Document ZaRZkKjg62J672rv2N8m2nNO

FILE NAME Johnson & Johnson JAJ DATE 0000 DOC JAJ217 DOCUMENT DESCRIPTION Report - Concentration of Amphibole and Serpentine asbestos from Talc by froth flotation CONCENTRATION OF AMPHIBOLE AND SERPENTINE ASBESTOS FROM| TALC BY FROTH FLOTATION mM a) Protected Document to Protective Order JNJAZ55_000007947 i 1 ! | < TABLE 1 Flotation Results of 0.5 Asbestos Sample Test Sample Fraction p.p.m. p.p.m. Crocidolite Recovery K A 1 1 Conc 0.0 0.0 2 Tailing 8.4 6.0 100 12 ~ 3 Conc 1 0.0 0.0 4 Conc 2 0.0 .0 0 0.5 Crocidolite 5 Conc 3 0.0 2 6 Conc 4 | 0.0 0.0 0.0 7 Middling 2.16 8 | Tailing | 12.6 1.5 8.5 91.0 17 B m , 4 9 Conc 0.0 10 Tailing 8.0 22 Conc 1 0.0 22 Conc 2 0.0 13 Conc 3 | 0.0 14 Conc 4 0.0 15 Middling 2.0 16 Tailing 13.1 0.0 8.0 0.0 0.0 0.0 0.0 1.5 9.0 * 100 12 0.5 Crocidolite + 95 Chrysotile 90.0 18 C S 6 17 18 19 - 20 21 22 22 24 Mg p.p.m. g Chrysotile Conc Tailing 0.0 4 .0.0 | 1.18 |" 8.5 100 17 Conc 1 0.0 Conc 2 0.0 Conc 3 | 0.0 Conc 4 0.0 0.0 0.0 0.0 0.0 0.5 Chrysotile a Middling | Tailing . 0.30 0.30 1.70 2.0 13.0 90 26 Protected Document to Protective Order JNJAZ55_000007948 e @ examination and the ray tube was operated at 30 KV and 20 ma ^ diffractometer scan rate of 26 per minute was employed and the inlet and outlet slits were 1" 20 and 0.2 mm respectively Diffractometer traces of Italian talc chrysotile crocidolite and actinolite used in the separation experiments are given by Figs 5 - 9 Results The results of a number of tests upon a talc sample ' containing 0.5 chrysotile and 0.5 crocidolite by weight and also a sample containing both crocidolite and chryso- tile in 0.5 portions are given in Table 1. In Table 1 test No. 1 represents a single stage flotation separation of crocidolite and talc It can be seen that the concen- tration of crocidolite in the tailings is 6 by weight no crocidolite being detected in the floated talc Test No. 2 in Table 1 represents a two stage separation of crocidolite and talc In the two stage separation the tailings fraction from four single stage tests have been combined together and retreated to give a final tailings and a secondary flotation product referred to as middlings By employing two stages of separation it can be seen that the final tailings is richer in asbestos than a single stage flotation tailings However some asbestos is lost in the middlings fraction Tests 3 and 4 in Table 1 show the results of the crocidolite separation from the mixture of crocidolite and chrysotile Again a 6 tailings assay in a single step and a 9.0 assay for crocidolite in a two stage separation The chrysotile did not therefore interfere with the crocidolite separa- Protected Document to Protective Order JNJAZ55_000007949 TABLE 2 Flotation Results of % Asbestos Sample Te Test st No. Sample Sample No. Fraction Fraction Fraction Fe p.p.m. g Crocidolite " | Recovery A 7 25 Conc 0.30 26 Tailing 30.60 0.25 21.00 75.90 27 Conc 0.40 0.25 00 28 Middling 9.60 7.00 29 Tailing 55.60 39.00 81.25 Concentration Ratio Ratio | K a} | | 21 i % Crocidolite 39 B 30 Conc 0.10 0.00 } 9 . 31 Tailing 23.60 16.00 32 Conc 0.00 0.00 0.00 100.00 % Crocidolite + % Chrysotile 10 33 Middling | 11.60 8.00 34 Tailing 46.60 33.00 66.00 33 Mg p.p.m. % Chrysotile A 30 Conc 0.00 0.00 ; 31 Tailing 2.70 21.00 100.00 21 i 32 Conc 0.00 10 33 Middling 0.50 0.00 4.00 m= % Crocidolite + % Chrysotile | 34 Tailing 4.80 37.50 90.62 37.50 C 35 Conc 0.00 0.00 | 11 36 Tailing 2.60 20.00 ' 37 Conc 0.00 0.00 | 100.00 20 % Chrysotile . 12 38 Middling 0.60 4.50 39 Tailing 5.10 40.00 ~ 87.32 40 * Protected Document to Protective Order JNJAZ55_000007950 Test No. A 13 TABLE 3 Flotation Results of % Asbestos Samples Sample No. Fraction Fraction Fe p.p.m. Crocidolite 40 Conc 0.30 0.25 - 41 Tailing | 37.60 26.00 % Recovery 88.35 i Concentration ; Ratio Ratio ; 13 | | 14 B 15 16 1 . a 15 1 16 C 17 18 42 Conc 0.00 43 | Middling 8.60 44 Tailing | 74.60 0.00 6.00 52.00 45 Conc 0.30 46 Tailing 39.60 0.25 . 28.00 47 Conc 48 | Middling 0.00 6.60 0.00 5.00 49 Tailing | 61.60 43.00 Mg % p.p.m. | Chrysotile 45 Conc 0.00 0.00 46 Tailing 3.50 27.00 47 | Conc 0.00 48 | Middling 0.80 49 Tailing 5.15 0.00 6.00 40.30 50 51 Conc Tailing 0.00 3.50 0.00 27.00 Su Conc 0.00 Su Middling 1.70 54 Tailing 5.25 ; 0.00 13.00 41.00 86.96 89.09 92.95 % Crocidolit I 26 | i 14 % Crocidolite + % Chrysotil fF 21.5 | 100.00 13.5 % + Chrysotil % Chrysotil | 91.38 20.15 100.00 , 13.5 2 Chrysotile : 75.93 20.5 - | Protected Document to Protective Order JNJAZ55_000007951 , tion 17-26 17-26 @ : 7 4 Mater : | ; Tests 5 and in Tab1l she ow the results obtained from the separation ofa 0.5 chrysotile mixture In Test 5 the tailings were found to contain 8.5 chrysotile while test 6 shows that the tailings produced : from a two stage separation assayed 13.0 chrysotile by weight a considerable upgrading from the original 0.5 Table 2 contains similar results to Table 1 except all the tests were performed with 1 additions of crocidolite and chrysotile and a % crocidolite and chrysotile mixture eS a From test 7 in Table 2 we see that in a single step tailings containing 21 crocidolite was produced while in a single step for chrysotile test 11 tailings with ee 20 chrysotile was obtained The two stage separation chrysotile results for crocidolite and t given by tests 8 and 12 respectively show an improvement to 39 and 40 ee as compared with 29 and 20 in the single stage tests . Table 3 contains the results obtained from the ee separation of a series of samples containing % crocidolite and chrysotile respectively and also the results from a % crocidolite and chrysotile mixture In single stage ee separation containing for crocidolite test 3 a tailings 26 crocidolite was obtained while a tailings containing ee 52 crocidolite was obtained in a two stage separation Fy test 4 For chrysotile tailings fractions containing 27 and 40.3 chrysotile for single and two stage separa- tions respectively were obtained tests 15 and 16 ee talc results for the % crocidolite % chrysotile in The samples gave 28 and 43 for crocidolite in the tailings fractions from single and two stage separations and 27 ee Protected Document to Protective Order JNJAZ55_000007952 JNJAZ55_000007952 TABLE 4 Continued | Test NoNo.. a 13 Sample - No. No. Fraction 40 Conc , 41 Tailings % Crocidolite % Chrysotile A.A.S. X.R.D. A.A.S. | X.R.D. 0.25 0.00 26.00 30.00 42 Conc 0.00 0.00 14 43 Middlings 6.00 7.00 44 Tailings 52.00 54.00 Remarks % Crocidolite 15 45 46 Conc Tailings Tailings 0.25 228.00 8.00 0.00 29.00 47 Conc 0.00 0.00 16 48 Middlings 5.00 7.00 49 Tailings 43.00 43.00 29 Crocidolite % Chrysotile | i 45 15 46 . 47 16 48 49 Conc Tailings |- Conc Middlings Tailings ; . 0.00 0.00 27.00 0.00 29.00 0.00 28 Crocidolite % Chrysotile 6.00 7.00 i 40.30 | 38.00 50 Conc 17 ; .51 Tailings | ; NM Conc : ' 18 53 Middlings ; 54 Tailings a : | 0.00 27.00 0.00 30.00 0.00 0.00 13.00 | 12.00 41.00 : 43.00 % Chrysotile j Protected Document to Protective Order JNJAZ55_000007953 y TABLE 4 Comparison of the analysis of flotation products by ray Diffraction and wet chemical analysis Test Sample Fraction No. . 25 Conc 7 . 26 Tailings % Crocidolite | * Chrysotile A.A.S. | X.R.D. | A.A.S. | R.D. 0.25 | 0.00 21.00 23.00 27 Conc 0.25 | 0.00 8 28 Middlings | 7.00 | 6.00 29 Tailings 39.00 | 40.00 Remarks 1 Crocidolite 30 = Conc 0 0.00 | 0.00 31 Tailings 16.00 19.00 ; % Crocidolite % Chrysotile 10 33 Middlings 8.00 7.00 . 34 Tailings 33.00 | 36.00 30 ~= Conc 9 31 Tailings 32 Conc 10 33 Middling 34 Tailings 0.00 | 0.00 21.00 20.00 0.00 4.00 0.00 5.00 37.50 | 35.00 % Crocidolite % Chrysotile . 35 Conc 11 j . 36 Tailings : : 37 Conc : 12 38 Middlings 39 Tailings 0.00 0.00 20.00 | 19.00 0.00 |; 4.50 0.00 6.00 40.00 | 41.00 oo % Chrysotile Protected Document to Protective Order JNJAZ55_000007954 , 1 ] oe ! Oe oe a CONCENTRATION OF AMPHIBOLE AND SERPENTINE ASBESTOS FROM _. TALC BY FROTH FLOTATION INTRODUCTION A great deal of concern surrounds the possible asbestos content of talc powders used in cosmetic pharmacutical and other industrial and consumer products Asbestos minerals are known to be associated with the increased incidence of certain types of cancer and it would be of some industrial importance if it were_ possiblteo t talc powder reduce the level of to an insignificant asbestos minerals in a level with respect to their possible health hazard Froth flotation is a technique used wideltyo separate fine mineral particles and over 90 of the world's non ferrous minerals are produced from crushed and finely ground rock using this technique This concentration technique has been applied to the concentration of commercial and non commercial forms of asbestos minerals from talc It has been shown to be very efficient in reducing the asbestos content of a powder and producing a residue which is referred to in mineral separation terms as a tailings in which the asbestos minerals can be easily detected and quantified The technique has therefore a second significant use in the detection and quantification of asbestos minerals in talc powder samples Most quantiative mineralogical techniques are only capable of detecting asbestos mineral impurities in talc powders down to the Protected Document to Protective Order JNJAZ55_000007955 FIG 1 Laboratory Flotation Cell Protected Document to Protective Order JNJAZ55_000007956 % by weight level These techniques include ray diffractometry differential infrared impromet Of these thermal analysis techniques ray and diffrac- tion would appear to be the most useful It allows both a positive identification of the mineral phase to be made and also an accurate determination of mass fraction by comparison of the relative intensity of the asbestos mineral reflections from the powders being tested to those of a set of standard reflections obtained from talc powder samples spiked with various quantities of different asbestos minerals The use of froth flotation to concentrate asbestos minerals from talc is so efficient that their detection by the ray diffraction method is accurate to an order or magnitude lower than in the untreated powder i.e 0.1 or less Efficient separation or concentration depends upon the selection of the most amenable chemical conditions under which the flotation separation should be performed The separation is made in an aqueous environment in which both talc and asbestos are in suspension One of the minerals has to be hydrophobic or made hydrophobic in order to remove it from the aqueous suspension using air bubbles Talc has a well known natural hydrophobicity can be improved however by use of suitable cationic chemicals e.g amines which selectively adsorb onto the talc particles and improve their hydrophobic character Asbestos minerals have no natural hydrophobic character therefore no natural floatability and will remain in froth flotation cell while talc is being floated Some care however has to Protected Document to Protective Order JNJAZ55_000007957 @ @ be exercised in the choice of frothing agent which is used to produce a froth at the top of flotation cell in which the floated mineral is held and removed to ensure that it does not impart hydrophobic properties to any asbestos mineral particles It must also produce a froth which drains easily removing as low an amount of water as possible from the cell in which asbestos mineral particles may be in suspension The pH of the aqueous medium is also of importance in the separation as this can also affect the efficiency of the flotation by interfering with the properties of the frothing agant | and also influencing the natural .* floatability of the talc and asbestos minerals ThepH produces floculated control also non floculated system in which particles of asbestos and talc are separated in suspension The control of pH is also desirable when a chemical is used ' to increase the hydrophobic nature of the talc as it can easily be adsorbed onto the asbestos minerals as well Selection of the pH to produce minimum adsorption of the chemical onto the asbestos should therefore be made METHODS MATERIALS AND APPARATUS The froth flotation tests reported here were all performed in a modified Knapp and Bates flotation cell with a capacity of 3 litres of mineral suspension An impeller in the flotation cell keeps the mineral in suspension and also draws in air for flotation purposes It then mixes the air with the mineral suspension to , . Protected Document to Protective Order 1 JNJAZ55_000007958 of promote rapid adhesion particles to air bubbles the impeller was operated at 1500 r.p.m. The amount of air drawn into the cell approximately 17 minute The flotation cell used is illustrated by Fig 1 The minerals used for experimentation were as follows 1 Italian talc 00000 grade supplied by Zach Cartwright Ltd. Its general formulae Mg6 Sis 029 OH 4 2 Serpentine asbestos chrysotile which is the most common of the asbestiform minerals It accounts for more than 95 of the asbestos fibre produced today Its general formulae is Mg12 Sig 020 OH Like a sheet talc is silicate which occurs as very fine rolled sheetosf magnesium silicate 3 Amphibole asbestos two varieties of which were used these were Crocidelite SiO22 OH 2 Actinolite Ca MgFe Si OH 2 The chrysotile and crocidolite samples were supplied by the M.R.C. Research Unit Penarth Glam as being representative of all commercial asbestiform minerals of the serpentine and amphibole varieties Protected Document to Protective Order JNJAZ55_000007959 JNJAZ55_000007959 JNJAZ55_000007959 The Actinolite sample was included to represent the type of amphibole more likely to be found associated with tale The actinolite itself came from the same mine as the talc used in the experimentation but was not but found in association with the talc It occurred with other minerals and before additiotno the talc in a powdered form it was concentrated into a pure fraction using a Franz isodynamic magnetic separator The chrysetile and crecidolite asbestos were already in a very finely powdered form and required no size reduction before addition to the Italian talc for separa- tion experiments The actinolite was however first ground to a size similar to that of the talc before addition a Ordinary tap water was used in the flotation tests and the pH of the suspensions was adjusted using sulphuric acid and sodium hydroxide The frothing agent used was a commercial product Aerofroth 65 manufactured by Cyanmide Ltd. it is essentially a propylene of high molecular weight which is totally soluble in water and is therefore easy to add to the flotation cell It was found that a suitable concentration of 1.5 ml of a % volume solution of the frothing agent gave an easily i ; managed froth removing very little liquid from the flotation cell Flotation separation tests were performed with talc samples in which asbestos was added represent 0.58 1.0 and 2.0 asbestos by weight A series of tests with Protected Document to Protective Order JNJAZ55_000007960 a mixturoef amphibole and serpentine asbestos was also performed to investigate the concentrating action in the presence of two forms of asbestos The talc samples were weighed and added to the flotation cell and mixed _ thoroughly with water the weighed asbestos sample was then added and also mixed thoroughly into the talc suspension Care was taken to ensure the talc was completely wetted . melted by mixing thoroughly no wetting agents were used When the asbestos mixture was considered to be well mixed the frothing agent was added The air inlet to the cell was then and pH opened adjustment made and the floated talc removed from the top of the cell with a scraper The test was run until no visible talc was found to be reporting to the top of the cell care was taken to ensure no tale froth was sticking to the cell sides which might contamin-- ate the asbestos material remaining in the cell as tailings From extensive tests the most advantageous conditions for advantageous conditions for asbestos talc separation was found to be as follows Water in the cell pH adjusted to 2.02.0 with 3 litres sulphuric acid Solids concentrat2i0o -2n5 grams in 3 litre Frothing agent 1.5 mls of % v in 3 litre All flotation tests were performed using these conditions the only variables being the type and quantity of asbestos mixed with the talc Protected Document to Protective Order JNJAZ55_000007961 S rn _ 100 a no) = CROIDLTE FOR 9. Ti CURVE ~ E a a b4 1 > CALIBRTON 2 IG, 7 * w ~ T CALIBRATION CURVE CROIDOLITE oO o CALIBRATION CURVE CROCIDOLITE o Oo o CALIBRATION CURVE CROCIDOLITE = . PHIOPIIOID *7, JNJAZ55_000007962 Document--Subject to Protective Order JNJAZ55_000007962 To measure the separation of asbestos from talc a combination of wet chemical and ray diffraction tech- EE - niques were used For measuring crocidolite the iron concentration in the floated talc and also in the tailings HE was measured and the results compared with a standard curve prepared from the iron analyses of crocidolite HE mixtures Chrysotile was measured wet chemically by digestion measuring the magnesium level obtained by in HE hydrochloric concentrated acid and comparing the results HE with a standard curve prepared from the magnesium analyses of chrysotile mixtures The analysis technique for HEH both iron and magnesium were as follows . He a Wet Chemical determination of Crocidolite in Talc , - HE A small amount _ 0.05 - 0.1 gram of the sample was_ fused in a P.T.F.E. crucible at approximately 350 Ere with 2 mls of 1 KOH and water The fused pellet was then disssolved in 3 mls of concentrated Cl The solution was made up to a known volume and assayefodr iron using an E.E.L. 240 atomic adsorption spectrophoto- & meter The amount of crocidolite was obtained by checking against a standard calibration curve as shown in Fig 2 EE b Wet Chemical determination of Chrysotile in Talc , ra Samples FF were dispersed in concentrated HCl talc is not affected by HCl and heated till dry The samples were then retreated with dilute HCl The resulting m solutions were made up to a known volume and assayed for magnesium using an A.A.S. From standard calibration fe Protected Document to Protective Order JNJAZ55_000007963 . ; o a ~ x [Io w w = ~ Oo o uy - [aa x= rs) ras ' \ tw >. 4 i . . sary ow = > = Eo _ c Lc * z x o - . < & wm 4 to) < aw [om ~ 4 o \ io Th YN . t o o Lo] o t oO & CALIBRATION = CALIBRATION CURVE q o Nn CHRYSOTILE Pas . o Protected Document--Subject to Protective Order JNJAZ55_000007964 0.6 0-51 0-51 | o & . Intesity 0.3 0.3 Relative o 0 0 6 0! co 3 0 Relative Composition by Weight FIG 4 DIFFRACTOMETER CALIBRATION \ CURVE FOR CROCIDOLITE IN TALC- a penn F s O a8 co Protected Document to Protective Order JNJAZ55_000007965 0.67 x 0.5 Intensity 0.4 . Intensity Intensity Intensity Intensity 0.3 . Z Relative .2- Relative a 0.1- : 1 6 0.2 0.4 0.6 0.8 1.0 Relative Composition by Weight FIG 5 DIFFRACTOMETER CALIBRATION CURVE FOR CHRYSOTILE IN TALC Protected Document to Protective Order JNJAZ55_000007966 . e curves the amount of chrysotile was determined after correction for acid soluble magnesium in the talc tailings due to the presence of carbonate minerals The carbonate magnesium was obtained by running flotation tests with no asbestos present and assaying the resultant tailings The magnesium calibration curve is shown in Fig 3 ray determination of Chrysotile and Crocidolite The tailings samples were also subjected to ray diffraction measurements using a Siemens ray diffracto- meter Quantitative readings were obtained by measuring the peak intensity of the amphibole reflection at 10.5 degrees 20 and the chrysotile reflection at 12.2 degrees 20 and expressing these as a ratio with the main talc reflection at approximately 9.0 degrees 28. This ratio figure was then compared with a calibration curve constructed from peak ratio figures obtained from mix- tures of talc and the various asbestos samples these are shown in Figs 4 and 5. The use of a ratio of chrysotile to talc peak and crocidolite to talc peak removed the necessity of using an internal standard for quantification purposes Care was taken in the preparation of ray standards to ensure good mixing and this was performed in aqueous suspension using the froth flotation cell as a mixer Xlray powder preparations were investigated also and both pressed and loose specimens were examined The loose powder preparation was preferred and used in all the measurements Copper radiation was used throughout the Protected Document to Protective Order JNJAZ55_000007967 and 41 for the chrysotile in the same tailings fractions The results show that quantity of asbestos in the tailings increases dramatically with increase in asbestos content of the original asbestos mixture Also the fact that two asbestos minerals may be contained in the same sample has very little effect upon the recovery of each mineral in the tailings The highest concentra- tion ratios K obtained in these tests were with the % asbestos mixtures where the asbestos was concentrated in the tailings from 1 to 35 approximately The tailings fractions were all subjected to ray diffraction examination as well as wet chemical analysis and the comparison of some of the quantitative results obtained are given in Table 4. 10-12 illustrate portions of diffractometer traces obtained from separated tailings fractions of tests performed upon 1 crocidolite 1 chrysotile 1 crocidolite and chrysotile in talc mixtures Tests with 0.5 additions of actinolite in talc were also performed and Fig.13 illustrates the diffractometer trace obtained from a single stage separation of actinolite from talc No quantification was performed for this sample as there was insufficient actinolite to prepare diffrac- tion standards Protected Document to Protective Order JNJAZ55_000007968 Conclusions . Froth flotation would appear to be a most efficient means of separating amphibole and serpentine asbestos from talc for both detection and quantification of the asbestos phase No interference appears to occur when two asbestos minerals are present and are being separa- ted Two stage separation is slightly more efficient than a single stage separation The most suitable flotation conditions for separation were found to be pH - 2.0 with a solids concen- tration of 6 - 8 grams per litre of water in the flotation cell The most suitable frothing agent was found to be Frother 65 produced by Cyanimide Ltd. H Protected Document to Protective Order JNJAZ55_000007969 _ Tit . pS TIT moe rg ef pT.Ee mp =i hi nae ^ oe o RATE A - COUNT . - |- or in MIN TRACE a j CHRYSOTILE he wR CHRYSOTILE eg --- we eee POLO te PT. p DI e os e Eo fo fe e me wee ae ey pet in ed oe es poy bef oy. we en eo pe ~~ eg ae pe. he - - fe e Pe ye pefo a te PaO ors oh ew ce - FoEo fe awe e we Cy ee ar me | YEPee Oo wee Sy pe [Ce yp rs = ns ap--f io Protected Document to Protective Order aT e ny erana - wees . e s - = - {eT ea a. ~ ae ~ ay 10 ba mT - - = ew rh ef en Cd a a an Sa - _ - a 4 - ver e na - len eas wmiqjerp:a e me aa ae en e _ es whe Es co ~ one _. t. ee A q Sh i . JNJAZ55_000007970 a Tee oe Tl == CT ; [3p JRE Ta aa 10- pT RATE PET RATE ry Ly PS COUNT OYE.MIN . 1"- 7 Ge a a - -- E. qe TRACE ne aie Protected Document to Protective Order FIGURE 7 aeLee ntram p. aO enytm oo af ie ~ , es e = ee - ed } -.|$ ~ wdc oe oe JNJAZ55_000007971 4. eh 7 Sy aed ee ef wf fo. ET ~ ed se ETL ed ~ -ee [Fo 10 me RATE ~e po dem wef COUNT e] - a 17MIN e ia 8 TRACE e J. wenie = ef - et- nee fe CROIDLTE _ ~ noncee | f= ~ s fp a carp a - os] = - eeod ware2. _ ~ ~ be , weonef oad ne TOL ~ wae ie oa _ oe e Se r ans ne e ae erage] ' et in i , ' 7 a ~ ae pI ~ le - - o- tena ea thor-d Bf. spocmer ansae - etTUE e-]- peat "4 Lr.oe' gotg wage th: ee _ : Uthe ad. cpt oa . Oe Je fa. oe PED ee -~Eap e} Ai 4 : { se eg 4 R Paes ee oe ee ail cli. Se a0 e. ee ed Tod. ET 2 77 T pT Tp. TE pt MPT OU RTP SOP DTI ~. T TO Ty mr! nr _ m= "SS JS JLT Ly ET PTSIRT Rnd : FIGURE FIGURE FIGUREFIGURE 8 > 4 fit : 16 Protected Document to Protective Order JNJAZ55_000007972 * : ~ es Ll we fe Ss en TE qSvefee e ced pe] ce ene ... es POUT ak. ree - 10 se TL 4 RATE COUNT re CUTIE =. Jo a [UROUSIL MIN IUNG 2p. ACTINLEa be. SONUCIE -ap a GOUINS SOTIURN) fob [UDOIRNTI OTE Sp Fon SUTRNONT | SS Searenaen SOUERNIGS - meneats paDURIOGEN ae fi DUK i SUNSIINE are feae RunisStelfi pana fa poe in Sl ae CpU L pe nee yee +a (nee St. rs a weanpo a m Jos. a whee 27 fe mp aT beesee DIUpo Aye ypo PIT Ci ne In. fl FE yp ee ray be te nie PO wef tic Tp ve : ay PLE ~ cob Cy mj : oe Se fl to a , : i oo i p- po ces f-L. ae tt mat EL cn rn : an ae ~ ee = cs ir oe es ee aoe Ped we - f a a Pees Sn FIGURE FIGURE 9 Protected Document to Protective Order , TT . ny ve nai on . J - we a ae ASS ot JNJAZ55_000007973 joops a ren temee-: | ae a ea TRACE FROM ~ DIFFRACTOMETER A of. TAILINGS SAMPLE PRODUCED IN Afi! % TWO STAGE SEPARATION OF CROCIDOLITE TALC to ctte eter mt TALC MIXTURE MIXTURE ae - - oe ae 16 18 14 ' FIGURE 10 Protected Document to Protective Order JNJAZ55_000007974 - DIFFRACTOMETER FROM A /- -b---1|<- s TAILINGS IN TWO <p ot {-= SAMPLE PRODUCED STAGE SEPARATION OF A % oc) port _t_ -- -o- omni Tp CHRYSOTILE TALC MIXTURE ee a = 7) poo ee os anaes bee ges -- - oe oe oe certo pe eo om eae Oe aa == = j a Per 1 JALC ten iad . i | piql i! 2 CLL j qd yey ij]:i ah ria fa eee oe |J CHRYSOTILE- ee 18 TE ZL 12 10 FIGURE 11 Protected Document to Protective Order JNJAZ55_000007975 DIFFRACTOMETERFROM i reas eel Seeeaal ioe arin TRACE A Say b= ae oe TAILINGSSAMPLE PRODUCED 1 TL Sih ab Pl af TWO STAGE SEPARATION OF A % Ply p= mofeco} ss: = pi jCROCIDOLITE % CHRYSOTILETALC espe 5 " oun - ---f EE Te Sos EE 2) I LE -- - Len feeeee ~- J fee ~- 2 Ee EEE SUSE SI i. o-f} |i ane ee ae aT. nay SOE Ll a ee wee fe ee veborr Sn NS RE a LST yp ae es _--. eam T.-- --. {owes feo on _ ares a. inane anen aaa Cee ome - Done ape eee ry oe eae ey _# - os. ft : }-[i---b- H 4 pl me i , cr: a * g verre z Desi i ores Poros ia i rr ee oa }- SS 5 mane = | eae ana vee BI reared plcorvent Wlerdbenld soeeneenll ser ieee a ge f = | ae t TALC ~ ba ee TALC ~ i TALC PLT i TALC - - om CHRYSOTIE CROIDLTErere 24 -; ~.. : > wee Ho CHRYSOTICE desapce!. . . = = need a N . 4 - ase ae 4 it! ae ~~ i 1 { ae fe ate _-- one a een Sperone ereerern leanne 20 Th 16 71 -12 10 B FIGURE 12 Protected Document to Protective Order JNJAZ55_000007976 STE UIL. rent ie . Saoasinael PRODUCE nope Init i Maeieaied ae Giamel mal ACTINOLITE Gna pa % SEPARTION_FQ.5 o.[2cep TAILNGSSEPARTION_OF_AQ.5 Ga oat e I FROM a TRACE . STAGE SINGLE sp [ DIFRACTOME| IN pore ase|ol-_ (espns rs Py | L biecorcTE op eces yp om T= es ' ies_ - a cco botFo} One oe _ - e ed oe tropelor ond . ane dee + _ wt ~ we pane oper tpricde jo aoe fee boom pier 1| + - ds - on a oe wif pf ae med ep ey _. apctbep- cpr} . : oa cp eit pe fhocpeoe en peinooffoe boc aes eee . ue - ACTINOLITEACTINOLITE aa - ees ACTINOLITE . |. ACTINOLITE , ACTIANOCLITTEINOLITE | _- we wi ae Se - nao) soe} tp poem Oe ae DRANG we to So o SONE fes pec we TALC pcp eae PANU2 fe TALC Be e AORN- . ] a Scypes [ELS gepblocrimepe --- SORA- ao venres pe SN On Poe _ PE decbpovfse ESL - CHLORITE CHLORITE SP Sern feo fee Ser fe cbs os Poo oO - pe fe be " cfs op. | <p Secarph Cipoechandavis ae ceee stop om faetn 2p 4 1 (alr TALE ACTINOLITE TALE ACTINOLITEACTINOLITEACTINOLITE ACTINOLITE ACTINOLITE oo e rans Uisecand TALE foe:oe pe Semen Ren po. dsery = vo rae a x oo i FIGURE 13. Protected Document to Protective Order a ras ~ T sevenwey OL | Meda bee ee. sole loi} 3h) jh} je - } el - cadd car : a tata Cai techMdae j- Pe | 15 o 25 7 = a 7 - JNJAZ55_000007977