-0130673 JNJAZ55_000017693 Protected Document--Subject to Protective Order D-8372 Page 142 of 247 FIGURE 1. Scanning Electron Micrograph :z FIGURE 2. Scanning ~lectron Micrograph x 500 500 J&J-013O67 4 Protected Document--Subject to Protective Order JNJAZ55_000017694 D-8372 Page 143 of 247 f!!' .. FIGURE 3. Scanning Electr~n Micrograph X FIGURE 4. Transmission Electron Micrograph x 10,000 10,000 J&J-0130675 JNJAZ55_000017695 Protected Document--Subject to Protective Order D-8372 Page 144 of 247 f½e. 593 FIGURE 5. FIGURE 6. Electron Microprobe Scan for Calcium Electron Microprobe Scan for Aluminium in Same Area as Above J&J-0130676 JNJAZ55_000017696 Protected Document--Subject to Protective Order D-8372 Page 145 of 247 J&J-0130677 JNJAZ55_000017697 Protected Document--Subject to Protective Order D-8372 Page 146 of 247 • • •• • ~ ' Pm!ROGRAPHJ:O IDENTIFICATION OF . .ASBESTOS SILICATES IN VAL CHISONE ...... - t (~O)'·TALO. 59 ·by The Mining Institute of The _Po1ytecnioal Sohoo1 of Torino • . The ana1ys1s was performed on two samples of SVC pulverized taJ.o produced by two different mills in di:f':f'erent times. Operation: Small amowite of the sampJ.es ha.ve been dispersed in eusenol and observed at the microscope under 5 dif~erent oonditionsi phase oon-trast, dark field, bright fie1d, polarized 11ght (paral.J.el and oroesed moo1e). BE3ULT8s The samples, though rather different in general. com~ositio are simi.J.a.r in regard to the content of :pa.rtioles morphological.l.y , oorresponden~ to asbestos mineraJ.s. No fibrous particles having the distinguishing features •· o~ serpentine asbestos (chryeotiJ.e) occur 1n the samples. There are no particJ.es having the optical. features of amphi.boie aebes~os llke ames~te or croc1dol1te. .. · , The onl.y particles that occasionally occur are thoae ones showing the optical feai.urea of tremolite. Their. proportions range in number between 1 and 2 per 10,000 parts; that means a weight .J · :;: oontent :Lesa than o.o~ %. . · 1:-•-. Thi.a 1ast result has been backed by a Vreeland epectrosoope test on the same samples after they were purificated of oa.:Lcium and magnesium carbonates. CaJ.ciu.m, which has a proportion oontent of 9.9.,, u th~ tremolite i'ormu1a, was :found cl.oae ~o "the iowest J.im.it of sens~tiVi.t7 or the speotrosoope (about 0.01 ~). ~orino, Yeb~ 1972 I • -·. ·.,' • ·t .. f ':/ . ., ; I J&J-0130678 ·Protected Document--Subject to Protective Order JNJAZ55_000017698 D-8372 Page 147 of 247 . ;•. ,·, :··.. ., '. 4:, . "·.: -~ ;•:, J.J ..J . . ,. ..--. : . . ~ . ·~· . . • ·, : .. •.... ' - ~~. '• .... . t..,.,iiG,~•- . . , . : .: . . . :; POtiHCNICO 01 TOIIHO •TUTO 01 ARTE M&NERARIA .. :.~ .. ·, ·; •:. -;_ : . . i,' ~ • • '· !. . .: ·.. . ' • •. = , :: 19110, . .••·.. ~ CERTIFICATO N. 71/ 7211/ · · . , . i. DETERMINAZIONE PETROGRAFlCA . DI SILICATI ASBESTOIDI •. \ .,: ~ ..·:..:··~ . .-:: · I ~ . ·. . ~ .: . . ·.. • :,. ··. Committente ·.".· Societa Talco e Grafite Val ch•isone - Pinerolo (Torino) :.::·: Ric:hiesta: ·1 ·_ . f::.: Campioni ;·: ,. ·• lettera VA/rb. P.S. del 4/2/1972 N. 2, contrasscgnati con le siglo "SVC :Extra 00000 San SeD bastiano" e "SVC Extra 00000 Malannaggio" consegnati pers~ nalmente all'Istituto da parte dell'Ing. Sartorio, Diretto re Tecnico della Committente, in data 4/2/1972. ;- .· .· ·. - ._ ··--:- DeterJninazione richiesta: "dosaggio del . quantitativo di tremolite e di. analoghi silicati asbestic:i". \. ..· : • . -'~ Modalita di analisi: Una porz .i one rappresentativa dei campioni in esame ~ stata dispersa in euge·n olo ed osservata al microscopio in S differenti con . dizioni: c:ontrasto di fase, campo oscuro, campo chiaro, ·1 uc:e polariz"lata - (a nicols paralleli ed incrociati) · I . ', Risultati delle determinazioni l .. ~ I due campioni, sebbene lievemente different! come compos1z1one generale, sono del tutto equivalenti nei riguardi del contenuto di elernenti bacil ·laTi, di:caratteristiche morfologiche corrispondenti ai minerali asbe•stoidi; · 2 • Nei campioni non si . riscontrano elcmanti fib1osi aventi le caratteri. stiche doll'arnianto di serpentino (cTisotilo); . ~ .. . :J ·--------------------------------------------J&J-0130679 JNJAZ55_000017699 'Protected Document--Subject to Protective Order D-8372 Page 148 of 247 • •01'!,"J1li :, .. ,.•.·.. :;.': :( ·,?-::·:•_.· .·.• ·., .- ,t . •. :1_, .~ . :.:-_:. . .·. "':· .~. -~~;. ·:·.-.·. •• 10:r~:-J iin, . ff' ~> ~t:) ·. .·. . J:·: ff,-;a:i . =----.. .. ,:-'Ir· ...~, .., ... , , •• "' I • ~ \ t, POUHCNICO 01 TOIINO • S.a•.,l•n.,rot. 71/7211 ISTITUTO DI ARTE MIN[RA~) NI 16/2/1977. µ·· l/ooflo__..2_ _ . · ei·cur/d~1ividuo ·:=·:. :,. 1,·..• , Non a presen;~ dotato delle caratteristiche ott,\Che . ··,: -~. degli amianti 'd • anfiVo..l'o d.i tipo · amosi te o c:rocidol ite; . ·. . ••: '·/ . :· 4 · ~ Sono presenti rari ·elementi bacillari aventi le caratteristiche ota tiche della tremolite·, in .propor~io~i corrispondenti a circa 1-2 paL ti per 10000 elemcnti (in numero); tenuto conto della forma degli elementi s~essi, _il contenuto ·ponder~le ~ cett~mente inferiore sllo· ·: \.'' 0,02\. . :: ,· ·. ·>: . .',." · Osservazion i: ,••.,,. · >. ·· l) Una prova di carattere rainero·g e11etico ·. dell'assenza dell 'amianto eris~ i, data dal~'Tncompatibilita paragenetica di tale amianto con le .\/,.: · ·.- rocce talcose; :i:.\, . :. tilo :t(· ·.2~··.· Unacostituito prova analitico-strumentale dcl ridottissimo contenuto di trernolite dal saggio spettroscopico alla fiamma sui campioni previa ~ .· •.: ·\.:: mente epurati dai carbonati ·di calcio. e magnesio per debole attacco ac!_ . ::". ·i:. ''.: :,. do; le linee corrispondenti al calcio {elemento contenuto nolla tremo• ·.. _:·'.\··. ;-:- lite in proporzioni :· stechiometriche del 9 ,9\) si . ritrovano presenti ai / · · .::_,:· limiti di sensibilita · dollo spettroscopio ·cii Vreeland utili:nato per :. ·.. · 1 •indagine~(pari allo O,Ol\ circa). ::· · .·. · · . ... '. .~• :. .• . .. • .~ •_-: ·. : ·. _' • . . . • • ·:· •. • -I.- •. ,·.. i.• •• ·,. ~ A Vis to: • •: I ~ i; I II :· ! :· ·. .. I ': • •·, ·; . .. .,· . .- . ·-·· :. ~: . . ·: : ·• ..·.. . .. . .. . ..:••. . ... . ~ .~ ·: .' .~ _.. ,.: . ·f . .•-~•, •~:: / • ' I•I\,; • i •• • . .. • • . ... . J&J-0130680 JNJAZ55_000017700 Protected Document--Subject to Protective Order D-8372 Page 149 of 247 >o rt 0 ~ ..I, (/) t" ~ ~ 5· J&J-0130681 JNJAZ55_000017701 Protected Document--Subject to Protective Order D-8372 Page 150 of 247 Sadeta .Anwma Talat Enrica Tron rJ C. J.eshona, lcaJy rrAI.IAN TALC AGENCIES G. A. Baldracco Torioo ~ Nip 597 CHARLES MATHIEU, . CA.BU Al>DU!lt .. MATllUCAR.•• A. a. 0. CCD& UlllD ..!),,.~ . Inc. (201) 277..0510 P.O. BOX AM 18-22 BANK STREET SUMMIT, ~EW JERSEY 07901 · REPRESENTATIVE IN U.S.A. ·op FOREIGN MINES September 18, 1972 Johnson & Johnson New Brunswick, New Jersey 08903 Att: Mr. Harold Hogan Dear Harold: Confirming our telephone conversation regarding the source of the basic rock from which 5/0 Italian Talc ·and 11615 AGI Italian Talc are made • . Both processed products are made from the s·ame basic rock and this rock is obtained from the Fontana mine located at Val Germanesca in the Italian Alps of Northern Italy. N~. 5/0 product is ground· and packaged for shipment in Italy. As you know, your Company has not been using any of this product for a number of years. No. 1615 AGI is ground and packaged in the United States at the Metropolitan Talc Company plant located in South Plainfield, New Jersey. This plant is jointly owned by Charles Mathieu, Inc. and Whittaker, Clark & Daniels, Inc. This is the product your Company has been purchasing and is also the product covered · by the attached analysis confirming the absence of any asbestos. ~ our Quality Control procedure at the Metropolitan Talc Co. calls for complete cleaning and checking before any changes of feed stock (rock) are packaged for . shipment. If you require further - information regarding our products, prease do not hesitate to call. Very truly yours, • DRF:as CHARLES t·IATHlEU, INC - · --~nail .-R:-;;;~ Hot na1'0""'11lc fiw do-iu htc»ncd by C4m",n. A!I ~t4tlON onil c:miracu lllbjcci to ccmd:i::cma l,~yond o~r concro:. Pncu 11rc ~ d v,l)on er.stint c,srijf r ~ ond cunonu ,c~iai:'Ofla. J&J-0130682 JNJAZ55_000017702 ·Protected Document--Subject to Protective Order D-8372 Page 151 of 247 ------··-··~:-·-· ~-:..-_~_--.....;__ . . :· :- - .. . ·- ... ·. -- . - . . - - ·- ·· --- -- . .·--~ . . . - -.- . -. -. . _ .. . _;.-.::.;:_::;;;__~--=-~a...;...;~~-__;:;.:..;o----.a..---,-- -- .- - ----- _,. ___ -.---_-- -_;,-- - . -·· -··- .. ·-- - .-. - . - . --·- _ -·- .. - . - . - ···-· - · Final Report · or X-Ray · D1.f.frat?t1•n- Analysis -- -- -- ------- _... _. ___ __ - - .. - -~ ---- ----- _:· __ _ ___- - ·-·- - -- - ·· -:-: ~~--- ···-· -- · __ - ...... ·····-.; ;;lf~ ~:= :-·~. ' :· -- ···--·-·~-·--~- . -·- ... .-· - · -Sample:: . ·-· . Ncf.-.=-16f5; Wh1 t take·~~-~'.Ciark~~ "a·n:a -Da-niels- .. ··-=-_:__~~ . -:::.-:: :.::.. .-:-..: ·.. -... -~-__ : .: ~--.- :::;~·-.. :...- :-.::..··: .: ::-::_:~~(r~lc, . AGI) _... _:_ _-< :..;_ _..::...;_~ -:._ ·. -_ ·-· ____·:_ _·_·:_· _ _· ___-,- , - ·--------~--------·--- -=-=-=-::..:. :-=.==-=-.:-·..!Uneral ..Cons.tituen t~- aJ.-::-85%--Ta1c--:(.±2%rr- - · · ·· - . · · _. · · ____ -10~ _-_··.__. · .Chlorite__-~2%i--- - - - - - - - - - - - - -- 2~ Dolom1 te ±2% · 1-2% Quartz. ±2% - - - - - - - 2 , ; Pli°logopite _(.±2%)'-- ·- - - - ----- b) No detectable amounts o.f any of the --asbes·t1:form m1.nera1s·. . .. . . . ---- - ·- -- - . . --- ·- ·· - . ---------· .----··- - ·- . ·-------- ------Nov.-2-, -1971- --· · ··· - ·- -. ··- . ..------~:.--- -- ---- - - --- - -- ~j;~~.~1;::,.,,,; - -- - ------- - - - - -·· - ·- - · - ·- ---- ----------.--·- - ---· Se~our Z. ~win Proressor 0£ Chemistry -- ·- -... ---- ---·---·- --- - --- --- ... ------------ ---·- . ----· - ------------------ -· ···- --- ·------ ------- ..... ______ ... - ···----· --· __ _ ____ . - .. --··--- --· . - ·- --- ----·· --- - ---- --- .. . -- - - .. - - - . -- --- ..------- - - . ··- ·- ·- -- . ...... . . -- - --_.,. ·- • '. ._ _, ---------··--··- - - .. .... - - - ·· - --- --- ---- ----- -- -- -------- ·- ··- - ··- - ·- . .. --· ...-• ·--'-----'---------------------·----- - ·----- - --- · - ···--- -- · ·------ ----------... -- .. - - - - --~ -.-- -· --- -·. - -- . . - - -- . ... ... -- - . -- - ·. -· ·---------· - --- ---- - ---- -- -------------·- - - - - --·---- .. -- -- ·--- - - - ····---·J&J-013O683 JNJAZ55_000017703 Protected Document--Subject to Protective Order D-8372 Page 152 of 247 _5.99 _. __-_,.--·--:. ~=-· ·--------------- . ____ -------~--- --- - - . . . -- __ ..__ . ·"'·---.- -- - - - - - · Final Report of X-Ray D1rrraction Analysis ------ ----- ~-- --- __: _Sample·: -- .. --· -- ------ -..Italian Talc Rock - - - - - . - - -- - -, --- (Hand Specimen) - ·-- - -------..;. __ ~_,-Mineral · Cons t1tuerits ·90% Talc ( ±2%) .:_. ·- -- - · -· - --.. - - . - -- - --·- . -- - - . -- .. - -- - - 5% Cblori te ( ±2%) . - · . :--- : "!""": .•• - ..• _ · - · - - --- - ·-··· - - -- ~ 5% Phlogop1 te (~)-?, l - -:· ------------- . --------···- - - -· -··------- - - ·- .. --- ------- Nov. 2-,.. 1971 of Cliem1stry ...___--- · - - - .. - --~~-- -- ---------.-------------------~- - • · - .., _ _ _ _ · - - - .-- __ .. _,, _ _ ...- . !... J&J-0130684 JNJAZ55_000017704 Protected Document--Subject to Protective Order D-8372 Page 153 of 247 J&J-0130685 JNJAZ55_000017705 Protected Document--Subject to Protective Order D-8372 Page 154 of 247 - -'"cl l-f 0 :-"' J&J-0130686 JNJAZ55_000017706 Protected Document--Subject to Protective Order D-8372 Page 155 of 247 600 Martin Julian Buerger Academic Training S.B., Mjning Engineering, S.M., Geology, Ph.D., M.I.T., Mineralogy, Academic Positions, M.LT., 1925 1927 M.1. T., 19Z9 Massachusetts Institute of Technology Assistant in Geo! ogy, 1925-1927 Instructor in Geology, 1927-1929 Assistant Professor of Mineralogy and Petrology, '1929- 1935 Assodaie Professor of Mineralogy and Petrology. 1935-1944 Profess or of Mineralogy and Crystallography, Institute Professor, 1944- present 1956-present Chairman of the Faculty, 1954-1956 Director of the School for Advanced Study, 1956-1963 Academic Pos _itions, University of Connecticut . University Professor, Department of Geology, 1968 · Graduate Advisor, Institute of -Materials Science, 1968 Society MembershiP, American Crystal Lographic Association Geological Society of America (Felio~) Mineralogical Society of America (F.cllow) National Academy of Sciences, Honorary Member ship, U.S.A . , 1953 foreign societies Academia Bras.ileira de Ciencias, 1952. Accademia delle Scienze di Torino, 1954 Deutsche Mineralogische Gesell~chaft, Accademia- Nazionale dei Linc:ei, 24, August, 1.957 1960 Bayerische Akademie der Wissenschaften (corresponding), 1960 Osterriechische Akademie der Wissenschaften (corresponding), Real Sociedad Espanola de Historia Natural of Madrid, . . ..... ... ., ~ .. "'.-. . ·- 1964 . :.· ... . . March, 1962 'I . . . .. , - ,~. - - ---- ·----J&J-0130687 Protected Document--Subject to Protective Order JNJAZ55_000017707 D-8372 Page 156 of 247 601 Offices Held Societies President., 1\merican Crystallographic Society, President, American Society for X-ray and Electron Diffraction, 1948 Pre::;ident, Mineralogical Socie.t y of America, Vice-President, • 1939- 1946 Councilor, 1947 Geological Socie_ty of America, t 948 American Academy of Arts and Sciences, 195 0-1954 International Union of Crystallography American Delegate to Preliminary Convent:i on, Council Member, Co-Edi tor, Member, U.S.A. 1946 1946-1951 1nternationa1 Tables for X-ray Crystallography, 1946-present Apparatus Commission, : 951- 1956 National Committee on Crystallography, 1966-1968 1951, 1952, \956-1. 962, National Research Council Representative of the U.S.A. to the Second General Assembly and Congress of the International Union of Crystallography, Stockholm, 1951 to the Fourth General Assembly and Co_ngress of the International Union of Crystallography, Cambridge, England, 1960 Representative -of the U.S.A. Member, Committee on Solids, 1949-1953, 1956-1962 Zeitschrift f:.;r Kristallographie Co-Editor, 1953-present Faculdade de Filosofia, Universid.ade de Rio de Janeiro Visiting Profess or, 194.8 Visiting Professor. -Consejo Superior de Investigaciones Cientificas, Madris, 1958 Institut~ de F{sica y M~them~ticas, Universidad de Chile, . Guest Lecturer, 19 6Z. Visiting P.rofe ssor, University of Minnesota, 1970 Visiting Professor, Univer-sity of Kentucky, 1971 J&J-0130688 Protected Document--Subject to Protective Order JNJAZ55_000017708 D-8372 Page 157 of 247 602 . Honors Day Medalist-, Geological Society of America, 19 !=1 . Roehling Medalist, Mineralogical Society of America, i 958 D. h. c. , University of Bern, 1958. Isador Fankuchen Awardee, American Crystallographic Society, 1971 Books The Optical Identification of Crystalline Substances. (1he M. I. T. Letter Shop, Cambridge, 1939) X-ray qrystallography. (John ·wi ley and Sons, Inc., New York, i 942) Elementary Crystallography. (John Wiley and Sons, Inc., New York, 1956) The Powder Method. (with Leonid V. Azaroff) (McGraw-Hill Book Co. , ·rnc., 1958) Vector Space. (John Wiley and Sons, Inc., New York, 1959) Crystal-Structure Analysis. (John Wiley and Sons, Inc •• New York, 1960) The Precession Method. (John Wiley and Sons, Inc., New York, 1964) Contemporary Crystallography (McGraw-Hill, New York, i970) Introduction to Crystal Geometry (McGraw-Hill, Nev., York, 1971) The La.ue Method 1973) J&J-0130689 i JNJAZ55_000017709 Protected Document--Subject to Protective Order D-8372 Page 158 of 247 603 DEPARTMENT OF EARTH AND PL.-.NETARY SCIENCES MASSACHUSETTS INSTJTUTE OF TECHNOLOGY CAMBRIDGE, MASSACHUSETTS 02t39 7 October 1972 Dear Dr. Goudie, I am enclosing a face copy and three Xerox copies of my report on the Washington meeting . which you requested in your letter of September 2 5. I have also taken the liberty of including some biographical material on myself in order to strengthen your hand if it is necessary to deferd ·. the authority of some of the remarks I make concerning the results of the meeting. In particular, I would like to draw your attention to the first book I ever wrote which you will find on the last page of the biographical information. I taught this subject for perhaps 20 years, so I feel that the remarks made concerning Lewin 1 s identification of chrysotile can be justified. Sincerely, - ---.. )/i -1 / /tc~-'L .t.,.,< ff 1 ~,__._._(,, ...-__ Martin J. Buerger \__ Dr. A. L. Goudie, Johnson & Johnson Research Center, New Bri.mswick, New Jersey. J&J-0130690 JNJAZ55_000017710 Protected Document--Subject to Protective Order D-8372 Page 159 of 247 604 In the following report (first paragraph, page 2). Professor Buerger' s statement indicating the use of step scanning by Professor Gordon Brown and Colorado School of Minea Research Institute should be corrected to Johnson & Johnson and Colorado School of Mines Research Institute. J&J-0130691 JNJAZ55_000017711 Protected Document--Subject to Protective Order D-8372 Page 160 of 247 60~ The Washington Meeting of Septernber 21., 1972 of Johnson and Johnson with the Food and Drug Administration and Conclusions to be drawn from the meeting by Martin J. Buerger October 7, 1972 J&J-0130692 JNJAZ55_000017712 Protected Document--Subject to Protective Order D-8372 Page 161 of 247 606 - 1 - As a prelimina~y.to the meeting with the Food and Drug Administration, those associated with Johnson & Johnson met early on the afternoon of the previous day. September 20, in the Holiday Inn, to review their findings. The Johnson & Johnson staff included Or. Fuller, Dr. Shelley, Dr. RollJ, Jack Sheltz and Dr. Nashed •. Associates of Johnson & Johnson included Walter McCrone and Ian Stewart, Fred Pooley, Sidney Pollack, Gordon Brown amd Martin Buerger. These reported to the other members of the group the results of their investigations of the purity of the talc used in the Johnson & Johnson talcum powder known as "Shower-to-Shower". The general conclusion was that none of the work revealed any trace of contamination of "Shower-to-Shower 11 talc by the mineral chrysotile. The meeting of the Johnson & .Johnson group with the Food and Drug Administration took place September 21, 1972, on the 6th floor conference room of ZOO Avenue C, S. W., Washington D. C. It was chaired by Dr. Schaffner. who introduced. before the meeting, Messrs. Weissler. Winniger. Carolla and a number of visitors whose names were not clearly given. Professor Seymour Lewin of the Deparbnent of Chemistry, New York University, consultant to the Food and Drug Administration, was also present but was not introduced. Dr. Schaffner asked the Johnson & Johnson group to present its findings first. Fred Pooley began by giving the results of his examination of the raw material used for 11 Shower-to-Shower' 1 talcum powder. from a mine at Val Chisone, Italy, just north of Turin. This talc is imported Pooley discussed his very extensive and exhaustive tests using various techniques including megascopic identification of minerals, petrographic microscopic examination and x-ray powder diffraction study. As a result. he concluded that there was no evidence for the existence of chrysotile in any samples, even in those assembled as far back as 1949. Thus, chrysotile does not exist in the source material from which the commercial product is made. The x-ray diffractometer work was reported independently by Professor Gordon Brown of the Department of Geology of Princeton University and by Dr. W. T. Caneer of the Colorado School of Mines Research Institute. J&J-0130693 JNJAZ55_000017713 Protected Document--Subject to Protective Order D-8372 Page 162 of 247 607 - 2 - Both used diffractometers. operated in the step-scanning method. The details of their experimental work can be described as elegant and conclusive. Neither of these competent mineralogists found any evidence for the contamination of "Shower-to-Shower" talcum with cbrysotile. An outline of the work which had been done under my direction using the Guinier camera This work had aho,nn that, if rJl/o chrysotile is added to was presented next. a sample of talc, the contamination is easily detectable and cannot be missed. With Long exposures, as little as 1% chrysotile can be detected as u contaminant. No contaminant was found in the "Shower-to-Shower" talcum. Walter McCrone demonstrated that chrysotile can be detected at levels as low as 1% by "optical staining" techniques. With the aid of this method, he was able to certify that "Shower-to-Shower" talc contains no chryaotile. Jack Sheltz demonstrated the power of differential thermal analysis in detecting chrysotile. That mineral produced a record which is characterized by two specific and sharp peaks by which its presence can be determined readily down to a level of 1%. Using this test, it was evident that the Johnson & Johnson product could not contain as much as 1% chrysotile. From these several independent investigations, it was most obvious that th: Johnson & Johnson "Shower-to-Shower" talcunl powder was made from a mine whose product was free from chrysotile, and that, after the product was made, it was still free fro:rn chryaotile asbestos. It must be emphasized that this common conclusion was reached by half a dozen competent scientist& applying the diverse tests of x-ray diffraction by three distinct techniques, petrographic-microscopic examination by two distinct techniques, and differential therT.'.lal analysis. There can be no doubt that "Shower-to-Shower" talcUin as made by J ~ son & Johnson is not contaminated l:7y any appreciable amount of chrysotile asbestos. J&J-0130694 ! Protected Document--Subject to Protective Order JNJAZ55_000017714 D-8372 Page 163 of 247 60l ., With this backgz-ound, it was a shock to hear Professor Lewin say that. while he agreed with these results, he now relied on certain optical tests which proved that chrysotile was really present in substantial quantities in "Shower-to-Shower" talcum. He then passed out to everyone in the room a set of ·five sheets containing 14 sequences of three pictures to support his view that he can easily detect chrysotile in certain samples. Professor Lewin's discourse, while beauti!ully delivered, contained points which cannot be accepted by trained mineralogists. His identification of chrysotile is, in my opinion, based upon an application of crystal optics which takes no account of the optics to be expected of plastically deformable layer-structures such as talc and chlorite. It also ignores crystal habit, especially the well-known habit of chrysotile. As a type example of his identification of chrysotile, Professor Lewin showed pictures of a piece of talc, immersed in a liquid whose refractive index was 1. 580, and called attention to the Becke-line test of its refractive index(~) when one edge was parallel to the vibration direction of the polarizer , and (~) when that edge was perpendicular to the vibration direction of the JDlarizer. The longer edge of the piece displayed a refractive index less than 1. 580 when the edge was in a horizontal position on the page. whereas the rest of the piece of talc showed a higher refractive index. Since a talc crystal has two of its _indices, 8 and y, approximately in the plane of (OOf ), both equal to about 1. 589, the talc crystal lying on the microscopic slide might be expected to display higher refractive indices than :1.. 580. But, Professor Lewin pointed out. one of the edges displays a lower refractive index. Ergo: the edge is not talc but chrysotile, whose refractive indices are lower than 1. 580. specifically. 1. 546, 1. 550 and 1. 557. But this deduction overlooks the well-known plasticity of talc. the very characteristic which ca.uses it to be soft and which recommends its use as talcum powder. Any bending of the edge of a talc crystal (and this cannot be avoided in the making of a microscopic slide, and is a characteristic which is bound to be exaggerated if its existence is ignored) results in the changing of the orientation of the edge of the talc platelet which is bent, so the lower a refractive index of J&J.0130695 Protected Document--Subject to Protective Order JNJAZ55_000017715 D-8372 Page 164 of 247 60' - 4 - t. 539 of talc begins to be displayed, Thus, talc edges are unsafe places to determine a refractive index unless it is first ascertained that the edge in question is undamaged. This applies also to the edges of upper and lower partial flakes of a talc crystal which have become bent; appear to lie within the crystal. index is_.!!£! talc, such bent flakes To prove that an observed low refractive i t ~ be shown that it is one of the principal refractive indices of chryaotile. Thia Professor Lewin has not done, nor did he seem to understand this objection to his identification of the bent flake as chrysotile when it was drawn to his attention. Thus, Professor Lewin has presented a.bsolutely no proof that any chrysotile is present in any of his samples. Thie negative result should be compared with all the negative tests shown by x-ray diffraction, with the competent crystal-0ptical studies by Walter Mccrone, with the results of differential thermal analysis tests. and with the fact that there was no chrysotile in the raw material as mined. to sta.rt with. Finally, the crystal habit of the part of the preparation which shows the low refractive index does ~have the well-known habit of chrysotile asbestos. This mineral is a pyrophyllite-type sheet rolled up to form a tube with neat parallel sides and, more generally, is characterized by a cylindrical contour. None of Professor Lewin' s photographed items labelled "CHR YSOTILE" conform to this habit properly. In fa.ct, his first example is so obviously a bent-edge effect that it displays its origin by the irregular black shape of the extinguished mass when the stage is at 0° and 90°. There ie another edge extinguished when the stage is a.t 45°. At the end of Professor Lewin' a discourse, I commented on the lack of conformity of Professor Lewin' s low-index areas with the known habit of chryaotile asbestos. He attempte_d to dodge this objection by pointing out that the compound Mg (Si o )(OH) is polymorphous, the polymorphs being 6 4 10 8 known as chrysotile, antigorite and lizardite. But, of these three, only chrysotile has the form of asbestos; the other two are la:ver structures and without any of the habit characteristics of asbestos (chrysotile asbestos itself has three polymorphs, o. , f3 and y, but all are known to have the asbestos J&J-0130696 JNJAZ55_000017716 ·Protected Document--Subject to Protective Order D-8372 Page 165 of 247 - 5 - 61 crystal form because all are sheet structures rolled into tubes.) Layer structures which do not have crystal habits consisting of rolled-up tubes are not more injurious to health than talc itself, for it is not thE- chemical composition but the asbesto :s-form crystal habit which is injurious. My conclusion is that no tenable evidence has been advanced to show that any Johnson & Johnson product was made with talc which contains chrysotile asbestos, and no tenable evidence has been advanced to show that the product as sold and manufactured contains chrysotile asbestos. J&J-0130697 Protected Document--Subject to Protective Order JNJAZ55_000017717 D-8372 Page 166 of 247 J&J-0130698 JNJAZ55_000017718 Protected Document--Subject to Protective Order D-8372 Page 167 of 247 61 1 CURRICULUM VITAt GORDON E. BROWN P------------------- Personal Data: Born i Redacted -Perso nal Informatio n i 1943, San Diego, California1 Married. one child. Education: s.s. M.s. Geology and Chemistry, Millsaps College, Jackson, Miss., 1965. Mineralogy, v.p.1., 1968. Ph.D. Mineralogy, v.P.I., 1970. Employment Experiences Assistant Professor, Dep~. of Geological and Geophysical Sciences. Princeton University, September, 1971- present. Post-Doctoral Research Associate, State University of New Yo~k at Stony Brook, May 1970- August 1971. Research and Teaching Assistant, Virginia Polytechnic Institute and State University, September 1966- April 1970. Research Assistant, Sun Oil Company, Jackson, Mississippi, June 1963- September 196S. Professional Societiesi Mineralogical Society of America American Geophysical Union American ASsociation for the Advancement of Science Research Experiences G.E. Brown investigated the crystal chemistry of the olivines as part of his doctoral research. The crystal structures of Ni-, Co-, (Pe,Mn)- (Mn,Mg)- (Fe,ca)- and (Mn,Ca)- olivines were refined from-single crystal X-ray data and cation ordering was studied in the (Fe,Mn)- and (Mn,Mg)- olivines. Earlier efforts were devoted to a study of bonding in the tetrahedral portions of silicates in collaboration with G.v. Gibbs- During post-doctoral work at Stony Brook, he collaborated with C•T• Prewitt and J.J. Papike on X-ray studies of the Apollo 12 clinopyroxenes and olivines. Included in this work are high-temperature X-ray studies of the P2 1 /ci=C2/c transition in intergrown lunar pigeonite/angites, design of several high temperature furnaces for single crystal X-ray work (also in collaboration withs. sueno), high temperature structural studies of pigeonite and cummingtonite, order-disorder studies of lunar olivines over a range of temperatures, and a neutron diffraction study of Al/Si ordering in sanidine. J&J-0130699 JNJAZ55_000017719 Protected Document--Subject to Protective Order D-8372 Page 168 of 247 612 Publications - G.E. Brown G-E• Brown and G.v. Gibbs (1968) The crystal structure of osumilite (Abstract) Geol. soc. Amer. s.E. Sec. Meet., ournham, N.c., 89. G.E. Brown and G.v. Gibbs (1969) Refinement of the crystal structure of osumili~e- Amer- Mineral. 54, 101-116. Brown, G.v. Gibbs and P-H· Ribb! (1969) The role of d-p r.-bonding in minerals containing Sio -, Alo 5- and Mgo 6 - tetrahedral 4 4 ions (Abstract) Geol. Soc. Amer. s.E. 3ec. Meet., Columbia, s.c., ll· G.E. BrO\rln, G.v. Gibbs and P.H. Ribbe (1969) The nature and variation in length of the Si-0 and Al-0 bonds in framework silicates (Abstract). Trans. Amer. Geophys. Union .:iQ, 358. G.E. Brown, c.v. Gibbs and p.a. Ribbe (1969) The nature and variation in length of the Si-0 and Al-0 bonds in framework silicates. Amer. Mineral • .2!, 1044-1061. G.E. Brown and G.v. Gibbs (1969) oxygen coordination and the si-o bond. Amer. Mineral. 54, 1528-1539. G.E. Brown and G.v. Gibbs (1970) The variation of the Si-0 bond lengths, Si-0-Si and O-Si-0 angles in - the chain and sorosilicates. (Abstract) Amphibole-Pyroxene Symposium, Blacksburg, Va. Amer. Mineral. ,ai, 298. G.E. Brown and o.v. Gibbs (1970) Stereochemistry and ordering in the tetrahedral portion of silicates. Amer. Mineral. ll, 1587-1607. G.E. Brown, G.A. Novak, K.G. Robinson, G.v. Gibbs and p.9. Ribbe (1970) Crysta1 chemistry of the orthosilicates (Abstract) Geol. Soc. Amer. Annual Meeting, Milwaukee • .!ill, 504. J.J. Papike, A.E. Bence, c.T. Prewitt and G.E. Brown (1970) Apollo 12 clinopyroxenes: subsolidus relations (Abstract) Geol. Soc. Amer. Annaul Meeting, Milwaukee. l.lll, 644. Bence, G.E. Brown, J.J. Papike, c.T. Prewitt and c.a. Wu (1971) Apol1o 12 clinopyroxenesa chemical trends, epitaxy, exsolution Proc. Apollo 12 Lunar Sci. and phase transitions. (Abstract) conf., Houston, Texas. 105-106. J&J-0130700 JNJAZ55_000017720 Protected Document--Subject to Protective Order D-8372 Page 169 of 247 613 J.J. Papike, A-E- Bence, G.E. Brown, c.T. Prewitt and c.H. Wu (1971) Apollo 12 clinopy~oxenes: exsolution and epitaxy. Earth Planet. Sci. Lett. 10, 307-315. c.T. Prewitt, G•E• Brown and J.J. Papike (1971) Apollo 12 clinopyroxenes: high temperature X-ray diffraction studies. Proceedings 2nd Lunar Science Conference. _l, 59-68. G·E· Brown, c.T. Prewitt and J.J. Papike (1971) Structural studies of intergrown lunar pyroxenes (Abstract) Trans. Amer. Geophys. Union 52, 270. w.c. Hamilton, c.T. Prewitt ands. Sueno (1971) Neutron diffraction study of Al/Si ordering in sanidine (Abstract) Geol. Soc. Amer. Annual Meeting, Washington. 1..ill, 514. G.E. Brown, G.E. Brown, c.T. Prewitt, J.J. Papike ands. Sueno (1972) A comparison of the structures of low and high pigeonite. Jour. Geophys. Res. (in press). s. Sueno, J.J. Papike, c.T. Prewitt and G.E. Brown (1972) The crystal structure of high-cummingtonite. Jour. Geophys. Res. (in press). J&J-0130701 JNJAZ55_000017721 Protected Document--Subject to Protective Order D-8372 Page 170 of 247 614 X-ray Diffraction Study of Johnson & Johnson's Shower-to-Shower Talcum Powder Gordon E- Brown Assistant Professor of Mineralogy and Crystallography Princeton University Princeton, New Jersey Abstract An x-ray diffraction study of Lewin's sample of Johnson & Johnson's Shower-to-Shower talcum powder using slow, continuous scanning, diffractometer techniques with monochromatized Cu radiation showed that two forms of chlorite, phlogopite, magnesite, dolomite and calcite are minor contaminants ( < 10% total) of the ta le. No evidence of chrysotile or tremolite in Lewin's sample was found. Examination of the 29 regions around 12° and 24° alone is not necessarily sufficient to establish the presence of chrysotile asbestos because of the similar peak positions of two other nonfibrous serpentine polymorphs, lizardite and antigorite. However, detailed examination of the range 5-80° 20 does permit discrimination between chlorite and serpentine peaks, assuming that these minerals are present in detectable amounts. The x-ray data on J&J's Shower-to-Shower powder presented by s.z. Lewin in a written report (May 16, 1972) to the Cosmetic, Toiletry and Fragrance Association and during a hearing (Sept. 21, 1972) before officials of the Food and Drug Administration show no evidence of chrysotile or tremolite when examined carefully. Moreover, the fibrous-looking particles in the photomicrographs also presented by Lewin at the Sept. 21 hearing can best be inter- preted as rolled talc particles, which are sometimes produced during grinding. Lewin's claim that chrysotile is present in J&J's Shower-to-Shower powder is not supported by his data or by any of the results (from x-ray and electron diffraction, optical dispersion staining, transmission and scanning electron microscopy, electron rnicroprobe analysis, differential thermal analysis, petrographic examination of the unchrushed Italian talc and detailed field study of the Italian mine) amassed by Johnson and Johnson's team of consultants. J&J-0130702 JNJAZ55_000017722 Protected Document--Subject to Protective Order D-8372 Page 171 of 247 615 Introduction Talc deposits can result from a variety of processes including hydrothermal alteration of ultrabasic rocks (steatitization) and thermal metamorphism of siliceous dolomites (Turner, 1948). In the former process serpentinization may or may not occur before the development of talc. In either case the resulting talc may contain minor contaminants which can occur from incomplete steatitization, retrograde metamorphic processes or more commonly simultaneous crystallization of additional phases necessary to maintain mass balance. Contaminants such as magnesite, dolomite, calcite, chlorite, secpentine, tremolite, actinolite, phlogopite and quartz may result. It is the purpose of this study to identify the contaminants present in Johnson & Johnson's Shower-to-Shower talcum powder using x-ray diffraction techniques. Because of s.z. Lewin's claim that this powder contains~ 5% chrysotile by weight, particular care was taken to verify or reject its presence using a continuous scanning x-ray technique similar to that employed by Lewin. The sensitivity of the continuous scanning technique to small concentrations of chrysoti le in talc is estimated to be detection of - 2-3¾ chrysotile by weight. Lewin in a report to CTFA (5-16-72), claims a sensitivity of 1-2°/4 chrysotile using a scanning rate of 1° 20/min. Therefore, if crysotile is present in the Shower-to-Shower powder in amounts of ~5% by weight, as claimed by Lewin, its presence should be easily detectable . · Experimental A powder mount of Lewin's sample of J & J's Shower-to-Shower powder was prepared by mixing 0.1 gr. of powder(< 325 mesh) with a mixture of acetone and duco cement on a glass slide. A very small quantity (~O.O1 gr.) of powdered Si metal (325 mesh), · for use as an internal standard, was sprinkled onto this mixture and stirred in. Powder mounts of three chemically diverse chrysotiles were also prepared in the same manner. Allx-ray data were collected using a Norelco vertical diffractometer mounted on a Norelco generator with a Cu standard focus x-ray tube. The diffractometer is equipped wi·t h a sample spinner, which is used to reduce the effects of preferred orientation , and a LiF crystal monochromator, which is set to produce a beam of Cu K~ x-rays. The PHA was tuned using the · 111 peak of Si-metal and 2 V baseline and window settings were found satisfactory. Diffractometer alignment was then checked using Si-metal peaks which were located within 0.01° 20 of their correct values. 1° source and receiving slits were used in all runs. Smaller receiving slits, which are used to increase resolution, were found J&J-0130703 Protected Document--Subject to Protective Order JNJAZ55_000017723 D-8372 Page 172 of 247 6l t to reduce intensity significantly. Enhancement of intensity was considered more impor~a.nt than increasing resolution because of the small amounts of impurities being searched for. All tracings were run at 40 KV and 20 mA using a scan speed of 1/4° 28/min. and a time constant =2. Scans from 5-80° 20 were run for the Shower-toShower sample and the three crysotiles. Table l contains the 20 values and d-spacings for all peaks in this interval for the Showerto-Shower sample and Table 2 lists the chemical compositions and positions of the three strongest peaks for the three crysotile specimens studied. Figure 1 is a copy of the diffractogram for the Shower-to-Shower sample. Interpretation The interpretation of a diffraction pattern from a complex mixture of phases is always difficult and necessitates great care. The standard philosophy employed in such an interpretation is outlined in Klug and Alexander (1954) and simply requires that all peaks be explained using the ASTM Powder Diffraction File or other standard patterns. The patterns in the ASTM file are for minerals of specific compositions, so the effects of solid solution on cl-spacings must be taken into account. Because of the paragenesis of talc, a number of specific contaminants are expected and were searched for. In addition to peaks due to talc and the Si internal standard, 22 extra peaks were recorded in the diffraction pattern of J & J's Shower-to-Shower powder (See Tableland Figure 1). These additional peaks are due to two varieties of chlorite ( ~ 5% by weight) , phlogopite ( 2%) , magnesite ( ,.; 2%) , dolomite ( 1%) and calcite (trace). Chlorite has the hypothetical composition Mg1zSiso 2 o(OH) 16 , however, Al can substitute for Mg and Si. When Al replaces about 3 Si per formula unit, the chlorite is called sheridanite; when about 1 Al substitutes for Si, it is termed a penninite. Because tetrahedral Al and Si ions differ by about 0.14A in size, penninite and sheridanite have different d-spacings (A.... 0.1..A) and 29 positions. The main peak at 7.15 A and its low angle shoulder are therefore interpreted to be due to sheridanite and penninite, respectively. with sheridanite and penninite constituting ,.,4% and 1% by weight. of the sample. For each of the contaminants listed above, identification was not accepted unless their peaks showed selfconsistent intensity relationships. The presence of tremolite was not confirmed because its three strongest peaks (8.38, 3 . 12 and 2.70ft) are absent. Likewise, chrysotile can be rejected as a component because its two strongest peaks , the 002 and 094, predicted to occur at 7.31 and 3.65 A, respectively, are missing. Al though the low angle shoulder (,,, 7. 2A) to the 002 chlorite peak (7.15A) overlaps the 7.3 ~ region, it is due to the 002 of penninite, not the 002 of crysotile. If the 002 of crysotile were present~ ~ ~ ~ J&J-0130704 Protected Document--Subject to Protective Order JNJAZ55_000017724 D-8372 Page 173 of 247 617 the 004 of chrysotile is required to be present at 3.651 and should have nearly the same relative intensity as the shoulder at Examination of Figure 1 shows no peak in the 3.65A region. Preferred orientation, which undoubtedly would have occurred for chrysotile if present. would enhance all of its basal reflections, not just the 002. One might argue that substitution of Al and Fe for Si and Mg in chrysotile would cause a shift in a-spacings such that the 002 and 004 of chrysotile are coincident with the chlorite peaks at 7.22-7.15A and 3.56A. To test this hypothesis, diffraction patterns of three chemically diverse chrysotiles were run and the results are reported in Table 2. The effects of these chemical substitutions on the basal spacing of crysotile appear to be small. Therefore, it • • 0 is doubtful that the 004 chlor1te peak at 3.65A obscures an 004 of crysotile. A word of caution is necessary even if peaks occur at 7.31 and 0 3.65A. Besides chrysotile, there are two other serpentine polymorphs known as lizardite and antigorite which differ slightly in structure and totally in morphology (both are platy} from chrysotile. However& the two strongest peaks of each polymorph occur near 7.36 and 3.66A (Whittaker and Zussman, 1956; Page and Coleman, 1967}. Whittaker and Zussrnan (1956) emphasize that correct identification of a serpentine polymorph is possible only if a complete and accurate diffraction pattern is obtained. Obviously discrimination of this type would be impossible i f small amounts of one or more of the serpentine polymorphs did occur in the Shower-to-Shower powder because of the weakness of the serpentine pattern and possible interference from other peaks. 7.2A. Conclusions The 22 extra peaks observed in the x-ray pattern of Lewin's sample of J&J's Shower-to-Shower talcum powder are interpreted as being due to sheridanite (4%), penninite (1%), phlogopite (2%), magnesite {2%), dolomite (1%) and calcite (trace). No evidence for chrysotile or tremolite was found. The diffraction patterns of three chemically different cbrysotiles were run to check the effects of cation substitutions on basal spacings. These effects were found to be minor and it is concluded that the 004 peak of chlorite does not obscure an 004 peak of chrysotile. Although the x-ray diffraction pattern from a multi-component mixture such as Shower-to-Shower is complicated, it can be interpreted by careful use of the ASTM Powder Diffraction File. J&J-0130705 JNJAZ55_000017725 Protected Document--Subject to Protective Order D-8372 Page 174 of 247 618 References Deer, W-A•, R-A- Howie and J. Zussman(1962) Rock-Forming Minerals, Vol. 3 Sheet Silicates270 PP·, Wiley & Sons, Inc., N-Y• Klug, H-P· and L-E· Alexander (1954) X-ray Diffraction Procedures716 PP·, Wiley & Sons, Inc., N.Y. Page, N.J. and R.G. Coleman (1967) Serpentine-mineral analyses and physical properties. U-S G S Prof- Paper 575-B, P· B103-B1070 0 0 Turner, p.J. (1948) Mineralogical and structural evolution of the metamorphic rocksGeol. soc. Amer. Mem. 30, 132 pp. Whittaker, E.J. w. and J. zussman (1956) The characterization of serpentine minerals by x-ray diffractionMineral. Mag • ..?.l, 107-126. J&J-0130706 JNJAZ55_000017726 Protected Document--Subject to Protective Order D-8372 Page 175 of 247 619 Table 1: X-ray Data for Lewin's Sample of Shower-to-Shower Powder hkl Mineral I/Io*** 001 Chlorite 001 002 002 002 003 004 020 ,111 020 004 022 Phlogopite Talc Chlorite(P)** Chlorite(S)** Chlorite (S+P) Talc Talc Chlori te (S+P) Chlorite(S+P) Phlogopite Phlogopite 60 100 100 003 111 006 220 Si Standard 005 Talc Cale i te Dolomite Chlorite(P) Chlorite(S) 104 Magnesite 200,131 Phlogopite Talc Chlori.te (S+P) Talc Chlorite{S+P) Talc Talc Talc Magnesite Chlorite(S+P) Si-standard Si-Standard Talc Magnesite Talc Si-Standard Talc Chlorite(S+P) 104 005 132 131,202 132,204 132,203 008 134 136 113 135,204 220 0-0-10 116 244,138 311 0-0-12 331,060 060,332 1-3-1:) 139,208 2-0-10 1·3•12 400 30 ~ 14-5-14-3 9- 9-9- 8 9-47 7-22 7-15 4-75 4-70 4- 59 40B 4-58 SO(S) or lOO(P) 3-56 20 100 100 3-37 3.35 3.14 3. 13 100 70 so 90 100 100 100 3.02 2-90 60 2-88 20 100 30 30 2-85 40 65 so 16* 20 20 2-75 2-63 2- 61 2.59 2-48 2.44 2.34 2.21 20 (deg-) 6-10-6-15 8- 90-9- 00 9-34 12-26 12-38 18-70 18-88 19-35 19-39 25-00 26-42 26-60 28-46 28-65 29-50 30-87 31-02 31-42 32-54 33-98 34-42 34-60 36-18 36.8 38-42 40-75 2. 11 2.10 42-85 40 2-02 60 1-92 1-92 44-85 47.18(Koe1) 40* 47.33(K9' 2 ) 1-87 48- 56 34 1-70 20B 1-68 54. 72° 35 1-64 1-56 56°02(K•1) 59-16 60.32 43 20* 20 Talc 40 Talc Chlorite (P) Talc Talc Si-Standard 8B 30 16 20 8 1-54 1-53 1.46 1.41 1-41 1.39 l-36 60.SS(K11t 63-2 66-2 67-0 67-1 69-20 J&J-0130707 JNJAZ55_000017727 Protected Document--Subject to Protective Order D-8372 Page 176 of 247 620 lli 0 · 0 • 14 264 331 Mineral Talc Talc Si-Standard .QJ& 20(deg.) 1.34 70-34 108 1.30 13 1. 25 72-90 76-30 I/Io 16 ... *Enhanced by preferred orientation **(S}= Sheridanite: (P)= Penninite *** ASTM Intensity J&J-0130708 Protected Document--Subject to Protective Order JNJAZ55_000017728 D-8372 Page 177 of 247 "D aID n ID C. C 0 n C: 3 11) :::l t C: J!. 11) !l 0 "D aID Table 2: !l Chemical and X-ray Data for Chrysotile <' 11) 0 Jeffrey Arizona Coalinga Tetrahedral Cations Si3,91Al0.07 Si3,9sA 1 0.02 Si3,92Alo . 18 octahedral cations Mg5,79Feo.19 Mg5. 93Feo. os Mgs.62A 10.41Feo.1s d002 ()\) 7,36 7.35 7.31 CA) 3,66 3-66 3,65 do60 {A) l,54 1.54 1.54 a. ~ D-8372 Page 178 of 247 doo4 c.. go c.. c.. zc.. b N 0 )> 0, 0, I 0 0 0 ~ ..... ..... I\) ID ~ w --1 0 tD °' N -·· .~ i) ,, -. ---- ~~e (g~d._ 1 Ft6u a& J..-. X•IA'I f '4i\E'fA IF l,6WJM 1m ~I\Mt ~ IF T & 'l's ~~ -11»--~~ P1wfefl I -- I I .. - a) () I - .. CD --: -- -.-- · ·- · ·-- . ' . --· ·: - -··· . ... . - ..... --- - - - - - - - ·- . ; _:__ ·--- - . .. - - :.. ·- . . - ---- ----· ._ ---- ··---- - . -. . . - -- -• • ✓-~ ·_ .r \ •• - - 1 . ~.~:~ ·' . :·: -----_-_-- - •-. . . .-. ·. ---- --·- -•. ·- - - -- ~. 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Lewin '·s Presentation at the FDA- Johnson Meeting (9/21/72) 643 & Johnson That Professor Lewin is a polished speaker is not questioned after his presentation on the morning of sept. 21~ however, his interpretation and command of the theory of x-ray diffraction and optics is suspectAfter a somewhat theatrical and generally nonrelavent discourse on the strucutres of talc and chlorite, he claimed that Shower-to-Shower did indeed contain chrysotile. It appears difficult for P~ofessor Lewin to decide on a fixed amount of chrysotile (his estimates· vary from 2-5% on a given date) or whether tremolite is present- The diffraction patterns of sample numbers 136 and 137 handed out by Lewin are totally useless in deciding almost anything except the presence of talc and chlorite. on the other hand they do show, if marked correctly, that a ~-filter was not used, a dangerous practice in general which only complicates an x-ray pattern. They do not show evidence of chrysotile or tremolite. His interpretation of the photomicrographs demonstrated a seeming lack of experience and little knowledge of the optical properties of talcIt is not uncommon for talc edges to be rolled or bent during mechanical grinding. This would explain Lewin's observation that some of the talc plates display two different refract i ve indices which he interpreted as indicating talc interg.rown with chrysotileAccording to Deer, Howie and Zussman (1962) the refractive indices of talc are "'" ~ 1-54,l'Ylf, ~ l-590, 1n'¥" ~ 1-590- When a talc plate has rolled edge~ one of the measured indices for the rolled edge will be near 1-54 with the unrolled plate exhibiting indices near 1-590Lewin also claimed that parallel extinction of these edges and other fibrous-looking particles precludes their being talc. Talc always shows parallel extinction when viewed parallel to the plates or when rolled into fibrous-looking tubes. His claim that the "intergrown chrysotile" represents a new variety with different physical properties and structure from the normal fibrous variety is totally without sound scientific evidence. No such discovery has been claimed in the rather extensive literature on talc and chrysotileNeither Lewin's x-ray data nor his optical data supports his claim that chrysotile is present in Shower-toShower. J&J-0130732 JNJAZ55_000017752 Protected Document--Subject to Protective Order D-8372 Page 201 of 247 ~ 0 • ..:i < :z0 C 0 () ;a 0 Q. (,J p. Ill al 5 = 0 .J"' Z Ill;:, ~ i-= ;t w Z 0 IJ "' :E !II: w fJ ~ >< U 0 w z >A -t Joi 2: ~ ~ ~ : !,: ~ ~ ~ iI(:::,a . "'z :ii p: ... ii ig 0 - p; :i: u ~ :z: ... ::, 0 ~ ~ f? 0 = LI Cl: i: ~ ~ ;di 3: u (1) •., ~ 2 .,Ill... • Inc = •. ;; "E E • II 0 ti !! 0 ~ C: 0 •OI 0 • 'Cl 0 'O . II • m Cl ~ 23-681 23-685 J&J-0130733 JNJAZ55_000017753 D-8372 Page 202 of 247 644 McCRONE, DR. WALTER C. JR, b. Wilmington, Del, June 9, 16; m. 56. CHEMISTRY. B. Chem, Cornell, 38, Ph.D. (chem. micros), 42; Chem. microscopist, Off. Sci. Res . &. Develop. Proj. Cornell, 42-44; Armour Res. Found, Ill. Inst. Tech, 44-45, supvr . anal. chem, 45-46, asst. chmn. chem. & chem. eng, 46-52, sr. scientist, 52-56; WITH McCRONE ASSOCS, 56-, McCRONE RES. INST, 60 Crystallography; chemical microscopy; polymorphism; crystal growth; correlation of solid state properties and performance; ultramicroanalysis; physical methods of analysis. Address: McCrone Associates, 501 E. 32nd St. Chicago, Ill. 60616. From: American Men of Science, 1966 J&J-0130734 JNJAZ55_000017754 D-8372 Page 203 of 247 645 IAN STEWART Born: Great Britain Education: B.Sc. University of Aberdeen, Scotland 1956 Geology and Petrology Employment: 1956-1970 Head Physical Analysis English Electric 1970-Present Manager of Electron· Optics ~ccrone Associates. J&J-013O735 JNJAZ55_000017755 D-8372 Page 204 of 247 waiter c. me crone associates, inc. 646 CONSULTING: ULTRA~ICROANALYSIS • MICROSCOPY• SMALL PARTICLE PROBLEMS· SOLID-STATE CHEMISTRY 21 August 1972 Dr, A. Goudie Johnson & Johnson Research Center 501 George Street New Brunswick, New Jersey 08901 Dear Al: I thought that before we met with Dr. Brown at Princeton you and be might wlsb t.o see the x-ray data that we bad produced on your Shower-to-Shower products. I am therefore enclosing a preltmlnary report on this work, together with Xerox copies of all the x-ray traces. I would also like to thank you for the very complimentary letter which you sent to Dr. Mccrone about our work on this project. Although you aimed your compllments specifically at me, I take it that you really mean the team as a whole. Without the work that Gene Grieger and Ralph Hinch put in, particularly on the midnight shift on the night of the 10th, any contribution that I could have made t.o the FDA meeting would ha.ve been only superficial. Finally, a lot of the credit for the FDA presentation must go to the J & J people who, as ever, were helpful, courteous and encouraglng while the work was in process, Yours sincerely, 1~. Ian M. Stewart Senior Research Physicist IMS:ajw Ref: MA 2540 Enclosure 2BW SOUTH MI CHIGAN AVENUE· CHICAGO. ILLINOIS 606 16 • 312/842 -7100 • CABLE: CHEMICRONE J&J-0130736 JNJAZ55_000017756 Protected Document--Subject to Protective Order D-8372 Page 205 of 247 647 PRELIMINARY NOTES ON THE EXAMINATION OF SBOWER-TO-6HQWER PRODUCTS FOR JOHNSON AND JOHNSON Because of allegations that a sample of Johnson & Johnson's Shower-to-Shower talcum powder contains approximately 4% cbrysotile, several samples of this pro- duct have been examined by x-ray diffraction, electron microscopy and, In some cases. optical microscopy. At the start of this investigation the sample alleged to contain cbrysotile was 11ot available and therefore 15 samples covering the production span during which thls sample would have been manufactured were examined by x-ray dlffractlon and electron microscopy. Neither technique revealed any evidence of cbrysotlle. Later. the sample which had been alleged to contain chrysotile was obtained and this was similarly examined: again no chrysotUe was detected. Two additional samples, fden- tlfled as sample BEG and sample MID, representing the start of the production run and the middle of the production nm from which the alleged chrysotile contalnlng sample was manufactured, were also examined and nelther of these showed cbrysotile. These last three samples were also examined petrographlcally and again no cbrysotile was found. To comment brlefiy on our results tn comparison with those of Professor Lewtn in the talc samples which we looked at we do have a doublet which occurs very close t.o the cbrysotile line and it ls possible that Lewin confused one of these peaks with the chrysotlle peak. However, if this is tbe case I would suspect that the level of cbrysotlle, 11 you really computed lt on this peak. would show as very much higher than the figure he ls quoting. Furthermore, as you know, we did not detect the higher order chrysotile line which we maintain should be present and which Lewin says is absent due to preferred orientation. Preferred orientation would not eliminate this line. since lt ts a fourth order refiectlon (004) from the same planes of which the 12. 210 28 le a second order reflection (002). orientation ls falactous. Thus it ls clear that the argument of a preferred To further substantiat.e that this line was not chrysotile, we ran both a cbrysotlle standard and our sample number 6 (the batch dated 3-2-71) which we spiked with 5% chrysotile -and clearly show a third peak occurring between J&J-0130737 JNJAZ55_000017757 Protected Document--Subject to Protective Order D-8372 Page 206 of 247 648 the previously mentloned doublet. Thus we are satlsfted that Lewin'a interpretation ts erroneous. I would stress that our argument with Lewin is on interpretation: the x-ray dlfiraction curves which he bas agree completely with those which we have. Finally. we also ran powder diffraction samples using a 57. 3 mm camera on our chrysotile standard and on t!le same talc number 6 and were unable to find chrysotile in sample number 6. although previous work with you had lndlcated that we were picking it up by photographic techniques at around the 1-2% level. In conclusion. then, we have identical x-ray diffraction data to those of Professor Lewin which in our opinion show no evidence of cbrysotile. To support our opinion the facts we present are firstly, the absence of a higher order reflectlon from the same pl~e as that on which Professor Lewin bases bls identification; secondly, when a sample ts intentionally spiked with chrysotile the presence of a new line near the peak on which Professor Lewln bases his conclusion together with lts higher order reflection; thirdly, the absence of any evidence of chrysotile by either light microscopy or electron microscope combined wlth electron diffraction. -2- J&J-013O738 JNJAZ55_000017758 Protected Document--Subject to Protective Order D-8372 Page 207 of 247 tD IC . 3z~ . :5 • .., 0 ;: 0 Q 0 !:) 0 ). lol ~ u al ol t: ] Ill < . z Ll ~ z .!: 0 Ill IE .." ci !: ui "'• «I :j m ::i "':E ~ w "'::> >< O 0 .., Cl :5 z • < w a: "" iii iH; J • IJ 0 !:J iii ... Ill~ Ill ::, ::,c ~ Ill U •Ll zIJ :C ~ 0 !J ,.J < a: z: ::i 0 0 z• 0 .a j:: M ~ fiIll ~ ~ !i ~ • ., E ~ :! 0 'O ........'"I ;;· ~ ~ ~ .• !: "0 . Q 'O Cl 'O Cl 'O • II Cl ID .• s: 23-681 23-685 J&J-013O739 JNJAZ55_000017759 Protected Document--Subject to Protective Order D-8372 Page 208 of 247 649 COMMENTS ON ~R. LEWIN 1S TECHNIQUE I will consider only his optical cryst.allograpbic techniques. As I understand Dr. Lewin he treats talc and asbestos as though they a.re both isotropic. Although this is not so ln either case, he justifies this action on the basis that talc in the plate view and asbestos in any orientation bas low birefringence - talc: 1. 594-1. 600 or o. 007). 0. 006; chryso~ile: 1.549 - 1.556 or This ls not too bad but he uses a re- fractive index liquid, 1.580, to differentiate between these two compounds. If an apparent needle shows an index less than 1. 580 it Is chrysotile. Yet, if talc plates are tipped only a few degrees, say 20-30°. the index of talc is no longer 1. 594-1. 600 but in one orientation relative to the plane of vibration of polarized light is less than 1.580. In other words, talc plates on edge are "chrysotile" by Dr. Lewfn's procedure. If, however. he simply rotated the stage 90° chrysotile would miraculously revert t.o t.alc. Every crystal of talc will always show one refractive index (in one orientation relative to the polar) higher than 1.580. It will show both indices higher than 1.580 only when lying flat or nearly flat. Cbrysotile will never show an index above 1.580. Dr. Lewin also uses birefringence to differentiate between chrysotile and talc. He seems to feel that talc always shows low birefringence and asbestos high The birefringence of talc ls low when viewed per- birefringence. This ls not so. pendicular to the plate but high (much hlgher than ch.rysotile) when the plate ls tipped. The figures are: N2 Nl Nl - N2 Talc (plate vtew) 1.600 1.594 0.006 Talc (on edge) 1.600 1.550 0.050 Cbrysotile 1.556 1.449 0.007 Concluslon-"a little bit of knowledge is a dangerous thing." ~~-"'-~ Walter C. Mc Crone Sc lentlf ic Advisor J&J-01307 40 JNJAZ55_000017760 Protected Document--Subject to Protective Order D-8372 Page 209 of 247 waiter c. me crone associates, inc. 650 CONSUL TING : ULTAAMICAOANALYSIS •MICROSCOPY• SMALL PARTICLE PROBLEMS• SOLID-STATE CHEMISTRY 29 September 1972 Dr. A. J. Goudie Johnson & Johnson Research Center 501 George Street New Brunswick. New Jersey 08901 Dear Dr. Goudie: Here are the comment.a you asked for on Professor Lewin's presentation at the last FDA meeting held on 21 September 1972. My remarks must naturally be made in the context of what occurred at previous meetings. I have also attached Dr. McCrone's comments. X-ray Diffraction At the early FDA meeting Professor Lewin had stated that chrysotile was present in your Shower to Shower product at about the 5% level. You wfil recall that there was some dispute between him and myself regarding the interpretation of this data. Basically the difference of opinion is that Professor Lewin was identifying chrysotile on the basis of one line which occurs at a 28 value of approximately 12° and I maintain that when this line is present it should be accompanied by a line of approximately equal intensity at the position of approximately 24.6° 29, the latter line being a second order refiection of the first line and both of them belng due to basal planes in the system. In the nomenclature of x-ray crystallography, the first line is referred t.o as a (002) line and the second a (004). Dr. Lewin, however, had claimed the absence of the (004) line In his data on the basis of preferred orientation, an argument that ls clearly preposterous: it would be equivalent to saying that opposite faces of a cube can be non-parallel and the cube would still be a cube. At the second meeting Professor Lewin seemed to deemphasize his x-ray data. The amount of cbrysotile which he was quoting for your material bad been revised to approximately 2%. He still had not step-scanned the peaks concerned. He still does not have the higher order reflection showing. I think the point that Professor Buegm.raised-that at least 3 lines are necessary for the identification by x-ray diffraction of a phase present-is important, but I think equally important in this case is the fact that the absence of the (004) reflection means that we certainly do not have cbrysotile. During the whole meeting, however. Professor Lewin played his x-ray diffraction data in very low key and in fact I cannot recall him mentioning it, except in reply to questions from other people. 2620 SOUTH '.llCHIGAN ,"V!;NUE • CHICAGO, ILLINOIS 60616 • 312/642 •7100 • CABLE · Cl-iEMICAONE J&J-01307 41 JNJAZ55_000017761 Protected Document--Subject to Protective Order D-8372 Page 210 of 247 651 Dr. A. J. Goudie Page Two Light MicroSCopY I think Professor Lewin's light microscopy is a little suspect. I do not think be has been sufficiently critical of his observations and I do not think that he has fully appreciated the optics of the serpentine and talc minerals. He repeatedly referred 1D the refractive index of talc where be clearly meant the mean refractive index of a plate section, but completely ignored the refractive index normal to the plates. From our electron microscopy, our own light microscopy and our scanning electron microscopy. we know that there are thin shards and rtbbons of talc which can be seen on edge in many sections. These I think are what Professor Lewin Is calling chrysotile. What adds credence tD my belief is that he refers to the chrysotile as being quite obvious on the basls of lts high birefringence. However, the birefringence of cbrysotile ls less than 0.01 whereas the birefringence of a talc plate, if observed on edge, is 0.05, thus bis high birefringence particles are more likely to be talc. Many of the particles which he calls chrysotile occur on talc plates and it is noticeable that many of those are parallel to the edges of the plate. This is farily typical of cleavage steps on a cleavage plate which are curling at the edges and I expect" he has been misled by this. Chrysotile Formation Professor Lewin'a speculation on the formation of cbrysotile within the talc plates is extremely interesting. In one fell swoop he has completely reversed the normal order of petrogeneeis. Talc may form in three ways; one of these ways is not clearly understood and is the development of talc in rocks which are high in gypsum. The second and third ways involve the formation of talc from other rocks by hydrothermal solutions. These are the two main types of talc formation. The first one is by the further alteration of serpentine, the second is by the alteration of rocks containing a high proportion of calcite, dolomite and quartz. From the description given by Dr. Pooley, the latter mechanism is the operative one in this particular mlne. To postulate this ''new mechanism" and ''new type" of chrysotile with its x-ray and optical data also differing from the well characterized forms of chrysotlle, I think ts rather fatuous and aD attempt to extricate himself from a position into which he should never have allowed himself t.o slip. My personal feeling is that when asked to do petrographic work on these samples he should have realized that he was getting further from bis own field and should have recommended to the FDA that they place this aspect of the work with a compet.ent mineralogist/petrologist. In this way all the parties involved could have been saved a lot of trouble. Yours sincerely, IMS:ajw Ref: MA 2546 Enclosure Ian M. Stewart Manager• Electron Optics Group J&J-0130742 JNJAZ55_000017762 Protected Document--Subject to Protective Order D-8372 Page 211 of 247 ID C Q ~ C u r •. .s 2 .,..;,, • < !! u; : :> : ~ E ~ "~ . ~ C 0 •"' V • .. "• • • 'Q CD . .,; () ,00 .., rot C..• s· oCl>' Ill {Al (') . ::r-: 0 ~ --, 0) .& ~ NATI ONA&. 23-681 23-68.S J&J-01307 43 JNJAZ55_000017763 D-8372 Page 212 of 247 652 MR. T. CANEER Born: USA Education; Employment: B.A. Geology, University of Missouri M.A. Geology, University of Missouri Assistant Manager Mining Division and Chi~£ Mineralogist -Present Colorado School of Mines Research Institute . if . J&J-01307 44 JNJAZ55_000017764 D-8372 Page 213 of 247 653 COLORADO SCHOOL OF MINES RESEARCH INSTITUTE P. O. Box 11 Z GOLDEN , COLORADO 80401 September 7. 197 Z Dr. Bob Rolle Johnson & Johnson West Research 501 George Street New Brunswick N.J 08903 Dear Dr. Rolle: In compliance with a request from Dr. Goudie I have made X-Ray diffraction studies on the sample of talc product (shower to shower) which he sent. The objective of these studies was to determine the nature of a reported double X-Ray diffraction peaks in the vicinity of 7 to 7. 5 angstroms. More specifically he wanted to determine if the reported data resulted from the occurrence · of chrysotile. The enclosed X-Ray diffraction scan for the sample indicate3 the presence of talc and chlorite. Since the major peaks of chrysotile occur near· the chlorite peaks. step scanning was used in order to better determine il any chrysotile peaks occur. The enclosed three charts show the results of these scans. I first scanned the vicinity of the second order chlorite peak (7. 0-7. 2 angstroms) since a major chrysotile peak occurs at about 7. 4 angstroms. As may be seen on chart 1. a chlorite peak occurs at 7.1 angstroms. This peak contains a shoulder which occurs at about 7. ZZ. angstroms. The position of this peak indicates that it is also a chlorite peak (the variety of chlorite called penninite contains a diffraction peak in this vicinity). Chrysotile should give a peak representing about 7. 3 6 angstroms (about 12. 0° z 8). However. realizing that X-Ray diffraction equipment alignment and compositional variations are critical. the area around the first order chlorite peak {6. o to 6. 5° Z 8) was also step scanned. If the 7. 22 angstrom peak (shown in chart l) results from a second order chlorite peak then its first order peak should occur at about 14. 4 angstroms. Chrysotile does not have a peak of these dimensions. As may be seen in chart ?., a major peak representing 14. l angstroms occurs which is the first order peak of the major chlorite peak shown in chart 1 (at 7.1 angstroms). However. this peak,also haS a shoulder which occurs at about 14.47 angstroms. This indicates that the shoulder (7. zzA or 1 z. 2.5° 28) shown in chart l is probably chlorite and not chrysotile. In order to be more complete. the region in the vicinity of 3. 7 to 3. 5 angstroms ( 24° to 25. 5° 28) was step scanned. As shown on chart 3 two peaks occur. One at 3. 54 angstroms. which is the fourth order of the 14. 1 angstrom chlorite peak.. The other occurs at 3. 61 ! which would be the fourth M1tum1J Industry R~seorclr J&J-01307 45 JNJAZ55_000017765 Protected Document--Subject to Protective Order D-8372 Page 214 of 247 COLORADO SCHOOL Dr. Bob Rolle OF MINES RESEARCH INSTITUTE Page 2 654 September 7, 1972 0 order of the 14. 47 A peak which is also likely to be chlorite. No peak was observed in the vicinity of 3. 66 angstroms where the ASTM file card shows the fourth order chrysotile peak. The above data does not indicate the presence of chrysotile. Sincerely. ~~ W. T. Caneer Assistant Manager Mining Division WTC/psk cc: Mr. Bill Ashton (without enclosures) Dr. Goudie (with enclosures) J&J-0130746 I JNJAZ55_000017766 Protected Document--Subject to Protective Order D-8372 Page 215 of 247 .,"' ~ ., oi ··. )l ... oi .~ ... N~ oJ . : r,.: · J. ('J : nJ ~ "' . !:: · ., · ~ = ILJb-~6--oL1 -~·e~~6---~f'-•~~~~6-~~-~1 ~ ~ •..-. :g .~ . ,; ~ ~ ;;; .~ ~ ·~~~- -0~--~0~~0~~0--- 0~~0~~0-Jo__OL_OL~o~ ~. ~ ~ .~ : . ~ .: N · 2, ~ ! !:: JNJAZ55_000017767 Protected Document--Subject to Protective Order D-8372 Page 216 of 247 1:J a~ n ~ I C. &5- - z :5 i • t 0 I) II. 0 I( IJ :: ..I DI Ill::, e •• u !: Z ~..: ~ ~ z "' ~ as lJ r.i ;:I . e e •• :iicoO w z >~ a: ... IQ ,( DI Q :!': ~ I; ~ z :z: • a, '0 ;r; ) • 'O GI ~i~ i::: < w 0 C zO - a: z ""::, a 0 :j 0 .,, ~ jl: < £ !! ::i :i:: I( al u IQ •E ... :E'0., ..; ~ ~ ..I Ill .fi en ,.•• t <( i:: • •• m . '0 ta :S ....c• .& )lj N,1/jTIONAL 23-681 23-685 J&J-0130750 Protected Document--Subject to Protective Order JNJAZ55_000017770 D-8372 Page 219 of 247 COLORADO SCHOOL OF MINES RESEARCH INSTITUTE 658 P. O. Box IIZ GoLOEN , COLORADO 80401 October 2,. 1972 REl'DTO Cl0704 Dr. A. J. Goudie Director. Analytical and Sterilization Section Johnson & Johnson West Research 501 George Street New Brunswick NJ 08903 Dear Dr. Goudie: I will first comment on my impressions of Dr. Lewin's presentation before the FDA board. I got the impression that Dr. Lewin was trying to be expert in perhaps too many fields. As a result he had only enough knowledge in many of the scientific fields to confuse the issue -- the identification of chrysotile in talc. I must adda howevera that he does give quite a convincing presentation if one has only a little. or, no knowledge of mineralogy. One example of his lack of knowledge in mineralogy was related to x-ray diffraction identification of minerals. He wasn't aware of the fact that chlorite occurs in more than one variety. He apparently has been indicating that chrysotile is present in a sample by wrongly using chlorite x-ray diffraction data. He was apparently very confused relative to optical microscopy based on his ideas on indices of refraction. He also stated to me that atomic packing or density had no bearing on indices of refraction. This is not so. I will next comment on the FDA meeting in general. Since the accepted FDA method for determining if chrysotile is present in talc is by first screening with x-ray diffraction. If the presence of serpentine is suspected then the sample is subjected to optical examination. The FDA is aware that x-ray diffraction will not pick up traces of chrysotile ( serpentine). They are probably also aware that if one looks long enough by optical methods he may find a fiber of chrysotile in any talc {or in anything else) which may have resulted from contamination from the air. Such a stray fiber should not condemn talc. However a /'.-fincral /,1dus1,y R,r,,r(lrch J&J-0130751 JNJAZ55_000017771 Protected Document--Subject to Protective Order D-8372 Page 220 of 247 COLORADO Dr. A. J. Goudie SCHOOL OF MINES Page 2 RESEARCH INSTITUTE October 2_. 1972 under the present scheme of things it apparently would be enough to cause a ban of the talc. The screening of talc by x-ray diffraction provides a method for not allowing this to happen. since this method is not that sensitive. My point in this is that Dr. Lewin apparently finds cause to go to optical methods based on the observation of a 7 A peak from x-ray diffraction. As I pointed out at the last FDA meeting,. the 7 A peaks in the Italian talc were caused by chlorite. Since practically all talc contains chlorite. the x-ray d{ffraction screening will be negated if one just looks for a 7 Apeak by x-ray scanning. I suggest that chlorite is checked for by x-ray diffraction when a 7 A peak is encountered before going to optical methods. This should be done by step scanning the 7 A and 14A regions. If a 14.A peak is found corresponding to the 7 A peak then they both belong to chlorite. Thus there is no need to go to optical methods. Sincerely., ~;,,,~ W. T. Caneer Assistant Manager Mining Division /laj cc: Wm. H. Ashton J&J-0130752 Protected Document--Subject to Protective Order JNJAZ55_000017772 D-8372 Page 221 of 247 J&J-0130753 JNJAZ55_000017773 Protected Document--Subject to Protective Order D-8372 Page 222 of 247 University College, Cardiff 660 Postal Address: University College, Newport Road, Cardiff CFz ,TA. Telephone Cardiff 44211 Telegrams: Coleg Cardiff from.- .... •________ Dr · .... F. D · ..... Poo_l ey ···-··························•·••········ Department oL ...J1.!.P.:~!:~.l.. .... ~~PJ9..1.c.t..<'.l-_1:j,QJ:l. ................ Examination of 'Shower to Shower' Talc Sample for Johnson and Johnson The tshower to Shower' talc specimen was subjected to electron microscope examination, X-ray analysis and also to density separation tests. The density separation tests were .performed in a heavy organic liquid composed of a misture of tetrabromoethane and carbon tetrachloride. The density of the fluid was set at an S.G. of 2.5. being intermediate between the density of chrysotile and talc. Visually all the sample suspended in the liquid was found to sink indicating the sample had a higher density than 2.5. An examination of the visually clear solution at the top of the separating vessel showed that no particles were present, thus indicating no free particulate material with a density below 2.5 thus precluding the presence of chrysotile. X-ray examination of the specimen indicated that no amphihole asbestos at the level of detection of the X-ray technique (i.e. 1.0%) was present. Electron microscope examination of the sample revealed no chrysotile fibres in the sample. Samples of 'Shower to Shower' talc diluted with chrysot~le at the 1 and 5% levels showed that if chrysotile were present it should be detected at below the 0.05% level by Electron microscope examination. The conclusions to be drawn from the examination are that no detectable chrysotile or amphibole asbestos is present in the 'Shower to Shower' talc sample. F.D. POOLEY 27th September, 1972. J&J.0130754 JNJAZ55_000017774 Protected Document--Subject to Protective Order D-8372 Page 223 of 247 J&J-0130755 JNJAZ55_000017775 Protected Document--Subject to Protective Order D-8372 Page 224 of 247 University College, Cardiff 661 Postal Address: University College, Newrort Ro3d, Cardiff CFl ,TA. Telephone Cardiff 442 1 1 T dcgrams: Coleg Cardiff .f rom ................_..Px.~.....f..~.P..~ .....?oo l eY. ............................................. . Department of.. ..........Mi.n.eX.g.l .. _.l;;.~pJ.QJ.t .~tlgn_...... .. FOP/MM 29th September, 1972. Dr. A.J. Goudie, Director, Analytical Research Section, Johnson and Johnson, New Brunswick, New Jersey, U.S.A. Dear Dr. Goudie, The results presented by Dr. Lewin at the F.D.A • . meeting would appear not to be capable of substantiating the presence of quantities of chrysotile asbestos. The x~ray procedure adopted was shown to be very insensitive to the detection of 1% chrysotile, while the major identification of chrysotile was based only on the observation of a slight difference in refractive index, which could have been explained by variation in orientation of talc particles or the presence of another mineral. As the refractive index of the unknown material appeared to be lower than that of talc, it was stated that chrysotile was present because it had a slightly lower refractive index. However, so have many other minerals, including magnesite which is a well known contaminent of talc. RI talc l. 539 -1. 550 RI chrysotile RI magnesite 1.589 1.594 1.532 1. 549 1.417 1.523 1.589 1.600 1.545 1. 556 1.507 l. 545: variation in refractive indices therefore only indicates an orientation difference or perhaps the presence of another mineral phase. J&J-0130756 JNJAZ55_000017776 Protected Document--Subject to Protective Order D-8372 Page 225 of 247 University College, Cardiff 662 Postal Address: University College, Newport Road, Cardiff CF2 rTA . Telephone Card iff 44211 T elegrams: Coleg Cardiff ·From ...... __Dr •.... F •. D •..... Poo.ley ............... ·--·-·····-.. ··-·-··-·.. ···· .. De partment of.. ..........~lm~.f .~J... -:,;;.?.CPJ.QJ.~-~.tJQ[L ...... . The positive identification of chrysotile can only be made with a transmission electron microscope because i t is with this instrument that the fibre can be observed and defined. The name Chrysotile and Chrysotile asbestos belong only to that material with a fibrous structure composed of fibrils 250-350 Angstroms in diameter if these are not observed in a sample i t must be concluded that the material is free of Chrysotile. It 1s suggested, therefore, that talc samples should be examined by a mineralOgical laboratory with transmission electron microscope facilities as it has already been shown to be the only way of detecting and assessing chrysotile in other materials. It would also be interesting to see whether the amounts of supposed chrysotile detected by Dr. Lewin do in fact vary with carbonate mineral contamination of the talc samples. DR. F.D. POOLEY J&J-0130757 JNJAZ55_000017777 Protected Document--Subject to Protective Order D-8372 Page 226 of 247 D-8372 Page 227 of 247 - I :1 Differ! 30758 663 --- ..... POLLACK. DR. SIDNEY S(OLOMON), b. New York, N. Y. Sept. 24, 29; m. 53; c. 2. CRYSTALLOGRAPHY. B. S, Mich. State, 51, M. S. 53; Ph.D. (soil sci), Wisconsin. 56. FEL. X-RAY DIFFRACTION, MELLON INST, 56Soil Sci. Soc; Mineral. Soc; Crystallog. Asn. Clay mineralogy; polymers; low crystallinity carbons; small-angle x-ray diffraction and crystallography; meteorites. Address: Mellon Institute, 4400 Fifth Ave, Pittsburgh, Pa. 15213. From: American Men of Science, 1966 J&J-0130759 JNJAZ55_000017779 D-8372 Page 228 of 247 Carnegie-Mellon Un1vers1ty Mellon Institute 4400 Fifth Avenue Pittsburgh, Pennsylvania 15213 [412] 621-1100 Division of Educational and Research Services September 27, 1972 Dr. A. Goudie Johnson and Johnson Research Center 501 George Street New Brunswick, New Jersey 08901 Dear Dr. Goudie: The meeting with the representatives of FDA was an enlightening experience for me and I am happy to give you some of my impressions from the meeting. Although Dr. Le,-rin said that chrysotile was present in t~o samples, he presented no objective evidence. Since x-ray diffraction cannot be used to make a positive identification of asbestos ~hen it makesup less than about three percent of a sa111ple, the combination of electron micrographs shtWing a hollow fiber, and then the characteristic electron diffraction pattern from the fiber, make the most definitive identification. Dr. Lewin did not show these. Optical microscopy is another sensitive technique for identifying very small amounts of asbestos but no evidence of crystals with the indices of refraction characteristic of chrysotile was presented. Dr. Lewin's identification of asbestos appeared to be based on the presence of particles which he thought looked like asbestos. He could not support his identification with any of the necessary electron microscopy, electron diffraction or optical microscopy evidence. To me, Dr. Lewin indicated his lack of fundamental understanding of crystallography at the very beginning of his presentation when he showed a scale model purporting to be the mineral talc. In this model, he had the basic platy units of talc which are about 10 Angstroms thick, 20 Angstroms apart because the£ unit cell is about 20 Angstroms. Dr. Lewin didn't understand that the manner in which the platy units pack and not the distance between them determined the£ unit cell dimension. It is disconcerting that the many capable government mineralogists were not consulted about this problem. Siiy:erely, ff J. _ -~t,,-L -'J I rl~ l S.S .. P~llack, Fellow L. SSP: jdf X-Ray Diffraction Laboratory J&J-0130760 JNJAZ55_000017780 Protected Document--Subject to Protective Order D-8372 Page 229 of 247 665 Carneg1e~ellon Un1vers1ty Mellon Institute 4400 Fifth Avenue Pittsburgh, Pennsylvania 15213 [412) 621-1100 Division of Educational and Research Services September 28, 1972 Dr. A. Goudie Johnson and Johnson Research Center 501 George Street New Brunswick, New Jersey 08901 Dear Dr. Goudie: The meetings with the people from Johnson and Johnson, the consultants and FDA were very educational and interesting. It is really hard to believe that Lewin still clings to the notion that there is asbestos in the talc. I did not carry out any significant experimental work. but based on all the x-ray evidence, I would agree that there is no positive evidence for the presence of chrysotile in the SHOWER TO SHOWER product. Since the least detectable amount is 1-3%. this means that the x-ray diffraction says there is less than l-3% serpentine. The nice DTA work indicates that there really is less than 1% chrysotile. In my view, the transmission electron microscopy and electron diffraction evidence are the best indicators that there is no chrysotile in the sample. The optical microscopy is also good evidence, but I suspect that in certain samples, one might have chrysotile fibers that could be seen using TEM and electron diffraction but not seen by optical microscopy. I am glad that you felt my discussion the day before the FDA meeting was helpful and hope that I might be useful at some other time. It was a pleasure to meet the people from Johnson and Johnson and the other consultants. Sincerely, --~-~-~ S.S. Pollack. Fellow X-Ray Diffraction Laboratory SSPjdf cc: J. J. McGovern J&J-0130761 JNJAZ55_000017781 Protected Document--Subject to Protective Order D-8372 Page 230 of 247 J&J-0130762 Protected Document--Subject to Protective Order JNJAZ55_000017782 D-8372 Page 231 of 247 666 Hew Brunswic,., N.J. September 28, 1972 Subject: ANALYSIS OF SHOWER TO SHOWER* POWDER FOR CHRYSOTILE ASBESTOS - PROJECT NO. 503 X-Ray Diffraction Qualitative analysis by means of a continuous X-ray diffractometer scan was performed on the sample of SHOWER TO SHOWER Powder which had been analyzed by Dr. Lewin. The following mineral content was indicated: Major: Minor: Trace: Talc Chlorite Dolomite, Calcite, Magnesite, Quartz In addition, an extraneous X-ray diffraction peak occurred at approximately 7.28A, at very weak intensity. This peak was thought to indicate a trace amount of either a second variety of chlorite, or kaolinite. The X-ray diffraction step-scanning technique was then employed for the purpose of further identifying this trace mineral impurity. Figure 1 shows a duplicate determination of the exact position of the extraneous peak (7.25A). Step-scanning revealed an additional diffraction peak at 3.62A (Figure 2) and a shoulder at approximately 14.49A {Figure 3). The existence of these three peaks was accepted as confirmation that the unknown mineral impurity was, in fact, a second variety 0£ chlorite. It was desired to determine the minimwn detectable level of chrysotile asbestos in talc by the X-ray diffraction technique. Homogeneous standards consisting of 1%, 3%, and 5% by weight of chrysotile in SHOWER TO SHOWER Powder were prepared and step-scanned in the vicinity of the chrysotile peak. The 5% sample (figure 4) showed a diffraction peak at 7.311 corresponding to chrysotile. This peak was easily detected in the 3% standard (Figure 5), but could not be detected at the 11 level. *A Trademark of JOHNSON & JOHNSON. J&J-013O763 JNJAZ55_000017783 Protected Document--Subject to Protective Order D-8372 Page 232 of 247 667 - 2 - The continuous X-ray diffractometer scans of SHOWER TO SHOWER Powder exhibited by Dr. Lewin indicate the absence of chrysotile in this talc. This is evident from the lack of diffraction peaks in the regions where chrysotile shows intense reflections (7.31A, 3.65A). Differential Thermal Analysis A differential thermal analysis (DTA) method was developed for the detection and quantitative estimation of chrysotile asbestos in talc at low concentrations. This is possible because of the existence of the two intense thermal transitions of chrysotile which are free from talc interference. These transitions consist a dehydroxylation endotherm with peak at 650°C. and an exothermic thermal decomposition peak at 820°C. (Figure 6). This thermal behavior is typical of chrysotile from sources all over the world. Thermograms of Italian talc (Figure 7} and SHOWER TO SHOWER Powder (Figure 8) indicate the presence of less than 5% each of chlorite and carbonate (mainly dolomite) impurities. Figures 9-11 show thermograms of standard samples of 5%, 3%, and 1% by weight of chrysotile in SHOWER TO SHOWER Fowder. The arrows indicate chrysotile transitions. The 1% sample represents the minimum detectable level of chrysotile in talc by DTA. The thermogram of the SHOWER TO SHOWER Powder examined by Dr. Lewin (Figure 12) shows no thermal peaks in the temperature ranges characteristic of chrysotile; while 1% chrysotile added to this sample is readily detectable (Figure 13). On the basis of this experimental evidence, there is no chrysotile asbestos in SHOWER TO SHOWER Powder at a 1% level or greater. of The theory of chrysotile fibers located within talc particles proposed by Dr. Lewin is erroneous with respect to detection of these fibers by DTA. The majority of the "fibers" detected by Dr. Lewin are located on the edges of talc platelets, not completely embedded in the talc particles. As such, and if these "fibersu were actually chrysotile, then they would of necessity undergo thermal transitions characteristic of the chrysotile structure. Since by OTA there is no chrysotile detected in the SHOWER TO SHOWER Powder at the proposed 2% level, the Lewin theory is shown to be in error. ab Senior Research Scientist Analytical Research J&J-0130764 JNJAZ55_000017784 Protected Document--Subject to Protective Order D-8372 Page 233 of 247 668 FIGURE 1 115 ,,o ,~ - 'l~ ioS" ~ ..., ~ :s 3 4o ,00 Vo.+----:~__,~----1--.------...... ·,,.w0 no , 111> , J&J-0130765 JNJAZ55_000017785 Protected Document--Subject to Protective Order D-8372 Page 234 of 247 669 FIGURE 2 ,~,oo '°o+---------------.... ----+--...-----------------.,o .eo ~DO •3o •of• ,1ro -~o ,?o p~o •Cfo -CS.co o;l(9 J&J-0130766 JNJAZ55_000017786 Protected Document--Subject to Protective Order D-8372 Page 235 of 247 ,,,,t,,., FIGURE 3 67{ \"° ,~ ,~..,_--P-_..,...._.,..._...,.__-r_-r---r----------------------5,,0 .,0 C..C0 .,o ,:2-0 ,30 - ~ 0~8 J&J-0130767 JNJAZ55_000017787 Protected Document--Subject to Protective Order D-8372 Page 236 of 247 67 FIGURE 4 /50 . . . --~------.---+----t---9--~~~---------------''·'° .11) ... ~~ .JO 0 ,t.oO ,10 •&D •So ."4• •S'O •CO oc2e J&J-0130768 JNJAZ55_000017788 Protected Document--Subject to Protective Order D-8372 Page 237 of 247 672 I~ FIGURE 5 ~-1---......--+---+---1~---,..,o-......--.~-~ . . -.~.,~.---,.------------------'-"' ,z.. •.ra /I••" •70 .tO .•• .,.. 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