EEO 2 UwE:m--EwE:uon_ ?.3022; :QExm. o ~\'.·;~·:· · · o· t:~~~.,: . .. •'l"~' ,.';.-, '0' : Protected Document--Subject to Protective Order JNJAZ55_000001033 I I I I I I I I I I PROGRESS REP OR T on STUDIES OF THE PHYSICAL PROPER TIES OF TALC, THEIR MEASUREMENT, AND COMPARISON to JOHNSON AND JOHNSON October 15, 1957 I I I I I I I I I I I .l) Protected Document--Subject to Protective Order by W. L. Smith BATTELLE MEMORIAL INSTITUTE 505 King Avenue Columbus 1, Ohio JNJAZ55_000001034 I I I I I I I I I I I I I I I I 'I I I I I II K-3262-2 cc: OK 1 d by O. F. Tangel and A. C. Richardson before typing. -(?) F. TaI1f5f1 (3) MA' C. Richarts1 .N(ll~tt@n emoria R. D. Macdonald ' W. L.,Smith (-3) nstitute " / \ K 50S 1 N A G V E N u E COLUMB U 5 OHIO I, October 25, 1957 Dr. W. H, Lycan Director of Re,search Johnson and Johnson New Brunswick, New Jersey De ar Dr. Lyc an: This letter transmits six copies of our report "Studies of the Physical Properties of Talc, Their Measurement, and Comparison". At the pre sent stage of this inve stigation it can be seen that the lubricity of the Italian talc is closely related to its purity,crystalline habit, and particle-size distribution and is expressed in bulk density, surface area, porosity, and average diameter measurements. The acceptable Italian talc was found to fall within a small range of physical measurements., Lubricity was found to be controlled by the shape of the relatively small content of comparatively larger particle s in the otherwise finer mixture. It appears feasible that the slip of the Italian talc may be improved by the removal of the coarser mineral contaminants. Your comments on the findin'gs o'f this investigation will be appreciated. Very truly yours, W. L. Smith Principal Geologist Minerals Beneficiation Division' WLS:rr Enc. (6) R E S Protected Document--Subject to Protective Order E A R c H F o R N o u s T R y JNJAZ55_000001035 I I I I I I I I I I I I TABLE OF CONTENTS SUMMARY. INTRODUCTION 2 DISCUSSION OF LUBRICITY . ,THE ROLE OF MINERALOGICAL PURITY IN LUBRICITY. :. 3 THE ROLE OF THE CRYSTALLOGRAPHIC HABIT OF TALC IN LUBRICITY 3 THE MEASUREMENT OF LUBRICITY 4 4 Discussion. The LUb~icity Board The Lubricity of Talc Sample s 4 7 9 THE RELATIONSHIP OF LUBRICITY TO PARTICLE-SIZE DISTRIBUTION 9 Discussion. Particle-Size Distribution in Italian Talc. Correlation of Lubricity With Particle-Size Distribution Data. 9 ·11 MOISTURE CONTENT • 15 MEASUREMENT AND CORRELATION OF OTHER PHYSICAL PROPERTIES RELATED TO LUBRICITY 15 Surface Area Determinations by Nitrogen Adsorption Average Diameter of Partic~e8 . " 15 15 Specific Surface Calculated FraIn Average Diameter. 17 Porosity Bulk Density 18 20 CONCLUSIONS 21 BIBLIOGRAPHY 23 APPENDIX A DESCRIPTION OF LUBRICITY BOARD AND TECHNIQUE OF OPERATION A-I APPENDIX B I I I I I I I I I PROCEDURE FOR PARTICLE-SIZE ANALYSIS B-1 LIST OF FIGURES Figure 1. The Lubricity Board, Showing Descent of Steel Puck Figure 2. Underside of Lubricity Board, Showing Microswitchea and Electric Tim.er Connected tu Lock-in Relay Figure B-1. • Standard Flowsheet for Sizing of Talc Samples 6 B-2 LIST OF TABLES Table 1. Typical Data From Lubricity-Board Measurement of Italian Talc Sample (Cranford, 12/22/56) Table 2. Lubricity_Board Measurements ~nd Per Cent Contamination o£ Talc Sa1Tlpled at Cranford, New Jersey Showing Relation of Lubricity to Purity of Sample BATTELLE Protected Document--Subject to Protective Order 7 8 MEMO R I A L JNJAZ55_000001036 LIST OF TABLES (Continued) Page Table 3. Lubricity-Board Data on Flotation of Contamination on Lubricity. Produ~ts 'of Italian Talc, Showing Deleterious Effect ' 8 Table 4. Previously Reported Particle-Size Distribution Data on Italian Talc 10 Table 5, Particle-Size Distribution of Three Samples of Italian Talc " 10 Table 6. Particle-Size Distribution of Talc Sampled 'at Cranford Plant l a. -30 Microns +15 Microns -15 Microns 65.72 10.76 10.78 7.75 56.66 16.49 13.46 8.30 7.85 60.76 10.23 11. 94 0.84 5.54 7.65 55.79 16.42 13.88 -,' 10-18-56 0.96 7.86 7.27 58.07 13.32 12.52 9-27-56 0.59 4.48 6.77 56.52 15.93 15.71 8-28-56 0.50 4.34 6.89 56.39 16. 18 15.71 10-4-56(a) 1. 22 6.38 9.36 40.02 31. 74 11.28 8-20-56 0.65 6.08 7.98 57.53 16.64 11. 12 12-22-56 0.88 3.42 12.30 52.27 20.01 11. 12 11-30-56 0.72 6.38 10.33 57.86 11. 21 13.50 11-15-56 0.88 6.93 9.91 48.72 22.08 11. 48_ +200 Mesh 9-6-56 0.47 5.44 6.83 11-6-56 0.51 5. 13 9-12-56 0.92 9-19-56 Date Collected III ~ Weight Per Cent of Size Fractions -400 Mesh -:325 Mesh +400 Mesh +30 Microns -200 Mesh +325 Mesh ~ 11'1 r r 11'1 ~ 11'1 ~ 0 lJ - > r - z CIl -f ..... tv -f c -f 11'1 (a) See comment under "Particle-Size Distribution in Italian Talc". c... Z c... ~ I~ o o o ~~ TABLE 18. -l SUMMARY OF PHYSICAL PROPERTIES OF SIZED FRACTIONS OF ITALIAN TALC -l m Tyler Mesh Size Lubricity-Board Measurements, seconds Average Diameter, microns Unseparated 0.990 2.60 +200 0.889 II -200+250 > r r m ~ m ~ 0 Specific Surface, cm 2 /g Porosity Ratio Bulk Density, Ih/cu ft 8392 0.448 23.030 7.40 2948 0.401 34. 261 0.951 3.60 -6061 0.426 26.645 -250+270 0.980 2.50 8727 0.439 20.721 -270+325 1.030 2.35 9284 0.446 19.335 -325+400 1.043 2.25 9697 0.442 19.139 -400 1.099 2.10 10390 0.455 16.894 N N - r Z l/l -l - -l C -l fTI c... Z c... ~ I~ o o o ~- '" 2 < 1 1 1-2 2 Trace 2 >2 O-trace O-trace Trace Trace Trace 1 <1 (n) Incidence determined petrographica lly. Grit is present in all size fractions, being somewhat more abundant in the fines. In the coarser fractions the mineral contaminants and the talc particles which are oversize in thickness are most readily sensed subjectively. The presence of grit in the fines is largely masked to the senses by the presence of larger platelets. In this regard no solution to, abrasiveness lies in the removal of entire coarse size fractions, inasmuch as the grit in the then remaining coarser fractions would be as readily noticeable subjectively and more abundant percentagewise. To remove the abrasive particles, it is necessary to remove both nonplaty talc and the mineral contaminants from the whole powder by such beneficiation methods as flotation(5) and classification by cycloning(6), the initial studies on which have been reported or are in preparation (Table 3). B A T TEL L E: Protected Document--Subject to Protective Order 'M E M OR , A L ~ INS T I. T UTE I I I I I I I I I I I I I I I I I I I I I I JNJAZ55_000000913 I I I I I I I I I I I I I I I I I I I I I I 5 TABLE 3. Talc Sample THE EFFECT ON LUBRICITY OF THE, REMOVAL OF MINERAL CONTAMINANTS AND NONPLATY TALC FROM ITALIAN TALC SAMP LES Incidence of Indicated Particle Type(a), per cent Platy Nonplaty Talc Talc Dolomite Tremolite Italian No. 1 Feed Float 88-90 95 Italian No. 2 Feed Float 90 98 8-9 <2 4 Trace Lubricity-Board Measurement, sec <1 0.990 Trace 1. 046 5 3 2 0.926 <1 Trace Trace 1. 051 (a) Mlneralogicallnc1dence determined petrographically. It is important to emphasize the difference between the incidence or frequency of contaminants and their per cent of total composition. The per cent incidence is determined petrographically by grain count. It is a two-dimensional measurement approximating area and does not consider the thickness of the particles observed. The incidence of a min~:I:al or crystal type is of primary importance inasmuch as a powder consists of a mixture of discrete grains, each with its particular size, shape, and other physical properties.' In eonsidering the behavior of a powder as a lubricant, we are dealing with the ;mechanical interactions of individual grains in lamellar movement and thus are concerned with the frequency of types of grains, not with their per cent of total composition. That is, for example, in considering lubricity or abrasiveness we must deal with the incidence of individual particles of dolomite rather than with the total volume oxt weight per cent of the sample which is dolomite, except when dealing with closely sized samples. Conversely, when considering acid solubility, moisture content, and the analysis and evaluation of beneficiation products, we, of neces sity, deal with total components; not the incidence of particles. While small differences in per cent incidence of contaminants in a powder may influence the physical properties of mechanical movement, in no case described here is the per cent incidence different from the weight per cent or the chemically analyzed component by more than 1 per cent of the whole sample. THE MEASUREMENT OF ABRASIVENESS Discussion A standard method of measuring the abrasiveness of high-quality talc has not been devised previously. Abrasiveness or grit has 'been measured subjectively by testing samples between the fingers or teeth. As in the case of lubricity, the final analysis of acceptability in regard to abrasiveness is subjective: consumer reaction. Objective tests are not designed to replace the subje~tive tests; however, to be able to determi~e BATTELLE Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000914 6 improvement in beneficiation procedures and to determine the correlative relationships of the physical properties of talc, it is necessary to be able to measure small differences in the phy~ical properties and to be able to compare them to other quantitative 'measurements. Knowiedge of these interrelationships s~rv:es as the basis for interpretation of improvement in quality and thus serves to make it po'ssible to visualize methods of beneficiation. Since the 'subjective tests are of little help in measuring small differences in one of the many physical properties encountered, and since such tests have no basis for correlation, a machine was built to measure objectively, or test for, abrasiveness, apart from other physical properties. The Abrasion Machine Because it was necessary to measure small differences 'in the abrasiveness of talc, a machine was built to test the wear effect of small concentrations of grit on standard material. The machine was built of a 1/20-hp l725-rpm electric motor' mounted vertically and fitted with a 5-inch lap covered by a Buehler Microcloth held in place by a rubber belt. The lap portion of the machine is set into a steel bowl and covered with a plastic lid. Mounted on a ringstand over the lap a SOO-ml open separatory funnel with stopcock is connected by a rubber tube with an adjustable pinch clamp to a feed spout. The separatory funnel contains the sample of talc to be tested in a slurry of 3 grams of talc to 350 ml of water. The feed spout and a cylindrical pellet holder are mounted in a removable crossbar over the lap. Accessibility to these parts is afforded through a hole in the plastic cover. $tandard 1 /2-inch-diameter pellets are held in the sample holder by a 16. I-gram weight to prevent their skipping or floating on the lap. A 1000-ml beaker mounted under a drain in the steel bowl catches the tested ,slurry. Figure 1 shows the over -all apparatus. Figure Z shows the detail of the feed and abrasion mechanism. A detailed description of the abrasion machine and the technique of its operation are found in Appendix A. In order to measure the abrasiveness of the talc in the slurry a test had to be designed where the object abraded wOlild have a great enough loss to be measured physically. Since the abrasiveness to be measured was that of a powder containing generally from only 1 to 3 per cent of abrasive gangue particles, the material to be abraded had to have a hardness greater than that of the talc, less than that of the grit, and also had to be coherent and homogeneous. After testing a large number of materials it was decided to perform the bulk of the tests on pellets made of minus 400-mesh Italian talc pressed under'50, OOO-psi pressure. The pellets average 5.20 grams and have dimensions of 1/2 by 7/10 inch. The pellets have a hardness greater than that of the raw talc and less than that of the contaminants (Table 4). Carbonate pellets were made to test specifically for the rarer, harder components, in a similar manner, but using alcohol instead of water in the slurry. , BAT TEL L E Protected Document--Subject to Protective Order ~ ,E M 0 ! R, I AL tNSTITUTE I I I I I' I I I I I I I I I I I I I I I I I JNJAZ55_000000915 I I I I I I I I I I I I I I I I I I I I I I 7 and 8 N45893 FIG URE 1. THE ABRASION MACHINE SHOWING RESERVOIR CONTAINING SAMPLE IN SLURRY TO BE TESTED FOR ITS ABRASIVENESS BATTELLE Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000916 a_ It n It c- o o - - - - - ------- - - - - - - - - - n l: 3 III :::l ~l: .E III !:lei "'0 ~ n ~ tD o » III a. ~ ... ~i!;: ITl r r . ITl __-II-Ii (.~.~ ,=,,~,.,,=,"~ ~f~J~_,t=·""",: ~~~',-','<~~"<1 . . . . ~~v--.' . ~ ITl ~ o ~. 1 :u ',' » r , ~ ~::;/~ ~ I ~ J~ n '" ~ If) ) n , [ - I o Z . . III C -4 ITl I ----~ FIGURE 2. c... Z c... I:~ o o o o o ~ ..... N45892 DETAIL VIEW OF ABRASION-MACHINE LAP SHOWING FEED SPOUT, CYLINDER IN WHICH PELLETS ARE HELD ON THE LAP, AND STANDARD PELLETS OF PRESSED TALC I I I I I I I I I I I I I I I I I I I I I I 11 TABLE 4. RELA TIVE HARDNESS OF THE TEST PELLETS AND THE GRIT PRESENT IN ITALIAN TALC Mineral Moh Hardness Talc I Pressed-talc test pellet ± 2 (scratches talc) Magnesite Dolomite 3. 5 (scratches talc pellet) 4 >4 (scratches dolomite) Pre s sed-carbonate te st pellet Apatite Titanite Tremolite Rutile Zircon 5 (scratches carbonate pellet) 5 6 6 7. 5 The abrasion-machine operation is timed electrically. The pellets are measured on a micrometer caliper before the test and afterward, after drying. The abrasion measurement is reported in decimal fractions of an inch per second. Although there are limitations to the use of a micrometer, the samples which were compared demonstrated differences in measurement large enough to be significant. Measurements based on weight were found to be entirely unsatisfactory inasmuch as some weight loss was due to spalling and abrasion of the pellet by the walls of the sample tube on portions other than that exposed to the lap and abrasive. This indicated losses which were no indication of the degree of loss due to action on the tested surface alone. The abrasion machine subjects the standard pellet to abrasion by the sample of talc being studied, at a high rate of speed. It has been calculated that the pellet receives wear equivalent to being rubbed over more than 1800 ft/min of surface of the talc being tested. As expected, the abrasion machine demonstrates that the slurry samples with the greater incidence of mineral contaminants produce the greater amount of abrasion on the pres sed pellets. It is also shown that those samples with primarily platy habit are less abrasive than those containing effective amounts of nonplaty talc. More precise abrasion machines could be built; however, the device used is satisfactory for the purpose of comparing samples within the. range of those tested and is an adequate means of obtaining comparable measurements of the effect of grit. Typical figures obtained by the abrasion experiments are shown in Table 5. BAT TEL L Protected Document--Subject to Protective Order E MEMORIAL INSTITUTE JNJAZ55_000000918 12 TABLE 5. TYPICAL FIGURES OBTAINED BY ABRASI()N TESTS ON FOUR SAMPLES OF ITALIAN TALC Test Incidence of ContalUinants(a), per cent 1 2 3 4 2 2 2 2 Pellet MeasurelUents, in. Before After O. 6453 O. 6435 O. 6184 O. 6442 Diffe renee in Measurements, in. Time, sec Abrasion(b), 10- 3 in./sec 0.0887 O. 0952 O. 0810 0.0743 38 41 36 32 2. 33 2. 32 2.25 2. 32 o. 5566 0.5483 0.5374 0.5699 (a) Determined petrographically. (b) Significant figure: 2.3 x 10- 3 in. /sec. The Abrasiveness of Talc SalUples Fifteen salUples of talc collected at the Cranford plant of Johnson and Johnson, the same samples used in the previously reported lubricity experiments(l), were tested on the abrasion lUachine. The results of the lUeasurelUents are shown in Table 6. The lUeasurements show a range of from 1.62 to 2.69 ,x 10- 3 in. I sec wear on the standard pellets. These figures are generally correlative with the incidence of contalUinants, as deterlUined petrographically, as reported in the Progress Report dealing with lubricity(l). As it will be shown further in the report, this relationship only holds in whole unseparated powder where particle size is not a fundamental controlling factor. The correlation of lubricity-board'lUeasurelUents with contalUination reported in Table 2 of the previous Progress Report(l) shows a silUilar general relationship between contalUination and lubricity. Where the lUbricity experilUents concluded that the samples containing the greater alUount of contaminants demonstrated the poorer lubricity, the' abrasion-lUachine experiments show that the, samples with the greater contamination produce the greater alUount of abrasion. Thus, when dealing with whole, UIlscreened powders, the relUoval of grit should also serve to ilUprove lubricity. Although the relUoval of grit ilUproves the lubricity of whole powders, the relationship of lubricity to abrasiveness cannot be considered to be lUathelUatically inverse. The properties which control abrasiveness are the size and shape of the contaminants and their incidence in the coarser fractions; whereas, the properties which cont'rol lubricity are the over-all size distribution, those previously described properties directly related to surface area, plus the incidence of the coarser components. When lUeasuring screened fractions of powders both abrasiveness ,and lubricity are influenced by the specific particle size, and abrasiveness will be directly related'to the grit COlUponent, whereas in whole powders the finer abrasive particles will be in part lUasked by the coarser platelets. To test further the effect of contaminants upon abrasiveness, the contaminants were removed from a sample of talc by froth flotation and the products were tested on the abrasion machine. The same samples had previously been tested for IUbricity(l). The test results, which are noticeable subjectively, are reported 'in Table 7. BAT TEL L E Protected Document--Subject to Protective Order MEMORIAL INSTITUTE I I I I I I I I I I I I I I I I I I I I I I JNJAZ55_000000919 I I I I I I I I I I I 13 TABLE 6. Date Sampled 9-12-S6 8 -1 0-S6 9-19-S6 9 .. 6-56 10-18-56 9-27 -56 10-4-S6 RELATION OF PURITY OF SAMPLE TO ABRASIVENESS AND LUBRICITY IN WHOLE POWDER Abrasiveness, 10- 3 in. {sec Incidence of Contaminants (a), per cent Lubricity-Board Measurement, sec 1, 62 <1 1, 030 1. 70 1 1. 021 1. 84 1. 87 <1 <1 1. 028 1. 083 1.88 1 1 2.32 2.32 2 1-2 2-3 1, 025 1, 017 0.982 0.971 1,'007 1. 053 0.936 1. 006 0.952 2.59 2.69 2-3 2 0.968 O. 965 1, 90 1, 90 8-20-56 1-2 2 1. 91 1. 97 8-28-S6 11-6-S6 2 1 2. 15 II-IS-56 10-29-56 11-30-56 10-12-s6 12-22-56 2.30 (a) Previously reported( 1). determined petrographically. I -I J I I I I I I I I TABLE 7. ABRASION AND LUBRICITY MEASUREMENTS ON FLOTATION PRODUC TS OF ITALlAN NO. 1 TALC Abrasiveness, 10- 3 in. {sec Product Lubricity-Board Measurement, sec Starting sample 2. 14 O. 990 Float producd a ) 1. 50 (superior)(C) 1.046 (superior) Nonfloat product{b) 3.03 (inferior) 0.873 (inferior) (a) Essentially pure talc. representing 90 per cent of starting sample. (b) 85 per cent talc. 15 per cent contaminants, representing 10 per cent of starting sample. (c) Less abrasive float products have been made from Italian No.2 talc. BAT TEL L E Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000920 14 The float products clearly demonstrate superiority over the starting sample in regard to both abrasiveness' and lubricity. The deleterious effect of contaminants is shown by the inferior measurements derived from testing the reject product of the flotation process. THE RELATIONSHIP OF ABRASIVENESS TO PARTICLE-SIZE DISTRIB UTION AND CONTAMINATION Discussion The abrasivenes s of the talc studied is determined by its component grit .. When dealing with the mechanics of a powder in lamellar motion, we are dealing with the interrelationship of individual particles, and thus are concerned with the per cent incidence and particular sizes and shapes of individual~. The distribution of the contaminants and nonplaty talc in the different size fractions is thus a primary consideration. The coarse contaminants are those which scratch and are quickly noticed subjectively. The finer contaminants clog the lamellar movement of the talc platelets and initiate rolling of the powder, introducing aggregate asperities. In the previous reports to Johnson and Johnson(l, 2,7) the problem of particlesize distribution has been thoroughly discussed. It does not seem requisite here but to re-emphasize the importance of establishing the particle-size distribution of a powder when studying its physical properties or the means of their improvement. Since the size of the abrasive particles, as well as their incidental abundance, contributes to abrasiveness, it was necessary to determine the size distribution of the contaminants. Correlation C?f Abrasiveness With Particle-Size Distribution and Contamination Portions of the same samples which were used to test for lubricity and other physical properties were used in the following experiments on abrasiveness. Size fractions were made of Italian talc and were measured for their abrasiveness on the abrasion machine. Results of the experiments show that the finer particle-size fractionsare more abrasive than the coarse. This is in agreement with the incidence of grit determined petrographically. Chemical·analyses for equivalent dolomite on these samples are also in agreement. These analyses appear in the section of this report dealing with acid solubility. Table 8 shows the results of abrasion tests of size fractions on standard talc pellets. When comparing size' fractions a parallel relationship exists between lubri'city and abrasiveness, as a function of particle size. Thus, were only the fines, the most lubricous fraction, used for baby powder, this fraction would also be the most abrasive. In order to retain the more lubricous particles yet remove the more abrasive, it is necessary to remove the contaminants only. Both lubricity and grittiness cannot be improved by the removal of particle ~s ize fractions. B A. T TEL L .E Protected Document--Subject to Protective Order M.E M 0 ~d I A ,L INSTITUTE I I I I I' I I I I I I I I I I I I I I I I I JNJAZ55_000000921 I I I I I I I I I I I I I I I I I I I I I I 15 TABLE 8. RELATIONSHIP OF ABRASIVENESS AND LUBRICITY TO PARTICLE SIZE AND CONTAMINATION IN SIZE FRACTIONS OF ITALIAN NO.1 TALC Lubricity-Board Measurement, sec Incidence of Contaminants(a), per cent Total Dolomite Tremolite Tyler Mesh Size Ab r a s i ve ne s s, 10- 3 in. I sec Unseparated 2. 14 0.990 ±2 <2 Trace +200 -200+250 -250+270 -270+325 -325+400 -400 1. 30 0.889 0.951 0.980 1.030 1. 043 1. 099 <1 1 1-2 2 Z >Z <1 1 1-2 2 Z >2 O-trace O-trace Trace Trace Trace-l < 1 1. 59 1.72 2. 00 Z.33 Z.48 (a) Determined petrographically. In order to show which effects are primary, and which are secondarily related because sized materials are analyzed, tests were made on the plus ZOO-mesh fraction of the talc as received from Italy, on the minus 400-mesh fraction, and on the plus 200-mesh material after it was crushed to pass a 400-mesh screen. The natural plus 200-mesh material had but a trace of contaminants compared with the more than 2 per cent present in the natural minus 400-mesh fraction. Abrasiveness and lubricity tests (Table 9) show clearly that the abrasiveness is controlled primarily by the contamination and only secondarily by the size fraction analyzed. It also shows that the lubricity is controlled primarily by the particle-size fraction tested, and only secondarily by the contamination present in the specific size range. This experiment serves as the basis of interpretation for relating the physical properties of sized material, and also establishes the controlling factors behind lUbricity and abrasiveness in whole powders. TABLE 9. COMPARISON OF LUBRICITY AND ABRASIVENESS TO GRAIN SIZE AND CONT AMINA TION Abrasivene ss, 10- 3 in. I sec Sample Natural +ZOO-mesh fraction Natural -400-Ine sh fraction +200-mesh fraction ground to -400 mesh Lubricity-Board Measurement, sec 1. 30 2.48 1. 12 (b) 0.889 1. 099 1. 10S(C) Incidence of ContaIninants(a), per cent Trace >2 Trace (a) Determined petrographically. (b) The abrasiveness of this sample is only slightly less than that produced by the same sample prior to grinding, much less than the natural minus 400-mesh fraction which contains more grit. (c) The lubricity of this sample is greatly improved by regrinding, but it is essentially like the natural minus 400-mesh sample despite the difference in the grit present, BAT TEL L E Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000922 "'0 0 It n It C- O 0 n l: 3 III ::!. in l: .E III !:lei "'0 0 It !:l- TABLE 10. <' III 0 0~ ABRASIVENESS AND LUBRICITY MEASUREMENTS OF IT ALIA..~ TALC SAMPLES FROM WHICH SPECIFIC PARTICLE-SIZE FRACTIONS HAVE BEEN REMOVED m X Represents Fractions Removed From Whole Powder U Represents Fractions Tested > ~ ~ IT! r r Tyler Mesh Size Incidence of Contaminants (a), per cent +200 -200+250 -250+270 -270+325 -325+400 -400 <1 1 1-2 2 2 >2 IT! 3: IT! 3: 0 :u -)r Z III Lubricity -Board(b) Measurement of Size Fractions., sec 0.889 0.951 0.980 1.030 1. 043· 1. 099 Abrasiveness, 10-3 in . /sec 1. 30 1. 59 1.72 2.00 2.33 2.48' Test Test 2 Whole Powder Test 3 Test 4 '. U U U U U U U U U X X U X X X U U U U U U 0.990 1.038 1.068 U U X X X Lubricity-Board Measurement, sec 0.945 Abrasiveness, 10- 3 in. / sec 1. 88 u· U U X 0.963 -- - - .-IncreaSe in slip and abrasiveness 1. 88 ....0"- 2.14 2.27 2.34 0.0 2.0 3.0 ~ - ~ .C Approximate Weight Per Cent of Fractions Removed 97.0 82.0 ~ IT! (a) Detennined petrographically; (b) Based on Table 10 of previous report(l). c... Z c... ~ I~ o o o ~- IV '" --------------------- I I I I I I I I I I I I I I I I I I I I I I 17 In the previous study of lubricity(l), measurements were made on powders from which different size fractions had been removed, and on mixtures of specific size fractions. The experiment demonstrated that the over -all lubricity was influenced primarily by the coarser particles. Similar experiments on abrasiveness have been made and show that it is not possible to increase the lubricity by removing total size fractions without increasing the abrasiveness (Table 10). Because talc contains tremolite and rare accessory minerals as well as carbonate as abrasive components, a test was devised to measure the abrasiveness of the harder contaminants. Carbonate pellets were made by fusing a three-to-one mixture of sodium carbonate and sodium borate into a melt. The fusion product was crushed and pressed into pellets under 15, 000 psi. The resulting pellets were harder than the talc or the carbonate contaminants but softer than the tremolite and accessory minerals. The pellets were slowly soluble in water; therefore, alcohol was used as the fluid in the test slurries. The test results are not necessarily correlative with measurements made on talc pellets, but demonstrate the distribution of the harder contaminants (Table 11). All other abrasive data contained in this report have been determined on pressed talc pellets. TABLE 11. Tyler Mesh Size THE DISTRIBUTION OF THE CONTAMINANTS HARDER THAN CARBONATE IN ITALIAN TALC AS SHOWN BY ABRASION TESTS MADE ON CARBONA TE PELLETS Abrasiveness (on Talc Pellets), 10- 3 in. I sec Abrasiveness (on Carbonate Pellets), 10- 3 in. I sec Incidence of Contaminants(a), pe r cent Total Dolomite Tremolite Unseparated 2. 14 0.9 ±2 <2 Trace +200 -200+250 -250+270 -270+325 -325+400 -400 1. 30 1. 59 O. 5 O. 7 <1 1.72 2.00 2.33 2.48 0.6 <1 1 1-2 O-trace O-trace Trace Trace Trace-l <1 0.6 0.8 0.9 1 1-2 2 2 >2 2 2 >2 (a) Determined petrographically. To demonstrate the effect of the rarer contaminants on the abrasion of pressed talc pellets, a series of sized fractions of Italian talc were leached free of the carbonate components and measured on pressed talc pellets. Table 12 shows the degree of abrasiveness produced by the leached samples. 8 A T TEL L E Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000924 18 TABLE 12. ABRASION TESTS USING LEACHED AND UNLEACHED SIZED FRACTIONS, DEMONSTRATING THE EFFECT OF DOLOMITE ON ABRASIVENESS , Abrasiveness, 10- 3 in. / sec Unleached Powder Leached Powder Tyler Mesh Size U~se:parated +200 . -200+250 ~250+270 -270+325 -325+400 -400 2. 14 1. 50 1. 30 1. 59 1. 72 2.00 2. 33 2.48 1. 60 1.72 1. 71 1. 90 1. 75 1. 34 An additional test, not relative to the beneficiation of Italian talc, but designed as an experiment to serve as a basis for study of lower grade talc, was made on a series of mixtures of Italian talc and minus 400-mesh calcium carbonate (Table 13). Although the data are not to be considered correlative withthose of Italian talc, they demonstrate clearly the increasing effect of contamination on abrasion. TABLE 13. Per Cent Italian Ta1c(a) ABRASIVENESS OF MIXTURES OF ITALIAN TALC AND CALCIUM CARBONATE Per Cent CaO· C02 (-400 Mesh) o 100 90 50 10 2. 14 2.89 5.09 8. 17 13. 65 10 50 90 100 o Abrasiveness, 10- 3 in. /sec Diffe renee in Abrasivenes s, 10- 3 in. /sec 0.75 2.20 3.08 5.48 (a) Contains about 2 per cent native carbonate. MEASUREMENT AND CORRELATION OF OTHER PHYSICAL PROPER TIES Moisture Content The previous Progress Report(l) introduced the problem of moisture content in talc, sugge sting that the fine-grain- size fractions should adsorb more moisture on its greater surface area per unit of weight. Table 14 shows the moisture content of size fractions of Italian talc, demonstrating an increase in moisture content with decreasing particle size. Because of the relationship of particle size to other physical properties, BAT TEL L E Protected Document--Subject to Protective Order M E M O.R I A L INSTITUTE I I I I I I I I I I I I I I I I I I I I I I JNJAZ55_000000925 I I I I I I I I I I 19 the moisture content of the s~zed fractions was found to be apparently correlative with a number of other measurements, indicating coincidental relationships which would not hold true in unsized sample s. TABLE 14. RELATIONSHIP OF MOISTURE CONTENT TO PARTICLE SIZE IN IT ALlAN TALC Tyler Mesh Size Per Cent Moisture{a) Unseparated 0.05 +200 -200+250 -250+270 -270+325 -325+400 -400 0.01 0.03 0.03 0.04 0.05 0.06 (a) Moisture content determined by method outlined in Johnson and lohnson's Raw Materials Specifications sheet. I I I I The lubricity of talc is related to its moisture content insofar as the moisture content of the finer fractions is higher. In lower grade talc the moisture content was found to be much higher. Six domestic tales, fabricated to a particle- size distribution similar to that of the Italian talc, showed from 0.08 to O. 20 per cent moisture on analysis. The higher moisture content of some inferior tales requires that moisture be determined on sample s prior to te sting for lubricity. Moisture tends to make talc pasty, producing a false indication of superior lubricity on the lubricity board. To demonstrate that the 0.05 per cent moisture content of Italian talc did not affect the lubricity, tests were run on talc from which the moisture had been driven off. A nonreproducible difference of only 0.006 second was recorded, and is not considered to be a significant figure. I I I I I I I I To further test the correlation of moisture content and particle size, the talc samples collected at Cranford were analyzed and the data compared with the percentage of fines in the sample. Table 15 compares the moisture content and the percentage of the powder finer than 400 mesh, as compiled from Table 6 of the previous Progress Report(l). The samples with the greater component of fines were found to contain the greater moisture content. No absolute interpretation should be given this relationship. The figure s are all very close and their similarity is of greater importance than the correlation. However, there is a theoretical basis for the variance, and the data are presented for whatever they may be worth in the light of future studies. The correlation seems more than coincidental. Moisture content shows no other correlation in whole powders. Inasmuch as the lubricity-board studies(l) showed that the lubricity variations depended upon the coarser fractions, the small difference in the fine component as re1ated to moisture content should have no expression in lubricity. BAT TEL L E Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000926 20 TABLE 15. THE RELATIONSHIP OF MOISTURE CONTENT TO PER CENT OF MINUS 400-MESH PARTICLES IN WHOLE SAMPLES OF TALC COLLECTED AT CRANFORD Per Cent Fines{a) (-400 Mesh, Tyler) Per Cent Moisture Date Sampled 88.28 88. 16 87.26 86.61 86.09 85.29 83.91 83.40 83.04 82.93 82.57 82. 28 0.06 0.07 0.06 0.06 0.05 0'; 05 0.05 0.05 0.05 0.03 0.03 0.04 8-28-56 9-27-56 9 -6 -56 11-6-56 9-19-56 8-20-56 10-18-56 12-22-56 10-4-56 9-12-56 11-30-56 11-15-56 (a) Repeated from previous report(l). Johnson and Johnson's Raw Materials Specifications sheet states O. 15 per cent moisture content to be the tolerable upper limit. The Crarlford samples, as well as the size fractions, contain considerably less moisture. This indicates that any beneficiation which would change the size distribution, hence the moisture content, would not produce a product of unsatisfactory moisture content. Inasmuch as a pasty consistency in talcum powder would be undesirable, samples which by exposure or otherwise have taken on exce ss moisture must be restored by proper drying. One problem arising from flotation experiments was the .tendency for the products to agglomerate after drying. It is possible that this moisture can be removed by spray drying. The problem of proper drying is to be considered further in the beneficiation phase of the program. A physical property closely related to moisture content and particle size is the absorptive power of talc. The hygroscopic property is highly important, inasmuch as it is a factor in deodorizing, coloring, in the carryirig of perfume or other agents, and in . the retention of moisture. Because this subject is only partly understood at this time, it will not be reported on here. The property is not immediately pertinent to the other me chanical and physical relationship s in this report except through moisture content. Protected Document--Subject to Protective Order M E M.O R I A L I I I I I I I I I Absorptive Power BAT TEL L E I I I I I I INSTITUTE I I I I I I I JNJAZ55_000000927 I I I I I I I I I I I I I I I I I I I I I I 21 Alkalinity The 15 samples of Italian talc collected at Cranford were measured for pH on a Beckman pH meter standardized at neutrality and checked with Beckman buffer solutions of pH 7 and pH 10. The figures are accurate to about O. 1. The samples were prepared by mixing 5 grams of talc with 10 cc of distilled water (pH 6.9). The solutions were agitated and permitted to stand for 2 hours prior to their measurement. The pH of the Cranford samples ranges from 9.0 to 9.3 (Table 16). TABLE 16. pH OF CRANFORD SAMPLES Date of Sample pH 8-10-56 8-20-56 8-28-56 9-6-56 9-12-56 9-19-56 9-27-56 10-4-56 10-12-56 10-18-56 10-29-56 11-6-56 11-15-56 11-30-56 12-22-56 9. 1 9.0 9. 3 9. 1 9. 1 9.2 9.2 9.2 9.2 9. 0 9. 1 9. 3 9.0 9. 1 9. 2 To see if there was any relationship of pH to other physical properties, a Cranford sample with a pH of 9. 2 was sized and the fractions were measured (Table 17). The size fractions each measured 9. 2, which showed that within the precision of the instrument there was no difference due to particle size or variation in the concentration of carbonates. Studies in progress will determine the practicality of removing the dolomite to the degree that the pH will'be lowered. Effective lowering of the pH would lessen Johnson and Johnson's expense of the acid additive. BATTELLE Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000928 I I I I 22 TABLE 17. pH OF SIZE FRACTIONS OF ITALIAN TALC Tyler Mesh Size pH Uns eparated 9.2 +200 -200+250 -250+270 -270+325 -325+400 -400 9.2 9.2 9.2 9.2 9.2 9.2 Acid Solubility Acid-solubility measurements were made as a part of the study of the carbonate component of Italian talc. It has been demonstrated that carbonate comprises the major amount of the contamination and that its removal decreases abrasiveness and improves lubricity. The per cent solubility was first determ.ined gravim.etrically by the m.ethod outlined in Johnson and Johnson's Raw Materials Specifications sheet. The figures obtained were considerably lower than the 6 per cent solubility lim.it perm.itted by the specifications; however, they were greater than the figures anticipated from. the sIUall amount of carbonate minerals observed petrographically. Solubility analyses determined gravim.etrically ranged from. 2.10 to 2.81 per cent, showed no relation to any of the physical property measurements. It was assumed that there was either a greater am.ount of soluble m.atter in the im.palpable fine fraction, or that there was a constant large sam.ple los s during handling. To resolve the problem the carbonate cOIUponent was determ.ined petrographically to be primarily dolomite, and a volumetric method of analysis was devised to analyze closely for small concentrations of dolomite in talc (Appendix B). The figures derived from these methods and computations are pre sented in this report as "equivalent dolomite". It is the measure of the total per cent of dolomite in the sample, not its incidence, which is a function of grain size. The equivalent dolomite analysis is recommended as a substitute for the previously used gravimetric analysis. The method is adjustable for larger concentrations, and other computations may be substituted when carbonates other than dolomite are present. Equivalent dolomite is correlative with petrographicall!y observed contamination and with related physical properties both in size fractions and in whole powder. A grab sample of Italian talc from the large bulk sample obtained from Cranford, containing slightly higher than average contamination, was analyzed for equivalent dolomite. The analysis showed 1.87 per cent. To check the analyzed percentage against the incidence, a series of grain counts was made on separate immersions, running 1.8, 1.8, 2.0, 1.8, 1.9, and 1.9 per cent. The average 1.8+ is essentially the same as the 1.87 per cent BAT TEL L E Protected Document--Subject to Protective Order MEMORIAL INSTITUTE I I I I I ·1 I I I I· I I I I I I· I I JNJAZ55_000000929 I I I I I I I I I I I I I I I I I I I I I I 23 determined volumetrically. In other cases a concentration of dolomite in the coarse sizes cuts down incidence, as a concentration of dolomite in the fines increases incidence. In the consideration of contaminants in regard to flotation, or of the measurement of lubricity or abrasiveness, the actual incidence of the contaminants is the important consideration. Within the range of Italian No. 1 talc, however, the difference is usually small. Table 18 shows a comparison of the gravimetric and equivalent dolomite analyses, the incidence of contaminants, and lubricity, as listed against increasing abrasiveness. Table 19 shows contamination and equivalent dolomite compared with decreasing lubricity. These show the primary relationship between abrasion and contamination, and the secondary relationship of abrasiveness to lubricity in whole powders. This was also demonstrated by Table 9 of this report. Table 20 compares the equivalent dolomite, contamination, abrasiveness, and lubricity of sized fractions of Italian talc, demonstrating that the fines contain the more abrasive particles. Inasmuch as the carbonate 'iil the Italian talc constitutes a rare component in all size fractions, it~ removal by sizing is not practical. Any practical beneficiation process would be concerned with effectively removing the carbonate from the whole powder, thus improving the slip while eliminating the major abrasive. The effects of flotation on lubricity, abrasiveness, and contamination are presented in a report(8) on the beneficiation of Italian No. 2 talc. REFLECTANCE AND WHITENESS Discussion The terminology of properties involving the behavior of light is very complex and for the purposes of this report the discussion will be limited to reflectance, whiteness, and gloss. Reflectance is the measurement of the return of light off of a s~rface in ratio to the intensity of the incident light. This may be measured in terms of brightness, apart from color. Whiteness may be measured in either terms of reflectance over the whole spectrum as "lightness", or in the sense of the absence of specific colors. Gloss is the measure of shininess of surface or specular reflection, as distinct from total reflection. Gloss, closely related to reflectance and whiteness, will be discussed in a future report when ample samples are prepared to enable assessment of the factors which control the property. Gloss is a separate measurement from those here reported. Although one may visualize the differences between whiteness, lightness, brightness, and gloss, one cannot subjectively differentiate one from another with any precision or determine the contribution of a specific property to over-all effect. The important consideration is the total subjective effect, which is quickly noticeable. However, in figuring means of improving the over-all effect we must relate the contribution of particle size, shape, and specific contamination to both the over-all effect and to specific properties. For example, fibrous talc is white, but less reflective than platy talc. Rutile is highly reflective, but not white. The beneficiation studies designed to BAT TEL L E Protected Document--Subject to Protective Order I MEMORIAL INSTITUTE JNJAZ55_000000930 "'0 o It n It C- O n o l: 3 III ::!. in l: .E III !:lei "'0 o It !:l- <' o III a. ~ c... Z c... ~ I~ o o o ~ TABLE 18. COMPARISON OF THE GRAVIMETRIC AND VOLUMETRIC ANALYSES FOR DOLOMITE AND THE RELATIONSHIP OF EQUIVALENT DOLOMITE TO THE INCIDENCE OF CONTAMINANTS AND LUBRICITY, AS LISTED AGAINST INCREASING ABRASIVENESS -- ----------------- - - a_ It n It C- o o n l: 3 III ::!. in l: .E III !:lei "'0 o It n ~ TABLE 19. III o a. ~ (II EQUIVALENT DOLOMITE, ABRASIVENESS, AND PER CENT CONTAMINATION LISTED AGAINST DECREASING LUBRICITY » ~ ~ ITI r Date of Cranford Sample Lubricity-Board Measurement, sec 9-6-56 11-6-56 9-12-56 9-19-56(c) 10-18-56 8-10-56 9-27-56 8-28-56 10-29-56 10-4-56 8-20-56 10-12-56 12-22-56 11-30-56 11-15-56 1. 083 1.053 1. 030 1. 028 1. 025 1.021 1. 017 1. 007 1. 006 o. 982 D. 971 0.968 0.965 o. 952 o. 936 Incidence of Contaminants(a), per cent Equivalent Dolomite (Volumetric), pe r cent Abrasiveness(b), 10- 3 in. / sec r 1'1 ~ ITI ~ o :0 » r Z f/I ~ ~ c ~ ITI c... Z c... ~ I~ o o o o o III a. ~ ~ TABLE 20. COMPARISON OF CONTAMINATION, EQUIVALENT DOLOMITE, ABRASIVENESS, AND LUBRICITY IN SIZE FRACTIONS OF ITALIAN TALC 1'1 r r 1'1 Tyler Mesh Size Incidence of Contaminants{a), per cent Total Dolomite Tremolite Equivalent Dolomite (Volumetric), pe r cent Abrasiveness, 10- 3 in. / sec Lubricity-Board Measurement, sec 1.9 2.14 O. 990 O. 1. 2. 2. 2. 2. 1. 30 1. 59 1.72 2.00 2. 33 2.48 0.889 O. 951 0.980 1. 030 1.043 1. 099 I: 1'1 I: o :u > r Z Unseparated ±2 <2 Trace +200 -200+250 -250+270 -270+ 325 -325+400 -400 < 1 1 <1 1 1-2 2 2 >2 O-trace O-trace Trace Trace Trace-l <1 1-2 2 2 >2 l/I ~ ~ C ~ rrI c... Z c... ~ I~ o o o '" (a) Determined petrographically. 6 1 0 0 1 1 N a- I I I I I I I I I I I I I I I I I I I I I I 27 remove specific particle sizes, shapes, or contaminants, in order to improve the appearance of the talc, will be best controlled when the reflectance and color properties can be assigned to particular components of the powder. As in the lubricity and abrasiveness studies, when the causes of variations are determined, it becomes possible to v:isualize the means of improving the subjective property. The reflectance properties of talc begin a new category of measurements. The reflectance properties are distinct from other physical measurements insofar as direct relationships are concerned, except when particle size, surface area, and purity are concerned, as the following experiments demonstrate. It is apparent at this stage of the. investigation that some degree of over-all appearance can be controlled by the selective removal of particular particles. The Measurement of Reflectance and Whiteness The Italian talc is nearly pure white and highly reflective. The work under way on reflectance and whiteness is designed to devise a means of improving these properties, particularly in lower grade talc, as the result of interpreting their variations in response to the variations of other physical properties. The program includes determining the effect on whiteness and reflectance of the removal of specific sizes, shapes, and contaminants by beneficiation. To date the measurements include only those made on a Photovolt Photoelectric Reflection Meter* and on a Gardner Color Meter*~~. The Photovolt instrument measures diffuse reflectance in terms ofllwhiteness ll or luminous apparent reflectance (LAR). Whiteness in this sense is a matter of lightness without regard to color. A green tristimulus filter is used in the measurement, a standard procedure which permits interlaboratory comparisons. The instrument is calibrated against standard enamel and porcelain plates. The LAR of the Cranford samples is presented in Table 21, showing a range in measurement of 95. 0 to 97. 5, with no discernible relationship to other properties of the whole powder. To determine the relationship between LAR and particle size, measurements were made on size fractions, which demonstrated greater reflectance in the fine s (Table 22). This indicates that particle size and surface area are important factors. To test if particle shape is also a factor, measurements were made on the products of cyclone classification. These measurements showed that the underflow (platy talc) has a greater reflectance than the overflow (fine acicular talc). A third test made on flotation products demonstrated that purity of sample is also a factor, the float product producing a higher reading than, the starting sample. The data related to shape and purity will be included in a report on the beneficiation of talc. The Gardner Color Meter, among other applications, measures properties designated as Rd and tb. The Rd measurement is one of reflectivity in the sense of brightness, apart from color. The higher the Rd value obtained, the greater the brightness. The tb measurement is one of color based on yellowness, but corresponding to whiteness in near white materials. The lower the tb value the greater is the whiteness. ·Model 610, Photovolt Corporation, New York. New York. "Gardner Instrument Company. Bethesda, Maryland. This is similar to the instrument used by Johnson and Johnson's Research . Laboratory. BATTELLE Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000934 I 28 Measurements made on the Cranford samples showed a range q.f 91. 30 to 93. 25 for Rd and 1.55 to 1.95 for +b, with no correlation as yet established with other physical properties (Table 21). To test if particle size has any effect on Rd and +b, measurements were made on a series of size fractions, showing that brightness increased in the finer fractions and that whiteness increased with fineness except for the minus 400-mesh fraction (Table 22), In order to interp'ret the aberrant figure the minus 400-mesh fraction will have to be subdivided and further +b values obtained. It is expected that the concentration of extremely fine acicular particles in the minus 400-mesh fraction accounts for the decr~ase in the +b measurement. It appears, since 1.60 is the value obtained on the whole powder, that whiteness is lower in the extreme. particle sizes, both coarse and fine. To test the effect of purity of sample on Rd and +b, measurements were made on beneficiated products, showing that the r~moval of contamination measurably improves Rd and +b. Measurements to be made on cyclone products will demonstrate the effect of particle shape on these properties. These studies will be presented in a forthcoming report on the beneficiation,of .talc. Further work is recommended in the matter of improving the sheen of talc. Further investigation is required in the tracing of the specific properties of reflectance to specific particle s prior to visualizing beneficiation for the improvement of sheen. It is hoped to be able to adapt a Glossmeter for use on powdered talc in order to be able to correlate properties and plan beneficiation for the improvement of specular reflectance. When sheen can conclusively be traced to specific physical propertie s of the powder, I,' then beneficiation for its improvement can be visualized. THE DUST COMPONENT ; For the purpose of this report dust may be defined as that fraction of the talcum which remains air borne when the powder is shaken from its container. The dust may be collected for examination by passing a moistened glass slide through the dust cloud which remains suspended in the air when talc is shaken from a container, or by similarly sampling the suspended material after an open container is struck on the bottom onto a table or similar surface. Such action produces two classes of matter, a cloud comprising the bulk of the talc which quickly settles, and a fine portion which does not. Material so collected has been analyzed petrographically and has been found to be composed primarily of platy talc, essentially free of contaminants or acicular particles. This talc represents the finer sizes of platelets - the maximum diameter being about 15 J1 in the larger particles. This roughly corresponds to the theoretical <5 -J1 sphere fraction(2) not including any amount of nonplaty grains or coarser platelets; The nature of the dust component has been established and it appear s likely that it is amenable to beneficiation. Work is at present under way devising a means of comparatively measuring the dust component of talc sample s, and to devise means for its removal should it be practically separable from the whole powder. a BAT TEL L E Protected Document··Subject to Protective Order MEMORIAL INSTITUTE I I I I I I I I I I I I I I I I I I I I I JNJAZ55_000000935 I I I I I I I I I 29 TABLE 21. Rd, +b, AND LAR MEASUREMENTS ON THE. CRANFORD SAMPLES Sample Date Rd +b LAR 12-22-56 9-12-56 8-10-56 10-18-56 11-15-56 9-6-56 8-28-56 9-19-56 9-27-56 8-20-56 11-30-56 11-6-56 10-29-56 10-12-56 10-4-56 93.25 93. 15 93.00 92.55 92.45 92.35 92.20 92. 15 92.10 92.05 91.80 91.75 91.55 91.35 91.30 1. 75 1. 80 1.90 1. 75 1. 75 1. 75 1. 65 1.55 1. 60 1. 90 1. 75 1.75 1.55 1. 60 1.95 97.5 97.0 97.0 97.5 97.0 95.0 96.0 96.0 97.0 95.5 96.0 96.0 97.5 96.0 96.0 I I I I I I I I I I I I I TABLE 22. Rd, +b, AND LAR AS RELATED TO THE PARTICLE SIZE OF ITALIAN TALC Tyler Mesh Size Rd +b LAR Unseparated 91.40 1. 60 96.0 85.60 . 89. 15 90.36 90.50 91. 50 92.55 1. 90 91. 0 92.0 92.5 93.0 96.0 96.0 +200 -200+250 -250+270 -270+325 -325+400 -400 BAT TEL L E Protected Document--Subject to Protective Order MEMORIAL 1. 45 1. 35 1. 30 1. 20 1. 50 INSTITUTE JNJAZ55_000000936 I 30 APPRAISAL OF PHYSICAL..,PROPERTY MEASlJREMENTS IN THE EVALUA TION OF ORE'S AND BENEFICIATION PRODUC TS The foregoing studies, and those previously reported(l), have established the relationships between many qf the physic::~l properties of talc and subjective evaluation. Many of the devices employed were relpful in establishing the interrelationships of physical properties, have served their purpose, and their use is not requisite to evaluate the acceptability of talc, inasmuch as the interr'elationsh,ip' of properties permits such an evaluation to be made on the basis' of a ~inimum of ~easurements. The subjective tests do not measure specific properties and thus are only of compara.tive value in deciding what is th,e specific problem in' a nonacceptable talc, or how it may be made acceptable by beneficiation. Such tests, however, must remain the final analysis of acceptability of beneficiation products or in the selection of naturai highgrade tales. The subjective tests are both,a matter of touch and visual comparison. Tested by touch, individual consid~ration may be given to slip and abrasiveness. , Quickly noted in nonacceptable tales or improper grinds of <;>therwise acceptable talcs are dry floury feelings, pastiness, the rolling of the powder', poor spread which leaves portions unlubricated, and coarse or sharp grit. Visually it may be quickly noted if the powder is colored or off-white, without sheen, spJ;'eads unevenly, C"ontains coarse brilliant particles, or contains a high compoI}ent of ex~remely fine dus~. To measure improvement'in'talc, to maintain quality control, or to visualize proper beneficiation for the improvement of a talc, 'it is necessary to measure specific physical properties of the powder as a whole, to know the size and shape of the talc particle s, and the nature of the contaminants. Following the subjective appraisal, of foremost importance is petrographic examination. Such a study esta~lishes the platy or nonplaty nature of a talc, identifies the contaminants, and should establish the general size distribution, incidence, degree of subdivision, habit of aggregation, and crystallographic varietie s, of the talc, carbonates, amphiboles, and accessor.y mineral compo~ents. In order to beneficiate for the, improvement of slip or the elimination of grit, it is necessary to know the size distribution,not'only of the crystallographic types 'of talc present, but also of the different impurities. Size-distribution procedures yield products which may be studied petrographically. These include screening, in the coarser fractions, and sedimentation in the fine s. The measurements assigned sedimentation products in usual procedures should be checked petrographically inasmuch as talc platelets behave in the manner of theoretical sphere s of much smaller dimensions. A practical method of comparing pow~er~, so lon'g as the theoretical measurements do not become mistaken for actual diameters~ is the Andreason sedimentation technique, previously reported( 2). When this method is employed with supporting petrography it should be a satisfactory device for evaluating beneficiation products. Without proper size and mine.ra~ knm,yledge of a sample of talc, beneficiation procedures cannot be developed.' Control'over the physical properties of a talc of known and fairly constant composition could be keptby the use of refinements of the experimental lubricity and abrasion-m'easuring devices. However, a knowledge of the Inineralogy and size distribution is recommended for, any talc. BAT TEL L E Protected Document--Subject to Protective Order ME~ORIAL NSTITUTE I I I I I I I I I I I I I I I I I I 1 I 'I JNJAZ55_000000937 I I I I I I I I I I I I I I I I I I I I I I 31 'The measurement of surface area, specific surface, porosity, and average diam ... eter will be considered further in regard to compactibility and ullage, and the absorptive power of talc; however, these are not necessary to consider as prerequisite to beneficiation studies for the improvement of the physical properties of talc. The lubricity board and abrasion machine were built to measure small differences in heretofore purely subjective propertie s and to relate them to established physical measurements. With proper mineralogical and size-distribution knowledge, these properties will be reflected in the other physical measurements. The following presents the measurements which should be attained in beneficiation products in order to produce material equivalent in quality to Italian No. 1 talc. Improvement of these properties will, of course, produce superior powder, when not improved at the expense of other physical propertie s. Beneficiation studie s on Italian No. 2 talc have produced powder considerably superior to grade No. 1 Italian talc in slip, purity, and the absence of grit. The following are the recommended requirements for beneficiation products to be the equivalent of Italian No. I talc. The items considered important at this stage of the investigation are marked with an asterisk. Mineralogy':' Platy talc, 90 per cent or more Nonplaty talc, less than 10 per cent Carbonates, less than 2 to 3 per cent Amphibole s, Ie s s than 1 pe r cent Accessory minerals, trace only Opaques, none. Size Distribution~~ (1) Whole powder: Gr·eater Greater Grea.ter Greater than than than than 150 200 325 400 mesh, mesh, mesh, mesh, none less than 1 per cent less than 10 per cent less than 20 per cent. The powder should have a size-distribution curve over its general range similar to that shown by Andreason sedimentation measuremend 2) of theoretical particle s. Many of the particles finer than the theoretical 5- J.l. sphere s are unde sirable, repre senting fine acicular grains and dust. Fines, however, should not be removed to the extent that the bulk density is raised beyond present specifi'cations. (2) Contaminants: ,Greater than 250 mesh, less than I per cent -250 to +400 mesh, not more than 2 per cent Finer than 400 mesh, less than 3 per cent. Note: There is reason to believe that the grind of Italian No. 1 talc is finer than optimum for the production of a superior beneficiated talc. Possibly talc 100 per cent minus 100 mesh would be fine enough. The principal reason for a minus ZOO-mesh grind for the currently used product may be to reduce the grit to a size where the platelets mask it. With beneficiated talc this would not be necessary and there would be less fines to discard. BATTELLE Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000938 32 Lubricity Measurement Greater than O. 93 second, preferably greater than 1 second. Porosity Approximately O. 45 to O. 50. Average Particle Diameter Approximately 2.4 to 3.3 jJ.. This measurement is made on the Fisher Subsieve Sizer, the figures are of theoretical particles but are not to be compared with those from 'the Andr~ason measurements. Bulk Density':' 22 to 24 lb/ cu, ft. Specific Surface, Theoretical Greater than 6600 cm 2/ g; preferable measurements lie in the 8000-cm 2 /g range. Abrasion- Machine Measurement Talc pellets - less than 2.7 x 10- 3 in. / sec, preferably less than 2 x 10- 3 in. / sec. Carbonate pellets - less than 1 x 10- 3 in. /sec. Moisture Content':' Less than 0.08 per cent, preferably 0.05 per cent or less. pH Less than 9. 4, preferably closer to 7 in order to lower the expense of the acid additive. Acid Solubility'~ Gravimetric, less than 3 per cent Volumetric, less than 2 per cent. LAR 95.0 or greater. Rd~' 91.0 or greater. MEMORIAL. Protected Document--Subject to Protective Order INSTITUTE I I I I I I I I I I I I I I I I I I I I I I JNJAZ55_000000939 I I I I I I I I I I I I I I I I I I I I I I 33 +b* Less than 2. O. (An additional color m.easurem.ent, -a, should be taken when tales with a yellow-green tint are studied. ) The above measurements concern purity, slip, and grit, and the measurement of acceptability of beneficiation products. Yet to be reported on are preferred measurements on the Glossmeter, preferred limits of the dust component, absorptiveness, and compactibility. Although specific problems may arise when other than Italian talc is considered, the above measurements should generally suffice formo st raw tales in the measurement of improvement by beneficiation or of acceptability in regard to Johnson and Johnson's present requirements. FUTURE WORK Future work related to' the physical properties of talc includes studies of the absorptive power to talc, measurements of gloss as distinct from whiteness and reflectance, mea~urements of compactibility, the dust component, studies on the effects of different methods of drying processed talc on its physical properties, and further evaluation of the physical properties and mineralogy of beneficiation products. Because of immediate pressure on other phases of work for Johnson and Johnson most of the above studies will be held in abeyance. REFERENCES (1) Smith, W. L., "Studies of the Physical Properties of Talc, Their Measurement, and Comparison", Battelle report to iohnson and Johnson (October 15, 1957). (2) Macdonald, R. D. , letter report to Johnson and Johnson on the Andreason Sedimentation Pro cedure (April 1, 1958). (3) Smith, W. L., and Snider, R. H., "Investigation of the Salgada and Casa Nova Talc Deposits of Brazil", Battelle report to Johnson and Johnson (May 28, 1957). (4) Smith, W. L., letter report to Johnson and Johnson on the talc deposits of Madoc, Canada (July 25, 1957). (5) Brown, W. E. , letter report to Johnson and Johnson on the flotation amenability of Italian and other tales (January 24, 1958). (6) Report in process describing results of classification of talc by cycloning. BAT TEL L E Protected Document--Subject to Protective Order MEMO'RIAL INSTITUTE JNJAZ55_000000940 I 34 (7) Sc1ar, C. B., Snider, R. H. , Macdonald, R. D. , and Tangel, O. F., "An Investigation of Selected Talc Deposits of the United States ll , Battelle report to Johnson and Johnson .(February 29, 1956). ( 8.) Brown, W. E., Smith, W. L., and Macdonald, R. D., liThe Physical Concentration of Talc Ore s - Flotation " , Battelle report to Johnson and Johnson (May 23, 1958). The original notes on the laboratory work described in this report are in Battelle Laboratory Record Books No. 13034, pages 78 through 96; No: 14187, pages 44 through 100; No. 14431, pages 7 through 100; and No. 14677, pages 1 through 8. The work was done in the period from October 21, 1957, to May 5, 1958. W LS:djo / gpi/bah SA T TEL L E Protected Document--Subject to Protective Order M E M 0 R I A L' INS T , T U T.E I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I I APPENDIX A DESCRIPTION OF ABRASION MACHINE AND TECHNIQUE OF OPERATION 8 A T TEL L E Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000942 I I I I I I I I I I I I I I I I I I I I I I A-I APPENDIX A DESCRIPTION OF ABRASION MACHINE AND TECHNIQUE OF OPERATION The experimental device described as the abrasion machine in this report (Figures 1 and 2) consists of a 1/20-hp 220-volt 60-cycle 1725-rpm three-phase Westinghouse electric motor, mounted vertically at operating height, fitted with a steel lap. The steel lap has a diameter of 5 inches and is designed so a lap cloth may be held in place by a rubber belt. A Buehler Microcloth was selected as a standard lapcloth. The lap is housed in a steel bowlS inches deep and 9-1/2 inches in diameter. A spout extends from the bottom of the bowl to carry the tested slurry into a beaker. A plastic shield is fitted over the top of the bowl to prevent spatter. A hole in the shield permits observation of the operation and access to the sample holder and slurry feed tube. The slurry feed tube and a cylindrical 1/2-inch-diamete r sample holder are fitted into a metal strip which is fastened in place over the lap. The sample holder is fixed 2 inches from the center of the lap. Directly behind the sample holder the slurry feed tube is fixed in a similar position so that the clockwise rotation of the lap brings the slurry which is to be measured under the standard talc pellet. The talc test pellet is held onto the lap by a 16. I-gram weight which prevents the pellet from skipping or floating on the rotating lap. The slurry feed tube is connected by a rubber tube with an adjustable clamp to a separatory funnel held in a ring stand. The funnel is a 500-ml open-top separatory funnel equipped with a stopcock, and serves as the reservoir for the slurry which is to be measured. The time of operation is kept on a Kodak electric timer. The pellets are made of minus 400-mesh Italian talc pressed in a F. S. Carver Laboratory Press under 50,000 psi. The pellets are 1/2 inch in diameter, and the 5. 2-gram samples used make a pellet about 7/10 inch long. In addition to the standard talc pellets used in the measurement of total abrasive particles, carbonate pellets were used to measure abrasion by the harder contaminants alone. The carbonate pellets were made by fusing three parts by weight of sodium carbonate to one part of sodium borate into a melt. The fused melt was then crushed and pressed similarly as the talc· pellets, under 15,000 psi. Because of swelling during drying the carbonate pellets must be measured wet, unlike the talc pellets. Also, because of slight solubility, the slurry to be te sted must be a mixture with alcohol instead of water. The carbonate pellets are less satisfactory than the talc pellets, however, they se rved a specific expe rimental purpose. In operation, the slurry, composed of 3 grams of the talc to be measured, in 350 ml of distilled water, passes onto the rotating lap at a rate controlled by a clamp on the feed tube. The slurry is carried under the standard pellet where the abrasive components wear the pellet at a rate approximating abrasion of the pellet by some 1800 ft/ min of surface composed of the sample slurry. Pure samples of talc were found to effect little abrasion, while contaminated talc was found to quickly wear away the pellet. The amount of abrasion loss as measured on a Starrett micrometer caliper is divided by the number of seconds of abrasion to provide figures representing the degree of abrasion. Should similar experiments be repeated, the following are important considerations. In any se~ies of tests the operation time of the machine should be essentially the same. The talc slurry should be kept in suspension by agitation. A new lap cloth should be used BAT T EL L E Protected Document--Subject to Protective Order MEMORIAL INSTITUTE JNJAZ55_000000943 I I A-2 as soon as any wear is noticed. All the talc pellets used in a series of tests should be pressed at the same time. Talc pellets should be dried overnight before measuring, to prevent any swelling effects of absorption of water. When any reruns are required on the abrasion machirie, the slurry feed should be adjusted to reproduce former readings before comparative data are sought. To make proper comparative measurements the abrasion machine should be operating so as to make replicate tests showing a difference of not ~~re than O. 1 x lO- 3 in. / sec of abrasion. 8 A T TEL L E Protected Document--Subject to Protective Order M EM OR I A L' INSTITUTE I I I I I I I I I I I I I I I I I I I I JNJAZ55_000000944 I I I I I I I I I I I I I I I I I I I I I I APPENDIX B DETERMINATION OF EQUIVALENT DOLOMITE CONTENT IN ITALIAN TALC BY VOLUMETRIC ANALYSIS by W. E. Brown BATTELLE Protected Document--Subject to Protective Order MEMORIAL INSTITUT~ JNJAZ55_000000945 : 'ffbf 0 \ f t.. '- /1 #~~/(--e ; cr/" ~ '~ #'" ) A' A 1/1~ ". . ',t.:., . I) , I , '...' !(/ )~" V ./ /. (. t ,j)" r t . "-0 / t~ ~ .' (j )( jJ~ \ I: 7 '7'