Document Rj1KE95jM5bN3MBQogxavKnzz

MINING AND METALS DIVISION p. o. box 579, Niagara falls, new york 14302 To (Noma) Division Location Dr. H. B. Rhodes UCC Mining and Metals Niagara Falls, NY 14302 Copy to Messrs. R. E. Byrne, Jr. ^ V. D. Holt F. H. Larrison ^ E. C. Madlangbayan 0. J. Malacarne^ R. 0. Marsten J. L. Myers ^ J. E. Skvarla W. C. Thurber^ R. G. Woolery File Dot* Originoting Dipt. July 11, 1974 "Calidria" Asbestos Aniworing litter dot* Subjoct RG-244 Quality Control Study V- The attached report, RG-244 Quality Control Study, deals with the findings and recommendations concerning the quality control of RG-244. The author made three trips to the King City, California plant since the first of the year for the purpose of this investigation (January 21-February 3, March 1021, and May 5-16). Considerable testing was performed at the Niagara Falls laboratory on production samples obtained during those visits. Understandably, in the evolution of the process, consideration has been given to those elements which have significant effect on production rate or product cost. In some cases, "the presently possible" rather than best performance has been the governing factor in standard establishment. For example, 25mm instead of 10mm cyclones are used for the final stage of classification because lOnin cyclones are difficult to maintain. Much of the equipment is second generation due to economic considerations. Chemical treatment is maintained at pH 7.0 rather than the preferred pH of 8 because slimes clog the press filters rapidly at 8. These factors are considered pertinent to the findings of this report. The most important evidence established by this study to date shows inadequate preparation of the feed prior to chemical treatment, i.e., insufficient particle size reduction and fiber liberation. According to Messrs. Byrne and Chwastiak, The Chemical Modification of UCC Chrysotile Asbestos I. Silica Modification for Viscosity Control, "The initial step in the (RG-244) process is the preparation of an asbestos feed which is sufficiently well liberated. A slurry of asbestos which contains less than 4 percent by weight of solids retained on a 10 micron sieve has been found to be acceptable feed material." At no time during the course of this study was feed material found to meet this qualification. The report presents evidence demonstrating problem areas and provides recommendations for improvements. BLI:cjb + arlimDn + Lite4 B. L. Ingalls RG-244 QUALITY CONTROL STUDY Test Work by: B. L. Ingalls R. J. Kennedy E. C. Madlangbayan T. C. Thompson Report by: B. L. Ingalls June 27, 1974 Supervisor: Dr. H. B. Rhodes UNION CARBIDE CORPORATION Mining and Metals Division Niagara Falls, New York , TABLE OF CONTENTS 1i Paae INTRODUCTION................................................................................................................................. 1 APPARATUS AND PROCEDURE.......................................................................................................... 1 DISCUSSION AND RESULTS........................................................................................................... 2 Performance Characteristics of RG-244 Circuit................................................... 2 Wet Beneficiation............................................................................................................ 3 Wet Refining............................................................................................................ 4 Cyclone Classification....................................................................................... 4 Results of Production Tests....................................................................................... 5 Tests During Off-Spec. Production............................................................... 5 Effects of Temperature onRG-244 Process.................................................. 5 Centrifugal Techniques.................................................................................................. 6 CONCLUSIONS.................................................................................................................................... 6 RECOMMENDATIONS................................ 7 ACKNOWLEDGMENTS........................................................................................................................... 7 APPENDIX A - TABULATED DATA (Tables X - XX)................................................................ 27-45 APPENDIX B - TEST PROCEDURES Centrifugal Test.............................................................................................................. 46 Laboratory Silica Treatment of Asbestos Samples............................................. 47 Wet Screen Analysis - Dispersed Asbestos............................................................ 48 Wet Screen Analysis - Flocculated Asbestos.......................................................... 49 Polyester Viscosity Test for RG-244...................................................................... 50 APPENDIX C - COMMENTARIES 1. Letter - R. G. Woolery to H. B. Rhodes, dated February 15, 1974, RG-244 Quality................... 51 2. Memo - J. E. Skvarla to H. B. Rhodes, dated February 22, 1974, Sources of Variability in RG-244 Quality..................................................... 54 3. Letter - R. E. Byrne, Jr. to H. B. Rhodes, dated June 17, 1974, RG-244 Quality............................................................................................................ 56 4. Letter - G. L. Dickson to H. B. Rhodes, dated June 27, 1974, RG-244 Production...................................................................................................... 59 LIST OF FIGURES Pa^e Figure 1 Schematic of RG-244 Circuit.......................................................................... 8 Figure 2 Effect of Drying Temperature on RG-244 Quality.................................. 9. Figure 3 Effect of Fiber Liberation on RG-244 Quality...................................... 10 Figure Figure 4 Performance Characteristics of Wet End Circuit.................................. 11 5 Wet Screen Analyses of Wet End Circuit................................................... 12 Figure 6 Dispersed Wet Screen Analyses of Wet End Circuit.............................. 13 Figure 7 Electron Micrograph of PMCOF........................................................................ 14 Figure 8 Electron Micrograph of PMCOF........................................................................ 15 Figure 9 Effect of Increasing Temperature of Circuit........................................ 16 Figure 10 Effect of Tergitol 07 & HAC on Dispersion of Asbestos Slurries 17 Figure 11 Dispersed +25^-Screen vs. Centrifuge % Sinks.................................... 18 Figure 12 Tapwater +200m Wet Screen vs. Centrifuge % Sinks........................... 19 LIST OF TABLES Page Table I Polyester Viscosity of Production Silica Treated Asbestos... 2 Table II Performance Characteristics of Circuit.............................................. 3 Table III Typical Performance Characteristics of The Bauer Mi11.i......... 20 Table IV Typical Performance Characteristics of the #1 Reitz Mill.... 21 Table V Typical Performance Characteristics of the #2 Reitz Mill.... 22 Table VI Typical Performance Characteristics of the Feed Prep. Cyclones............................................................................................................ 23 Table VII Typical Performance Characteristics of Primary Cyclones..........24 Table VIII Comparison of Feed Stock Made During Normal and Off-Spec. Production Runs.............................................................................................. 25 Table IX Effect of Temperature on Cyclone Performance................................. 26 Table X Centrifuged Dispersed Asbestos Slurries............................................ 27 Table XI Polyester Viscosity of Production Silica Treated Asbestos... 28 Table XII Polyester Viscosity & Percent Magnetite of Silica Treated Asbestos Slurries......................................................................................... 29 Table XIII Polyester Viscosity of Silica Treated PMCOF................................... 30 Table XIV Wet Screen Test Data................................................................................... 31 Table XV Main Plant Recycle to 30' Thickener.................................................... 35 Table XVI Percent Solids Variations of 24' Thickener Underflow & #1 Reitz Mill........................................................................................................ 36 Table XVII Centrifuge Test Data.................................................................................... 37 Table XVIII Replicate Determinations - Centrifuge Test Data........................... 38 Table XIX RG-244 Production Data................................................................................ 39 Table XX RG-244 Production Lab Data....................................................................... 40 INTRODUCTION For sometime, there has existed a problem with controlling the quality of RG-244. The problem usually manifests itself at random, evidenced by erratic and low-polyester viscosity test specifications which defy obvious explanation. A program was started in January of this year, the purpose of which was to determine those variables that relate to product quality and to implement proper control. The RG-244 circuit consists of six stages of operation; wet beneficiatlon chemical treatment, filter press dewatering, rotary drying, dry grinding, and packaging. An initial survey of the entire plant showed that conditions In the wet beneficiation portion of the circuit varied widely and undoubtedly affected the rest of the process. It was, therefore, decided to concentrate first on the wet end. This is an interim report limited primarily to those implications. Testing included viscosity measurement, tap water and dispersed wet screening, and a newly developed centrifugal technique for determination of fiber liberation. Parameters such as pH, temperature, and % magnetite were also monitored. Overall, a considerable amount of data was collected and is recorded in tabular form in Appendix A. Only the most important results have been abstracted for presentation in the main body of the report. References are made to the appropriate tabulated data in the appendix for pertinent back ground. Commentaries by R. G. Woolery, J. E. Skvarla, R. E. Byrne, and G. L. Dickson concerning the RG-244 process are appended - Appendix C. Early in the program, their counsel was solicited as preparation for discussions with the production staff. APPARATUS AND PROCEDURE Principal equipment used was the Brookfield Viscometer, International Clinical Centrifuge - Model CL, and Standard Tyler U.S. sieves. Details of the test procedures and pertinent comments are given in Appendix B. All polyester viscosity test data referred to in the report were measured at 6 rpm in accordance with the "Niagara Falls Laboratory Analytical Procedures for Calidria Asbestos Products." (NFLP) Unless otherwise stated, centrifugal conditions were 1950 rpm ("600 GF) for 5 minutes. Centrifugal test data are reported as % sinks; i.e., percent of sample remaining in the bottom of test tube. Wet screen tests were performed according to standard laboratory procedure (NFLP) with the following exceptions; one and a half (1.5) gm dry weight of sample was used for 65* through 2a screening tests. One gram (1.0) dry weight of sample was used for lQ^. screening. The slurries were not mixed in the Hermann Disintegrator in order to avoid additional shearing. Over the course of the past several months, the writer has observed several areas where improvement or updating of standard laboratory procedure would be beneficial. However, further study is necessary prior to any recommendations. / DISCUSSJON AND RESULTS A schematic of the RG-244 circuit is illustrated in Figure 1 to assist the reader. For the purpose of brevity, the following abbreviations are used throughout the report: 355 Reitz (#1 Reitz), 340 Reitz (#2 Reitz), 25mm Doxie cyclone overflow and underflow (Primary COF and CUF), 3" Bauer Cyclone overflow and underflow (Feed Prep. COF and CUF). All data referenced in the report are based on laboratory test results unless specifically referred to as production data. Performance Characteristics of RG-244 Circuit Samples of silica treated asbestos were taken at various stages in the plant circuit at a time when the plant was operating "normally." The samples were processed to finished RG-244 in the laboratory and tested for polyester thickening efficiency. The results are shown below. TABLE I POLYESTER VISCOSITY OF PRODUCTION SILICA TREATED ASBESTOS Sample Point^ Treatment Tank (TT) Press Feed (PF) Press Cake (PC) Dryer Discharge (DD) Raymond Milled Product Average(' 2)' Polyester Viscosity (cps x 10"3) % Loss Between TT & PF PF & PC PC & DD ^ All Sanples with the exception of Product were opened one pass through a micropulverizer. (21 v ' Data Reference - Table XI, Appendix A Some loss in product quality is evident in the press feed due to agitation and the Moyno pump. Major degradation occurs in the press and dryer sections accounting for over a 50% loss in product thickening efficiency. Degradation in the press is presumed due to shear under high pressure. The lump breaker and shearing by extrusion through the screw feeder face plate also account for some degradation. The adverse effects of rotary drying have yet to be satisfactorily explained. The effect.of drying at_elevated tenperatures is illustrated in Figure 2. Outlet temperature of the plant dryer is approximately 150C. -2- Temperature of product In the dryer would not be expected to exceed 100 C due to the endothermic action of vaporization. However, should temperature exceed 100C, some degradation would be expected. The recent purchase of a larger dryer makes any further investigation academic prior to Its Installation. Wet Benefielation Figure 3 shows polyester viscosity of laboratory silica treated asbestos slurries obtained from several points in the process. These samples were subjected to varying levels of shear in a Waring Blender prior to silica treatment. The. data illustrate the most important evidence established by this study to date; i.e., feed to chemical treatment tank (PMCOF) can be significantly improved by additional wet benefi elation. With sufficient wet grinding, even #1 Reitz discharge is comparable to present PMCOF despite the fact it has not been cycloned. The changes which take place in the asbestos slurry during "typical" plant operation and the corresponding effect on polyester viscosity are shown in Figure 4 and Table II. Some supplemental screen analyses data are also provided in Figures 5 and 6. These data emphasize the inportance of the cyclones in the feed prep, circuit. In fact, according to the polyester viscosity tests, the cyclones are largely responsible for beneficlatlon of the feed stock. TABLE II PERFORMANCE CHARACTERISTICS OF CIRCUIT Test Bauer Feed Bauer Disch Wet Ci rcui t #1 Feed Reitz Prep. Disch COF n Reitz Disch Primary COF Total Reduction(-) or Increase(+) Across Circuit Percent Contribution by Mills Cyclones Centri fuge % Sinks 58 50 41 30 29 21 -37 492 51% %+ Retains 45 39 25 12 9.5 3.1 -41.9 54% 46% Polyester Vise, after si lica treatment (cps x 10"'3) 1 4.5 25 17.5 61 +61 7% 93% Data Reference: % Sinks - 181 Table X, Appendix A + 2* Retains - 9, 18 , 27 , 32A, 56, 65, Table XIV, Appendix A Poly. Vise. - Table XII, Appendix A -3- Wet Refining Typical operating results for the Bauer and #1 Reitz mill are given in Tables III and IV. Results show wide variations in percent solids of 11.117.9% and 4.2-14.6% for the Bauer and #1 Reitz, respectively. The solids content of mill feed is usually considered an important factor to grinding efficiency in basic attrition mill technology. Thus, wide variations in the feed would be expected to contribute to erratic mill performance. Methods for improvement are currently under consideration by the Engineering Department. Typical operating results for the #2 Reitz are given in Table V. The evidence shows the #2 Reitz to operate at a lew level of efficiency. Wet screen and centrifugal tests show only marginal inprovements across the mill. Polyester viscosity test data show a decrease in thickening efficiency across the mill. However, this is attributed to limitations of the viscosity test - accuracy 10%. It can be concluded that #2 Reitz contributes very little to fiber liberation. This inefficacy is due, presumably, to low solids of the feed (^2%) which is necessary for proper performance of the feed prep, cyclones. The #1 Reitz discharge is monitored by production six times per day. The samples are tested for % solids and +200m wet screen performed on every other sample (production spec. <20% +200m). The #2 Reitz discharge is sampled once a day, analyzed for % solids, and +200m wet screen (production spec. 2-5% <+200m). Generally, the mills are serviced as problems occur. No preventative maintenance program as such is currently in effect. Mr. E. C. Madlangbeyan and the writer recently began a record keeping program to establish a maintenance history for each of the mills. A preventative maintenance program will be initiated when sufficient data have been conpiled. Mr. Madlangbeyan will be responsible for compilation of the data. * Cycl one Cl assi fi cati on Typical performance characteristics of the 3" feed prep, cyclones are shewn in Table VI, p.23. The magnetite level is reduced^45% by the feed prep, cyclones. A significant degree of gangue and fiber bundles are also removed as evidenced by the test data. The cyclone overflow is monitored by the plant six times daily and analyzed for % solids. A +200m wet screen is run on the composite (production spec. 5-8% +200m). Typical performance characteristics of the 25mm primary cyclones are shown in Table VII, p.24. Percent magnetite is reduced to^O.33% (prod. spec. <0.35%) at this point. Centrifugal tests show a significant amount of liberated asbestos fiber in the underflow of both cyclone operations. These results would indicate that classification can be improved. Primary cyclone overflow is sampled by production approximately every 1-1/2 hours and analyzed for percent solids. Percent magnetite and +200m wet screen tests are run once daily on a composite sample. Production samples of PMCOF are obtained directly from the discharge of the cyclones. It is virtually impossible to obtain a representative sample by this procedure. The cyclones operate at varying degrees of efficiency and it is difficult to obtain a uniformly > representative composite (refer PMCOF, Table XIV - ref. 28-38, 57-79, and 90-99, Appendix A, p.31. Sampling from the hold tank during the later stage of the fill '/ cycle would assure a more representative sample. -4- ' Hold tanks in the circuit constitute a time lag of several hours between the cyclones and final product. As a result, problems are sometimes not detected until several hours after the fact. In the opinion of the writer, both the feed prep, and primary cyclones should be monitored more often. Instan taneous grab samples as well as composites should be tested. Cyclone performance is critical to product quality and more frequent sampling would assure better quality control. Results of Production Tests The preliminary objective of this study was to identify those parameters most critical to the production of RG-244. Efforts to date have been devoted to sampling test programs and the compilation of data necessary for proper definition of those parameters. However, some cursory production tests have been implemented. Tests During Off-Spec. Production During the week of 5/12/74, the plant experienced problems with RG-244 quality typical of that described earlier. The writer was present at the time and samples were obtained during the production of off-spec, product. Wet screen tests of PMCOF indicated higher than normal +200m. Centrifugal % sinks of the PMCOF were also high. Some differences were observed with the #1 Reitz mill but the data was not consistent (refer Table VIII, p.25). Subsequent laboratory tests showed silica treated PMCOF to exhibit very low thickening efficiency in polyester (44M cps). However, efficiency of the PMCOF was improved 59% (70M cps) by additional wet grinding* prior to silica treatment. This is indicative of inadequate refining and/or classification. Electron microscopy showed many large unopened bundles of asbestos fiber in the PMCOF (refer Figures 7 and 8). Unfortunately, a statistical comparison of the samples was not possible due to the limitations of available equipment. The following day, 5/14/74, sodium silicate and acetic acid addition were increased to 110%. Product polyester viscosity tests increased from 33M to 48M cps over the next 12 hours and then began to decrease (data reference - Tables XIX and XX, Appendix A, pp.39 & 40). At approximately the same time, a marked increase was noted in the +200m fraction of the #1 Reitz discharge. As a result, the mill hammers were changed on 5/15/74. Consequently, it was impossible to determine whether the problem was a function of chemical treatment or simply inadequate grinding. The evidence strongly suggests the latter. Effects of Temperature on RG-244 Process During the week of 3/10/74, tests were run to determine the effects of increasing the temperature of the RG-244 circuit. The average quality of_RGr244^ improved slightly during the six-day run at elevated temperatures .(105 - 130F).\ As illustrated in Figure 9, the most significant effect of increasing^emperature was on product uniformity. The average deviation from the mean for production j viscosity data was approximately 3% during the test run as compared to 6% for / the control periods. :4' * 3 minutes in Waring Blender at high speed. -5- Why.elevated temperature improves product quality Is not fully under stood. However, higher temperature was found to improve cyclone performance (refer Table IX). Both the + fraction of wet screen tests and centrifugal % sinks decreased in the cyclone overflows during the run at elevated temperatures with the expectation of +200m on the PMCOF. However, the data by and large are indicative of improvement. This is attributed to lower slurry viscosity which would improve separation. No significant effects by temperature were observed on Reitz mill performance. Temperature may also effect chemical treatment, i.e., precipitation, pH, etc. Limited stucjy has been done in this area and further investigation is required prior to conclusions. Centrifugal Techniques A new centrifugal technique for determining fiber liberation was devised during the course of this investigation. Although asbestos fiber does not meet the exact definition of a collodlal particle (because of its fibrous shape), dispersed suspensions can be made that closely approximate a sol. Many procedures for obtaining asbestos dispersions have been developed over the years, i.e., R. G. Woolery, S. Chwastiak, et al. Aside from minor differences, the procedure consisted primarily of adding BaCl2 (to remove sulfates), Na or Al acetate, and reduction of pH to 4.0-4.5 with HC1 or acetic acid. More recently, Tergitol 07, an anionic surfactant, has been used (J. E. Skvarla). During the course of this stucjy, it was found that more effective dispersion could be obtained with Tergitol 07 by adjusting the pH to 4.0-4.5 with acetic acid. A comparison of asbestos dispersions produced with Tergitol 07 only and Tergitol plus acetic acid is shown in Figure 10. Centrifugal conditions used during the course of this investigation were 5 minutes at 1950 rpm, approximating 600 G forces. The asbestos slurried samples were dispersed by the above method prior to centrifuging. Results were reported as % sinks. The finer the particle size distribution and the better the fiber liberation, the lower the % sinks. The centrifugal data illustrate a linear relationship with +2^ dispersed wet screen tests. This is shown in Figure 11. These data and screen tests at IQ* are indicative of particle size separation below lQ*with the centrifuge at the conditions stated. This test supplements wet screen analyses as further demonstrated by Figure 12, a comparison of +200m wet screen and centrifugal data. The centrifugal test is considered an accurate (est. 10%) and definative method for determination of fiber liberation, however, the present procedure is too laborious for practical production application. Further investigation of procedural technique is planned. CONCLUSIONS Further investigation and testing are in progress. The following conclusions are based on the evidence to date. 1. Primary cyclone overflow (feed to the treatment tanks) can be significantly improved by additional wet beneficiation. This demonstrates inefficiencies in the present process. -6- 2. Wide variations were evident in the percent solids of the feed to the Bauer and #1 Reitz mills, affecting erratic mill performance. 3. The #2 Reitz mill contributes relatively little to particle size reduction and fiber liberation comparable to other stages of the ci rcui t. 4. Elevated temperature in the range of 105* - 130F improved cyclone performance. . Results also indicated more uniform product quality during the production run at high temperature. 5. The use of Tergitol 07 adjusted to a pH of 4.0-4.5 with acetic acid has been found to produce superior asbestos dispersions compared to conventional techniques. 6. Chemical treatment, rotary drying, and cyclone classification require further investigation. RECOMMENDATIONS 1. Results were indicative of inadequate preparation of the feed prior to chemical treatment. It follows, that more effective wet refining and/or classification is required. 2. More effective control of percent solids is recommended throughout the RG-244 circuit in general with priority on the #1 Reitz and primary cyclones. 3. Preventative maintenance programs are suggested for periodic servicing of the mills and cyclones. (A program to this effect has been started.) 4. Both cyclone operations should be monitored more often with inclusion of instantaneous as well as composite samples. It is also recom mended that sampling of the primary cyclone overflow be made from the hold tank during the late stage of the fill cycle rather than the individual cyclone discharges. 5. Further investigation of the drying process pending installation of the new rotary dryer. 6. Further investigation of the chemical treatment process with particular emphasis on the effects of pH and temperature. ACKNOWLEDGMENTS Contributions to this effort were by so many it would suffice to say that several departments were involved, including Engineering, Production, and Research and Development. The many courtesies and assistance of the production staff during ny visits to King City were most appreciated. Much of the sampling and test work were performed by Bob Kennedy, E. "Paco" Madlangbayan, Jack Olearczyk.and "Tomy" Thompson, without whose efforts this report would still be in its infancy, special thanks to Bob Byrne and Harry Rhodes for their assistance, particularly on those occasions when I forgot "the original objective was to drain the swamp!" -7- > @1 it l5\>i&*tc$ CveuL i* % nO J lrtll<l T~~>' <0 <0 9WA rt S N IX IW i"> m V O C tO IQ tt t t* i z AVt/mZ &9UV3&U V3/7*S JO fcjsysthj Jj'S03S//\ y3U.S3A'10cJ 10 < 9 N lfc lV /V \ t rV C K E U F f t L at t f t t E f t C O . **61 2 CYCLES X 84 O IV IS IO N 2 RciTI reeppRtp a-2fUiTZ P//viARr BAufcR pjMCoF 0 Fl6uRC 1 \ 14 '5~` tTLEcTfiolJ M/CRo SfiAPH oF ^*5 . 2 SooX PM CoF (isr-i3-7yj Fl& S ( -15- ! tooWTH oF K ftffcn l^ 7 * f t IGO \ 0 . -11- FiCrone it. FIG-uKt. >1 TYPICAL PERFORMANCE CHARACTERISTICS OF THE BAUER MILL CoT s- tO u <A o m 4- zcan) a\ fN. 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I CM II I CM CM *3- U3 Wt H'-'CON ro o ^ 'O' cH CM' O <It CM O CM VO O *3" -H <-H CT> CM O CM CM CO hh O ro CM --->s0o_)V >c--mo<oo>S--mOQoocrs3e_>)f >iomorn> <--i0S>>uonM_)-,1_o1iXou-n_4. th+c<<a<Ssta(uo-O->ua>-u_O-4tmcr->-)wC+Ooo+"1ooC+MNuC+Oi QitC0wonUJl3-Cvuca0tOE-1> --HiOwctM--olc+OmNtr+folinc+\.mo+--.\ --wCOfp**auiCa>C-*O->D-ie4-Ca>i0CSs3Co<-nOn_u)_X.Jtx-tcoCrn- 22 a> 01 4- cn s- <i-0 Ta3t ionio co UJ -(UC/) =C3 co o >o- *- I U V CM CM > CM o <a3/jl oc Iiii iiIi r^*4 aio> III III Hi- ^H II ii o\ *in* iinn II II CfHMfHN II o* oo CM a> luO u u. o a. ,>i CoO TJ a) La m Lau> t os 111 CJ act 1--o- 11 1 in1 S3- o 5a: o' T j--J- in co iooi ihjs in to 1 CM CO & T3 C01 a. at Q. i- c a.r^ m r-- in o at 4a-t to L. 40J) aMt 3 e t-- A > X mo M P0 E TD E in -o ' tco o 01 fe. CJ LClJI at O M 4a-t l/l to 0L). 4-> 4E as_. 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CO 1/1 -Iam-) *cia-- +* Mid .2 t-- OOC+M cCC+nMO c 7ai 9s)i lc/l 1C oTS aa>. co a-> iow ,\ 4 QUf-) 4<-1> 3 W X NO+ MC+MCU+Mf-H+O' >L*> ri3"m "O CO ao>i-o *+3S-">- 1O<CLU/J1L1Jic/--C1 C IA IA Uu acO>l z<e: M i</ui < X co "O O >u1 c0J cQQ.. >1sC_ *Es"_ OL <a c. +0ia) 4o-> -(ocU- E Tja-3>> ns a> 4(a-/>>) 3 C e E in s_ 4o- > X -c<oa k X f1--/1 aOc>.) +-> i<o--e t-- ra auE. Oomi*li JloO/l m 4- G *5 NM cac> o p>M-1 o 4o3a-)> I/I O1o/1 ~ir--4C-> C=*Mx > oa> H CM CO k X (0A) -rQd 1-- aC>J ca%>.a> DaC/ 4<-e> ns o -24- COMPARISON OF FEED STOCKMADE DURING NORMAL AND OFF-SPEC. PRODUCTION RUNS Grab san^le at 9:30A 1/31/74 Data Reference: Production q u a lity control data Is not appended due to the bulk o f the data, however, the Information Is available at request. Other supplemental data may be found in Tables X, X II, XIV, and XIX. CO -o I <sU- -M> -<MD O-- +> *r-- (O Ll-- co i/I <D O X >a> ,ooii--Zo in i--0-1<S>-4- O- OQ. O. > O -- co ID p- Lool-- Tca3>nw IS !-(/) -p- C CsL-. Oa) Ta3j aUj b C+M o<j a) oo 10a. 0r- ) ICC+DMO (O c o ia. o3 a o zoCo+M: Qs-- ra cn cn o *3" OCO rr id co IC--M CCMO CM ocn CCOJ o\ iiii CJ o 00 o cr--n <o/i "o -o-pNI--* MCo3!-J->tOtC^Oo-cpam-i -Scat->_> r=-= cj 0w<r_-> ^oO)0c0) Q+QNf-">)(<0O!/U-).103+/UE0J) tC+rVAMy, CCI+DMO <-- oCM cn Cp-O* CO CJ 1111 mCCMO CO CCMM *0s | i! iiii OgOCDMO1'+o-QcOOLC3Jp.J- -->+wiw>OUp--JrOo1IQUX/I. fa cn in OCCMO o CM -- <ID a4(0-O) po+oOSC---_prcC^C--nM1O- cn Cp4oOtC-~J-> ^CCprIDOM-l- $ a--X5<3T1J vP'IC*vD3O--. roS--CCoJ rNCr^--^D.. ID or i r<-u* & </) J-(V-Z> -5opOc-l 4o--oQpL0o-).. L. c<<ia-Qu>n coI >>0 | O1i-0) ^f.H1 ^ CM C* TABLE IX EFFECT OF TEMPERATURE ON CYCLONE PERFORMANCE* FPCOF Ant>ient Conditions High Temperature PMCOF Ambient Conditions High Temperature Wet Screen +200 Disp. +25 12.2 13.7 10.i 11.3 2.8 3.0 4.0 2.9 Centrifugal % Sinks 30.8 28.6 23.5 19.3 Data Reference: Tables X and XIV, Appendix A, dates 3/12-19/74. 3/12 and 3/13 were used as controls. -26- APPENDIX A TABULATED DATA TABULATED DATA X- CENTRIFUGED DISPERSED ASBESTOS SLURRIES (REPORTED IN PERCENT S IN K S ) Average o f th re e o r more te s t measure measurements. O Cd o- in iOb ooi o r-r~r'r^r~r~r-P-r^f''C0 -- co CM m -3" W NO oo co oo oo co E -- u_ L ZD Q- O E -- Ll_ LO CL CJ __ o CO CM rO CO r- SO m pn ** * CM CN vo in CO CM in CN cm m o r- CN CM CN CM CN CN VO CO fn ** m go CM Os CN -- VO vO <3 -- CN in NO cn CM NO NO CM IM 4- -C --O cd -- CM =*fc Ox -- r- PO CM O to co vO CM CM CO Cl GO CN CM <T\ CM 4- "O <d <x> cd li. CM =*fc CM -- 00 CO CN CN CL L_ CL L_ o Zo> 0) CM CM vO Oin CM r- CD O' CM CN CN Ov CN in in vo in CL L 0. U_ o -O o . Ll_ in O --o K> m o Os O' CN CM co co O' CN CN NO -3CM N --+- -(CJ Cd -- _Q % m 00 o GO fn * CN m m CN O' CO r>* NO o N* o m -3- L JC (J 3 -- CO Q * r^* Os GO vO vO CN Os in *3 * Os o Os o *3 in Jd O -- -C t4-= Uin -o TT CM CD I 4-1 ID O CN r* in in 0in0 CN O' m in iOn' o vO * * ** mm *4--- 4- 4--- * * * <c cxKo\ o (A o <o iCnL COL O. e o o o -- CN ^3 in o p o < Oo.mO EO o <in CoL n - m -- CM <in -- o o O -- --* -- *3 r* P* p* CN pn pn pin CO 1 Os mmm m m m pn CM CinO O) L. oc. m mo moo. << o CM < in > in <-- -S' -3- 1 CN P1^ mp. mi -3t* 1 m 1 in mI in in mi o 2 JO 42 NT I o CL (0 o "<OD 4 3 T5 in <D O 4C3 ID C r" e -- in O 4- L O-TMoL t-- L .c 4- O 2 o 4- Ltn 4- Q. L 2 2 O) W M3-- -- I- 0.4c (J -- -- JZ <tr * * TABULATED DATA XI- POLYESTER VISCOSITY QF PRODUCTION SILICA TREATED ASBESTOS/ ________ I \ The wet samples were f ilt e r e d and d rie d In an oven 6 I05C. A ll th e samples w ith th e expectlon o f RG-244 product were opened in a M lc ro p u lv e rlz e r (one-pass). OO LAvOmVO SD vf* vO vp no -a- cm \OM> N LTV iO- *>J* Ec 10 10 \c mo mvo nin.31 m NvO (TWO lACM^TCM in N N\D u\ v> oo < f'. r^. co co Nmvooco r>. o\no md r* no no focorom -- m a; no cn -a- m ro m to T3 &9 --O lO no ctn co co un no CO CO NO no --C*" PN -- -- -- -------O'! CO NO 4<iLa.a.<<a.a. IOOOfOUOUn--OfOOOlOIA-NO < QE.QE.CEL-O3" ^ a. a. a.o Eo Eo Eo O l_> (_>(_> -- o< -- a. a. a.zo Eo Eo Eo O** <m o a. a. a. EO Eo EO <Tm\...--.a...N.U...N.U...Nr.O..O..M...n..c.M...J...1 ....o. o<_>ooo o woll r-| - Qcd I | cn CM I r0m--i1 r^i . ro r<>ir oi ipn cim mi ni cnro^i . -i cim mi mi r*H r** r-* i iii m O'* o -- CM N pom i N ^i --i i 1 r** r*- r**. r** ini CM iii o\ cm ocn --cn i CM ^i mi-- i co --o0). --<a-> Eu (/1>0 a(0oO JcC CO <0 0 UV0o_) Jo01*0 C(I01LOO_. o(0u1O1.0 3u o10 a ou>. aoL.. --CTM CcOc 28 IA b U L A ItU DATA - X I I POLYESTER VISCOSITY 4 PERCENT MAGNETITE OF SILICA TREATED ASBESTOS SLURRIES * L. >. PA VI m*->i --in EQ. --O --> UiOn iCl. X aO. -- <ft> iaun V0-T -3" LA-3- oi -- cs -s- r^co N fSN -- -- LA -3- CO vO AnvO r-oo co co owe a> iu c -- ro 4-0 U CL. LC0g)O-0 a_ N (AN CO PA LA in "O iW o I/) PAN I VO -3- 0 P- (TIVC o 0 -- 0 tn^ocaffinooooo PAPA P*A PA PAPSPAPA PA PA PA OOOOOOOOOOO cm IA* o LA O -- N N N U JP U -C .e CM CO NiT LAf^LALALALALACO euc eoc * <<<&. a. a. Q.LA LA o o EO EO EO--...--....P..A..P.A. u u u a\ <rco -- < << < c c a a auuAO o oo OLALAOOOOOOOOO Eo Eo Eo--...--....p..a..p.a.....p.a..p..a o o o <n cnco co oo co PAPA-WLAO -- PAPAPAPAPAO CO -- -- pa-3- <n oi cncn nn u -a- a- -a- -a- 4-1 to o rs r- r** i iii LA <n o -- CM PS PA PA 1 111 CM -- -- -- -a" ^ rs> ii in m CM -- it cm m -a- -a- .ap^ iii <n o -- PS PA PA 111 -a* ii i LA LA OA CM CM CM 111 CM CM a- ^ LA IA PS -- VI PS IA Co 4-> O. tEtoo ain =*b =t T3 J-- U U- u. o o N 4J Q_ t Q. CP PS TO U in a U. o u 4N-4 >* L_ to 0 E-- PS u o. 4-1 *4 44Ec-1) 4c4-4) 44Ec->4 wI4D> 4wI4D-) UI4D) --K conao.. wI--UD IA w +o4 IUD -- IA 4O-* --IOD * IA 4O-1 wL-. "ouuOV3 La.. >* u oLQ.. iuaVno. OVl JC U --O uQ. iVCnoL .--oc x: --uo Q. TiUUQn3. JOCl * mi L. 4o-1 ir_e oo --re a> c E CA cM E -- Ol C E LA c 1 1 A *a> -44tua--o>4 - u 4OL. -4cVo) --au toI--A> 0ua5>) XI :<cru*eV71 J4C4 w tOt"LO4c4).) XI ccn LID. 4V-1 ILoW. 1C14 ucuo 1C cc XX X Ocl mccm, to 3Ln xw: X4- 4A> c c --C c -- CL e rina .Kc "Op Co5 -o u ao2e T-cOOLt2OcPt. XJ1L(. O052P 1C -- 4PS fA -a- -29- TABULATED DATA - X I I I POLYESTER V IS C O S IT Y OF S IL IC A TREATED PMCOF (cps x IO ^ )- (1) The u n tre a te d s lu r r y was reworked in a Waring blender fo r 3 m inutes @ high speed p r io r to S ilic a treatm ent. (2) Average v is c o s ity over 8 hour period fo llo w in g the sample tim e. co > ex MW 4- ^w ex GO -a- o D Mo pa ex N 1 O -oo L u m -- cc Q. > r*s -a*> a- o -i- o -- in JVd i>_* oiOn +l0(0-. -- > in a3oVe &O LCD. --(0i +i0>n-) -- -- o CO 0- < O IPA** --33*- --33"" LPA"s veOx PL^As PCX^v\0O 10 o -- LOA -- WW (N> <t--o/) cx rL*%A --3y" -- WW \CoA *m V --E GO. ca a. oCA 1- W-- MW <CoM I<A 3" * W-- -- L*Q--A. PA a- -3" -3* -3" J* 40-1) eix o 1 4) CA -C rx. U o 1 4) 1 4) LA -C -3- JC o<0 -- -- U i i a> w- U w- o 1 4) 1 4) LA IA L. LA LA U rA L c o *" 0) 4-1 a o EL CD O in in 4) Q U. O o > L. CD E i L. Q. 30 01_) -3o 4U) oL. a >u* 4O-> <L0. jQo(0 ^w "LO. 4CcCu-DD1 in .a>* "4O4-)i CD 4) U 4-1 CD U in 4) U 4) 2 in 4) CL E CD in .4c) -- -JC i-- c\j ro >tj- lo lo m co d <d o^-cMco^-mior** oo aot oioi-cvico^tiflto k m --CM CM CM CM CM CM CM CM CM cO as 0) + 1 iu go I in 4J CM 0) + I 3: o LO 1 0J CM to ro 1 t- 40) o. to O o Q CM + CM CM ^ to to LO to................................... V'v'MMLOOOCMin ZZZIOinM'lflM' ro LO i--LorooLOLOi-- oo CM O *-- M CM "3" C\l LO in LO ^^ ^ m 'S- 'f lo 'S- co . ininininin OONCON'sNNS nnozzzzz 00 ro r- O* IO io to to to to CO r-- ID XXXX'S nnnzzzzz LO ro NOOnM COCOCO SNSifli-noai ZZZ LO 'S' 00 -- O cococo N.'s'SCONOlNM' d d zzz'S'rocococo ro ro cocococococococo ---------------------------------------ZZZZZZZZ cocococococococo V.N.N.'v's'sV.^. ZZZZZZZZ o lo ro lo ro cococo zzzrocMtororo ro ro cm i-- dCMfOOr'-ro io co in n in io co in CM r-- CO CM CM CM CM in CM Nint CO to CO co to cm in m v wxs, CMi-- -- ZZZZZ LO M LO to CO to CO CO VOOOOO'SN.'S'n's 1-- ZZZZZ Xc a I < to a ULlJI OC OOO LO CM ro c+ 0) 0) s_ o oo (/) CM + i. <D 4-> o fO o 3 + Q. <o f-- LO io + ooooinscMoioio in co cm <cr in o in concooicocoSco LO 00 CMO^NNriCONN CMCOininioodd CM O psNNrsioNlOID r-* r** a* m Is* to to to to CO CMCTlO^'X'^'X-X minio z z z z z 00 in d 'S' o to to to <o to CMNCMNXNVS m'3-mzzzzz in IOCMOIPOMJINN 4-ioNcoaoQinco r*rrs,oorN.oor>.r^ Ol f--CMCMd'--LOO'S" O) r* N f- O) N N ro in inmtototor^inin LO to d O -- * CO CO LO LO CO r- fOct N.N WX 'S-'t'tZZZZZ ro COON CO CO CO CO CO WMOSSNSS cocoiozzzzz ro CMdLO'--CMd'S'f'O dOOcoNoo^-om o* lominNrvNioN LO mo n cm in in m o i-CMCOinCMdQN (-- LO rocvji-- rororororo ro ro m CO CO CO CO CO in m x. ZZZZZ in l- i- CO CO CO CO to -- t-- H- ZZZZZ i. i-- m T3 cocoro3'_r^o oo o oo 00 US 10 ^ CM CM CM 10 'S- d00io'S"Ln>--loo CM l^-UOlOtO>--U3 n cmtooo now ^ co'ctocococo't-co c <<c O O LO ooooooo^OOCJr-- C_) O r-- f-- ox <o: <in g-g-g-- g-g--- OOOOOOlO-- OUOUOi-"I---- < < <x O o LO i-g-g-" g-g-^'n C0J0O0O0i--000>>---- d d a* as r-- a> a) d <a ro CIQT> ro on>> co *** u i * * * L. I *** i asa> cm ro in d p* p at CM > r* Ol Q CM Ifl OI CM n CO r- i-- i-- r-- >as CM Ol O r-CM (O in cn CM CM O ro r-I-f-r-r- ro I I I I I I I I lll I I I I Ia iii11 c ro ro ro ro ro CO < i-- i-- r- (O (O (O (O fO ro r--i-- >--rororororo < ro r---- <o ia <a +J as o> 1-- < >*-> ai o < <*- o a>s o r* -C M o a. in H mu 6ion u t/7 *r r-- a N a as t. Si <o to CM coa Temperature 105 - 130F o0s5 CcMo 0CM1 oCO C--O cCmO < CM CO fo^intoN oo co <o co co <o co oio^-CMCO^-mio c TABULATED DATA - XIV (CONTINUED) WET SCREEN TEST DATA Jenperature 105 - 130 F Niocnotco mNioN^ r- r-- f-- i-- i-- N000<0 ^ ^ Cf>rs cm (ON rs n, i-- lO U) Z NNOOO t--Ci--M iC--O ip---- at rC--M CO 00 CM CM ^ iNn4C'M<-^(Ot^ZN 05 C/1 in in in *C '<^.'<^<N.moocro^cioo iooocoo in Z Z Z r_ *" *" r" 0--5--0UO*5^0CUM )OiJnCiN-JQCO in Ol CO CO 00 0 <<<<< (ON( >.NNN.N CO </5 1/1 C/1 GO CO C/1 C/1 C/1 </1 < iC-OCCMO rC--MCONC.ONCN/1 .CNO NC/1. O CM oiuc00o-5) l_ CCL+OMO oCo+M ^*C3O" rC--O 00CO50 CO z rC"M* ^P3"* CCMO CoM o 0055 0co5 " *" rr*- in rLi--OT5 N 10 io < z 1005 CiinnO 0CO0 in 3 CCinMM <c z oino o CSJ 0CCMM5 0iCnO0 ICiOnM ccCoMo 0OCM0 101----5 CM N* i-- 05 cm in CO O 05 00 r- 05 00 05 05 05 34*-0> Q<0. oo + iinn + 'CZx/1 NCZ/5 cn z to z cn z CZ/S1 C--Z/1. C/1 Z 1/1 z C/5 z cn z cn z cn z c-ZNn. <N. Z cn z cn z cn z cn z "zcN CM CO rv. r" NZC V<Z N<Z << ZZ *C3M" CoO oo ioo c < < z: <c z c z Or-- C/5 -o oi Lei cn co co oiCO N CO CM n CO UI O <t 5t ^ Ul 05 co cOo CM CM CM r-- CM CM UIUX'IOZ ^}- CM CM CM CM CM CM CM i" CM < 8 <o <ui i-mr: rO-Uo UO rO-rf--- < s O O O O N. i-- C_> C_) -- z Qc <ifc) &&&*&!- OOOOOOOt-- UUUr-UUUr- 05 4-5 iq CM CO O*- L*fl 0*5 CIO COI COI CIO COI 0) 05 <II0>Q_5 CM CO * U*I 0+5 CiO CiO CiO CiO TCO <0<0>0u0555 **+ O'O I-CM CO Q-Ul 05 CM CO CO -- t-- -- r-- -- I III II II i--i----COCOCOCOCO 05 05 05 ItQ- CIO 05 CM > CO IQ IQ O O4-> 4-> 4IOQ4 <0>5 o +a3 "oC oUo. C/1 05 CL 'll IQ 00o55 C/1 Ll_ O 00o55 CL a. N 4-5 5 .0055 CM _-J9_ TABULATED DATA - XIV (CONTINUED) WET SCREEN TEST DATA Temperature 105 - 130 F a0a1:t +1-0> 4 C^OvOrluOiirn-CinMucoiuiuini ttno < VtnO O<0 NtnCtOn Otnl vOo rt--o CM CO < VO VO to ivno VVOONUC1OVOOlVOOr-NCMNNCON < fN. c0) o*' t+ o to Jk 0M) CM + -a ai CaaO a tCCnMO + ooCM + tototo o m o o r** VZ WZ ZNC-- fO-- 1l--flf^--Of-- CM r-3*" f*x CO o CO CO CO CM VO tn CO 00 Ol Ol cro- Ol rO- Ol VO Ol Ol V OOC^1^<<^<^<^< VO tnvomzzzzz tn oicorx.<<<<< WXN.NS r-- CM<-- ZZZZZ o CM i-- VO CO Ol 40 N VO < CM r-- CM CO Hu- O rto- u CO VO l--OO N r-- IX VO CM O CO CO CO CO r""* to oo to r-- r- o U1NVO r-- i-- ^ rco ui co CO CM in rr"f"p" * co in i-- ooo o UI UI CM IX O U3 Ol UI to CO VOtOtOVOfX'tOCO^S' to vo O W r* N 00 r*^ CO o COCOx^POCMCOCOi-- CO CO z <X.<X.<--<x.><s<--<W< ZZZZZZZZ <x.<----<----<----<----<----<---< ZZZZZZZZ in CCMO Oc) + jCa->J to t. OoC+M 40->) <0 3 Q<0. 1-- oo + 4tXn3 + Cx CO <T ^ LO CO r- CO CO rin-CCOKCTZ1 C'vOff^-CCM rO- iC--O CO 'S'Ol to r-NCOO to Ol cr-ops.rr-- wZ ooivovn co to Ur-- 1i--U r--1 C^Z1^Z<^Z<<^Z<^Z< l-t'oxt'oxt'ost--o.t'Vo 't/s1Nto. J1-- zzzzzzz I-- Ol r- oi rt--n Ol cm CO VO CM Ol ui vo a* <<< zzz <<< zzz CO VCOM oCM CO <co << ZZ << zz rx n to CcMo tCoM COMl CM CM IX CO tn vo vo UI < zzz <<< 2 Z Z Ol CO CO UI O CO r-- CO fx. co Vi--0.--Cf0--<COM<r-Cr-MCr--lCiM- to 0*1 Ulf-- |xN<r-r- CO CO CM CO CO CM CM VO CO CM CO <CC<C<<<<C ZZZZZZZZ <\<w<<--<w<<--<-- ZZZZZZZZ 4/1 T3 T-- fOoir- OONnCO o to/i CM I-- CM I--CM CM CM f-- CM CM 00 m inrsN vo rxrsiocors>4or^'t ui o c_> o o o o o r- OOVOJ OO ti----- < < Qo m in co co a- 00 l-- r- <oLO aoo. i-- CO <0.0. Ol CM < <oco O g.<oo a>m--. aoo. Or-CM <to OOr--- r-- Or- O Of-- 4t * . oior-w co <a-moi CMCOCOi-- r--i-- i--i-- II II I I II i--r--f--COCOCOCOCO < r-- *x. CO 01 <> Ol CM I r- PQC"1O* rcT-o1~* <>aaaOt_>s)l CM CO ^CO1 pCO1a ph4<o->-e *< *in *oi pCa1O pC1Oa pCO1 Ol CXCMO1 . CO <0Oe1l <(>U <0>) ---o4IS-* o 0l. 4/1 4/1 N ai 1 (O CM V/l OOU. e oo <0 * TABULATED DATA - XIV (CONTINUED) WET SCREEN TEST DATA Temperature 1 0 5 - 130VF CD CC to in r-~. id ri--*. co r^. oi oco i-- cm n ^ in to ^ os n COCOOOCOCOOOOOCO 00 o >-- cm co ^ Ot Ol Ol Ot mOl OIO >ON Ol Ol 00 01 Ol 01 A co 01 01 + u u m * irv 4-> CM a> + 2 T3 Lf> a) C\J i/i ro s- + 0) CL l/l o *o o CM + lOOOIr-__ < ID 00 00 CO ^ CM CM CM CM Z r-- ID CM 01 _ < i-^P)ON CM CM CM CM Z c < <t < < ---------------------zzzzz <<< zzzzz in CM CO c+ 01 01 S- o oo oo CM + J- 01 4J o to o 3 + a. to 1-- in VO + NCMinN ^ ^ r-- 3- -S. co co co cm z r-CONN CO CT> CM o -- i-- -- f-- Z < c < < < -z------z------z------z------z- ct < c c < \ ^ 'SN, ^ ^ zzzzz oiNionoifl^N locMOoaiooiom tofCMMM,minin loon^voNooi ^s-c^r^ro^s-iomco *t < < C < t C < zzzzzzzz wzzwzzsz.z'n.z'sz'v r>. cm *3- ID CO o *3- CM 00 00 P-- CM CM r CM CT1 <c \N. c < << w zz c< ZZ o in r-- *---co as r-- r. O ID CM CO r-- co CM CM r-- ID M* CO << W zz t c ^z --z. < c zz << zz ^ CO M- CM CO CM m rs. D p-- O r-- CD Ol CM r-- CM CM co in CM f-- *=c < <c c \V zz c t zz << N. \ zz r** ct> f". ** CO cm CM 00 r- 01 00 88 o in CO o r-- CM << zz << `z--'z's. c< ^ -V* zz c< zz 1/1 -o n in id <M- < ^ o CM CM CM CM Z in ** < <c o in 3 g-g-g-'H O o O O I-- r-UUUi- LooioocoinioNoo p- r-- ^ -- i-- p- r* r* <CC0.Q_0.t0.Q- ooooom>m--o--ocom*--ocm CTlr--CMCMCOcXlCMM" in in m id f-- OO O O CM CM << 8 8 oo O f-- CO CM 3- O CM CM oo o o CM CM << 88 oo *** CMCo^moi p-- r* ^ t-- p-- 11111 CO CO CO CO CO a% 8 CM CO 1 11 P"" CO CO r ^ 11 CO <o ** r-- f-- 11 CO CO ro co P" ^ 1f CO CO ** pa pn 1I CO CO c_> u >l_>- >o- u <_> >o- >o- O CJ >- ><_> u ou >u >u- c CM *ll C4Ob CM CO <Ne CM CO CM CO <i Cftn to LU u. LU U. O O o u O O3 0)to EE EE r-- pa i- fc. i- l_ o. O- a. o. TABLE XV MAIN PLANT RECYCLE TO THICKENER Date 5-15-74 5-16-74 5-17-74 5-18-74 5-19-74 5-20-74 5-21-74 5-22-74 5-23-74 5-24-74 5-25-74 5-26-74 5-27-74 5-28-74 Tons of Open Product Packaged 45.6 48 0 4.2 54 33.6 13.2 0 42.4 37.6 13.5 51.4 61.8 18.6 Tons Average RG-244 Recycled . Production Viscosity 6.68 N/A 4.0 N/A N/A 3.3 3.3 N/A N/A N/A N/A N/A 4.5 7.3 41.2 35.0 43.5 39.9 36.4 FB 41.4 39.8 39.4 44.1 42.0 37.3 38.9 36.2 32.4 Flow Bin -35- TABULATED DATA - XVI PERCENT SOLIDS VARIATIONS OF 24' THICKENER UNDERFLOW & #1 REITZ MILL 24 ' Thickener Underflow Date Time % Solids 1-29-74 1-30-74 1 31-74 3-12-74 3-12-74 3-13-74 3-13-74 3-13-74 3-14-74 3-15-74 3-18-74 3-18-74 3-19-74 Shear Composite Shear Composite Shear Composite 10:30A 1:45P 1:30P 2:15P Composite Composite 10:30A 2:20P 3:05P 11:15P 18.8 15.8 16.4 15.1 11.9 11.3 12.4 12.6 12.1 12.4 13.8 14.7 16.0 #1 Reitz Discharge Date Time % Solids 3-26-74 3-26-74 3-26-74 3-26-74 3-26-74 3-26-74 3-26-74 3-26-74 3-26-74 3-26-74 3-26-74 3-26-74 3-27-74 3-27-74 3-27-74 3-27-74 3-27-74 3-28-74 3-28-74 8:10A 9:30A 10:00A 10:30A 11:10A 12:00N 1:05P 2:00P 3:00P 4:00P 6:00P 10:00P 2:00A 6:00A 11:00A 1:35P 8:00P 2:00A 6:00P 7.3 7.8 10.4 14.6 14.5 14.3 14.0 13.1 12.3 7.3 8.5 7.5 9.8 8.5 13.9 13.9 10.2 14.4 6.9 -36- 10 p GO O' o -- CN PO in VO p CO O' o CO CO O' O' O' O' O' O' O' O' on O' o CN TABULATED DATA XV I I- CENTRIFUGE TEST DATA ' (REPORTED IN PERCENT SINKS) Two grams (bone d ry w+) o f sample was used th ru o u t. Average o f 2 o r more te s t measurements. 2O 0. in x co CN 7o X in x ON z? o Xo X -- in m vO VO p CM in O' CM CM m in p p * co in CN IIII ** O' On NO O O' VO O' -- in in -- CN CN m in ** * i i CO VO m GO VO i O' CM 00 in p VO im p vO o p VO VO p CO -- CN CM CN m m * CN ON i , i i 1 i 1 i i 1 GO CN i | i 1 N- -- i 1 i 1 o 3CO -->+- ECD C i_--------- +- K E Cw OD in in in in in in in in in in in in in in o o o o o o o o in in in in in pppppppp in in in in in in in in o o p o o o vO vO VO VO VO VO VO vO m rr to O< O04 QX i_ o oo o oo CN CN VO CM CM CM CO CT) D *3- CM VO CD in "O co O' m in ON in vO VO VO o -- _ -- CN co _ _ 00 -- _ CO -- ____ ___ V*. D < in < in c in ST in < in < in < in < in X o X o a o r in < m <r in E mm------ -- 1- CM CN CN -- -- -- ^3- -FD p p p p P p p p p p r- p p p O<0 O' O' O' O' O' O' O' O' 00 CO GO ON ON ON rA 1 PO 1 m pA 1 m 1 m 1 pn 1 m iA 1 m 1 pn 1 m 1 pn 1 rn c o -- CD. -P "" CL Q. E L. IT3 o CO 10 o o JZ X -C -C u "O o o "0 o (0 CD o (0 D 10 X -- CD -- CD X -- X u ll u. U. U, ooX o NN a Xo o ooo o o o Cl o o o o o o o CD N N IM >- +- f 1_ -i- -iu -- X -- -- > L- m+mm > >- p > > p l_ L. L. L. L- l_ CD CD CD CD CD CD CD ID {n <T3 <n (0 (0 E X X "O X X E X o *-- E c F F F F 1- CN CN CD CN L. L. l_ L- L. L. 1. X *fc =*fc X =*t =*fc X s*te X X X X X X (SXNIS !N30d3d Nl 031M0d3M) VIVO XS31 39fljlHiN33 o cr II -- pm n in no r* S S S S 8 S n in CnM (SI PM -I on| CM ON KS -- PM --PM PPMM nO| On -- -- PM IA| tO On PM -- PM NO *-- PM " m n HS| om PoM --PM p* NO -- K PM NO -- PM I no PM PM ON -- s> oin PPMM --CN ON " KS * On p -- M PM -- o in o PM . m mo pm POM _ o OPM p --* s 8om mo om Om ion oin ON On On ON On ON ON ON in m in in m in in in *_5* in > (ft A > > in i>n. in > <A > in 9> in r- so r- 0. < < CL au. m a.-- a. q r\ a. in o ^m J oS o8 --o o8 --- 5 | p* <01 KS KN o| t K> C r* p* P- in in i m i Ki| Ki> 1 *n c o --Q.--+a* 4IED0 uOin a o. u. oin o o O L>.- l. to E i o in u_ oa oN L>. 4- _ 9O E <r L. -- 0. h o o &0 ofe >* L>. >L. 11 il a -38 t tr RG-244 PRODUCTION DATA Data Reference: Production Data - available on requiest. IM *--* -M .O r- lO 0) L. OS CS CM ' oo r-- CM CO O rH LO 1 1 1 *111 ^ CO 1 1 1 1 1 o LO LO oi t1 1 1 CO CM r-t CM N +-> 'N *P~ CO CO CO io cn lt> =! o CM ---- 00 CO CO CM CO CM c cxz > rHCVKf K^-COCOCO co r- co co 3- co 0) < CM iH rH H rH r-H H rH pH pH rH CM OJ cH =*= o Ul 4-> 0) ;2 LL. Si JZ 00 a. o a) Ll_ U s: ----- 1 1 a\ 1 1 CO | 1 1 1 ttHfflt-IN in co in co rH '-- LO --1 CO 3- Lf) CO *3" *3" *3^ ^ CO 1 1 o o CM + Ll_ . -- LO LO 00 O CO 00 CO ^ CO P* 00 CO Si z: o Q. O - o o 0^000 f> rH H H n rH 4J pH u 3 a) CM o > 1 o <c CD S- W. oc Q. O CM *3LO LO LO ooo O co in co ^ N N Pv vo N ooooo OOOaiOOOH IvOOcONlflOO oo oooo m "O (/) a) Z (U a) a> Q. > Qu o --< 00 r~~ r-- O. N LfUO a. VO LO LO LO LO C- O- 00 O VO 00 co O CO VO lO (O N N u_ o ao. Cto7> OE. o z: o Ll. 1 CM I LO 1 1O 1 1 1 > ^OCMNN oo r^. to ooooo O CO Ps, LO LO 11 ^o3- 11 o O O 1 -* 1 Uu o cn QE. o <o o i. a. z o 1 LO LO 1 CM CM 1 oo I--I !--1 eg CT> CM CO *3" CO CM OOOOO CM CO CM CM CO CO co co ** co a* ooo oo o "Op--. oLU i- 1-- a) (> n ^ 00 C a. fl'CMOl M* in m H H --4 o CO co CO co c^ vo vo vo to H H H r-H ^4 00 00 O'! LO CO CO ccicoNcomm rH H H H H +-> U 0) rd 10 > r- <C a. > w| "* ^ > r ^ CM ^ r^. cti to CO CO CO * VO ^ P CT> NQOlOQ CO CO ^ IT) CM VO OV CO 00 3- ^3" 3" 3- * xt- ^ r^. iii N1 N1 N1 N1 N1 r- i-- r--. r-- ii iiii CT1 Q CVJCOM'lflO. o CM CO *7 in o CM1 C1O CO1 rH H H rH rH 11111 H rH rH H rH H 1111t1 fH pH rH CO CO CO CO CO to in to to to to r-i~ IO LO r-- C0T)> i vo 'O 0 o # s3 cd o o 1 { f 1 \ 5 u z r\ t to O oto > Ci\. l/> x iw w > rr *1 % >^ * % (V- t rl > Sj "n t 1 to n *i IN. da i i i T *o i.e .jg r 0 z be At tv, r*\ * \ *V S \5 ca < N /V *N r> T Cl & V/ ar cr1 n c o, \ z /M a Uk O' k> c N MS l<7 i/ fv. C V V/ vS oc V/ u> < ? > -i f? 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V/ I &21 t?t* * Ii D P yal D.O.P. % \ uuaz u >u 8N '+ oo + 5 n + \o \D 3 _L Vo jd \ { auu! t Oiun i* 0 > O' \ & *! <3 ifl ft <3 K iV A > <5 c O' O' X c\ < wC CNf `c ii1 "H i NN 3 CO CO i c w o 2 ;u *o =? >i iL~ o d 1i1 t z0 * za O c> v "s. t & & vs Vo r r2 l IV V Uc VS v& a < lg PV V) uS vc 'rf ^ vi \i vS N cV VV O' CC K) tv; ) V vC v vi vO Q Oo VV V/ Oc if /V N C Qc f<6- IS )2 /X tv U 2 P Is S*>3 `Vj r< S Y5 cr 1 rv iVn A*. rt1 uH<a rr $ - -XV X X IV U 5 q; 91C VA o csl V CE t <3 4 1 t a 5?. 1 S 5v <3 ? On S'f ?> fs ts to v ; l o <5; tM 5 Sj Sir' VX. X. X w {J X P - m* - XX - X % X X x X* & f'l fca > > 9\ <C % u j 0. z < (0 u u ce 3 0 Jin ^3 S s uV* v s. *v 6= QC \ f* 'i ti V*. fV N' Q& r 'l 0 1 -e <c V c > m, a: U! >x C Vl vS. C oVa C1 \ * V w+. - j.^,-Q ' ^ v- ____ f*it-__ 1V OV.' 0 cv r f * <5. 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V <c I J C\ -v- l, :> .1 (V 'I i \S r- Vn % v) tf\ r V) \i V '<0 > V > * -j c *> 3 <2 i v! ^5 e C v> VI p IS bi 9g- <s 0. c. a* J {. a* 'i ,c Q 1 -*o V. 1Q LL LL 0 v/) J) o0 Cb C73 1 C <J -7 x* M V J k *60 -C0 ~Cw a LL s. vA y 3 2 * O c0 \L V c h IL w 0 Vd J CJ ~7 Cu OT) 3^ <53 "5 * "S > ri -i* i *A 6 2 >s > M N <A Q. C _ -cCul *0j3 U Li a J >o *8 / S* C VJ 7 o --r . j> w s w 7 > c- O o D u *w *. i 1 i\ i f i 1 i1i i 1A 244 LAB U A IA ^ 4 / ThGLS 'J<& - mT T " O.O.P. .V iIzldl 8N '+ e o 8 0+ tk $ n + i > O' 3< OQ CN O' OC Q v5 v; a0 O'4 o< c c cC d ^ Q (V i i i > NO tii --i i i --i IE 0 ou Si 0 5 3 * < CC 3 3 01 ff fe or CO 3 > 01 {V' / l > c0 Fi \ % o d \ 4 ii i 0i X / * fc 0. v OC or pr es N < N< N. NN N G V. v; nC 0 's ic za vo s: Cr vS *0 to w O' v vr is QC vl cc (V U1 rs Q0 Cc N v K QC <K N ac N OC 0- OC V od 6< d .Xi <Ox <s Q O <: I r a: O' O' fa - - - %0 Vo N Pi C\ c\ < 1 s1 f w 0 cv cv< %tn LT 1 < a % % a. V c 9 cv <L ai i a o CP c\ i Oil cl: L'J U. s 3? 4^ > \n Vr N 0 = c w * 0 N. ^0 Id J a. Z < 4IA 1 1Id U S3e a3 0 3 10 8 ~r n o~ o CNJ cv N c 5 1 cv ,w* 2 C O' cv cv 'C \s O' NS V c^ . if a ts CL p 0 o6 Q C*J 3 8 1 S' "G o UJ Uj 11 UJ a 4 C4 S fS1J * J a * rsj vj i O -X CJ c/3 C <n if U o: a a C i QC Ql IL 1 r S' c 0 V- 3 1 c CV <0 a Q w <\ 5 K sj N t c a u N U] q c\ ***^ (1 8 c Uj U, a q u a S c wC 4J U. ll rr in fsl CJ V C O Cj Q Uj Uj U OC (nh n\ rc \v 1 c $ 1 V Q jr < t, _5 >? P 01 1 0" 3 Leu ] <2 ?> a O' in o: o 3 CN * 3CV X cC c/j c u. 3CC c. c3 CN >< c 0 cr c/ ii Q a c or co Uj C q 3 CN > q: > > q a q cr. or ty c 2 o: a 3 3 <N o: vC Gu V ni i > VI V! > C>H 4 o V, ato ce 1<5 r1 I * 1 1 i i i ! APPENDIX B TEST PROCEDURES CENTRIFUGAL TEST Equipment Clinical Centrifugue Model CL Acetone Tergitol 07 Acetic acid 400 ml beakers 250 ml beakers Lab stirrer (Lightnin) #41 filter paper 15 cm dia. Procedure 1. Prepare a 2 gm (dry wt.) sample. If sample is not in slurry form, wet with 100 ml distilled water. Mix with Lightnin mixer. 500 rpm for 5 minutes. Distilled water should be used throughout; tap water will cause flocculation. 2. Add 4 gm Tergitol 07 and mix with Lightnin mixer (same speed as above) for 1 minute. 3. Adjust pH to 4.3 with HAC and mix additional minute. Dispersion should be visibly evident. 4. Transfer dispersed sample to centrifuge glass containers, transferring any residue with distilled water. 5. Centrifuge for 5 minutes at 1950 rpm in Clinical Centrifuge; other models may be used. Rpm should be adjusted to exert-'600 GF. Calculations for G Force: GF = 0.0000142 n2 Dfa n = speed of rotation rpm D^ = bowl diameter - inches Important: The speed should be adjusted to 1950 rpm within the first 30 seconds. 6. After centrifuging, the supemate is decanted. A small amount of supemate remaining with the settlings (sinks) is desirable rather than to lose any sinks during the decanting process. 7. The sinks are transferred by washing to a 400 ml flask and flocculated with acetone (~50 ml is usually adequate. 8. Filter on preweighed #41 Watman filter paper (15 cm diameter recommended). Dry on hot plate, taking care not to scorch the filter paper. Then transfer to oven @105C for 15 minutes. % Sinks net wt. of filtrate ,, 100 -46- LABORATORY SILICA TREATMENT OF ASBESTOS SAMPLES Procedure 1. 25 gm dry weight of asbestos are treated. 2. Dilute to 2500 ml with tap water in 10 liter bucket. 3. Mix with Lightnin mixer @1750 rpm for 2 minutes. 4. Add 10.0 gm (12% based on the asbestos) of 30% solution. Technical Grade NaSiO^. Mix for 2 minutes. 5. Adjust pH to 7.8 with HAC^28-30 ml 6% acid solution. Mix for 2 minutes. Note: pH may rise slightly after mixing; adjust to 7.8, if necessary. 6. Filter with #41 filter paper. Dry 18 hours @100#C. 7. Open dry 3-4 gm quantities with Waring Blender at high speed. -47- WET SCREEN ANALYSIS - DISPERSED ASBESTOS To determine the basic particle size distribution of dispersed products. Indicates the degree to which a product has been refined to either liberate fiber or to remove coarse particulates. Apparatus - U. S. Sieves, 8-in. diameter, mesh size 200, 325, 25*, and IQ*; fritted glass filters, lab. stirrer (Lightnin), Tergitol anionic 4 or 7, pan or tube to hold 4 liter water. Procedure - For each screen size to be determined: 1. Place sufficient quantity of asbestos slurry in 400-ml. beaker to equal 1.5 gm dry wt. of asbestos. (1 gm(l.O) is required for IQ* screen test.) Make volume tO/^300 ml. with tap water. 2. Add 6 ml. anionic Tergitol to beaker while stirring at low speed to disentangle asbestos floccs. 3. Pour the dispersed slurry into a sieve. 4. Jig the sieve in a tub of water containing 2% by volume Tergitol anionic 4 or 7 until a constant quantity of oversize remains on the screen. 5. Wash oversize material into tared, fritted glass filter, dry, cool to room temperature in desiccator, obtain net weight of oversize asbestos. Report - Cumulative weight % retained on each screen. net wt. oversize ,nn dry wt. of sample x u -48- WET SCREEN ANALYSIS - FLOCCULATED ASBESTOS To determine the particle size distribution of asbestos slurry. Indicates product fineness and quantity of liberated fiber. Apparatus - U.S. sieves, 8-inch diameter, mesh sizes 65, 100, 200, 325; water basin, fritted glass vacuum filters. Procedure - For each screen size to be determined: 1. Place sufficient quantity of asbestos slurry on sieve to equal 1.5 gm dry weight of asbestos. 2. Jig the sieve in basinful of tap water in order to break up asbestos floccs and to wash undersize material through the screen. Continue jigging until a constant quantity of oversize remains on screen. 3. Wash oversize into tared, fritted glass vacuum filter. 4. Dry filter, cool to room temperature in desiccator, obtain net weight of oversize. Report - Cumulative weight % retained on each screen; net wt. oversize ,, 175 x iuu -49- POLYESTER VISCOSITY TEST FOR R-G244 equipment Stirrer 1750 50 rpra, 5-cm. diam. propeller type, three-bladed Viscometer Brookfield LV Mixing Cup 400-ml graduated, disposable, polypropylene Viscosity Cup 100-ml. graduated, disposable polypropylene PROCEDURE 1. Mix by hand 4.0 g. sample into 196 g. of the following homogeneous polyester mixture in a 400-ml. mixing cup: 450 g. Rohm & Haas P-43 resin 50 g. Styrene monomer (or a similar mixture) to provide a viscosity of 550 25 cps at 25 * 2C. Note: The viscosity of this polyester mixture should be checked periodically (about every 8 to 10 determina tions) and adjusted to 550 25 cps at 25 * 2C. 2. Stir 10 minutes with the propeller stirrer. 3* Allow the stirred mixture to stand for one hour, during which it should equilibrate to 25 2C, and pour slowly into a clean 100-ml. viscosity cup. 4. After exactly 5 minutes, measure the viscosity at 6 rpm with a No. 4 spindle. Read the viscosity after 6 revolutions of the spindle. (Disregard any prior dial readings.) -50- APPENDIX C COMMENTARIES JC. w.t.9 internal correspondence MINING AND METALS DIVISION To (Ham*) OiWiioa Ucofeo 0r> H> Rhodes Building 94 Niagara Falls, NY 14302 Copy to P. 0. BOX 579. NIAGARA FALLS, NEW YORK 14302 Oofo Originating D#pfc Annraring Utiir Join Sobjnd February 15, 1974 Technology Department RG-244 Quality In response to your request for comments on RG-244 production, 1 submit that the following conditions must be met in order to produce consistent high* quality RG-244. 1. The fibers to the RG-244 circuit must be highly liberated. 2. The feed must contain a minimum of rock dust and fiber bundles. 3. Conditions for silica coating must be optimized. 4. During filtration only modest pressure must be applied. 5. Only minimal work energy should be applied during pellet (extrusion) forming. 6. Drying conditions must be adequately controlled. 7. Full opening of the dried final product must be achieved without breakage of the silica coating. My recommendations for achieving these requirements are: 1. Fiber Liberation (a) Apply maximum shear energy to fiber bundles (b) For ultimate liberation, this energy should be applied in the presence of chemical agents (A)Cl3, acetic acid, etc.) which enhance liberation. I assume, however, that pollution requirements prohibit this approach. 2. Minimal Rock Dust & Fiber Bundles (a) Cyclone efficiently following each stage of wet opening using smaller diameter cyclone on each -51- Dr. H. B. Rhodes -2- February 15, 197^* successive stage. This will permit the removal of rock dust before it becomes too fine to remove effectively. It also removes the "greenbiaded" product which Is considered a transitional product between serpentine rock and chrysotile asbestos. 3. Optimize Conditions for Silica Coating (a) Ensure that the asbestos slurry and sodium silicate are homogeneous prior to adding acid. (b) Add acid slowly to ensure that localized zones of high pH do not occur. (c) Take care that the pulp pH rise Is slowed at pH where silica precipitation occurs. This would ensure a uniform, smooth coating on the fiber rather than a lumpy coating consisting of a series of pre-precip]tated silica gobs. A. Apply Only Low-Pressure Filtration Pressures (a) The silica coating Is quite fragile at this time and care should be exercised that dis turbance of this coating is minimized. 5. Minimal Work Energy in Pellet Forming Stage (a) The same truths apply here as in A(a). 6. Controlled Drying Conditions (a) Care should be taken that the silica coating is cured carefully so that the proper silica surface conditions are achieved. 7. Full Opening of Dried Product Without Breaking Coating (a) If all the proceeding steps have been achieved satisfactorily, normal opening energy has little or no effect on the final product. (b) An abuse of Item (a) can result in product degradation if sufficient energy is applied so that the fibers themselves are actually breaking down as evidenced by the poor quality of product produced by opening in a Waring blendor at high speeds for prolonged periods. -52- Dr. K. 6. Rhodes -3- February 15, 197A (b) Product degradation Is largely attributed to exposed, noncoated, asbestos fibrils. This may occur as a result of fiber bundles being coated In the silica addition step and a subsequent opening of these bundles in the dry opening'step. Normally, a second pass opening results In a higher quality product. However, where the initial product consisted of coated fiber bundles, a second pass opening can result In a lower quality product. it is, of course, Impossible on this short notice to discuss in detail a theory of RG-244, but I believe the above statements summarize fairly well the theories I have held regarding this product. RGW/bsn -53- i ** Technology Department Mining and Metals Division-UCC Niagara Falls, New York February 22, 197** MEMORANDUM TO: Dr. H. B. Rhodes^ COPY: Mr. R. G. Woolery FROM: J. E. Skvarla SUBJECT: Sources of Variability in RG-244 Quality The following is a list of RG-244 process procedural variations that are believed to be contributing to variability in product quality. Items (A). The recommended corrective measures are noted as Items (B). 1A - Degree of fiber liberation in feed material IB - Two stages of cyclone classification would improve feed quality. The 12 each, 1" scalping cyclones are not presently being used. They should be utilized for first-stage fiber classification with their overflow feeding the 22 second-stage cyclone. The feed solid and pressure to the first-stage cyclones should be increased to produce overflow solid and volume equal to that presently feed ing the 22 primary cyclones. The 3" cyclones on the first-stage Reitz mill product should be moved to the second-stage Reitz mill product. This will increase the useful fiberizing work of the second-stage mill by a factor of four. 2A - Quantitative acid addition to treatment tank 2B - Acid addition should be by pH control and the pH should not go be low 8.0. 3A - Temperature variations in treatment tank 3B - Control temperature with regulated steam sparge to cyclone feed or indirect tank heaters. 4a - Continuous operation of press feed tank agitator 4b - Operate agitator only for a short, fixed time period sufficient to blend the feed batches. -54- Memo re Sources of Variability in RG-244 Quality . # -2- 5A - Overpressure of filter press feed, 45 psi- February 22, 1974 5B - Limit press feed pressure to 40 psi. 6A - By-pass valve on filter press feed pump. . 6b - Replace by-pass valve vith pressure limit switch on pump motor. 7A - Overpressure when air blowing press coke 7B - Regulate air blown pressure to 40 psi. 8A - Variations in dryer product moisture 8B - This is probably due to dryer bed fluidization. Correction would require larger area distribution of inlet gas, deeper bed, or reduced gas velocity. These items, as well as others, were covered in the King City value engineering session. Obey are considered to be those most critical to product quality and product consistency. JES:ms -55- UC 14* INTERNAL CORRESPONDENCE mining and metals division To (Nam*) H. B. Rhodes Dimion Mining & Metals location Niagara Falls, NY copy to 6. L. Dickson B. L. Ingalls J. L. Myers P. 0. BOX 579, NIAGARA FALLS, NEW YORK 14302 Dot. June 17, 1974 originating Oopt. "Calidria" Asbestos Antworing lottor dot* Subject rg-244 Quality Some time ago you asked for my thoughts on the most significant factors regarding the production of high quality RG-244. I have itemized them below, but it should be pointed out that by "high quality" I usually think first of high viscosity in liquid resins, followed closely by resistance to degradation by shear and stability in a polyester resin system. All these factors are usually present in a high viscosity product. The production of RG-244, as you know, consists of the deposition of polymeric silica on asbestos fibers and fibrils. The polymerization of silica is, at best, a tricky business and is dependent on the factors listed below. There is really one_ overriding requirement for the production of good RG-244 which is a well liberated feed stock of asbestos. In the laboratory it is always possible to make good material. This, along with other important factors are as follows: 1.) Well liberated, colloidal asbestos. 2.) Controlled solids content of the slurry. 3.) Temperature of the slurry. 4.) Adjustment of'pH during precipitation of silica. 5.) Time allowed for precipitation. 6.) Careful filtration and drying of the product. Each of the above areas deserve explanation and are detailed below. 1.) Well liberated, colloidal asbestos. High viscosity product can always be produced from almost any of our products, if sufficiently well opened. For example, we have made RG-244 from SG-200 by extensive opening of a water slurry thereof in a Waring Blender. The preferred starting material, however, is high purity slurry which has been passed first through a 25 mm cyclone followed by a 10 mm cyclone. The resulting "COF 10" is characterized by 95% -1Q by a dispersed wet screen test and a low magnetite content. Our present plant circuit is a bastardized arrangement to approximate the same slurry. Attempts to control the plant feed stock by a 200 mesh screen analysis have been universally unsuccessful. -56- In the light of some of Ingalls recent work it seems that the present arrangement of mills and cyclones may not be optimum for producing a uniform feed stock. Regardless of the reasons for varying feed stock quality, it is likely that recourse to a bank of 10 mm cyclones could bail us out. 2.) Solids content of slurry to be treated. Solids content of feed stock is probably only important in so far as it affects cyclone and mill efficiency. We have successfully made RG-244 in the laboratory up to 5 or 6% solids. In order to obtain maximum mill efficiency solids content should probably be high, i.e. 5% +. Our cyclones, however, operate best at 1-2% solids. We have, therefore, recommended feed stock at about 1-1.5% solids. 3.) Temperature of slurry. Due to the polymeric nature of the silica deposited on the asbestos, temperature during silica precipatation can be critical. It was established by Chwastiak and later by me that good product can be made over a wide temperature range, 65 to 150F, assuming adequate pH and time control. It was also shown that both time and pH become more critical as temperatures fluctuate outside those limits. 4.) Adjustment of pH. Here, again, pH control is essential to depositing a reproducible polymer of silica. In extensive lab tests Chwastiak and I showed that the desired silica polymer formed best and quickest at a final pH range of 7.0 - 8.0. Any attempt to control this type of process without regard to pH must be fraught with failure or, at best, wide variations in end result. 5.) Time for precipitation. At pH 7.0 - 8.0 and temperatures 65-150#F.the silica polymer formation is very fast. We could never really establish a lower limit, but certainly 5-10 minutes is adequate. Not too much work was done outside these ranges, but it is certain that time is a more important factor as these limits are exceeded. 6.) Careful filtration and drying. Extensive experiments have shown that filtration of RG-244 slurries above 50 psi result in poorer product. It has also been shown that drying at excessive temperatures, such as 150C, also results in lower viscosities. It is probably true that as we make better product we may be able to violate these limits with minimal effect, but they are useful guidelines during marginal periods. In summary, I believe we need means to insure uniformly - well liberated slurries, treated with soduim silicate neutralized to a controlled pH of about 7.5 at a temperature of SJO-IOO'T, filtered at 50 psi and dried in such a way that the RG-244 does not "see" a temperature above 150*C. In this way we can attain a uniformly high quality product. -57- i You may notice I have not mentioned the dry grinding of RG-244. This is done with malice of fore thought because I believe that a high quality product at the treatment tank will not be unduly sensitive to degradation during subsequent dry grinding. Our focus for attempts to improve RG-244 quality should be directed first to feed stock preparation and controlled silica precipitation. When that is done, most other factors will "wash out." It should be mentioned that it is essential that the operation of the RG-244 circuit should be automatic and reproducible by close control. Stray fluctuation cannot help but affect product quality. In this regard it is important that there be regular maintenance which should include scheduled scale removal and clean up and, most important of all, strict control and supervision. REB:mlv -58- UC 14 1 internal correspondence MINING AND METALS DIVISION To (Naim) dvu!m Location Dr. H. B. Rhodes UCC Mining and Metals Niagara Falls, NY 14302 cop,.. Messrs. R. E. Byrne, Jr. B. L. Ingalls J. L. Myers File P. 0. BOX 579, NIAGARA FALLS, NEW YORK 1002 D"'* AnsworinQ lottor data June 27, 1974 "Calidria" Asbestos Sub'"1 RG-244 Production Bob Byrne's letter, dated June 17, to you on this subject also pretty much reflects qy feelings on the variables which effect RG-244 product quality. However, qy one exception is that dry grinding is an important factor in our process. Based on observations made at King City last year, and a limited amount of laboratory work subsequently carried out by our lab people in Niagara Falls, it appears to me that inproper grinding can be detrimental to even the best product which we can produce up to that point in the system. I do agree that a properly treated material will not be degraded to the same extent that a poorly prepared material will be when subjected to the same grinding conditions. However, as previously reported, I recommend that we review our present dry grinding system, which consists of two Raymond Mills, and evaluate other commercial grinding equipment. GLD:cjb Gordon L. Dickson -59-