State CiBOLOGiCAi tan ILLINOIS STATE GEOLOGICAL SURVEY 3 3051 00000 1184 STATE OF ILLINOIS DWIGHT H. GREEN, Governor DEPARTMENT OF REGISTRATION AND EDUCATION FRANK G. THOMPSON, Director DIVISION OF THE STATE GEOLOGICAL SURVEY M. M. LEIGHTON, Chief URBANA BULLETIN NO. 71 USE OF ILLINOIS COAL FOR PRODUCTION OF METALLURGICAL COKE F. H. Reed, H. W. Jackman, O. W. Rees, G. R. Yohe, AND P. W. Henline Released for publication by the Office of Production, Research and Development of the War Production Board, under Contract WPB-75 with the University of Illinois. PRINTED BY AUTHORITY OF THE STATE OF ILLINOIS URBANA, ILLINOIS 1947 ORGANIZATION STATE OF ILLINOIS HON. DWIGHT H. GREEN, Governor DEPARTMENT OF REGISTRATION AND EDUCATION HON. FRANK G. THOMPSON, Director BOARD OF NATURAL RESOURCES AND CONSERVATION HON. FRANK G. THOMPSON, Chairman NORMAN L. BOWEN, Ph.D., D.Sc, LL.D., Geology ROGER ADAMS, Ph.D., D.Sc, Chemistry LOUIS R. HOWSON, C.E., Engineering CARL G. HARTMAN, Ph.D., Biology EZRA JACOB KRAUS, Ph.D., D.Sc., Forestry GEORGE D. STODDARD, Ph.D., Litt.D., LL.D., L.H.D. President of the University of Illinois GEOLOGICAL SURVEY DIVISION M. M. LEIGHTON, Chief (37563— 3M— 6-47) 5"S*7 SCIENTIFIC AND TECHNICAL STAFF OF THE STATE GEOLOGICAL SURVEY DIVISION 100 Natural Resources Building, Urbana M. M. LEIGHTON, Ph.D., Chief Enid Townley, M.S., Assistant to the Chief Helen E. McMorris, Secretary to the Chief Velda A. Millard, Junior Asst. to the Chief Effie Hetishee, B.S., Geological Assistant GEOLOGICAL RESOURCES Ralph E. Grim, Ph.D., Petrographer and Principal Geologist in Charge Coal G. H. Cady, Ph.D., Senior Geologist and Head R. J. Helfinstine, M.S., Mech. Engineer Charles C. Boley, M.S., Assoc. Mining Eng. Robert M. Kosanke, M.A., Asst. Geologist Robert W. Ellingwood, B.S., Asst. Geologist Jack A. Simon, B.A., Asst. Geologist Arnold Eddings, B.A., Asst. Geologist John A. Harrison, B.S., Asst. Geologist Raymond Siever, B.S., Research Assistant Mary E. Barnes, B.S., Research Assistant Margaret Parker. B.S., Research Assistant Oil and Gas A. H. Bell, Ph.D., Geologist and Head Frederick Squires, B.S., Petroleum Engineer David H. Swann, Ph.D., Assoc. Geologist Virginia Kline, Ph.D., Assoc. Geologist Paul G. Luckhardt, M.S., Asst. Geologist Wayne F. Meents, Asst. Geologist Richard J. Cassin, B.S., Research Assistant Sue R. Anderson, B.S., Research Assistant Industrial Minerals J. E. Lamar, B.S., Geologist and Head Robert M. Grogan, Ph.D., Assoc. Geologist Mary R. Hill, B.S., Research Assistant Clay Resources and Clay Mineral Technology Ralph E. Grim, Ph.D., Petrographer and Head Henry M. Putman, B.A.Sc, Asst. Geologist William A. White, B.S., Research Assistant Groundwater Geology and Geophysical Exploration Carl A. Bays, Ph.D., Geologist and Engineer, and Head Robert R. Storm, A.B., Assoc. Geologist Arnold C. Mason, B.S., Assoc. Geologist (on leave) Merlyn B. Buhle, M.S., Assoc. Geologist M. W. Pullen, Jr., M.S., Asst. Geologist Gordon W. Prescott, B.S., Asst. Geologist Margaret J. Castle, Asst. Geologic Draftsman Robert N. M. Urash, B.S., Research Assistant George H. Davis, B.S., Research Assistant Engineering Geology and Topographic Mapping Mineral Resources Records Vivian Gordon, Head Ruth R. Warden, B.S. Research Assistant George E. Ekblaw, Richard F. Fisher, Ph.D., Geologist and Head M.S., Asst. Geologist Areal Geology and Paleontology H. B. Willman, Ph.D., Geologist and Head Chalmer L. Cooper, Ph.D., Geologist C. Leland Horberg, Ph.D., Assoc. Geologist Heinz A. Lowenstam, Ph.D., Assoc Geologist Subsurface Geology L E. Workman, M.S., Geologist and Head Elwood Atherton, Ph.D., Asst. Geologist Paul Herbert, Jr., B.S., Asst. Geologist Marvin P. Meyer, M.S., Asst. Geologist Elizabeth Pretzer, M.A., Asst. Geologist Physics R. J. Piersol, Ph.D., Physicist GEOCHEMISTRY Frank H. Reed, Ph.D., Chief Chemist Carol J. Adams, B.S., Research Assistant Coal G. R. Yohe, Ph.D., Chemist and Head Eva O. Blodgett, B.S., Research Assistant Industrial Minerals J. S. Machin, Ph.D., Chemist and Head Tin Boo Yee, M.S., Research Assistant Fluorspar G. C. Finger, Ph.D., Chemist and Head Oren F. Williams, B.Engr., Asst. Chemist Chemical Engineering H. W. Jackman, M.S.E., Chemical Engineer and Head P. W. Henline, M.S., Assoc. Chemical Engineer James C. McCullough, Research Associate James H. Hanes, B.S., Research Assistant (on leave) Leroy S. Miller, B.S., Research Assistant (on leave) Earl C. Noble, Technical Assistant X-ray and Spectrography W. F. Bradley, Ph.D., Chemist and Head Analytical Chemistry O. W. Rees, Ph.D., Chemist and Head L. D. McVicker, B.S., Chemist Howard S. Clark, A.B., Assoc. Chemist Lewis E. Moncrief, B.S., Research Assistant Emile D. Pierron, B.S., Research Assistant John C. Gogley, B.S., Research Assistant Elizabeth Bartz, A.B., Research Assistant Albertine Krohn, B.S., Research Assistant Phyllis K. Brown, B.A., Research Assistant MINERAL ECONOMICS W. H. Voskuil, Ph.D., Mineral Economist Douglas F. Stevens, M.E., Research Associate Nina Hamrick, A.B., Research Assistant Ethel M. King, Research Assistant EDUCATIONAL EXTENSION Gilbert O. Raasch, Ph.D., Assoc. Geologist LIBRARY Regina Yoast, B.A., B.L.S., Librarian Ruby D. Frison, Technical Assistant PUBLICATIONS Dorothy E. Rose, B.S., Technical Editor Meredith M. Calkins, Geologic Draftsman Beulah F. Hopper, B.F.A., Asst. Geologic Draftsman Willis L. Busch, Principal Technical Assistant Leslie D. Vaughan. Asst. Photographer Consultants: Ceramics, Cullen W. Parmelee, M.S., D.Sc, and Ralph K. Hursh, B.S., University of Illinois Mechanical Engineering, Seichi Konzo, M.S., University of Illinois Topographic Mapping in Cooperation with the United States Geological Survey. This report is a contribution of the Geochemistry Secti Aug. 1, 1946 PERSONNEL Below is given a complete list of all who were employed on the work of Project WPB-75 for all or part of the period July 1, 1943-June 30, 1945. Supervisors Frank H. Reed, Chemist in Charge H. W. Jackman, Chemical Engineer O. W. Rees, Analytical Chemist G. R. Yohe, Organic Chemist P. W. Henline, Chemical Engineer Technical Personnel W. T. Abel, Research Assistant, Laboratory and Pilot Plant Operation Carol J. Adams, Secretary H. S. Clark, Associate Chemist, Laboratory J. E. DeVries, Research Assistant, Laboratory D. M. Fort, Assistant Chemist, Laboratory J. H. Hanes, Research Assistant, Pilot Plant Operation H. N. Hazelkorn, Research Assistant, Labora- tory H. S. Levine, Research Assistant, Laboratory and Pilot Plant Operation L. D. McVicker, Chemist, Laboratory L. S. Miller, Research Assistant, Pilot Plant Operation Elizabeth Mills, Secretary J. Mills, Research Assistant, Laboratory and Pilot Plant Operation M. A. Rebenstorf, Research Assistant, Labora- tory W. G. Tilbury, Assistant Chemist, Laboratory W. F. Wagner, Assistant Chemist, Laboratory Supervisor Non-Technical Personnel J. C. McCullough, Research Associate W. J. Retzolk, Laborer CONTENTS PAGE Introduction 9 Purpose of investigation 9 War Production Board contract with Illinois State Geological Survey 9 Acknowledgments 9 Summary 10 Summary and conclusions 10 Status of Illinois Coals 12 Historical review 12 Early tests on Illinois coals in metallurgical coke ovens 12 Use of Illinois coal in Roberts ovens 12 Other tests on Illinois coals 12 Impending depletion of best Eastern high- volatile coals 13 Illinois high- volatile coals 13 Procedures and Results 14 Approach to problem 14 Coal samples 14 Laboratory tests and analyses 15 Pilot plant coke oven 15 Design of oven 15 Temperature control 19 By-product recovery 23 Operation of oven 23 Coking results on duplicate samples 23 Comparison of experimental and commercial results 24 Cooperation with Koppers Company, Inc. 25 Pilot plant oven and laboratory cooperation 26 Early plant tests 27 Full oven battery tests by Koppers Company 27 Effects of Illinois coal 28 Oven operation 28 Coke properties 28 By-products 29 Coal storage 29 Blast furnace operation 29 Economics and transportation 29 Cooperation with Inland Steel Company 29 Early pilot plant oven tests 30 Cooperative research program 30 Scope of research 30 Testing procedure 30 Results 31 Coal expansion pressure tests 31 Pilot oven tests at Urbana 31 Full-scale oven tests 32 Three-week oven and blast furnace tests 32 Coal drying tests 33 Remarks 35 General coking tests 35 Illinois coal 35 Franklin County 35 Saline County 36 Madison County 36 Woodford County 36 Indiana No. IV seam coal representing deposits in Illinois 36 Non-Illinois coal 36 Low- volatile coals 36 High-volatile coals 37 Trends in pilot plant oven tests 37 Effect of coking time and temperature on coke properties 38 Preparation of coal 38 Pulverization — effect on coke properties 38 Moisture— effect on coke properties 39 Coal cleaning — effect on coke properties 40 Weathering of Illinois coals 41 Effects of blending Pocahontas coals of different characteristics with Illinois coal 43 Effect of increasing the percentage of low- volatile coal in Illinois coal blends 44 Effect of using petroleum coke as a substitute for Pocahontas coal 45 Comparison of No. 6 seam coals from different Illinois mines 45 Comparison of No. 5 seam coals from different Illinois mines 46 Blends containing both No. 5 and No. 6 seam coals 46 Addition of Eastern high-volatile coal to the blend 47 Effect of Illinois coal on ash fusion 48 Special tests 48 Plasticity study 48 Carbon and hydrogen determinations on cokes 55 Ash analyses 55 By-products 55 Scope of by-product tests 55 Gas 55 Light oil 55 Tar 59 Discussion of by-product tests 59 Effect of carbonizing conditions on tar characteristics 59 Effect of varying the proportions of high- and low- volatile coals 59 Substitution of Illinois high-volatile for Eastern high- volatile coals 62 References to publications 62 Appendix A — Complete tabular data on experimental coking runs made through June 30, 1945 63 Appendix B — Laboratory procedures for tar analysis 128 Drying 128 Distillation 128 Specific gravity and water content 128 Free carbon 1 29 Separation of tar distillate into acidic, basic, and neutral fractions 129 Determination of phenol and cresols in tar acids 130 Analysis of the neutral fraction 131 ILLUSTRATIONS FIGURE PAGE 1. Discharging and quenching coke from slot-type experimental oven 16 2. Sketch of slot-type experimental coke oven 17 3. Details of slot-type oven construction 18 4. Door and buckstays for slot-type oven 20 5. Slot-type coke oven — wiring diagram 21 6. Time-temperature recording chart 22 7. Flow diagram of coke oven and by-product recovery system 23 8. Gas evolution and B.t.u. value 24 9. Low sulfur coal area of southern Illinois showing mines sampled 63 TABLES TABLE PAGE 1 . Duplicate runs on pilot oven 25 2. Comparison between coking results in commercial ovens and pilot oven on same coal blend. ... 26 3. Effect of addition of Illinois coal to a Beckley-Elkhorn coal blend 32 4. Heat drying tests on Link-Belt drier 34 5. Effect of coking time and temperature on coke properties (I) 38 6. Effect of coking time and temperature on coke properties (II) 39 7. Effect of coal pulverization on coke properties 39 8. Effect of moisture on coke properties 40 9. Effect of removal of non-coal impurities 40 10. Effect of weathering Illinois coal (I) 41 11. Effect of weathering Illinois coal (II) 42 12. Effect of weathering Illinois coal (III) 42 13. Weathering of Illinois coal stocked in plant storage pile 43 14. Effect of blending different Pocahontas coals with Illinois coal 43 15. Effect of increasing the percentage of lower volatile coals in Illinois coal blends 44 16. Effect of using petroleum coke as a substitute for Pocahontas coal 45 17. Comparison of No. 6 seam coals 45 1 8. Comparison of No. 5 seam coals 46 19. Effect of adding No. 5 seam coal to a blend of No. 6 seam coal and Pocahontas coal 46 20. Addition of Eastern high- volatile coal to the blend 47 21. Comparison of ash-fusion temperatures of Eastern and Illinois coal blends 48 22. Ash fusion of cokes from blends of various Illinois coals 49 23. Gieselei- plasticity data for individual coals 50 24. Comparison of determined and calculated Gieseler data for coal blends 52 25. Correlation of coal blend fluidities and coke characteristics 54 26. Ash analyses 56 27. Effect of carbonizing conditions on tar characteristics 58 28. Effect on tar characteristics of varying the proportions of high- and low- volatile coals 60 29. Effect on tar characteristics of substitution of Illinois high- volatile for Eastern high- volatile coal. . 61 30. Names and sources of coals tested with abbreviations used 64 31. Analyses of coals and coal blends Part A. Coals — proximate analyses 65 Part B. Coals — ultimate analyses 69 Part C. Coal blends — proximate analyses 70 Part D. Identification of coals in blends by laboratory number 84 32. Coke oven operation and results Part A. Oven charge and operation 86 Part B. Coke yields 101 Part C. Screen sizes of coke produced 103 Part D. Coke — analyses 105 Part E. Coke — physical tests 109 Part E. By-products 113 33. Special coke analyses. Carbon and hydrogen determinations compared with volatile matter and coking temperatures 115 34. Properties and composition of tars Part A. Yield, moisture, gravity, free carbon, distillate to 350°, loss on manipulation 116 Part B. Neutrals, bases, acids 120 35. Phenol and cresol content of tars 124 36. Index to coals used in experimental coking runs 124 USE OF ILLINOIS COAL FOR PRODUCTION OF METALLURGICAL COKE BY F. H. Reed, H. W. Jackman, O. W. Rees, G. R. Yohe, and P. W. Henline INTRODUCTION Purpose of Investigation THIS PROJECT was planned, set up, and conducted for the purpose of saving transportation. Midwestern by-prod- uct coke ovens in the Chicago and St. Louis areas use annually from 12 to 15 million tons of bituminous coals which are trans- ported 500 to 700 miles from the Appa- lachian coal fields of Pennsylvania, West Virginia, and eastern Kentucky. Approx- imately two-thirds of this coal is high-vola- tile bituminous. The critical transportation problem con- fronting the nation in 1943, and the grow- ing scarcity of the best Appalachian coking coals, prompted the Illinois Geological Sur- vey to propose a research program in which would be studied the coking properties of blends of low-sulfur, high-volatile Illinois coal with the high- and low-volatile coals from the eastern fields. Such blends con- taining Illinois coal, if substituted for the all-eastern blends normally coked, would result in important transportation savings. War Production Board Contract with Illinois State Geological Survey To investigate this problem of producing metallurgical coke from Illinois coals, the Illinois State Geological Survey, through the University of Illinois, entered into a contract with the Office of Production, Re- search and Development of the War Pro- duction Board on July 1, 1943, for a six- month period. This contract was renewed January 1, 1944, July 1, 1944, and January 1, 1945. The contract terminated on June 30, 1945. Since this date, the project has been continued by the Illinois State Geo- logical Survey under the sponsorship of the State of Illinois. Acknowledgments This study was made possible through the cooperation of the Office of Production, Research and Development of the War Production Board, Washington, D. C. Valuable counsel w T as received from A. C. Fieldner, U. S. Bureau of Mines, in the initiation of this project. M. D. Curran, Coal Carbonizing Company, furnished fabricated steel for oven construction and for coke and by-product testing. Walsh Refractories Corporation furnished fire- brick, bonding mortar, and refractory insu- lating brick. Without the extensive cooper- ation of Koppers Company, Inc., and In- land Steel Company, it would have been impossible to compare the results of experi- mental work with those of commercial oper- ation. The Coal Division of the Illinois State Geological Survey has given valuable advice on the location of Illinois coals to be used in this study. The following companies have been generous and cooperative in fur- nishing samples of coal : Bell and Zoller Coal Alining Co., Walter Bledsoe and Co., Chicago, Wilmington and Franklin Coal Co., Consolidated Coal Co., Franklin County Coal Corp., Inland Steel Co., Kop- pers Co., Inc., Old Ben Coal Corp., Pea- body Coal Co., Pocahontas Fuel Co., Sahara Coal Co., W. G. Sutton Co., Troy Domestic Mining Co. To all of these organizations and indi- viduals we express our sincere appreciation. [9] SUMMARY Summary and Conclusions As a result of the tests made with Illinois coals which, on the basis of chemical com- position and immediate availability in quan- tity, are the most promising for metallurgi- cal coke production, the following con- clusions may be drawn. 1) Illinois No. 6 seam coal from the Franklin County low-sulfur area can be used continuously in blends with eastern coals in modern slot-type coke ovens for the production of coke which is practical for use in commercial blast furnaces. The ex- tent to which Illinois coal can be used to replace eastern high-volatile coal for this purpose is dependent primarily upon the economics of each individual application. Experimental pilot plant tests and commer- cial full-scale operation have shown that up to 75 percent of this coal may be used satis- factorily. 2) Such use of Illinois coal in metal- lurgical coke plants of the Chicago and St. Louis areas does result in sizeable transpor- tation savings. 3) Cokes of satisfactory physical and chemical properties can be made from blends containing up to 75 percent or more of Illinois No. 5 seam coal from the limited low-sulphur area in Saline County. 4) Cokes with equally good physical properties can be made using other No. 5 seam coals of medium sulfur content from Saline and Williamson counties. These coals and others similar to them are worthy of consideration as small percentage con- stituents of coal blends. 5) Illinois coal fines should not be used for coking. Fusain tends to concentrate in the fines, and the tendency to weather is increased by the large surface area. No lower limit on screen size, as prepared at the mine, has been determined, but in actual applications no size smaller than ^ inch has been recommended or used for coking. 6) Sized and cleaned Illinois coal can be safely stocked without hazard of spon- taneous combustion. 7) Consideration of all weathering test data obtained to date on Illinois No. 6 seam coals indicates that where prepared sizes of such coals are to be used as not over 25 percent of the total coal blend, storage of from three to six months is allowable. Like- wise, where as much as 80 percent of this Illinois coal is to be blended with a fluid medium-volatile coal (such as that tested in this work), six months storage may have no detrimental effects on the physical prop- erties of the coke. 8) Due to the extensive use of cleaning plants in the low-sulfur area, the coal shipped from this area is very uniform in preparation and composition, and coals from the mines of the various producing compa- nies are interchangeable. 9) The bulk density of Illinois coal when charged to coke ovens is almost identi- cal with that of eastern coals. However, due to the higher inherent moisture content of the Illinois coal, a correspondingly lower yield of coke is obtained. 10) In general, the low-sulfur Illinois coals tested in this program become less fluid during carbonization than do the higher ranking eastern high-volatile coking coals. Our tests have shown that the coke structure of an Illinois-Pocahontas coal blend may be improved by including a por- tion of a more fluid eastern high-volatile coal in the blend or by substituting certain medium-volatile coals for the low-volatile Pocahontas coal that is normally used in production of metallurgical coke. These conclusions have been reached through laboratory investigations, pilot plant carbonization of experimental coal blends, and cooperation with commercial producers of metallurgical coke. [10] SUMMARY 11 The Koppers Company, Inc., at its plant in Granite City, Illinois, has carbonized Illinois coal blends since April 1944, and as of the date of this report was coking a blend containing 65 percent of No. 6 seam Illinois coal mined within 80 miles of the plant. At the expiration of this contract, Koppers Company had carbonized 228,107 tons of Illinois coal which represented a transportation saving of 2,326,700 car miles, not including return of the empty cars to the mines. The Inland Steel Company of East Chi- cago, Indiana, has cooperated actively and had made commercial coke oven and blast furnace tests on coal blends containing No. 6 seam Illinois coal. Other producers of blast furnace and foundry cokes in the Chicago and St. Louis areas have shown keen interest in the progress of this pro- gram. It seems quite probable that this interest will result in a continued increase in the use of Illinois coal for metallurgical coke. STATUS OF ILLINOIS COALS HISTORICAL REVIEW Early Tests on Illinois Coals in Metallurgical Coke Ovens Although Illinois coal was not being used in the production of metallurgical coke at the initiation of this project, it was known that certain areas of this state produced coal of sufficiently low sulfur content and uniform chemical composition to be used for this purpose. The use of Illinois coal in by-product coke plants is not without precedent. Dur- ing the first world war, southern Illinois coal was used for production of blast fur- nace fuel in the Chicago area. The use of this coal was discontinued at the close of the war, due to the large reserves of the more strongly coking eastern coals then available. In the spring of 1918, the Bureau of Standards supervised the coking of 4800 tons of midwestern coal, mostly from Franklin County, Illinois, in Roberts type ovens at Canal Dover, Ohio. Although the breeze was high (8.1 percent of the coke), and the ovens did not produce sufficient coke to operate the 500-ton blast furnace except by admixture of 30-50 percent of other coke, the furnace superintendent was of the opinion that he could operate satis- factorily and at full capacity with this coke alone. 1 (See References to Publications, p. 62.) A detailed description of tests involving the use of 7600 tons of Orient coal (Illi- nois No. 6 seam, Franklin County) in Kop- pers ovens at the coke plant of the Minne- sota By-Product Coke Company at St. Paul, Minnesota, has been published by the Bureau of Standards in cooperation with the Bureau of Mines. 2 Chemists of this company and of the Koppers Company com- mented favorably upon the coke from Illi- nois coal as a blast furnace fuel. It was reported to carry a normal basic burden well, to burn faster than the regular coke, and to increase the iron tonnage from the furnace, which operated with the regular coke at about 175-185 tons per day, to an average of 198 tons per day for the test period. Work was also done on the coking of blends of Illinois coal with eastern coals, and as a result of these tests and others by the Bureau of Mines, Fieldner and co- workers stated in regard to the Orient coal that "on blending with 25 percent of low- volatile coal, however, it makes an excellent metallurgical or domestic coke." 3 Use of Illinois Coal in Roberts Ovens Following these early tests, the Roberts coke oven plant at Granite City, Illinois, 4 produced coke of metallurgical quality from 1921 until 1935, using from 85 to 100 per- cent of southern Illinois coal. Illinois coals from Franklin and the surrounding coun- ties were carbonized. The coke produced was used in blast furnaces at this plant. It was reported to be faster burning than eastern coke, to have good burden-bearing qualities, and to produce basic iron consist- ently with low coke consumption. Best results were obtained when blending from 10 to 15 percent Pocahontas with the Illi- nois coal. Other Tests on Illinois Coals In 1942, Illinois coal was tested in the Carnegie-Illinois Steel Corporation plant at Gary, Indiana. The results of these tests have not been published. No attempt is made here to review all work done on coking of Illinois coals. Laboratory and small-scale carbonization of these coals by various processes has been done by Parr at the University of Illinois, [12] STATUS OF ILLINOIS COALS 13 Fieldner and others at the U. S. Bureau of Alines, Thiessen at the Illinois State Geological Survey, and others. Results of these tests have been cited by Thiessen. ' IMPENDING DEPLETION OF BEST EASTERN HIGH-VOLATILE COALS In all of these tests with Illinois coal, it appears that satisfactory metallurgical coke has been made. The availability of quantities of high quality eastern coking coals has resulted, however, in a return to the use of eastern coal. Eastern coking coals in general are of higher rank than Illinois coals, and as such have a lower moisture content, and in many cases stronger coking properties. The continued use of eastern coals, and especially their increased use in World War II, has seriously reduced the reserves of the better coking coals. Many of the re- maining coals are higher in ash and sulfur. During the first ten months of 1942 in the Chicago district, the average analysis of by-product coke showed an increase in ash of 0.72 percent. The increase in the St. Louis-Western district was 0.68 percent. Both ash and sulfur continued to increase during the war years, and this tendency has been accelerated by the increased use of mechanical mining equipment. With this growing scarcity of the better eastern coking coals, it is becoming more important to locate other sources of high- volatile coal to use in production of metal- lurgical coke in the midwestern area. The low-sulfur coals of Illinois offer one possi- ble solution. ILLINOIS HIGH-VOLATILE COALS Illinois has larger reserves of high-vola- tile bituminous coal than any state east of the Rocky Mountains; only Colorado ex- ceeds Illinois in reserves. Although Illinois coals can all be classed as coking, unfortun- ately, with the exception of certain areas, most of these coals are too high in sulfur to be used for metallurgical coke produc- tion at this time. The principal low-sulfur coal area of Illinois centers in Franklin County and ex- tends to portions of the surrounding coun- ties. In this area, washed and sized No. 6 seam coal is obtained containing from 0.7 to 1.2 percent sulfur. Fifteen of the princi- pal mines in this area have the capacity to produce more than 50,000 tons of coal per day. In Saline County, southeast of Franklin County, there is a limited area of No. 5 seam coal containing 0.7 to 1.0 percent of sulfur in the washed sizes, and large de- posits of coal containing 1.7 to 2.2 percent sulfur. This is the highest rank coal mined commercially in Illinois. Other smaller areas of relatively low- sulfur coal are located in Vermilion, Wood- ford, and Madison counties. The Franklin County low-sulfur coal area lies about 300 miles south and a little west of Chicago, and 80 to 100 miles south- east of St. Louis. Both Franklin and Saline counties are well provided with railroads, having several routes to each of these indus- trial districts. The proximity of this Illi- nois coal to the midwest coking plants favors its use because of the short rail haul and low freight rates. PROCEDURES AND RESULTS APPROACH TO PROBLEM The problem of investigating the coking properties of Illinois coal has both technical and economic aspects. It is necessary first to determine whether or not suitable coke can be produced, and next to develop the economics of the process. The comparison of costs of coking Appalachian coals alone or in combination with Illinois coals in any given plant can be determined only by com- mercial operation over an extended period. The suitability of the coke for blast furnace operation, the yield of coke from the coal, and the amount and value of the by-prod- ucts are important factors which must be considered. Freight rates and cost and uni- formity of coal must be considered also in determining the overall economic picture. However, experimentation with various blends of coal in commercial coke ovens is costly, and it interferes with regular pro- duction. Consequently, only a minimum of such experimentation is conducted. The first step in the present program was, therefore, the design and construction of a small scale slot-type coke oven in which coal blends could be carbonized under con- ditions approximating those obtained in commercial ovens. The coke produced under these conditions should have physical and chemical properties directly compa- rable to those of coke produced commercially from the same coal blend. An experimental oven of 500 pounds coal capacity was built. Its operation was stand- ardized by coking coal blends that were being used at the time in commercial ovens, and comparing experimental results with those from average commercial operation. Blends containing Illinois coals were then carbonized in the experimental oven and their coking properties were determined. This experimental oven was connected with the by-product recovery train formerly used in our experimental work with the sole-flue oven." Tar and gas were collected and evaluated. Early pilot oven tests indicated that the Illinois coals tested had different plastic properties than the eastern high-volatile coking coals normally used in coke produc- tion. This necessitated special studies on the technique of blending Illinois coals with coals from other areas, and laboratory tests involving plastic studies of both Illinois and eastern coals were made. Data ob- tained have been applied successfully to coal blending procedure in our pilot oven studies. Early in the experimental program, it became possible to cooperate with commer- cial producers of metallurgical coke who had an interest in using Illinois coal in their plants. Through these valuable connec- tions, certain blends of Illinois coal, after preliminary pilot plant tests, have been car- bonized in commercial ovens over extended periods of time, where their behavior in plant equipment, their yields of coke and by-products, and the economics of their extended commercial use were studied. These cooperative studies have played a valuable part in carrying out this project. COAL SAMPLES Samples of Illinois coals for pilot plant and laboratory tests were collected at the mines in the desired screen sizes under the supervision of a member of our staff. Special care was taken to collect these samples in increments over a sufficiently long period of time to cover the entire working area of the mine. The coal samples were brought in our truck directly to the laboratory and used within a few days in order to avoid possible oxidation in storage. Eastern coals for blending with Illinois coals were obtained largely from the plants of the Koppers Company at Granite City, Illinois, and the Inland Steel Company of [14] PROCEDURES AND RESULTS 15 East Chicago, Indiana. The coals were sampled from cars in such a way as to be representative, and were also brought to the laboratory by our truck. LABORATORY TESTS AND ANALYSES Coals collected in the above manner were prepared for analyses in the laboratory by approved methods. Analytical determina- tions were made on individual coals and on coal blends by standard A.S.T.M. methods for proximate analysis, sulfur, B.t.u. 7 and Free Swelling Index (F.S.I.). S An ultimate analysis 7 was also made on one sample of coal from most of the mines tested. The cokes produced in the pilot oven were analyzed by standard A.S.T.M. meth- ods for proximate analysis, sulfur, B.t.u. and ash fusion. 7 Physical tests were made, also by standard A.S.T.M. methods, for shatter test, 9 tumbler test, 10 apparent and true gravities, and porosity. 11 All these results are tabulated completely in tables 31 and 32. Plasticity studies on coals, carbon and hydrogen determinations on cokes, and analyses of coal and coke ashes are presented in the section entitled "Special Tests." Details of laboratory work on tar are presented under the section entitled "By- Products," and in tables 34 and 35 of Ap- pendix A. Special methods of tar analyses are described in Appendix B. PILOT PLANT COKE OVEN The primary objective in design of the experimental slot-type coke oven 12 was to construct a unit which would duplicate essentially a small section of a commercial oven, and in which the process of coking would be controlled rigidly. Only in the width of the oven was an attempt made to duplicate any dimension of a commercial oven. The average width for most com- mercial ovens ranges from 13 to 21 inches. The actual width of the experimental oven is 14 inches. The oven was designed so that it could be operated to give the same heat penetration (average width of oven in inches divided by coking time in hours) and final coke temperature as obtained in com- mercial practice. Figure 1 shows this oven being discharged and the coke being quenched. The uniform oven wall temperature up to the top of the charge and the slightly cooler space above for gas collection are apparent. Design of Oven Figure 2 is a diagrammatic sketch of the oven showing detailed cross-sectional views from front and side. As in all slot-type ovens, heat is applied from vertical flues on both sides of the oven chamber (fig. 2, 1 ) . The inside of the chamber is designed to have approximately \4 inch taper in width. Due to small irregularities in the shapes received, the oven as constructed averages 14 inches in width and has very nearly parallel walls. The coal space in the oven chamber is 36 inches in length, 35 inches in depth, and holds approximately 10 cubic feet of coal per charge. The side walls (4) and floor (5) of the oven are made of silicon carbide tile, 2 inches thick. Each side wall consists of a single tile, and the floor is formed from two tiles laid end to end with an overlap- ping joint. The walls are anchored at the back of the oven and left free to expand vertically and horizontally. They are held in place at the top and bottom by the sur- rounding brickwork, and are further sup- ported on each side by two rows of long firebrick (6) which touch the oven walls and are, in turn, strengthened by steel angles (7) running the full length of the outside w r alls of the oven. These support- ing firebrick are spaced from front to back of the flues, leaving 4.5 inches between bricks, so that approximately 50 percent of the flue space is left open (fig. 3, section C-C). These flue openings are staggered in the two rows of supporting brick in each flue. This leaves the three sections of each flue closely interconnected and allows the heat to equalize from top to bottom of each oven wall. The oven chamber is surrounded on the sides and top by vermiculite insula- 16 ILLINOIS COAL FOR METALLURGICAL COKE Fig. 1. — Discharging and quenching coke from slot-type experimental oven. tion (8). This insulation acts not only as a heat baffle but, being soft, as a cushion against thermal expansion or swelling pres- sures which otherwise might crack the sili- con carbide walls. The top of the oven chamber (9) is cast of refractory concrete. Coal is charged through a 6-inch pipe (10) extending through the casting, and a 6-inch blank flange (11) serves as a charge hole cover. PROCEDURES AND RESULTS 17 CC D I- < U) a. oc uj O a \- I Z o 18 ILLINOIS COAL FOR METALLURGICAL COKE SECTION A-A / ANGLE I i ^ -A ANGLE I 1 I k SECTION B-B J*- 1 3 kt^*| |^I3 3 /4^| SECTION C-C BACK VIEW / ANGLE / / ^ SfcS M : 1 m : 1 it : 1 1 3 £ lr- ; ^ 1 1 * i r§ 1 £ ^ i S I 1 ^ i • ( £ ^ i i % ANGLE 1 1 II 1 1 1 1 1 1 1 III 1 1 II 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 n.|.--;-kln 1 1 GLOBAR 1 1 1 1 r ; OPENINGS^ ;l II: : 1 1 : 1 /f=t> i 1 ^~~S-^ v^ b 1 ' i 1 <9> | | 1 ^^©' P 1 1 : ll II! '(Q) | | THERMO- 1 1 1 : l°l : COUPLE 1 l | | ~^~-L '/R\ 1 "t— S^ ill: J® 1 1 ll 1 1: 1 1 (FsJ Ifpfo 1 1 <8> y i i ' ' ' ' VWX&bCXA 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 II II 1 1 1 1 II ^1 M M M \X\ 1X1 ) FIRE BRICK SPECIAL INSULATING SHAPES R^SSSS HIGH-TEMPERATURE INSULATORS V////A VERMICULITE HEATING FLUE OPENINGS SILICON CARBIDE Fig. 3. — Details~of slot-type oven construction. PROCEDURES AND RESULTS 19 Gas escapes from the oven through a 3-inch pipe (12) extending through the top and connected to the by-product recovery equip- ment. The back of the oven chamber con- sists of permanent brickwork, whereas the front is covered by a refractory concrete door (13) which is raised or lowered by a chain hoist and is mudded into place be- fore the oven is charged. After charging, the coal is leveled through a rectangular opening (14) in the door located 35 inches above the chamber floor. This level bar opening is then bricked and mudded. Be- tween the door and the coal charge a tem- porary brick wall (15) (9 inches in depth) extends from the floor to the coal level. This wall, which consists of one layer of firebrick next to the charge and one layer of insulating brick next to the door, is re- moved before a coke charge is pulled, and is replaced immediately after the oven is discharged. The oven structure is held together by tie rods (16) extending through the top brickwork and foundation. These rods are anchored to heavy buckstays (17) at each corner of the oven. Figure 3 gives more details of the oven brickwork construction. Horizontal sec- tions A-A, B-B, and C-C, which refer to figure 2, show the brick arrangement just below floor level, at the oven floor, and at a plane between the lower and middle flue sections. The back view shows the arrange- ment of the openings for heating units and thermocouples into the heating flues and the oven chamber. Thermocouples are never placed in all of the holes shown dur- ing any one run, but the holes are built into the oven to be available when and if desired. Temperature Control Accurate control of the temperature and heating rate of the coal is maintained by regulation of the Globar heating units which are powered from a three-phase 230- volt 60-cycle source through a 50 kv.-amp. rap transformer as shown in the wiring dia- gram of figure 5. Six AT type Globar brand nonmetalic heating elements (2, lig. 2), 67 inches long and having a middle heating section 36 inches in length and 1.25 inches in diameter, designed to carry a capacity load of 100 amperes at 136 volts, are placed horizontally in each flue and spaced as shown so that heat may be applied uniformly from top to bottom of the oven walls. The two Globars in each top flue section are connected in series, and the two units thus formed are connected in parallel across one secondary of the transformer. Globars in the center and bottom flue sec- tions are connected in a similar manner across the other two secondaries. In this way there are formed three independently variable single-phase circuits. Tempera- tures in the two vertical flues are controlled separately by two Wheelco Capacitrols connected to thermocouples in the center flue sections adjacent to the oven walls. These units actuate the secondary circuits from the transformer (see fig. 5). The even heating of the walls that is hereby ob- tained, together with the high heat con- ductivity of the silicon carbide tile, results in a very uniform application of heat to the oven charge ; these factors are believed to be responsible for the uniformity of the coke produced. Temperatures inside the oven are record- ed by a four-point recorder actuated by thermocouples inserted through the back of the oven chamber (fig. 2, 18). Three thermocouples are located just inside the silicon carbide wall near the top, center, and bottom of the coal charge, and extending horizontally to the center of the oven. A fourth is placed in the exact center of the coal charge, and a fifth, located in the gas space above the coal, is made to record by manipulation of a double-throw switch. A 20 ILLINOIS COAL FOR METALLURGICAL COKE j . o „H ^ : 1 o c = — — - — o x •" T ^ ..9 = _J * Z r> < n QC 1 7 o x 1 J I to f< (/■) O D CD UJ > O LLl o u o o Q z UJ > o UJ *: o (J PROCEDURES AND RESULTS 21 22 ILLINOIS COAL FOR METALLURGICAL COKE -ft* '# 4*: 100 200 100 2O0 300 400 500 600 700 .600 900 £t 1000 1100 f ;.> / fv .,-,4* , ,... j , ; $ , „*„ „ i j , m im~- wto _£ 1! IS i '// ,' . . . j.) 300 400 900 600 TOO 800! .' 900 1000 1100 1*00 Oil 1200 700 .1 800 «** 1000 1100 1200 : A . . . . /i __I_^ i «bCi 100 200 000 400 500 «j&0^2^700 / afOO 000 1000 1100 — — { • — 7^*ym i — ; - — — 1200 Fig. 6. — Time-temperature recording chart. typical time-temperature chart is shown in figure 6. Curve ( 1 ) was recorded by the thermocouple just below the gas riser in the gas space; curves (2), (3), and (4) represent respectively the temperatures at the top, middle, and bottom of the charge next to the side wall, and curve (5) indi- cates the temperature at the exact center of the coal charge. It is seen that the coke next to the oven wall increases in tempera- ture uniformly throughout the coking period, and that the center of the charge remains constant at about 100° C. for the first six hours, then increases rapidly and finally reaches the temperature of the coke at the side wall. PROCEDURES AND RESULTS 23 Gas Line + Liquid Line A — Coke oven B — Circulating liquor spray C — Washer-cooler D — Circulating liquor tank and tar separator E — Tar scrubber F — Tar separator G — Waste liquor tank H — Gas exhauster I — Hydrogen sulfide scrubber J — Iron-oxide catch box K — Light oil scrubber (not in use) L — Gas meter M — Gas calorimeter N — Gas sample holder O — Gas line to atmos- phere P^-Ps— Circulating pumps Q — Tank for soda-ash solution R — Tank for straw-oil Fig. 7. — Flow diagram of coke oven and by-product recovery system. By-Product Recovery Equipment has been provided for the re- covery of tar from the gas that is evolved during experimental coking runs. The gas is purified of hydrogen sulfide and metered. A representative gas sample is collected and the heating value determined. A flow dia- gram of the by-product recovery system is shown in figure 7. Operation of Oven In operating this experimental coke oven, the flue temperatures are controlled to give the same average heat penetration through the coal charge and the same final coke tem- perature as attained by commercial oven bat- teries. As the silicon carbide walls of the experimental oven have a higher thermal conductivity than the silica brick walls of large-scale ovens, it is possible to obtain approximately the same average heat pene- tration rate at much lower flue temperatures in the experimental oven than are required in commercial ovens. Results that dupli- cate closely those of commercial practice have been obtained by charging the oven at an initial flue temperature of 1600° F. and raising this temperature 30° per hour to a maximum of 1850° F. The coking time under these conditions is found to be 12.75 to 14 hours, or the average penetration is 1.10 to 1.0 inches per hour, depending upon such factors as bulk density, moisture con- tent, and plastic characteristics of the coal. The final average coke temperature is 1770- 1800° F. Coking is usually continued until the temperature of the coke at the center of the oven has remained constant for li/£ to 2 hours, depending on the volatile matter de- sired in the coke. The original method, used with many of the experimental runs, was to discontinue coking when gas evolution dropped to a rate of fifty cubic feet per hour, but this method was found to give less consistent results. At the end of the run the oven is opened and the coke is pulled by hand and quenched with water. Yields of tar, gas, and coke are computed on the basis of the coal as charged to the oven. Coking Results on Duplicate Samples To check the operation of the oven and to determine how closely coking results can be reproduced, duplicate runs on two coal 24 ILLINOIS COAL FOR METALLURGICAL COKE 5 6 7 6 9 10 II HOURS AFTER CHARGING 300 Fig. 8. — Gas evolution and B.t.u. value. blends are shown in table 1. Note that coke yields check to within one-half percent. Of the physical tests, the closest checks are obtained on "Tumbler Stability," which is a test used extensively in the industry to evaluate coke quality. Satisfactory checks are also obtained on shatter test, coke siz- ing, and apparent gravity. In figure 8 the data on gas evolution per hour and B.t.u. value are plotted from ex- perimental data taken during these dupli- cate runs. B.t.u. values are not shown for the gas beyond the tenth hour. Gas evolved during the balance of the coking period is very high in hydrogen, and the calorimeter is not, adjusted to read accurately in this low range. These curves are typical of the results obtained under normal operating conditions. Because of the close control of operation possible with the experimental oven, which can not be realized in a gas-heated com- mercial size oven, the results on the experi- mental oven have been shown to be more dependable and more easily duplicated than those obtained from individual ovens of a commercial battery. Comparison of Experimental and Commercial Results A number of checks have been made be- tween experimental oven runs and commer- cial plant operation on the same coal blends. Four series of comparisons are shown in our previously published paper. 12 It has been found that pilot oven results, which are obtained under uniform operating condi- tions on coals blended accurately by hand, do not necessarily check the results of indi- vidual commercial ovens, but do check aver- age plant results over an extended period of time. Table 2 shows such a comparison between the average results of a 57-day test on a commercial oven battery and one experimental run made with the same coal blend in the pilot oven. The total coke yields are shown to be identical. However, as the commercial oven coke has rougher handling than the experimental coke, it undergoes more breakage, and the amount of furnace size coke is somewhat less and the fines are somewhat greater than are ob- tained from the pilot oven. Here again the "Tumbler Stability" checks very closely, PROCEDURES AND RESULTS 25 Table 1. — Duplicate Runs on Pilot Oven Blend A No. 113 No. 116 Blend B No. 1 18 No. II'' Coke analysis, % Volatile matter Fixed carbon Ash Sulfur Coke yields, % of dry coal Total Furnace ( + 1 in.) Nut (1 x y 2 in.) Breeze ( — 34 in.) Coke screen test, % of coke Total +4 in Total +3 in Total +2 in Total +1 in Av. size, in Tumbler test Stability (+1 in.) Hardness (+M in.) Shatter test % of +2 in %o(+\y 2 m Apparent gravity Gas Cu. ft./ lb. drv coal B.t.u. ' B.t.u. in gas/lb. coal 1.2 90.9 7.9 0.83 71.7 68.7 0.9 2.1 4.1 31.6 79.3 95.8 2.61 55.9 69.2 64.0 88.8 1.1 91.3 7.6 0.73 72.2 68.7 1.0 2.5 1.8 29.2 78.2 95.2 2.54 55.4 68.9 68. 87. 0.824 0.825 6.50 6.42 486 496 3159 3184 1.7 92.1 6.2 0.68 73.3 69.9 1.0 2.4 2.8 29.7 77.1 95.4 2.55 55.0 67.9 65.3 88.9 0.842 1.6 92.1 6.3 0.76 72.8 69.4 1.2 2.2 2.8 25.2 75.4 95.3 2.48 55.3 69.6 64.8 87.0 0.838 6.14 6.15 545 541 3346 3327 and satisfactory checks are obtained on other physical tests. It is noted on all experi- mental runs that the apparent gravity of the coke made in the pilot oven is about 0.045 less than that made in commercial ovens. This figure can be used as a correction con- stant. COOPERATION WITH KOPPERS COMPANY, INC. At the time the pilot oven was being built in our laboratory, it was learned that Koppers Company, Inc., was considering the use of Illinois high-volatile coal for the production of blast furnace coke at its plant in Granite City. Illinois. The Granite City plant consists of one battery of 49 Koppers Underjet type coke ovens of 17-inch aver- age width and 17 tons coal capacity, by- product recovery equipment for tar, light oils, ammonium sulfate and gas, and two blast furnaces, one of 17 feet 9 inches hearth diameter and 86 feet overall height, and the other of 19 feet 6 inches hearth diameter and 92 feet overall height. The coke oven battery at the Koppers Company plant, which was built by the Defense Plant Corporation, had been oper- ating since it was started in March, 1943, on an all-eastern coal blend of 70 percent high-volatile Hernshaw seam coal and 30 percent low-volatile Pocahontas No. 3 seam coal. A very satisfactory coke was made and used as blast furnace fuel. How- ever, as there is a freight differential of $2.12 per ton between West Virginia and Illinois coals delivered to the Koppers plant, a research program involving the use of 26 ILLINOIS COAL FOR METALLURGICAL COKE Table 2. — Comparison between Coking Results in Commercial Ovens and Pilot Oven on Same Coal Blend Coke analysis % Volatile matter Fixed carbon Ash Sulfur Coke yields, % of coal Total Furnace ( + 1 in.) Nut(l xV 2 m.) Breeze { — Yz in.) Coke screen test, % of Coke Total +4 in Total +3 in Total +2 in Tumbler test Stability (+1 in.) Hardness (+/4 in.) Shatter test % of +2 in %of+l^in Apparent gravity Commercial Ovens 57 days average Pilot Oven Run No. 102 1.5 87.4 11.1 0.77 1.0 87.8 11.2 0.69 65.0 58.1 3.4 3.5 65.0 62.2 0.7 2.1 8.4 35.8 78.3 6.4 48.4 87.2 49.3 67.9 49.0 66.8 66.0 94.9 63.6 96.4 0.848 0.802 Illinois coal was justified. Realizing that this was an opportunity for mutual assist- ance, the Illinois State Geological Survey and the Koppers Company have cooperated in this program. Pilot Plant Oven and Laboratory Cooperation Our cooperation with Koppers Company was started immediately after completing construction of the pilot oven. The opera- tion of this oven was standardized by first coking the all-eastern coal blend being used at the Koppers Company plant, and com- paring experimental with commercial re- sults. Proper control of flue temperatures was obtained on the second experimental run, and coking results checked plant opera- tion closely. The operating procedure de- veloped in these tests has been continued with only minor changes. Following the test runs on all-eastern coal, coking tests were made on blends of Illinois No. 6 seam coal and Pocahontas coal. In the first Illinois coal studies, the percentages of high- and low-volatile coals were varied, and Illinois coals from differ- ent mines were tested. Petroleum coke was tried as a substitute for low-volatile coal. The coking temperature was also varied and the effect on the coke structure was noted. The first plant test in the Koppers ovens on an Illinois coal blend was made after twenty-one experimental runs had been made in the pilot oven. It was noted that physical properties of the coke made in the full-scale ovens again duplicated the prop- erties of experimental coke made from the same coal blend, thereby indicating that the pilot oven coking results could be used as a dependable guide in predicting commercial oven practice. During the entire period of our coopera- tion with Koppers Company, the pilot oven has been used in exploring the coking prop- erties of coals from the different Illinois mines, in determining the effect of variations in the proportions of high- and low-volatile coals, in establishing proper carbonizing PROCEDURES 4ND RESULTS 27 temperatures and rates of coking when using Illinois coal blends, and in determin- ing the effect of coal density, coal pulver- ization, surface moisture, and inert material on the physical properties of coke. The' plastic properties of coals have been studied in our laboratories, and the findings applied to the proper blending of coals to produce the physical properties desired in blast furnace coke at the Koppers plant. This has involved a study of eastern coals as well as those from Illinois. These studies have been evaluated, and experi- mental data have been made available to the Koppers Company. Early Plant Tests In the first plant test made by Koppers Company on Illinois coal, referred to in the preceding section, five full-scale ovens were charged with a blend of approxi- mately 60 percent Illinois No. 6 seam coal and 40 percent Pocahontas. The regular coking time of 16.3 hours was maintained at normal oven flue temperatures. The coke produced was tough and blocky and gave satisfactory shatter and tumbler tests. At this time it was found that petroleum coke fines could be purchased in Wood River, Illinois, about ten miles from Granite City. It was thought that this fuel might be substituted for Pocahontas coal in the lllinois-Pocahontas blend and result in a further savings in cost and transportation. Experimental runs were made in the pilot oven on Illinois coal-petroleum coke blends. These were followed by full-scale oven tests at Granite City. The coke produced was found to have low resistance to break- age and to result in more than the normal amount of fines. These results, together with the nonuniform composition of the petroleum coke, convinced Koppers Com- pany that such a blend would not be satis- factory. Experimental pilot oven tests had shown that Illinois No. 5 seam coal from Saline County, which is the highest rank coal mined commercially in Illinois, has excep- tionally good coking properties. This coal when blended with No. 3 Pocahontas pro- duced low breeze, and the furnace coke was Strong and somewhat smaller in size than that made from No. 6 seam coal. Excellent shatter and tumbler tests were obtained. Koppers Company tested a blend of 65 per- cent No. 5 seam Illinois coal and 35 percent Pocahontas in the oven battery. The coke produced had excellent physical properties and a pleasing appearance. However, pre- vious commitments on this coal prevented further plant tests of longer duration in which the coke could have been evaluated as blast furnace fuel. Full Oven Battery Tests by Koppers Company The experience gained in the early plant tests at Granite City, and in the pilot oven tests in our laboratories, enabled Koppers Company to place the entire Granite City coke oven battery on a blend of 60 percent Illinois No. 6 seam coal and 40 percent Pocahontas coal on April 25, 1944. Just before the change to Illinois coal, the larger blast furnace was shut down and it was necessary to lengthen the coking time to approximately 24 hours. As Illinois coal has been shown to coke better at faster coking rates, considerable experimental ma- nipulation of oven heats was required to determine best operating procedure to pro- duce a maximum yield of furnace coke hav- ing the physical properties required for blast furnace fuel. It was found that with this long coking period, a rapid coking rate fol- lowed by a soaking period in which the coke temperature reaches 1900° F. or higher produces a good structure coke. Illinois coals of \\/i inches x Y\ mc h an d 2 inches x }i inch sizes have been used ex- clusively by Koppers Company. Finer coal sizes than Y% inch have been avoided be- cause fusain tends to concentrate in the finer sizes, and as the tendency for weathering is greatly increased by the large surface area of the fine size coal. Koppers Company continued to test llli- nois-Pocahontas coal blends, increasing the amount of Illinois coal from time to time 28 ILLINOIS COAL FOR METALLURGICAL COKE from 60 to 65, to 70, and to 75 percent, with corresponding decreases in Pocahontas coal. These blends produced large, blocky coke tending to have irregular surfaces and pebbly seams. The coke was tough, having exceptionally high shatter and tumbler sta- bility. More coke fines were produced than when all-eastern coal was used. Blast fur- nace results indicated that the coke sup- ported the burden well. There was, how- ever, a decrease in furnace tonnage, accom- panied by other indications pointing to a too-open stock column, a condition which might have been improved by a reduction in the size of the coke to the furnace. Un- avoidable changes in ores used were made throughout the tests which reduced the accuracy of any direct comparisons in ton- nages and coke rates. In October 1944, Koppers Company be- gan charging a coal blend containing 75 percent Illinois No. 6 seam coal, 15 per- cent eastern high-volatile coal, and 10 per- cent Pocahontas. The blend was later changed to 65 percent Illinois, 25 percent eastern high-volatile, and 10 percent Poca- hontas. This blend, and others similar to it, have continued to be used. Addition of eastern high-volatile coal resulted in reduc- tion of the coke size, elimination of pebbly seams, and reduction in the amount of coke fines. The oven battery has operated smoothly on these blends. Blast furnace operation has improved, and iron tonnage increased. Effects of Illinois Coal The problems involved in the use of Illi- nois coal at the Koppers Company Granite City plant have not all been solved. The effects of using Illinois coal in the produc- tion of metallurgical coke during this test- ing program may be summed up, however, as follows. OVEN OPERATION The coke oven battery at the Koppers plant has operated smoothly on Illinois coal blends during the entire testing period. Less trouble due to heavy tar and carbon deposits has been experienced than when all-eastern coal was used. This may be due in part to the longer coking time. It has not been necessary to leave ovens empty for decarbonization. The coke has pushed easily with no increase in power for push- ing. Coke shrinks from the oven walls and there have been no stickers. Approximately the same tonnage of coal is charged per oven as when all-eastern coal was used. The heat for underfiring has increased about 30 percent due, in part, to the longer coking time and higher final coke temperature, and probably in part to the nature and higher moisture content of the Illinois coal. No comparison has been made between under- firing Illinois coal and eastern coal under the same operating conditions. COKE PROPERTIES When Illinois No. 6 seam coal from the mines furnishing coal to the Koppers plant was blended with Pocahontas coal of 17 percent volatile matter, a large, blocky coke of high stability was produced. The coke had irregular surfaces, contained pebbly seams, and produced a greater than normal yield of fines. Reducing the Pocahontas coal from 40 percent to 25 percent had little effect on these properties. Addition of 15 to 25 percent of eastern high-volatile coal with more fluid plastic properties improved the coke structure, eliminated the pebbly seams, and decreased the coke fines. Coke of uniform chemical composition, containing about 0.75 percent sulfur, has been produced consistently from the washed Illinois coals used at this plant. The yield of furnace coke has been de- creased about 1 percent for each 10 percent of Illinois No. 6 seam washed coal which replaced the eastern Hernshaw seam coal in the blend. When the percentage of Poca- hontas coal was also decreased, as in the later tests at the Granite City plant, the coke yield was naturally reduced further in accordance with the fixed carbon content of the coal blend. PRO C E DUR ES . / \ I) R ES I ' L TS 29 BY-PRODUCTS The total by-product yields from the carbonization of Illinois coal are somewhat less than from the best high-volatile eastern coals for the same ratio of high- and low- volatile coal in the blends. The tests at the Koppers Company plant show the following trends, part of which may be due to the different conditions under which the Illinois coal has been coked. a) Gas — Total yield in therms is not appreciably different from Koppers' former experience with the all-eastern coal blend. The B.t.u. value of the gas is reduced, how- ever, from 5 to 10 percent, depending on the coal blend being used. b) Tar — Yield is reduced about 1 gal- lon per ton. Tar gravity is also lower. c) Ammonium Sulfate — Yield is in- creased 20 to 30 percent. d) Light Oils — Little change in yield. Present yields are greater than before Illi- nois coal tests were started due, in part at least, to improved plant operation. COAL STORAGE To avoid any tendency toward weather- ing, the Koppers Company has not stocked Illinois coal. The proximity of this plant to the mines, a distance of only 80 miles, has assured a dependable daily supply of coal. Our pilot plant data indicate that the Illinois coal being used at this plant could be stocked without detrimental effect on the coking properties for a thirty day period, and perhaps much longer, but no controlled plant tests on weathered coal have been made. BLAST FURNACE OPERATION A complete correlation of blast furnace practice with the various coal blends cannot be made for reasons previously stated. In general, it appears that the production of iron per day is lower and the pounds of coke per ton of iron are higher than would be expected from a direct comparison of the eastern and the Illinois cokes. This con- dition is due in part to the more open stock and higher top temperature resulting from the larger size of the Illinois coke. The latter condition might be corrected by the installation of adequate crushing facilities. ECONOMICS AND TRANSPORTATION No figures on the relative economics of the use of eastern high-volatile and Illinois coals are included in this report other than the fact that there is a freight differential to Granite City of $2.12 per ton. In June, 1945, at the conclusion of W. P. B. sponsorship of this project, the Kop- pers plant at Granite City was consuming Illinois coal mined within 80 miles of the plant at a rate of approximately 600 tons per day. Indications are that the rate of consumption will continue at about this level until it is again possible to operate two blast furnaces simultaneously. When this occurs, the consumption of Illinois coal will increase. From the start of the Illinois coal tests in April 1944, until the termina- tion of our W.P.B. contract on June 30, 1945, Koppers Company carbonized 228,- 107 tons of Illinois coal, representing a transportation saving of 2,326,700 car miles not including return of the empty cars to the mines. COOPERATION WITH INLAND STEEL COMPANY Early in April 1944, we were invited to consult with officials of the Inland Steel Company in East Chicago, Indiana, on the possible use of our pilot oven in connection with their research program. Inland Steel carbonizes about 8,000 tons of coal daily, 4,700 tons in four Koppers oven batteries at the main plant, and 3,300 tons in two new batteries of Koppers Underjet type ovens in the plant built in 1943 by the Defense Plant Corporation. About 70 per- cent of the total coal used is high-volatile bituminous, that used in the main plant being supplied from Inland's captive mine in the No. 3 Elkhorn seam of eastern Ken- tucky, and that used in the D.P.C. plant being allocated by the government from miscellaneous eastern Kentucky and West Virginia mines. 30 ILLINOIS COAL FOR METALLURGICAL COKE Inland Steel Company holds extensive coal reserves in the low-sulfur area of south- ern Illinois. No coal has been mined from this holding, but other areas near this property have been mined extensively in the No. 6 seam, and drill tests indicate that the Inland Steel reserves are similar to those coals. It was thus of mutual advantage to Inland Steel Company and to ourselves to determine the coking characteristics of blends of this Illinois coal with the coals normally used in the Inland Steel plant for production of blast furnace coke. Early Pilot Plant Oven Tests In order to check the ability of our ex- perimental oven to give results comparable to commercial coking practice, a sample of the coal blend being used at the Inland Steel plant was coked in this oven under condi- tions approaching the operating practice in the Inland plant. Experimental results checked average plant results remarkably well. Other coal blends used at both In- land plants were carbonized in the experi- mental oven, and results checked closely with commercial practice, thereby indicating that the pilot oven could be used as a guide for large-scale coking experiments on com- mercial ovens. Cooperative Research Program In June 1944, the officials of the Inland Steel Company requested the loan of Mr. Harold W. Jackman (Chemical Engineer in charge of our pilot oven operation) for a period of three months to direct their re- search program and to correlate it with ex- perimental work of the Illinois State Geo- logical Survey at Urbana. Believing that this arrangement would be of value to the progress of this project, the Survey com- plied with the request and Mr. Jackman worked with the Inland Steel Company for the period of July 1 to October 1, 1944. The cooperative work between the two organizations was carried out largely under this arrangement. scope of research The research program as planned by Inland Steel Company at this time con- templated a general study of coal expansion and carbonization properties, and a critical examination of Beckley seam low-volatile coal from an area in Raleigh County, West Virginia, to determine its coking and expan- sion properties when blended with Inland's eastern Kentucky Elkhorn seam coal. This program was expanded to include tests on these coals in blends with Illinois No. 6 seam coal similar to that in Inland's reserve in Jefferson County, Illinois. TESTING PROCEDURE The following procedure was used in the Inland Steel Company coal testing pro- gram. 1. Expansion pressure tests were made (by Inland Steel Company) on coal blends in a movable-wall Koppers type test oven. This test gives an indication of the pressure that is developed on the oven walls during carbonization. 2. Coal blends under consideration were carbonized in the pilot oven in Urbana to determine their coking properties. 3. Full-scale oven tests were then made on each coal blend which warranted further investigation. Each blend being tested was charged to four ovens on three successive days and carbonized under normal plant operating conditions. The coke was sampled and tested on each day for its physical and chemical properties. 4. As a final check on coke properties and oven operation, and as an indication of blast furnace performance when using the test cokes as fuel, certain coal blends were charged to one entire coke oven battery of 73 ovens at the D.P.C. plant for periods of three weeks each, and the test cokes were used exclusively on one blast furnace where their performances were studied and com- pared. 5. Following the above research pro- gram, series of coal drying tests were made in cooperation with the Link-Belt Company of Chicago, the objective being to remove PROCEDURES .IS I) RESULTS SI the surface moisture from wet washed coals without injury to their coking properties. Coking and expansion pressure tests were made on blends of these coals before and after drying. Results coal expansion pressure tests No attempt is made in this report to de- scribe the Koppers movable-wall test oven in detail or to elaborate on the many coal expansion tests made during this investiga- tion. Reference to these tests is made, how- ever, because of the importance of coal ex- pansion data in coke oven practice, and be- cause of the information obtained on the expansion properties of Illinois coal blends. The Koppers Company was one of the first to realize the damaging effect of ex- panding coal on by-product coke ovens. Based on the experience gained from actual oven failures, Koppers has concluded that the maximum wall pressure which can safely be developed during the carbonization of any coal is 2 pounds per square inch. To measure this wall pressure, Koppers has developed the movable-wall oven which was used in these tests. Generally speaking, high-volatile coals contract and low-volatile coals expand during carbonization. Low-volatile coals from different seams, and even from different sections of the same seam, have different expansion characteristics. By avoiding the use of highly expanding coals, and by using experimental blends to deter- mine the expansion pressure developed, it is possible to avoid blends which may exert damaging pressures on the oven walls. In addition to the inherent expansion properties of the coals used, there are other factors which strongly influence the pressure developed in an oven during the coking period. The most important of these is the bulk density of the coal as charged, which is influenced by coal moisture and pulveriza- tion. Ash and petrographic composition also have a bearing on the pressure developed. The effects of these factors were studied at this time. From the standpoint of our research, two important conclusions were reached from the study of expansion pressure. 1. The Beckley coal under consideration was found to produce higher expansion pressures when blended with Inland's Elk- horn coal than the Pocahontas normally used at the Inland plant. 2. The expansion pressure of a Beckley- Elkhorn blend can be reduced materially by including a relatively small proportion of certain Xo. 6 seam Illinois coals in the blend. For example, a blend of 70 percent Elkhorn, 30 percent Beckley developed an expansion pressure of 4.21 pounds per square inch. Substituting 25 percent of a Xo. 6 seam coal for an equal amount of Elkhorn reduced the expansion pressure to 2.58 pounds per square inch. This property of decreasing the expansion pressure of a highly expanding blend is regarded as important. In this way, low- volatile coals not now in general use for carbonization because of their expansion properties might be made usable in the cok- ing industry by the inclusion of certain Illi- nois coals in the blend. PILOT OVEX TESTS AT URBAXA The tests in the pilot plant at Urbana were made to determine the coking proper- ties of many coal blends of interest to this cooperative research. In all, 35 pilot plant runs were made in connection with the Inland Steel cooperative program. Of special value to the general knowledge of carbonization were the runs made to de- termine the effect of such factors as coal density, moisture, pulverization, and mine preparation on the properties of the coke. The trends noted here will be described in more detail in that section of this report entitled "Trends in Pilot Oven Tests." One point of interest brought to our attention by these tests was the use of Poca- hontas coal of 22 percent volatile matter to improve the plastic properties of coal blends containing a large percentage of Illi- nois Xo. 6 seam coal. This medium-vola- tile Pocahontas coal is much more fluid when in the plastic condition than is the 32 ILLINOIS COAL FOR METALLURGICAL COKE regular Pocahontas coal of 17 percent vola- tile matter. The Illinois No. 6 seam coal used in these tests has a low fluidity, and its coking properties are improved by addition of the more highly fluid Pocahontas coal. A series of coking tests was made on Beckley-Elkhorn coal blends in which the Beckley coal was increased by increments of five percent from 15 percent to 30 per- cent of the total blend. This series showed an improvement in coke properties consist- ent with the increase in Beckley coal. To show the effect of substituting 25 per- cent Illinois No. 6 coal for a portion of the Elkhorn coal in blends of Elkhorn and low- volatile, three sets of comparative tests were made both with and without No. 6 coal from the Orient No. 1 mine. Results indi- cated consistently that the No. 6 coal blends produced a slightly blockier coke with very little change in stability, but with a slight increase in size and shatter index, and a lower apparent gravity. Physical tests indi- cate that coke made from blends containing this amount of No. 6 coal would be satis- factory as blast furnace fuel. FULL-SCALE OVEN TESTS In addition to tests in the pilot ovens. Inland Steel tested nine coal blends under plant operating conditions in full-scale Koppers ovens at the D.P.C. plant. Ten to twelve ovens were charged with each coal blend tested. Of interest to this proj- ect is the comparison in properties of the coke made from two similar coal blends, the difference being the inclusion of 25 per- cent of Illinois No. 6 seam coal in one of the blends. Illinois No. 6 coal from the Orient No. 1 mine in Franklin County was chosen as being representative of Inland's Illinois reserve. The 2 inches x j£ inch size coal was used. Minus ^ inch Illinois coal was not used in any of the Inland tests because of concentration of fusain in the fine size of coal. Significant coke properties as shown in table 3 indicate that the Orient coal produced a small increase in the size and strength of the coke, a decrease in apparent gravity, and a slightly rougher and darker coke structure. THREE-WEEK OVEN AND BLAST FURNACE TESTS In the final phase of the Inland Steel research program, three-week oven battery tests were made on selected coal blends, con- suming about 35,000 tons of coal per test, and the coke was Used as blast furnace fuel. Here again two similar coal blends, one of all-eastern coals, and the other containing 25 percent Orient coal, were compared. The coke from the Orient coal blend was Table 3. — Effect of Addition of Illinois Coal to a Beckley-Elkhorn Coal Blend Furnace coke yield (% of coal charged) Average size (in.) Shatter (+2") Tumbler Stability (+1") Hardness (+M") Apparent gravity True gravity Porosity (%) Appearance 25% Elkhorn Egg 45% Elkhorn Slack 30% Beckley 67.3 2.25 59.6 52.7 69.7 0.899 1.86 51.8 Gray — normal. Smooth surfaces. Blocky — tough. 25% No. 6 Illinois (Orient) 45% Elkhorn Slack 30% Beckley 66.0 2.30 61.4 54.8 69.3 0.886 1.88 53.0 Slightly darker than normal. Surface somewhat rough. Blocky — tough. PROCEDURES AND RESULTS 33 again slightly larger with a higher shatter test, and with tumbler stability very similar to that of the coke made from the all-eastern coal blends. Coke oven operation was satis- factory with both blends. Operation of the blast furnace was erratic during the first half of the three-week test when coke containing Orient coal was used as fuel. Iron tonnage for the entire period was nearly 4 percent lower than when no Orient coal was used. During the last half of the test period, furnace operation became more uniform and this decrease in tonnage dropped to 1.8 percent. Fuel consumed per ton of iron was high. This likewise improved as the test progressed. It was unfortunate that this test could not be con- tinued longer to evaluate more accurately this coke as blast furnace fuel. Average efficiencies obtained in the blast furnace during the period in which Orient coal was used indicated that the Illinois coal blend was comparable to the all-eastern blend being used at the D.P.C. plant. Allowing for time in which to adjust blast furnace operation, an advantage should be gained from use of Illinois coal of uniform chemical composition in place of an equal amount of eastern coal from a number of mines in which the chemical composition is variable. Inland Steel, therefore, expressed a desire to place both batteries of the D.P.C. plant on a blend containing 25 percent of Illinois coal for a period of one month. It was found, however, that Illinois coal in that quantity was not then available, and no further tests were made at that time. COAL DRYING TESTS In addition to the major cooperative re- search program described above, we have cooperated in this project with Inland Steel Company and Link-Belt Company of Chi- cago, Illinois, in coal drying tests on No. 6 seam Illinois coal, Beckley seam coal, and Inland's Kentucky Elkhorn coal. Mechanical mining is making it more imperative to remove coal impurities at the mines with washing equipment. Anticipat- ing the use of washed coal in the plant, Inland Steel has realized that surface moist- ure remaining on the coal causes it to freeze in the cars in winter weather and to give trouble in handling. Surface mois- ture also lowers the bulk density of the coal charge in the ovens and reduces oven capac- ity. Link-Belt Company is developing a coal drier in which coal can be heat dried quickly and at a relatively low temperature. It is hoped in this way to remove surface mois- ture without oxidizing the coal and injuring its coking properties. The coal drying tests described below were made on the pilot size drier located in the Link-Belt plant in Chicago. Slack coal from the Beckley and Elkhorn seams, and 2 inches x % inch sized coal from the Orient mine, were drenched with water and surface dried to approximately the moisture content of the coals as mined. Blends of these coals were coked in our pilot coke oven before and after drying. The heat dried coal blends produced cokes of lower tumbler stability than did the blends of the untreated coals. (See Runs 113 to 121 inc., in Appendix A.) This series of coal drying tests was repeated in the Link-Belt drier, and care was taken to use somewhat lower tempera- tures than before. Here again lower stabili- ties were obtained on the cokes made from the heat-dried coals. Expansion pressure tests made by the Inland Steel Company on coal blends from both of these series of tests showed in every case that heat drying caused a reduction in the pressure exerted on the oven walls by these blends during the coking period. It was therefore concluded that heat dry- ing these three coals had resulted in some oxidation which manifested itself primarily in reduction of the tumbler stability of the coke, and in reducing the expansion charac- teristics of the coal blends. In the tests just described, no attempt was made to determine the effect of heat drying on each individual coal. Subse- quently, a third series of drying tests was made and the heat dried coals were substi- tuted one at a time in the coal blends. It was found that the use of heat dried Elk- 34 ILLINOIS COAL FOR METALLURGICAL COKE horn (2 inches x 0) coal caused a reduction in the tumbler stability as in the previous tests. Use of the Beckley (^8 inch x 0) heat dried coal caused a small increase in coke stability. No effect was noted when Illinois (2 inches x ^ inch) heat dried coal was substituted for the undried coal. Expansion pressure tests on this third series of coals showed that heat drying again caused a reduction in the pressure developed by the blends containing heat dried Elkhorn and Beckley coals. Heat dry- ing Illinois coal caused no change in the expansion characteristics of the coal blend. This last series of tests leads us to be- lieve that the coal fines, with their large surface area, undergo appreciable oxidation in this type of heat drying. We believe that both the Elkhorn and Beckley fine coals show oxidation. The coking properties of the Elkhorn coal, which is not strongly coking, are somewhat injured by this oxi- dation of the fines. The Beckley coal, which is much more strongly coking, appears to be one of those which produces more blocky coke when slightly oxidized. The Illinois coal, containing no fines, and thus having much less surface area, was not oxidized appreciably in the drying process. Pertinent data on these coal drying tests are shown in table 4. We believe that the problem of drying coal without injury to its coking properties is one of great importance to the Illinois coal producers. Illinois has pioneered in coal washing, and the removal of surface moisture is a problem which should be solved if quantities of washed Illinois coals are to be used for coking. Table 4. — Heat Drying Tests on Link-Belt Drier Tumbler stability % + 1 inch. Expansion pressure lb/sq. in. Series I 75% Elkhorn 25% Beckley Coals as mined 55.1 52.7 55.6 52.4 52.1 49.7 53.3 50.2 43.8 41.0 46.8 47.2 47.9 1.60 Drenched and heat dried 1.35 25% Illinois 50% Elkhorn 25% Beckley Coals as mined .... 1.10 Drenched and heat dried 1.00 Series II 75% Elkhorn 25% Beckley Coals as mined 2.75 Drenched and heat dried 2.68 25% Illinois 50% Elkhorn 25% Beckley Coals as mined 2.46 Drenched and heat dried 2.35 Series III 75% Elkhorn 25% Beckley Coals as mined 2.25 Elkhorn drenched and heat dried Beckley drenched and heat dried 2.18 1.90 25% Illinois 50% Elkhorn 25% Beckley Coals as mined 1.82 Illinois drenched and heat dried 1.81 PROCEDURES AND RESULTS 35 Remarks Inland Steel Company has considered this cooperative research program with the Illinois State Geological Survey to be suc- cessful. The Beckley seam coal was pur- chased, thus assuring a supply of low-vola- tile coal which tests have shown can be blended with eastern Kentucky coal and with the coal similar to that from Inland's reserves in Jefferson County, Illinois. Although Inland Steel has not been active in testing Illinois coal since this series of tests was completed, it has used Franklin County coal in the plant during periods of coal shortage. The progress of this project has been followed with interest, and the testing program with Illinois coal is not considered to be completed. During the tests just described, there were approximately 10,000 tons of Illinois coal used in the Inland Steel plant. This coal was mined at a distance of 319 miles from the Chicago area and replaced eastern Kentucky coal mined at 546 miles from this area. Freight on the Illinois coal is $1.14 per ton less than the all-rail haul from eastern Kentucky, and $0.50 less than the combination rail and lake boat rate. Any continued use of Illinois coal at this plant would, of course, be dependent on the eco- nomics of the process, and this can only be determined by plant tests of long enough duration to establish operating procedures and determine accurate yields and costs. GENERAL COKING TESTS In addition to the pilot oven tests made in direct cooperation with the Koppers Com- pany and with Inland Steel Company, coals from most of the low-sulfur Illinois mines have been tested to evaluate them for use in production of metallurgical coke. As all Illinois coals which have been tested must be blended with other coals to produce metallurgical coke with satisfactory physi- cal properties, a study has also been made of low-volatile coals and of certain eastern high-volatile coals for blending with Illi- nois coal. LLINOIS Coals FRANK I.I X COUNTY The low-sulfur coals tested in the Frank- lin County area, including adjoining areas in Jefferson, Perry, and Williamson coun- ties, are from the No. 6 Illinois seam. The washed coals from this area are of uniform chemical composition, with sulfur ranging from 0.7 to 1.2 percent, depending upon the location of the mine. No. 6 seam coal in the Franklin County area has relatively low fluid characteristics when in the plastic state, and has a tendency to form a rough structure coke when blended with Pocahontas coal of about 17 percent volatile matter. This tendency toward a rough structure can be overcome by replacing this Pocahontas coal with cer- tain more fluid coals of about 22 percent volatile matter, such as the medium-vola- tile Pocahontas used in a number of our experimental runs, or by addition of a third coal to the Illinois-Pocahontas blend. This third coal may be either a high- or low- volatile coal possessing more fluid plastic characteristics than the Illinois No. 6 seam coal. Rapid coking also improves the coke structure. Coals from certain mines in the north- western portion of this area have been shown to have somewhat more fluid plastic properties than other coals mined farther south and east. Pilot plant tests indicate that these more fluid Illinois coals can be blended with Pocahontas of 17 percent vola- tile matter with production of a desirable coke without the addition of a third more highly fluid coal. Generally speaking, coke made from a blend of Illinois No. 6 seam coal from Franklin County and Pocahontas coal is rather large and strong. Shatter and tum- bler tests indicate that this coke should sup- port satisfactorily the burden in a blast furnace. The coke is lighter and slightly more porous than coke usually made from all-eastern coal. By proper blending, such as is practiced at the Koppers Company plant at Granite City, Illinois, No. 6 seam 36 ILLINOIS COAL FOR METALLURGICAL COKE coal can be used successfully in production of blast furnace fuel. SALINE COUNTY No. 5 seam Illinois coal which underlies Saline County, south and east of Franklin County, tends to have the strongest coking properties of any Illinois coal which has been tested. This is the highest rank coal mined commercially in Illinois. Washed coals obtained from this area contain less moisture than Franklin County No. 6 seam coal, and about 1.5 percent less oxygen on the dry ash-free basis. Sulfur in this coal ranges from 1.7 to 2.1 percent, except for one low-sulfur area where washed coal of 0.75 to 1.0 percent sulfur can be produced. No. 5 seam coal can be coked successfully in blends with Pocahontas to form a blocky coke high in stability, with a desirable sur- face structure. It does not appear to be necessary to increase the fluidity of the No. 5 seam-Pocahontas coal blends by the addi- tion of more fluid eastern coals. Pilot plant results and commercial oven tests at the Koppers Granite City plant bear out this statement. MADISON COUNTY There is a small low-sulfur coal area in the No. 6 seam in Madison County, near Troy. Coal sampled from this area con- tained high moisture, high ash, and about 1.5 percent sulfur. No attempt was made to clean this coal. Laboratory tests indi- cate very weak coking properties, but when 20 percent of this coal from Madison County was blended with Franklin County coal and Pocahontas of 22 percent volatile matter, a very strong coke was produced. WOODFORD COUNTY There is also a low-sulfur area in the No. 2 Illinois coal seam in Woodford County in the north-central part of the State. Previous mine samples taken here had analyzed about 1 percent sulfur. The Minonk mine is operating in this area. It is without coal washing facilities, and pro- duces coal of about 13 percent moisture. The samples taken at this mine on the stoker size coal showed 1.5 to 2.0 percent sulfur. Indications are that this sulfur would have been reduced by cleaning. Mi- nonk coal is somewhat more fluid than the Franklin County coals tested, and produces a fairly smooth coke with a low percentage of fines, even when blended with 40 percent of Pocahontas coal. The coke strength is fair, but can be improved by proper blend- ing. This coal might be used in small quan- tities to improve the fluidity of a coal blend. INDIANA NO. IV SEAM COAL REPRESENTING DEPOSITS IN ILLINOIS The Saxton No. 1 mine, located in Vigo County, Indiana, just across the eastern Illinois state line, produces low sulfur, low ash coal with high moisture content. The coal has a low fluidity and produces a sandy appearing, but fairly tough coke. Proper blending should improve the coke structure. This coal is of interest because of its low sulfur content of less than 1 percent, and because it may be representative of the un- developed No. 4 seam in adjacent areas of eastern Illinois. Non-Illinois Coals low-volatile coals As stated, it is necessary to blend Illinois coals with coal from other areas to produce coke having the desirable characteristics for metallurgical use. Coal commonly used for this purpose in the Chicago and St. Louis areas is from the No. 3 Pocahontas seam in West Virginia, and contains about 17 per- cent volatile matter. Plastic tests on this Pocahontas coal show it to have a low fluidity. In normal coal blending procedure, this low-fluid Pocahontas coal is blended with highly fluid eastern high-volatile coal. The blend produces a good coke. Experimental data have led us to the belief, however, that when Illinois coal is used to replace the eastern high-volatile coal, the resulting PROCEDURES AND RESULTS 37 blend may not have sufficient fluidity to produce the desired coke structure. In line with this belief, it has been found that improved coke structure results from in- creasing the fluidity of the blend through inclusion of more highly fluid coals, either high- or low-volatile. It has been found that a Pocahontas coal of about 22 percent volatile matter becomes much more fluid when in the plastic state than do the lower volatile Pocahontas coals. When this more fluid coal is blended with Illinois coal of low fluidity, the blend pro- duces a smooth coke structure with a low percentage of coke fines. Coke stability and size are somewhat reduced. Three-way blends in which Illinois coal is blended with both low- and medium-volatile Pocahontas coals have produced cokes combining high stability with a good appearance and low percentage of coke fines. The medium-volatile Pocahontas coal mentioned here, and subsequently in this bulletin, is from one West Virginia mine which is not identified by name. It must not be construed that all medium-volatile coals have coking properties similar to this coal. However, two other coals of similar volatile content have been investigated, one being the Buccaneer Carey seam coal men- tioned in this bulletin, and the other being from the No. 6 Pocahontas seam. Both of these coals develop high fluidity in the plastic stage. When blended with Illinois coal and coked in the experimental oven, desirable coke structures have resulted which are similar to those resulting from use of the medium-volatile Pocahontas coal first mentioned. Other low-volatile coals from the Beck- ley seam of West Virginia have been blended with No. 6 seam Illinois coal. These Beckley coals are also more fluid than the regular Pocahontas and can be blended to advantage with Illinois coal. HIGH-VOLATILE COALS Another means of improving the structure of the coke from an Illinois-Pocahontas coal blend is by including a percentage of fluid eastern high-volatile coal. In pilot oven blends run in cooperation with Kop- pers Company, and in coal blends used at the Koppers Company plant, No. 2 Gas and Hemshaw seam coals from West Vir- ginia have been used for this purpose. Ex- perimental and commercial coking results indicate that addition of either of these coals to an Illinois-Pocahontas coal blend improves the physical properties of the coke. TRENDS IN PILOT PLANT OVEN TESTS No attempt is made in this report to discuss in detail all of the 183 experimental coke runs made on the pilot oven during the period of W.P.B. sponsorship. Many of these runs were made at the request of the cooperating industrial companies to aid in their choice of coal blends, and to help determine proper operating procedure. Other runs, as previously stated, were made in our survey of low-sulfur coals of the State, and in our study of coal blending. Detailed data on all pilot oven runs, includ- ing oven operating conditions, coal and coke analyses, physical properties and yields of coke, and yields and composition of by-prod- ucts, are presented in tabular form in Ap- pendix A. Certain later data supplementing those obtained in the original 183 coking runs have been included at this point in the dis- cussion of coking trends. These data are presented to substantiate trends noted in the early work but which could not be verified until later. Pilot oven tests have shown definitely that coal from the low-sulfur area of Illinois can be used in blends for the production of coke having physical and chemical proper- ties similar to the cokes now being used in industry for metallurgical purposes. In evaluating the experimental cokes, we have been handicapped by lack of accepted speci- fications for blast furnace fuel. Cokes have been compared one with another, and with commercial coke, by such standard physical tests as shatter, tumbler, and gravity. It 38 ILLINOIS COAL FOR METALLURGICAL COKE has only been through our cooperative work with industry that certain of these cokes have been evaluated in terms of blast furnace operation. Experimental runs in the pilot oven have shown the effects on coke properties of oven operating conditions and coal preparation and blending. Trends have been shown which are of value to an understanding of the coking properties of Illinois coal. Dis- cussion of certain of these trends follows. Effect of Coking Time and Tempera- ture on Coke Properties In table 5 are shown the results of car- bonizing Illinois coal blends at increasing temperatures. It is noted that an increase in the rate of coking is shown to decrease the average size of the coke produced, with a corresponding decrease in shatter index. Coke stability is reduced, and the hardness factor is increased. The breeze (-^-inch coke) decreases as the coking rate is in- creased, and the coke appearance is im- proved, judging by color and uniformity of cell structure. Further studies made on the effect of coking time and temperature, in which coal blends were coked at five different rates corresponding to coking times of 24, 22, 20, 18 and \6]/2 hours in a 19-inch oven, are shown in table 6. Here trends similar to those noted in table 5 are shown as the coking time is decreased. Other experimental runs (Nos. 102 and 108) in which the coal was coked at a normally fast rate and then allowed to remain in the oven for a four-hour to six- hour soaking period, during which time the coke temperature gradually increased about 90° F., did not show any decided change in coke quality attributable to the soaking period (compare with runs 103 and 126 respectively in which no soaking periods were employed). It is concluded that it is the rate of coking that is largely responsible for coke quality. It is also concluded that a fast coking rate is desirable when coking such Illinois coal blends in order to produce the best cellular coke structure, and to keep coke breeze at a minimum. Preparation of Coal pulverization effect on coke properties Many modern metallurgical coke plants pulverize coal to pass 80 percent through a j/6-inch screen. Other plants pulverize to only 65 percent minus i/^-inch size and a few plants are known to carbonize coal passing 90 percent through a J/6-inch screen in order to improve the quality of the coke. Table 5. — Effect of Coking Time and Temperature on Coke Properties. (I) Run No. Final flue temp. °F. Coking time Hr.: Min. Shatter +2" % Tumbler Av. size in. Breeze Stability Hardness % + W -Vi" % of coal Coal Blend 60% Energy No. 5. (l%" x %" Washed) 40% Pocahontas-Carswell 8 7 14 15 1850 1900 1950 2000 12:15 11:35 11:05 10:23 Coal Blend 62.2 50.0 68.2 58.4 47.1 69.5 50.2 47.8 70.0 45.6 47.1 70.8 : 60% Orient No. 1. (\ l A" x %" Washed) 40% Pocahontas-Carswell 2.77 2.74 2.50 2.38 4.2 4.0 2.7 2.8 25 9 1750 1850 17:30 12:03 83.8 56.2 59.2 60.7 52.2 69.1 3.48 2.85 6.0 3.3 PROCEDURES AND RESULTS 39 Table 6.— ■Effect of Coking Time and Temperature on Coke Propertu s. (ID Run Final Hue temp. °F. Coking time Hr.: Min. Shatter +2" % Tl MBI.I.R Av. size in. Breeze No. Stability Hardness % + Va" % of coal Coal Blend: 75% Orient No. 1. (2" x 25% Pocahontas-Carswell Washed) 262 1760 17:42 83.9 51.7 58.1 3.21 6.1 261 1810 16:13 81.1 51.9 61.7 2.97 5.0 260 1860 14:44 70.9 52.1 63.7 2.58 4.3 259 1910 13:16 67.4 50.3 66.7 2.44 3.7 258 1960 12:15 61.3 49.2 66.9 2.31 4.1 Coal Blend: 75% Old Ben No. 11. (2" x \y 2 " Washed) 25% Pocahontas No. 4 Seam 233 1760 17:42 77.9 45.8 62.7 2.99 3.4 232 1810 16:13 73.1 46.8 64.8 2.79 3.0 231 1860 14:44 67.0 46.2 65.8 2.52 3.0 230 1910 13:16 59.8 44.1 66.1 2.34 2.9 229 1960 12:15 55.2 43.1 67.0 2.21 2.8 Table 7. — Effect of Coal P ULVERIZATION ON COKE PROPERTIES No. Pulver- ization -8m % Shatter +2" % Tumbler Av. size in. Breeze Run Stability Hardness % + i" 1 % + M" - l A" % of coal Coal Blend: 25% Orient No. 1. (2" x %" Washed) 45% Wheelwright Slack— 30% Glen Rogers 76 62.7 76.9 51.0 62.1 3.30 63 78.4 72.7 53.7 65.6 2.95 77 92.7 66.6 59.1 70.5 2.82 Coal Blend: 25% Orient No. 1. (2" x %" Washed) 40% Wheelwright Slack — 35% Medium- Volatile Pocahontas 68 81.1 63.0 48.3 68.2 2.92 57 91.5 66.1 54.7 67.5 2.72 3.0 3.2 2.1 2.2 Table 7 shows the effects of pulverization on two coal blends when carbonized in the experimental oven. Increasing the degree of pulverization produces the following changes in coke quality. ( 1 ) Reduction in average coke size. (2) Increase in coke stability. Fine pulverization of the Glen Rogers blend is shown also to decrease the shatter index and increase the amount of coke fines. MOISTURE EFFECT ON COKE PROPERTIES Moisture is considered under the heading of "Coal Preparation" because of the effect of preparation methods on the moisture content of coal as delivered. Wet washing processes add surface moisture to the pre- pared coal. Shaker screens and coal driers remove moisture. A number of coke plants are adding moisture to the coal before pul- verization as an effective means of reducing bulk density in the coke ovens, thereby reducing the expansion pressure developed by the coal during carbonization. The fact that surface moisture does affect bulk density has been evident throughout this entire testing program. It has been necessary to air dry washed coals partially before charging to the experimental oven 40 ILLINOIS COAL FOR METALLURGICAL COKE Table 8. — Effect of Moisture on Coke Properties Coal Blend: 25% Wheelwright Egg 50% Wheelwright Slack 25% Glen Rogers Coal moisture % Bulk density lb./cu. ft. Shatter + 2" % Tumbler Av. size in. Breeze 1/ " — 72 % of coal App. Run No. Stability % + 1" Hardness % + M" gr. 83 62 84 2.4 3.2 5.8 54.6 51.1 47.7 63.5 69.0 73.1 53.1 68.2 53.3 68.2 53.1 65.6 2.93 2.94 3.36 2.2 2.5 2.1 0.878 0.855 0.805 in order to obtain the desired bulk density of about 50 pounds per cu. ft. Table 8 shows results of a series of tests in which the coal moisture is increased from 2.4 to 3.2 and 5.8 percent. The bulk density of the coal charge in the oven is shown to drop from 54.6 to 51.1 and 47.7 pounds per cu. ft. This decrease in bulk density results in a corresponding decrease in the apparent gravity of the coke. Coke size is increased. The shatter index also increases, probably due to the larger coke, and tumbler stability remains constant. COAL CLEANING EFFECT ON COKE PROPERTIES No general statement can be made rela- tive to the effect of coal ash on coke proper- ties. When ash is reduced in a coal cleaning process, the ratio of the petrographic con- stituents in the coal may be changed, along with removal of high ash coal and free impurities such as pyrite and slate particles. It is known that free non-coal impurities shatter into fine particles when coal is pul- verized, and that these particles may form points of weakness in the coke structure which cause cracks and shattering. Removal of such impurities before crushing will eliminate this condition. Tests made on coal from the Jefferson No. 20 mine, with and without removal of free impurities, illus- trate this fact. Raw coal from this mine contained visible pieces of free non-coal impurities. It is shown in Table 9 that removal of these impurities from the coal by flotation at 1.5 gravity produced a much stronger coke with higher shatter index and increased tumbler stability and hardness. Coke fines were reduced. Visual examina- tion of coke made from the raw coal showed that small particles of free impurities formed nuclei, about which radiated many cracks in the coke structure. Table 9. — Effect of Removal of Non-Coal Impurities Coal Blend: 80% Jefferson No. 20. (1- 20% Pocahontas-Carswell Run No. Condition of Jefferson coal Coal ash % Shatter + 2" % Tumbler Av. size in. Nut + breeze - 1" % of coal Stability % + 1'" Hardness % + M" 173 178 Raw Float at 1.5 gr.... 8.1 6.9 67.6 71.8 43.5 61.4 53.2 65.1 2.63 2.58 3.9 3.2 PROCEDURES AND RESULTS 41 Weathering of Illinois Coals When Illinois coal from the No. 6 seam is stocked for an extended period of time after mining it is known to weather with a gradual loss of its coking properties. This is true especially with the fine coal sizes where large surface areas are exposed to oxidation. Consequently, it has not been considered advisable by certain operators to stock Illinois coal, even temporarily, when it is to be used for production of coke. Preliminary coking tests made on blends containing Illinois No. 6 seam \Yz x H- inch coal, in which the Illinois coal was stocked for approximately three-month and six-month periods in a roofed but other- wise open bin, indicated that storage of this coal did not seriously impair the coking properties of the blends in which it was used. (See table 10.) Following these preliminary tests, other series of weathering tests have been made at regular intervals on Illinois coals which were stocked in the open in conical piles of from two to four tons. The coals were exposed in this way to maximum weather- ing conditions during the storage period. Certain of these tests are still in progress. Data are shown in tables 11 and 12. Plant storage. — Illinois coal, largely of the 6x3 inch and 3x2 inch sizes from a number of mines, was stocked in a ridge- shaped pile approximately 150 feet long and 25 feet high on a concrete pad at a midwest coke plant. This coal was sampled and tested by us one, two, and six months after stocking. The first two samples were taken from the top of the pile where the coal had been exposed directly to the air for the entire period. The six-month sam- ple was taken from near the bottom of the pile as the coal was exposed when being removed from storage. Data in table 13 show that six months storage had not re- sulted in sufficient weathering to be notice- able when the coal was used as 25 percent of the total blend. It was noted also that the coal in the pile still showed the original bright surfaces, and that there was no noticeable size degradation. At no time had there been any evidence of heating. Consideration of all of the weathering test data obtained to this date on No. 6 seam Illinois coals indicates that where washed, prepared sizes of Illinois coal, ex- clusive of fines, are to be used as not more than 25 percent of the total coal blend, storage of from three to six months is allow- able. Likewise, where as much as 80 per- cent of this Illinois coal is to be blended with a fluid medium-volatile coal such as is shown in table 11, six months storage has no detrimental effects on the physical prop- erties of the coke. Blending of weathered No. 6 seam Illi- nois coal with Carswell-Pocahontas of low fluidity apparently gives a blend with borderline plastic characteristics. In table 12, Series I and II, the Orient coal blends Table 10. — Effect of Weathering Illinois Coal. (I) Run No. Age of 111. coal since mining No. days Shatter Tumbler Breeze — y 2 % of coal + 2" % Stability Hardness % + l A" 25% Orien 45% Wheeh 30% Glen F tNo. 1. (VA •ight Slack .ogers " x%" Washe d) App. gr- 63 104 94 141 Coal Blend: Fresh 83 72.7 74.4 53.7 49.3 65.6 63.2 Coal Blend: 80% Orient No. 1. i\\ 20% Medium- Volatile Pocahontas Washed) Fresh 186 58.2 57.5 47.4 47.8 67.6 68.0 3.0 2.0 1.8 2.7 0.842 0.830 0.813 0.802 42 ILLINOIS COAL FOR METALLURGICAL COKE produced very good coke after 30 days in storage. The 2 x ^g-inch size continued to produce good coke after 60 days, and showed only minor deterioration after 90 days weathering. The 3x2 inch size, on the other hand, showed' considerable weather- ing effect in 60 days, and still more in 90 days. It can be assumed from these data that Orient coal can be safely stocked for a period of 30 days and blended with Cars- well-Pocahontas using as much as 80 per- cent Orient in the blend. Stocking this coal in a pile of commercial size where only the surface is exposed directly to the weather has been shown to reduce the effect of weathering and should minimize the oxida- tion shown in our laboratory tests. No evidence of heating in storage has been found. No. 5 seam Illinois coal is shown in table 12, Series III, to withstand three months' weathering with only a small effect on its coking properties. As this is a higher rank coal than that from the No. 6 seam, it is to be expected that its weathering charac- teristics would be superior to those of the No. 6 seam coal. In all these tests, it is shown that weather- ing is first evidenced by an increase in breeze Table 11. — Effect of Weathering Illinois Coal. (II) Coal Blend: 80% Orient No. 1. (2" x %" Washed) 20% Medium- Volatile Pocahontas Run No. Age of Illinois coal since mining No. days Shatter + 2" % Stability Hardness % + l" % + M" Av. size in. Breeze \/ " — 72 % of coal App. gr. 195 13 61.8 48.7 66.6 2.24 3.5 0.808 212 72 63.1 47.9 65.8 2.35 2.8 0.785 225 132 61.5 46.0 66.2 2.34 3.0 0.798 239 ' 198 66.2 48.2 66.4 2.33 3.1 0.779 256 258 69.3 42.8 62.3 2.46 4.2 0.785 Table 12. — Effect of Weathering Illinois Coal. (Ill) Run No. Age of Illinois coal since mining No. days Shatter + 2" % Tumbler Stability %+l" Hardness % + l A" Av. size in. Breeze — 72 % of coal Series I— Coal Blend: 80% Orient No. 1. (2" x %" Washed) 20% Pocahontas-Carswell App. gr. 246 31 63.3 49.4 67.2 2.43 3,0 0.809 255 62 71.8 47.1 66.5 2.42 •3.5 0.774 263 94 63.5 48.4 64.8 2.51 4.2 0.756 270 122 65.4 42.5 59.8 2.49 6.1 0.823 279 153 69.2 37.0 51.5 2.37 9.5 0.806 Series II — Coal Blend: 80% Orient No. 1. (3"x2" Washed) 20% Pocahontas-Carswell 249 31 62.7 51.4 67.2 2.48 3.1 0.792 257 59 63.3 46.5 63.9 2.45 4.4 0.811 265 91 65.1 44.8 59.6 2.39 6.2 0.818 273 122 68.3 38.9 53.0 2.37 9.8 0.834 282 154 64.9 29.4 39.9 1.89 22.4 0.835 Series III- -Coal Blend: 80% Harco No 47. (2" x 1 " Washed) (No. 5 seam Illinois Coal) 20% Pocahontas-C? rswell 250 32 66.5 55.5 67.9 2.33 2.3 0.822 266 90 69.1 55.1 66.7 2.39 3.5 0.838 283 153 69.6 45.0 59.0 2.47 7.1 0.865 307 244 63.6 40.1 52.4 2.32 10.5 0.841 PROCEDURES AND RESULTS 43 Table 13.— Weathering of Illinois Coal Stocked in Plant Storage I'm i Coal Blend: 25% Illinois No. 6 Scam 25% Eastern Kentucky 50% Pocahontas No. 4 Scam Run No. Time in storage, months Shatter + 2" % Tumbler Av. size in. Breeze % of coal Stability % + l" Hardness % + X A" App. gr. 220 226 254 1 2 6 64.0 62.2 62.9 31.3 64.0 28.3 62.7 34.5 65.4 2.55 2.63 2.63 3.0 3.1 3.1 0.887 0.889 0.892 and a lowered hardness factor. Coke size usually increases slightly after the first one or two months and then remains constant. The shatter test is not greatly affected by weathering, and the tumbler stability factor decreases very slowly, and has never been shown in these tests to drop below 42. Like- wise, the hardness factor has never dropped to less than 58.4. Judging from these physical tests, it would not appear that the maximum weathering shown here would greatly affect the use of these cokes as blast furnace fuel. Effects of Blending Pocahontas Coals of Different Characteristics with Illinois Coal It has been shown, as previously stated, that Medium-Volatile Pocahontas coal of 22 percent volatile matter, which has a high fluidity when in the plastic state, is effective in reducing coke breeze and rough coke appearance when blended with No. 6 seam Illinois coal. Comparisons are made in table 14 between blends of Illinois coal with (1) Pocahontas coal of 17 percent volatile Table 14. — Effect of Blending Different Pocahontas Coals with Illinois Coal Run No. Coal blend Shatter + 2" % Tumbler Av. size in. Breeze -Vi" % of coal App. Stability %+l" Hardness % + H" gr. 152 80% 20% Zeigler Pocahontas- Carswell 60.0 49.2 66.5 2.43 2.8 0.795 153 80% 20% Zeigler Medium- Volatile Pocahontas 53.9 48.7 68.3 2.31 2.3 0.788 148 80% 10% 10% Zeigler Pocahontas- Carswell Medium-Volatile Pocahontas 59.7 49.4 67.1 2.35 2.5 0.803 149 70% 15% 15% Zeigler Pocahontas- Carswell Medium- Volatile Pocahontas 57.7 50.7 68.3 2.31 2.2 0.828 150 60% Zeigler 20% Pocahontas- Carswell 20% Medium-Volatile Pocahontas 63.2 52.7 67.3 2.42 2.2 0.846 44 ILLINOIS COAL FOR METALLURGICAL COKE matter, (2) Medium-Volatile Pocahontas coal, and (3) combinations of these two blending coals. Comparisons shown in table 14 between blends of Illinois coal with ( 1 ) Pocahontas of 17 percent volatile matter, and with (2) Medium-Volatile Pocahontas coal indi- cate that blending the medium-volatile coal produces coke with lower shatter index and tumbler stability but with increased hard- ness. The coke size is reduced by the medium-volatile coal, and less breeze is pro- duced. Coke gravity is normally higher; in this respect Run 153 is not typical. It is further noted in this table that a stronger, heavier coke can be made by com- bining equal quantities of Carswell-Poca- hontas and Medium-Volatile Pocahontas coals in blends with 80, 70 or 60 percent of Illinois coal, and that the breeze pro- duced remains small. It is this property of Medium-Volatile Pocahontas coal which indicates its value for blending with coals of low fluidity. Effect of Increasing the Percentage of Low-Volatile Coal in Illinois Coal Blends Table 15 shows the effect of increasing the amount of lower volatile coals in Illi- nois coal blends. Table 15. — Effect of Increasing the Percentage of Lower Volatile Coals in Illinois Coal Blends Run No. Coal blend Shatter + 2" % Tum BLER Av. size in. Breeze -Vi" % of coal App. gr. Stability %+ 1" Hardness % + M" Series I — Orient- -Pocahontas -Carswell B lends 140 90% 10% Orient Pocahontas- Carswell 49.8 37.4 67.4 2.20 2.6 0.774 130 85% 15% Orient Pocahontas- Carswell 62.3 46.3 64.9 2.53 3.1 0.788 131 75% 25% Orient Pocahontas- Carswell 66.5 54.8 67.2 2.47 2.8 0.798 3 70% 30% Zeigler Pocahontas- Carswell 57.2 49.5 65.0 2.76 4.4 0.798 4 60% 40% Zeigler Pocahontas- Carswell 59.7 51.4 65.9 2.69 • 4.7 0.811 5 50% Zeigler 50% Pocahontas- Carswell 63.2 52.7 70.9 2.78 3.9 0.827 Series II — Orient — Me dium-Volat ile-Pocahon tas Blends 96 90% 10% Orient Medium- Volatile Pocahontas 50.9 39.7 69.6 2.52 2.0 0.792 138 85% 15% Orient Medium- Volatile Pocahontas 54.3 45.6 68.4 a 2.23 2.3 0.798 94 80% 20% Orient Medium- Volatile Pocahontas 58.2 47.4 67.6 2.66 1.8 0.813 a Size not comparable with other two runs. PROCEDURES AND RESULTS 45 Table 16. — Effect of Using Petroleum Com. as a Substitute for Pocahontas Coal Run No. Coal blend Shatter + 2" % Tumbler Stability % + l" Hardr % + Vv. size in. I freeze -Vi" % of coal App. gr. 18 90% Orient 10% Petroleum Coke 37.0 26.6 65.2 2.40 2.1 0.775 20 85% Orient 15% Petroleum Coke 46.8 39.3 66.8 2.32 3.2 0.794 21 80% Orient 20% Petroleum Coke 48.2 39.5 61.3 2.45 3.5 0.789 In Series I of this table where Carswell- Pocahontas is increased from 10 to 25 per- cent and from 30 to 50 percent, it is seen that increasing the low-volatile coal tends to increase the coke strength. The appar- ent gravity of the coke also increases con- sistently as the percentage of Pocahontas coal is increased. In Series II where Medium-Volatile Pocahontas is blended with Orient coal, the coke strength again increases as the medium-volatile coal is increased from 10 to 20 percent. No runs were made in which a larger percentage of medium-volatile coal was used. The coke breeze remains low. Apparent gravity increases as the amount of the lower volatile coal is increased. The gravities are consistently higher than those of the corresponding cokes of Series I in which the lower volatile coal used was from the Carswell mine. Effect of Using Petroleum Coke as a Substitute for Pocahontas Coal The petroleum coke used in these experi- mental runs contained about 13 percent volatile matter and formed a very weak button in the standard volatile-matter de- termination. Table 16 shows the quality of the coke produced when petroleum coke was blended with Orient coal and coked in the experimental oven. Petroleum coke is seen to cause the for- mation of a soft coke with poor shatter and tumbler tests. As the amount of petroleum coke used in the blend is increased to 20 percent, the hardness factor drops and the amount of coke breeze increases. These same trends were noticed in plant oven tests made by Koppers Company at Granite City, Illinois. Comparison of No. 6 Seam Coals from Different Illinois Mines Coals from the low-sulfur area of the No. 6 seam vary somewhat in their plastic properties. Of those subjected to test in this program, the ones from the northwest part of the area give evidence of somewhat higher fluidity than the others and produce less breeze when carbonized in blends with Poca- hontas (see table 17). Lower breeze is also Table 17. — Comparison of No. 6 Seam Coals Run No. Illinois coal used Breeze -Vi" % of coal Coal Blend: 80% Illinois No. 6 seam coal 20% Pocahontas-Carswell 152 165 182 178 154 Zeigler No. 1 and 2 Old Ben No. 14 Majestic Jefferson No. 20 (Float 1.50 gr.) Old Ben No. 11 2.8 2.6 2.4 2.3 2.2 Coal Blend: 60% Illinois No. 6 seam coal 4 8 9 166 183 174 164 Zeigler No. 1 and 2 . . . . Energy No. 5 Orient No. 1 Old Ben No. 14 Majestic Jefferson No. 20 (Raw) Old Ben No. 11 4.7 4.2 3.3 3.3 3.0 2.9 2.6 46 ILLINOIS COAL FOR METALLURGICAL COKE Table 18. — Comparison of No. 5 Seam Coals Run No. Illinois coal used Breeze -Vi" % of coal Coal Blend: 80% Illinois No. 5 seam coal 20% Pocahontas-Carswell 44 Sahara No. 16. 180 HarcoNo. 47. 176 Buckhorn 2.4 2.0 1.9 Coal Blend: 60% Illinois No. 5 seam coal 40% Pocahontas-Carswell 49 Sahara No. 16. 181 HarcoNo. 47. 177 Buckhorn 3.5 2.1 2.1 accompanied by an improved appearance of the coke. It is not to be inferred that the coals which produce higher breeze are of inferior quality, as by proper blending they may be made to produce equally satisfactory cokes. Comparison of No. 5 Seam Coals From Different Illinois Mines Coals have been tested from four No. 5 seam mines; three in Saline County and one, the Buckhorn mine, in Williamson County. Coal from this last mine proved to be high in sulfur. No. 5 seam coal when blended with Poca- hontas has consistently produced a strong coke with desirable physical properties. Coke with smooth surface structure and a small amount of breeze is produced. Here again differences in coal plasticity are found to exist; coals from Harco No. 47 and Buck- horn mines are the most fluid. The breeze produced from carbonizing Illinois No. 5 seam-Pocahontas coal blends is shown in table 18. This table does not list the Sahara No. 4 and No. 5 mine coals which are com- bined at the tipple and have also been tested but not in the same blends as shown in the table. These coals also produced low breeze when carbonized with Pocahontas coal (see Run No. 54). Blends Containing Both No. 5 and No. 6 Seam Coals Having shown in pilot oven tests that No. 5 seam coal tends to be more strongly coking than that from No. 6 seam, it was desired to find the effect of addition of a percentage of No. 5 seam coal to blends con- taining No. 6 seam and Pocahontas coals. Two comparisons are shown in table 19 be- tween similar blends with and without the addition of No. 5 seam coal. Table 19. — Effect of Adding No. 5 Seam Coal to a Blend of No. 6 Seam Coal and Pocahontas Coal Run No. Coal used Shatter + 2" % Tumbler Breeze -Vi" % of coal App. Stability %+l" Hardness % + l A" gr. 140 90% 10% Orient (No. 6 Seam) . . . Pocahontas-Carswell 49.8 37.4 67 .4 2.6 0.774 106 50% 40% 10% Orient (No 6 Seam) .... Sahara No. 16 (No. 5 Seam) Pocahontas-Carswell 60.5 45.5 65.1 2.7 0.773 130 85% 15% Orient (No. 6 Seam) . . . Pocahontas-Carswell 62.3 46.3 64.9 3.1 0.788 109 60% 25% 15% Orient (No. 6 Seam). . . Sahara No. 16 (No. 5 Seam) Pocahontas-Carswell 61.9 53.3 68.7 2.4 0.794 PROCEDURES AND RESULTS 47 It is seen that where coal from the Sahara No. lb mine is added to blends of Orient and Pocahontas coals, the quality of the coke is improved. Not only is the strength in- creased, but the general appearance of the coke structure is better. Addition of Eastern High-Volatile Coal to the Blend In the description of the cooperative work with Koppers Company at Granite City, Illinois, it was stated that Koppers Company had reduced the size and breeze content of the plant coke made from Illinois coal blends by reduction in the Pocahontas coal and ad- dition of from 15 to 25 percent of eastern high-volatile coal of high fluidity. Pilot plant results shown in table 20 indicate the effect of this eastern high-volatile coal on the quality of the coke produced. A comparison is made of coal blends containing 10 percent of Pocahontas, with and without eastern high-volatile coal. A further comparison is made of coal blends containing 65 percent Orient coal where the amount of eastern high-volatile coal is reduced and the Poca- hontas is increased. Examination of Runs 140 and 122 show that when 25 percent of Midvale eastern high-volatile coal is added to the blend con- taining 10 percent Pocahontas, the coke strength and size arc both increased, the breeze is decreased, and the coke is heavier. The coke made without Midvale tends to be pebbly, and when Midvale is added the pebbly structure disappears entirely. The second comparison, where Midvale is decreased and Pocahontas increased, indi- cates that the coke becomes more resistant to breakage, and somewhat larger. Breeze is not increased until Midvale is cut to 15 percent. In this last blend, the fluidity is low, and a tendency toward pebblyness is noted in the coke. Koppers' Company has carbonized these three blends in the plant at Granite City, and the same trends have been noticed in the commercial coke. Higher carbonizing temperatures were used in the plant at this time than those used on the pilot oven, and the tendency to produce stronger coke as Midvale was reduced w T as more pronounced than in the pilot oven. The plant coke also increased in size as the amount of Midvale was reduced. It was not possible to obtain actual yields of coke breeze during the plant tests with 17i/ and 15 percent Midvale in the blends, but visual observation indicated that coke breeze increased. The coke had occasional pebbly streaks when only 15 per- cent Midvale was included. Table 20. — Addition of Eastern High-Volatile Coal to the Blend Run No. Coal used Shatter + 2" % 140 90% Orient 49.8 10% Pocahontas 122 65% Orient 63.4 25% Midvale 10% Pocahontas 122 65% Orient 63.4 25% Midvale 10% Pocahontas 167 65% Orient 70.4 173^% Midvale 173^2% Pocahontas 170 65% Orient 71.4 15% Midvale 20% Pocahontas Tumbler Stability %+l" Hardness % + M" Av. size in. 47.9 46.6 50 65.1 63.8 63.3 Breeze % of coal 2.63 2.65 2.73 2.1 2.0 2.6 App. gr. 37.412 67.4 2.20 2.6 0.774 47.9 65.1 2.63 2.1 0.815 0.815 0.824 0.811 48 ILLINOIS COAL FOR METALLURGICAL COKE Table 21. — Comparison of Ash Fusion Temperatures of Eastern and Illinois Coal Blends Run No. Coal blend Ash softening temp. °F. 2 3 37 42 41 54 2 16 37 24 53 89 90 Comparing eastern high-volatile with Illinois coal 70% Wharton (West Virginia)— 30% Pocahontas 70% Zeigler— 30% Pocahontas 70% Energy— 30% Pocahontas 70% Sahara 16—30% Pocahontas 70% Sahara 16 (Raw)— 30% Pocahontas 70% Sahara 4 and 5—30% Pocahontas Decreasing eastern— Increasing Illinois coal 70% Wharton— 30% Pocahontas 30% Wharton— 50% Energy^20% Pocahontas 70% Energy— 30% Pocahontas * 45% Wheelwright Slack— 20% Wheelwright Egg— 35% Pocahontas. . 45% Wheelwright Slack— 20% Orient— 35% Pocahontas 40% Wheelwright Slack— 25% Orient— 35% Pocahontas 25% Wheelwright Slack— 40% Orient— 35% Pocahontas 2120 2156 2240 2261 2308 2090 2120 2192 2240 2154 2341 2320 2333 Effect of Illinois Coal on Ash Fusion Ash fusion determinations were made on all cokes produced in the experimental oven. Fusion data were obtained on only a few of the individual coals used, but a compari- son of the fusion data on cokes from the various coal blends indicates the effect of Illinois coal on the ash fusion of the blends. In table 21 is shown a comparison of ash fusion data on similar blends of Whar- ton (West Virginia) and Illinois coals with Carswell-Pocahontas. The effect of replacing increasing percentages of Wheel- wright (eastern Kentucky) with Illinois coal is also shown. Examination of this table shows that all Illinois coal blends listed; with one exception, have higher ash fusion temperatures than do the correspond- ing blends of all-eastern coals. Table 22 contains further ash fusion data on cokes from similar blends of various Illinois coals. It is noted that blends con- taining No. 6 seam coals all produce cokes having ash fusion temperatures in approxi- mately the same range. No. 5 seam coals, with the exception of Sahara No. 16, pro- duce cokes having the lowest ash fusion temperatures of any of those tested. No. 16 Sahara coal, on the other hand, when blended with Pocahontas as shown produces cokes having exceptionally high ash fusions. SPECIAL TESTS From the preceding discussion of coking results in the pilot plant oven, it is obvious that studies of coal plasticity have played an important part in planning the experi- mental program and in interpreting the results obtained. Other special laboratory tests made in conjunction with the pilot plant studies have also contributed to the interpretation of experimental results, and their application to industrial situations. A discussion of these special tests follows. Plasticity Study Plastic properties of many of the indi- vidual coals and blends carbonized were studied. For this purpose, the Gieseler plastometer was used. The equipment was similar to the modified form of the Gieseler plastometer described by Brewer. 13 In order to obtain somewhat greater sensitiv- ity in the instrument, use was made of a smaller pulley on the dial than on the stirring head of the plastometer. The dial pulley was \\/\ inches in diameter and the stirring head pulley was \Y\ inches in PROCEDURES AND RESULTS Table 22.— Ash Im sion of Cokes prom Bi i ntds of Varioi s Illinois Coai s 40 Run No. 29 28 3 4 5 140 124 131 9 33 173 174 36 37 7 15 154 164 165 166 193 180 181 176 177 54 93 92 48 127 44 42 41 59 49 80 Coal Mend Ash softening temp. I'. No. 6 seam coals - 100% Zeigler 2358 80% Zeigler— 20% Pocahontas 2141 70% Zeigler— 30% Pocahontas 2156 60% Zeigler — 40% Pocahontas 21 60 50% Zeigler — 50% Pocahontas 2146 90% Orient 1—10% Pocahontas 2309 85% Orient 1— 15%Pocahontas 2232 75% Orient 1—25% Pocahontas 2224 60% Orient 1 — 40% Pocahontas 2140 60% Orient 1—40% Pocahontas 2237 80% Jefferson No. 20—20% Pocahontas 2158 60% Jefferson No. 20—40% Pocahontas 2212 70% Energy No. 5—30% Pocahontas 2188 70% Energy No. 5—30% Pocahontas 2240 60% Energy No. 5—40% Pocahontas 2131 60% Energy No. 5—40% Pocahontas 2135 80% Old Ben No. 11—20% Pocahontas 2207 60% Old Ben No. 11—40% Pocahontas 2183 80% Old Ben No. 14—20% Pocahontas 2272 60% Old Ben No. 14—40% Pocahontas 2241 No. 5 seam coals 100% Harco 2124 80% Harco— 20% Pocahontas 2070 60% Harco— 40% Pocahontas 2095 80% Buckhorn— 20% Pocahontas 2063 60% Buckhorn— 40% Pocahontas 2148 70% Sahara 4 and 5—30% Pocahontas 2090 25% Sahara 4 and 5—65% Orient— 10% Pocahontas 2171 15% Sahara 4 and 5—75% Orient— 10% Pocahontas 2202 90% Sahara 16—10% Pocahontas 2446 85% Sahara 16—15% Pocahontas 2390 80% Sahara 16—20% Pocahontas 2353 70% Sahara 16—30% Pocahontas 2261 70% Sahara 16 (Raw)— 30% Pocahontas 2308 65% Sahara 16 — 35% Pocahontas 2323 60% Sahara 16-40% Pocahontas 2299 40% Sahara 16—60% Orient 2242 diameter. This differs from the Russell- Soth modification in which the two pulleys are the same size, being 1% inches in diameter. 11 By using different sized pulleys, the maximum fluidity readings obtained are somewhat higher than with the Russell - Soth modification. However, this differ- ence does not appear to he in direct ratio to the sizes of the pulleys of the two instru- ments. 50 ILLINOIS COAL FOR METALLURGICAL COKE Table 23. — Gieseler Plasticity Data for Individual Coals Description County No. samples Softening temp. °C. Fusion temp. °C. Max. fluidity temp. °C. Solidi- fication temp. °C. Max. fluidity dial Div./Min. Illinois Coals Orient No. 1 No. 6 seam i\W xM" Washed) Orient No. 1 No. 6 seam (2" xVs" Washed) Orient No. 2 No. 6 seam (2" x V 8 " Washed) Old Ben No. 11 No. 6 seam (2" x23^" Washed) Old Ben No. 14 No. 6 seam (3" x 2" Washed) Zeigler No. 1 and 2 No. 6 seam W *%" Washed) Jefferson No. 20 No. 6 seam {Wl" *H" Raw) Sahara No. 4 and 5 . . . . No. 5 seam (3" x \y 2 " Washed) Sahara No. 16 No. 5 seam (6" x 28 mesh Washed) Sahara No. 16 No. 5 seam (3" x 2" Washed) Buckhorn No. 5 seam 0H"xM" Washed) Franklin Franklin Franklin Franklin Franklin Franklin Jefferson Saline Saline. Saline. Williamson Harco No. 47 No. 5 seam (3" x 2" Washed) Other Coals Pocahontas-Carswell . . . No. 3 seam Pocahontas-Inland Steel No. 3 seam Glen Rogers Beckley seam Eccles Beckley seam Saline. McDowell- West Virginia McDowell- West Virginia Wyoming- West Virginia Raleigh- West Virginia 378 409 445 4 4 372 av. 407 av. 422 av. 448 av. 11.1 av. 387 401 417 444 18.4 371 405 418 442 13.3 358 403 419 439 12.1 361 403 413 438 8.8 402 420 449 43.5 367 404 422 453 23.4 382 419 430 459 20.5 375 411 423 453 7.5 363 390 414 456 345 360 397 426 455 52 437 av. 467 av. 475 av. 492 av. 13.8 av. 419 456 465 499 14.7 411 av. 441 av. 466 av. 498 av. 81 av. 420 455 472 502 62 PROCEDURES AND RESl LTS Table 23.— (Concluded) 51 Description County No. samples Softening Fusion temp. °C. temp. °C. Max. fluidity temp. °C. Solidi- fication temp. C. Max. fluidit) dial ' Div./Min. Medium-Volatile No. 3 seam McDowell- West Virginia 1 382 414 450 483 1224 Buccaneer Carey seam Buchanan- Virginia 1 385 415 455 497 1840 Wheelwright Slack Elkhorn No. 3 seam Floyd- Kentucky 2 384 av. 415 av. 434 av. 462 av. 97.5 av. Wheelwright Egg Elkhorn No. 3 seam Floyd- Kentucky 1 382 407 432 466 590 Amherst Eagle Eagle seam Logan- West Virginia 1 371 401 437 479 8000 Wharton Hernshaw seam Boone- West Virginia 1 354 388 427 471 > 15000 Midvale No. 2 Gas seam Fayette- West Virginia 1 357 400 439 484 > 15000 The Gieseler plastometer gives the fol- lowing information : Softening Temperature — temperature (°C.) at which movement is 0.5 dial divisions per minute. Fusion Temperature — temperature (°C.) at which movement reaches 5.0 dial divisions per minute. Maximum Fluidity Temperature — temperature (°C.) of maximum rate of dial movement. Solidification Temperature — temperature (°C) at which dial movement stops. Maximum Fluidity — maximum rate of dial movement in dial divisions per minute. It should be stated that duplication of results in our Gieseler plastometer is not sufficiently precise to warrant more than a qualitative interpretation. Gieseler plasticity data for certain indi- vidual coals used in the work of this project are tabulated in table 23. Unsuccessful at- tempts were made to secure such data for several other coals studied. In general, the Illinois coals tested, especially those from the No. 6 seam, show low fluidity. Poca- hontas No. 3 coals are in general also of low fluidity. The Medium-Volatile Poca- hontas has a much higher fluidity, whereas the high-volatile eastern coals such as Whar- ton, Amherst Eagle and Midvale arc also quite fluid. In this work it has been found impossible to estimate fluidities of coal blends from known fluidities of the individual coals mak- ing up the blends. In table 24 comparison is made of determined and calculated Giese- ler data for several coal blends studied. Cal- culated values appearing in this table are weighted average values arrived at from known data for individual coals and known percent composition of the blends. It is seen readily that determined and calculated critical temperature values are not greatly different, but that determined and calculated maximum fluidities differ widely. The importance of plasticity data, as de- scribed above, for this work lies in the pos- sibility of its use in choosing proper coal blends and predicting the properties of coke to be made therefrom. Table 25 has been compiled by choosing six ranges of maximum fluidity of coal blends carbonized, and averaging character- istics of cokes made from coal blends ha\ ing fluidities within each range. The number of cases falling within each range as well as maximum and average deviations are shown. Unfortunately, insufficient data are available for a reliable correlation. The number of cases in each group is too small 52 ILLINOIS COAL FOR METALLURGICAL COKE 3 > rt ""3 4J Q c •-5 £ CO -6 4-1 Q .M . X 6 rt £> "If ■M U "2 Q bO r v J3-I "c3 U "2 Q C §4 «2 5 rJH o CO r^ vO VO ^ Tf -* oo r^ VO VO TF Th $ 3 f*. CN r^ o o CO CO 7— I CO *H TtH ^ TjH TJH CO CO o CO SO OS oo 1% CO CO CO CN CO "* TjH ^ tJH "tf <* -* <* 3 ? OS CN ON r-« OO h- CO CO co os rh \o r- CO CO M J* -^ OD O be ^ §g^^ %J1 cu CU W53 4^ 4-. .5 ^S rt rt U VO rt u 2 s -cun 2 _d-c.o *~^ -^J 3 '""Co O v> heelwrig leelwrig en Roge heelwrig heelwrig edium-V c o -C rt CJ Z *'§ E C - cu .3 rt c o u o'\^> cahonta ££o £££ U O^S £ 6c£ u Cu 6c£ 6c W J5g & j53Sp: S&&S ^S^ &S $&S c^ c^ ^ c£ ^ ^ ^ ^ ^ ^ v)ioo iflOvi vo o vo o o vo vo VO w-i wi VO LO VO CN tjH CO CO Tin cN CN vo CN OO CN OO T_l oo '"" ' OO 1—1 OO i—i r^ ON r^ "* -* vo r- °i VO VO oo ON CN CN CN CN PROCEDURES AND RESl f/ES 53 Tf oo vfi CO OS CO CN CO Os CO oo O _ OO ON OO oo © CO cs cn Os O cs CO 3 on vr> CN CN ^ "* * _ \o CO CN Tfrl "* u-> u-> ^n VO CN T— 1 cs CN ^ "^ rf Tf o VO r^ CN O o\ ^ tF CO •<* CO o oo r^ Os CO CO CO OO o\ f» OO CO CO vn CN VD >o CO CO g CO 1— 1 «-l CO S e CO . rt rt*Z3 cj ^ ol 3, rt cn « cd JLJcT} - J* U .U .U <~7 CO U °* -w ,„ rNo. ontas ontas- k5 <* d CO W be o> c c c <" c c £ c £ C herst eelwr n Ro; m O o3 c * vo Wl vO l"» f* r^ 54 ILLINOIS COAL FOR METALLURGICAL COKE 3 o CO ON o ON rt > oo CN ^H oo w-> Tf CN '-' o on *3 ON oo 7h u Q cn •^ ^ d -* ^ d d so 8^ cn 3 ;§< TlH -- 1 CN CN CO CO d o ON on 2 *> Q 3 r-~ CN 2 «5 CO r- oo >* CN On CO r— ' CO o 7h § so CN LT) x^' to ^ d o 8- 1—1 S 1) O CO 00 oS 3 CO CO vn NO O ON ?— i sO CN oo U r-~ oo CN VO On r- CO CN CN SO oo to \o r-- 3 w ON h CN CN u C . OO sO O cs CO tO CN o i— i o < o > 05 "S< CN d oo WO d d d d DC U On en . 4-1 > CO w On ft CN ON O oo -* oo ^ o CN o ui § TjH d CN r-~ d d d d o oL U b=,<^ Q < rf 3 NO oo -* VD r~- 1-1 5 to £ c . to r~~ "^ , — i wo CO CN i— i CN o j >> .2 > to CO i— 1 CO CN CN CN d d •3 Q 2 '3 On £3 > Q 3 CN OO -1 s On CO vO rt^' *f" xf d o _) qo - ^ o < a to T^ 3 . to ON O ^ CN o 1— 1 O O .2 > "* CO ^ ^ <* d d O U 1 On o> si s 7h r> x* CO CO CN CN OO oo CO o CO CN o so CN O to CN S*n SO W ,-H t2 3 CN so CN 3 . .2 > SO T-H oo »o © ON rJH T-H CO O ^ CN CN ^ ^ CO d o 00 '> r- On £ «*< CO r^ CO o f* VO so to to co o OnL_, S CO r^ CN r^ ^h" d CN 1-H or- y— < '-"' 1—1 co On 3 n SO r-» CN 00 d Oh Pl -3 CO co CO CO < w < PROCEDURES AND RESULTS 55 and maximum deviations are large. Further- more, no attention has been given to other variables in compiling this table. For these reasons, application of generalizations ap- pearing in these data to individual cases should be made with caution. However, certain trends do appear which would seem to be worthy of further confirmation. The two trends which are most evident in this table are: 1. As the maximum fluidity of the blend increases, the percentage of breeze decreases. 2. As the maximum fluidity of the blend increases, the apparent specific gravity in- creases. Carbon and Hydrogen Determinations on Cokes Carbon and hydrogen determinations were made on most of the cokes produced in the first 95 pilot plant runs using micro methods. Data obtained are tabulated and compared with volatile matter and final coke temperature in table 33 of Appendix A. These analyses were made in order to learn whether such data could be used satisfac- torily in determining the end of the coking period. Variations in hydrogen content were found to be too small to permit the use of these data for this purpose, due probably to the fact that, with but few exceptions, carbonizing conditions fell with- in a limited range. In a few cases where operating temperatures were decidedly dif- ferent, corresponding changes in the hydro- gen content of the coke were shown. These tests were discontinued when it became ap- parent that no practical results were being obtained. Ash Analyses Ash analyses w T ere made on a number of individual coals and coal blends to deter- mine the general characteristics of the ash which would enter into the slag reaction in blast furnace operation. A few coke ash analyses also were made to compare with the ash from the coal blends, and good checks were obtained. In general, there is about the same ratio between acids and alkalies in the ash from Illinois coals tested as in the ash from the eastern high-volatile coals tested. Ash analyses are tabulated in table 26. BY-PRODUCTS Scope of By-Product Tests The examination of by-products was not complete. Primary emphasis of the project has been on the coke, and although all tars were tested in the laboratory, light oils and aqueous liquors were not collected. An out- line of the by-product tests that were made follows. gas The gas was metered and a continuous record of its heating value was obtained from the recording calorimeter. At 30- minute intervals during each run a small sample (usually 0.002 times the preceding half hour's make) was diverted into a 5 cu. ft. gas holder. The resulting composite gas sample was used to determine the heating value of the gas for that run. The locations of meter, calorimeter and gas holder are shown in figure 7, and data on gas yields and heating values are given in table 32, Part F, of Appendix A. LIGHT OIL Although the available equipment and personnel did not permit collection and examination of light oil, the composite gas samples from several runs were subjected to the freezing method of estimating light oil. 15 The results were of the order of magnitude of half that obtained in com- mercial practice, and w T ere not significantly different for different blends of coal, whether all-eastern coals or part Illinois coals. It is thought that two factors nia\ have contributed to these low values: loss of light oil in the gas purification train and low top temperature in the oven. It was not possible to investigate this phase of the problem in more detail. 56 ILLINOIS COAL FOR METALLURGICAL COKE C/5 , . CJ fct; <-0 O C 8** 3* IF < CO »-• CN "* ^ ^ o _H CO OO NO _ NO ^ o CN 1-1 oo to NO CN CO CN H CO t-H CO on -*< to r^ u S 3 '-3 °^ > ^3 © (V ^ HI pj ~ •sj S O iU "O T3 So <" CN ^> o W| UT) O CO U Tt CN CO C ^, r^ f ) u~> io w^ oom>o O CO CN i-hcOD ,— N C o c 6 1—1 4_, £w ^ oe u *&s o c 3 £ o 58 ILLINOIS COAL FOR METALLURGICAL COKE 50 3 w h la U g < a O co g.S > t«i < * p4 4-1 m UJ W O. rt £ c «-n -— ir^OO'— lOOcocsxO'fl'oOtNH O O ^o^oomooooooo^o -T-* 1 ^ "f -tf r-H CO CO < ~ " CO CO CO w, un vn ur> \0 tjm ON, ov OOO^O^OOOOOOOOOO' i^oooolooloooot^ooxooooa)a\^< ooo?2o°°oooooooooO' OOOiOToOOOOOOOlo^' w-> vO vO .A. vO.-i.vO vO ^O vO vO vO vO vOvDvO ooo wi u-> uo ■' ^ 7 7 vo .o co 7 7 J. tA J> ^ ^f ^ ^> °° °° J, J, uk ^ ^ 222s 6667 VO vO 'O ' CN CN > Oh Cm H 0%%-ss & **& " ti \00\00 Cm Cm Cm X X^PhCm U Cm ^ lli ^ CN CN IH^^A uuuus Cm Cm Cm Cm Jg ^^T^T^^r^^^ in >o >o >o _T v> ioco^ooootNLocor-vooo^cooor^TjHiocN CN CO O CO O ON O co CO OO CN CN hh(S PROCEDURES i.m) RESULTS 5<) TAR The tar samples from the tar separator (Jig. 7) were measured by volume and taken to the laboratory for moisture, free carbon, and specific gravity determinations. Sub- sequently, the dried tar was distilled to 350° C. in a 1-liter, short-necked distilling Mask analogous to the flask used in standard tar distillation procedures 1 ' 1 and the distil- late extracted and the extracts distilled for the determination of tar acids, bases, neu- trals, and naphthalene. Phenol, o- } in-, and />-cresols were determined where tar acid fractions were of sufficient size, and in a number of other cases the tar acids from similar carbonization runs were combined and the phenolic compounds were deter- mined on the combined samples. For the examination of these tars, modi- fications of standard and published proce- dures were developed to suit the needs of the problem and the size of samples available. For example, it is known that simple extrac- tion with aqueous alkali and acid does not give a clean-cut separation of the weak acids (phenols), weak bases, and the neu- trals, 17 and for this reason the somewhat involved extraction procedure was used. Inasmuch as the methods used have not been described elsewhere, they are given in considerable detail and with supplementary notes in Appendix B. Tabulated results of composition of tars tested are given in tables 34 and 35 of Ap- pendix A. Discussion of By-Product Tests An attempt has been made to ascertain whether changes in carbonizing conditions and composition of coal blends have caused any significant changes in tar properties. The following paragraphs with tabulated data indicate that certain trends are dis- tinguishable. It might be well to point out that the tar studies are subject to some error, due to the fact that each tar may have been contaminated by a small amount of tar which remained in the collecting system from the previous run. It is be- lieved, however, that such error was not great enough to affect the direction of trends herein noted. EFFECT OF CARBONIZING CONDITIONS ON TAR CHARACTERISTICS The trends observed in this phase of the investigation are in line with those usually noted in commercial coke oven operation. Table 27 presents data which support the following general conclusions: with increas- ing severity of carbonizing conditions, one may expect an increase in tar specific gravity and in naphthalene content, and a decrease in tar acids; the trend in "free carbon" may be upward, although the data are not con- clusive. The last two entries in this table compare the pilot oven tar with commercial tar (Koppers Company) for the same coal blend, and indicate that the tar in the com- mercial oven was subjected to considerably more drastic cracking conditions. EFFECT OF VARYING THE PROPORTIONS OF HIGH- AND LOW-VOLATILE COALS The runs made on various blends of all- eastern coals w T ere insufficient in number and of too low a range of blend composi- tion to warrant drawing conclusions. A number of comparisons are possible in cases where the percentage of Illinois high-vola- tile coal was changed w T hile operating con- ditions remained constant, and these are pre- sented in table 28. Tar yields and data are less reliable for the early runs than later when more ex- perience had been gained. An operating difficulty encountered on Run 125 affected tar results on that and several subsequent runs; these are excluded from comparisons. In general, it will be noted that specific giavity and naphthalene content show no significant trend in variation as the percent- age of high-volatile coal in the blend is decreased, but total tar yield and percent- age of acids in the tar decrease. The last group in the table comprises runs made on Mends containing only Illinois high-volatile coals. 60 ILLINOIS COAL FOR METALLURGICAL COKE -X OTl ^cS(S«oi-«-OiOU->u->OOO x -O v -OOO v O' OOMOOOOM(^^ONOOQOa\0\ClOiX(?\(>a\CT\0000000000000000000000«100000C)000000(»«)(»000000 OOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOOO OOOOOOOOI^-OOOr^I^w^u^uouovo^OOOOOOOOOOOOOOOOOOOOOOO W) w> "sD O ^O 'O vo "-O vO \D\00 ^O ^D ^D VD ^D VD VO ooooooooo OOOOOOOOOOOOOO^oOOOOO O OO v>0 U~> OO OO *o OO 8 <^ooo i ooo«oo77T OOOOOOL0OOOOOOOL0O^-l l ^ L n'7' C | 4r T < T' C i 1 '^ , C ) C , PhPh uuuuuuuu -*V P-iPhPhPhPhP^PhPh^ uu PhPh uuuuuu^^ PL, PL, P-| Ph Ph Ph ~ ~ fc % % % % fc OO OO UU xxxxxxxx uuu UUPhPhPh PhPl, « „ „ .^PhPmPh PHPn^-Hyy^^ J^vo vo ^ ^^^^^^^PhPhPhPh^^^^-^cOC/^c/} „PQjf_CPQPP ~ - " ~ £ C " ^ ^ ^° ^ ^ ^^^ ^^ 1 J?rJr? r J?^' ^* r £ 1 -?r4 T J?& N N N N N t-^i-^i-^O OW«OOffiKSS^^£$££^££c7)c/3c7)0000 NNO O O O O O CS(N r^r^r^vDVD^I^w^\ooooOOOOOv^\OOO^rtirrTf^^Ou^r^c^C^cOTtivort Z X u PC fc w H e/5 < *- s UJ a; o b < w H X < o -a c «&* > X o < o-9 E o CO o 2 /. rt u ■3 -< .2 J c ofe o c ^° > So P4 H en £> H CO c - o go > u o wx 3 £ < V ta — H CO O « >. H * o < rt ^ U * < H fc T3 N O s O _a | T3 c o vr> w-> OOOOOOOOOOOOOOOOOOQOOOCOOOCX)OOOOCX)00 OOOOOOOOOO OO OOO OO"!^ '■o o >^ i ^'i , oo v i'V i ^ ir i ir ' i ^7 r i c i l ^^A^n7o7777'A^7o7'A : »o^^^00 0000 O r ">A t "' cOO CU Q-i Oh D-i ^ < PL, ™. — ^ •£ a, ^ j£ S cu ^ c/3 2 2 cu Ph v> vj j^ w £ OOOOOOOOOOOOOOOOOO | if i 8 8 8 I > > > > 2 2 2 2 arranged alphabetically by coals used. It is cross-indexed. M A R I O N W A Y N E I J E F F E RSON i Jefferson 20 PERRY 7 j F R A N KLIN . . < Old Ben II Majestic 14} • i — m j. ' Zeigler I •Orient I AMI L_ T O N Old Ben 14 Zeigler Z% •Orient 2 ! gr cm — Energy 5 Buckhorn ! W I L.L.IAMSON J_ S A l_ I N E • Harco 47 • Sahara 16 Sahara Sahara 5 4 U M I O N J O H M SO N POPE Fig. 9. — Low-sulfur coal area of southern Illinois showing locations of mines sampled. [63] 64 ILLINOIS COAL FOR METALLURGICAL COKE Table 30. — Names and Sources of Coals Tested with Abbreviations Used Coal Designation Abbreviation County Amherst Eagle Buccaneer Buckhorn Corban Eccles Energy No. 5 Glen Rogers HarcoNo. 47 Jefferson No. 20 Kentucky White Ash Madison County Majestic No. 14 Medium- Volatile Pocahontas Midvale Minonk Old Ben No. 11 Old Ben No. 14 Orient No. 1 Orient No. 2 Petroleum Coke Pocahontas-Carswell Pocahontas-Inland Steel Pocahontas-Inland, D.P.C Sahara No. 5 (and No. 4 + No. 5) Sahara No. 16 Sahara No. 5 + No. 16 Saxton. . . . Wharton Wheelwright (egg) Wheelwright (slack) Zeigler No. 1 4- No. 2 AE Eagle W. Va. Logan Be Cary Va. Buchanan Bh 5 111. Williamson C Eastern Ec Becklev W. Va. Raleigh E5 6 111. Franklin GR Beckley W. Va. Wyoming H 5 111. Saline J 6 111. Jefferson KWA Adair Ky. Daviess MC 6 111. Madison M 6 111. Perry MVP Pocahontas 3 W. Va. McDowell Md No. 2 Gas W. Va. Fayette Mn 2 111. Woodford OB11 6 111. Franklin OB14 6 111. Franklin Ol 6 111. Franklin 02 6 111. Franklin PetC PC Pocahontas 3 W. Va. McDowell PI Pocahontas 3 W. Va. McDowell PDP S5 5 IU. Saline S16 5 111. Saline S516 5 111. Saline Sx IV Ind. Vigo Wn Hernshaw W. Va. Boone We Elkhorn 3 Ky. Floyd Ws Elkhorn 3 Ky. Floyd Z 6 111. Franklin APPENDIX A 65 Table 31. — Analyses of Coals and Coal Blends Part A. Coals — Proximate Analyses (On the "as received" basis) Mois- Volatile Fixed Ash % Total B.t.u. per lb. Lab. No. Coal ture matter carbon sulfur F.S.I. % % % % C-3585 Amherst Eagle 3.0 30.8 59.9 6.3 0.71 13962 8.0 C-4032 Buccaneer 0.9 21.3 66.3 11.5 1.51 13676 8.5 C-4151 Buckhorn (iy 2 "x%" Washed) 5.9 35.3 48.9 9.9 3.15 12343 4.0 C-3381 Corban (Raw) 4.2 33.3 53.7 8.8 1.24 12963 4.0 C-3967 Corban (Raw) 4.2 32.6 55.7 7.5 0.84 13374 6.0 C-3833 Eccles (^"xO Washed) 0.9 17.3 75.1 6.7 0.80 14516 9.0 C-3845 Eccles (^"xO Washed) 1.2 17.2 72.9 8.7 0.98 14067 8.5 C-3862 Eccles (^"xO Washed. Heat Dried.) 0.9 17.9 73.7 7.5 0.96 14316 9.0 C-3027 Energy No. 5 (3" x2" Raw) 7.6 34.2 48.5 9.7 0.63 11969 4.5 C-3040 Energy No. 5 (iy 2 "x %" Washed) 8.7 32.7 50.9 7.7 0.73 12144 4.5 C-3086 Energy No. 5 i\Yi" *%" Washed) 10.5 31.2 51.2 7.1 0.67 11960 5.0 C-3279 Energy No. 5 (IK2" x ^" Raw) 8.5 32.4 51.1 8.0 0.81 12163 5.0 C-3524 Glen Rogers (Mine Run— Raw) 0.9 18.8 70.1 10.2 0.98 13824 9.0 C-3532 Glen Rogers (Mine Run— Washed) 4.1 18.8 69.7 7.4 0.73 13784 9.0 C-3569 Glen Rogers (Float— 1.5 gr.) 1.1 19.1 74.3 5.5 0.73 14620 9.0 C-3579 Glen Rogers (Float — 1.4 gr.) 1.6 19.6 74.9 3.9 0.56 14872 9.5 C-3624 Glen Rogers (Mine Run— Raw Course Grind) 1.2 16.7 70.0 12.1 0.55 13437 7.5 C-3632 Glen Rogers (Mine Run— Washed) 2.9 17.7 70.9 8.5 0.75 13812 7.5 C-3704 Glen Rogers (Mine Run— Washed) 2.4 18.1 71.1 8.4 0.72 13900 9.0 C-3782 Glen Rogers (Mine Run— Washed) 4.4 17.6 69.7 8.3 0.72 13661 8.5 C-4175 Harco No. 47 (3" x 2" Washed) 6.8 32.2 53.8 7.2 1.83 12701 5.5 C-4139 Jefferson No. 20 (lK"xM"Raw) 8.7 30.8 51.8 8.7 1.16 11979 5.5 C-4158 Jefferson No. 20 (13^" * Z A" Float at 1.5 gr.) 9.0 32.7 51.2 7.1 1.15 12272 4.5 C-3986 Kentucky White Ash (Brazil Lower Block — Raw) 11.4 34.7 50.9 3.0 0.62 12510 2.5 C-3775 Madison County (3" x \y 2 "Raw) 15.5 29.1 43.9 11.5 1.26 10334 3.0 C-4182 Majestic No. 14 (3f x \y 2 " W ashed) 8.6 33.7 49.7 8.0 1.27 11956 4.0 C-3498 Medium- Volatile Pocahontas (Slack— Raw) 2.1 22.2 69.5 6.2 0.62 14518 9.0 C-3562 Medium- Volatile Pocahontas (Slack— Raw) 1.0 22.7 69.3 7.0 0.56 14506 9.0 C-3825 Medium- Volatile Pocahontas (Slack— Raw) 2.3 21.9 69.7 6.1 0.56 14492 9.0 C-3913 Medium- Volatile Pocahontas (Slack— Raw) 2.5 21.7 69.0 6.8 0.54 14265 9.0 66 ILLINOIS COAL FOR METALLURGICAL COKE Table 31. — Part A. — (Continued) Mois- Volatile Fixed Ash % Total B.t.u. per lb. Lab. No. Coal ture matter carbon sulfur F.S.I. % % % % C-3980 Medium- Volatile Pocahontas (Slack— Raw) 3.8 21.8 67.3 7.1 0.54 14014 9.0 C-4109 Medium-Volatile Pocahontas (Slack— Raw) 1.7 23.3 69.3 5.7 0.63 14541 9.0 C-3886 Midvale 2.1 34.9 57.6 5.4 0.75 14250 7.5 C-4094 Midvale 2.1 33.1 56.2 8.6 0.83 13513 7.0 C-4051 Minonk (4" x 2Y 2 "Hand Picked. Crushed and Screened to 13.4 32.8 46.8 7.0 1.38 11653 5 5 C-4079 Minonk (Same size as C-4051) 12.1 33.0 47.4 7.5 1.79 11767 5.5 C-4038 Old Ben No. 11 (2" x \Y 2 " Washed) 8.2 32.9 51.5 7.4 1.03 12088 6.0 C-4052 Old Ben No. 11 (2" x \y 2 " Washed) 7.6 33.5 51.2 7.7 0.95 12176 5.5 C-4081 Old Ben No. 11 (2" x \y 2 " Washed) 8.4 33.1 51.3 7.2 1.10 12185 5.5 C-4086 Old Ben No. 14 (3"x 2 "Washed) 8.6 32.4 51.7 7.3 0.98 12153 5.0 C-4116 Old Ben No. 14 (3" x 2" Washed) 8.1 33.4 50.7 7.8 1.11 12147 4.5 C-3045 Orient No. 1 {\y 2 " xM" Washed) 9.8 32.1 50.9 7.2 0.80 12067 5.0 C-3061 Orient No. 1 (2"x \y 2 " Washed) 9.3 33.1 50.4 7.2 0.73 12162 5.0 C-3067 Orient No. 1 (6" x 3" Washed) 8.0 33.0 51.3 7.7 0.88 12276 4.5 C-3123 Orient No. 1 WxO Air Cleaned) 8.8 31.4 50.6 9.2 0.92 11892 5.5 C-3129 Orient No. 1 WW *%" Washed) 8.6 32.3 52.4 6.7 0.98 12310 5.0 C-3154 Orient No. 1 Wx%" Washed) 9.0 32.5 52.1 6.4 0.84 12309 4.5 C-3195 Orient No. 1 W *%" Washed) 9.1 31.9 51.7 7. .3 0.65 12186 5.0 C-3313 Orient No. 1 (lM"x%" Washed) 8.1 33.2 52.1 6.6 0.80 12286 3.5 C-3441 Orient No. 1 Wx%" Washed) 9.4 31.7 51.3 7.6 0.78 12084 4.5 C-3470 Orient No. 1 W *%" Washed) 8.3 32.7 51.7 7.3 0.80 12260 5.0 C-3535 Orient No. 1 0- l A" x%" Washed) 8.5 32.5 51.6 7.4 0.81 12202 4.5 C-3561 Orient No. 1 (1M"xM" Washed) 8.9 32.6 51.2 7.3 0.78 12152 4.5 C-3625 Orient No. 1 (W x%" Washed) 8.1 32.5 52.0 7.4 0.80 12265 5.0 C-3640 Orient No. 1 (Wx%" Washed) 9.1 31.2 51.8 7.9 0.65 12047 5.5 C-3730 Orient No. 1 (13-2" xM" Washed) 8.9 31.6 52.6 6.9 0.76 12225 4.5 C-3750 Orient No. 1 (\ l A* xH" Washed) 8.7 31.4 51.9 8.0 0.75 12054 5.5 C-3791 Orient No. 1 (2" xV 8 " Washed) 9.7 31.3 51.3 7.7 0.79 12101 5.0 C-3887 Orient No. 1 (2" x^" Washed) 7.7 32.6 51.9 7.8 0.70 12377 5.0 C-3931 Orient No. 1 (2" x y 8 " Washed) 8.3 31.7 52.6 7.4 0.73 12252 5.0 C-3979 Orient No. 1 (2" x^" Washed) 8.1 32.3 52.4 7.2 0.84 12366 5.5 APPENDIX A 67 Table 31. — Part A. — (Continued) Lab. No. Coal Mois- ture % Volatile matter % Fixed carbon Ash % Total sulfur % B.t.u. per lb. F.S.I. Orient No. 1 W *%" Washed Weathered 6 months) Orient No. 1 (2" x^" Washed) Orient No. 1 (2" x %" Washed) Orient No. 1 (2" x y 8 " Washed) Orient No. 1 (2" xy 8 " Washed) Orient No. 2 (2" x%" Washed) Orient No. 2 (2" x^" Washed) Orient No. 2 (2" x^" Washed. Heat Dried) Petroleum Coke ( — 34" Screenings) Petroleum Coke 7.6 31.9 52.7 0.80 12315 4.0 Pocahontas-Carswell Pocahontas-Carswell Pocahontas-Carswell Pocahontas-Carswell Pocahontas-Carswell Pocahontas-Carswell Pocahontas-Carswell Pocahontas-Carswell Pocahontas-Inland DPC Pocahontas-Inland Steel Pocahontas-Inland Steel Pocahontas-Inland Steel Pocahontas-Inland Steel Sahara No. 4 and 5 (3" xiy 2 " Washed) C-3459 Sahara No. 4 and 5 (3" x 1W Washed) C-3752 Sahara No. 5 (3" x 2" Washed) C-3314 Sahara No. 16 (6" x 1" Hand Picked) C-3324 Sahara No. 16 (3"x 1" Washed) C-3399 Sahara No. 16 (3" x 1" Washed) C-3515 Sahara No. 16 (6" x 28 mesh Washed) C-3641 Sahara No. 16 (6" x \y 2 " Raw) C-3805 Sahara No. 16 (3" x V/ 2 " Washed) C-3914 Sahara No. 16 (3" x 2" Washed) C-3542 75% Sahara No. 16 25% Sahara No. 5 (6" x 28 mesh Washed) C-3724 Saxton (2" x \\i" Raw) C-4065 Saxton {2"x\y Raw) 8.9 32.5 51.4 7.2 0.91 12202 5.0 8.1 32.9 51.5 7.5 0.81 12263 5.5 8.9 31.7 51.8 7.6 0.64 11970 5.0 8.6 31.4 52.8 7.2 0.79 12234 4.5 8.6 32.6 52.6 6.2 1.07 12424 3.0 7.0 31.9 53.5 7.6 1.12 12432 5.0 6.6 32.5 53.6 7.3 0.92 12559 4.0 4.9 12.9 82.0 0.2 2.53 14994 1.0 4.4 12.9 82.5 0.2 2.44 15008 1.0 2.9 17.7 73.2 6.2 0.67 2.0 16.5 75.5 6.0 0.66 i4494 9'6 2.6 16.2 74.4 6.8 0.72 14294 1.9 16.5 75.9 5.7 0.62 14587 9'6 2.9 17.2 74.2 5.7 0.61 14349 9.0 2.8 16.4 74.4 6.4 0.65 14251 9.0 2.0 17.5 74.1 6.4 0.61 14338 9.0 1.7 16.8 74.3 7.2 0.72 14345 8.5 4.2 17.5 69.4 8.9 0.73 13471 7.0 3.0 17.1 71.6 8.3 0.59 13972 9.0 4.4 17.2 69.5 8.9 0.60 13633 9.0 4.0 16.2 71.9 7.9 0.55 13863 9.0 4.0 17.1 70.4 8.5 0.55 13758 9.0 7.1 33.6 52.1 7.2 1.69 12617 5.5 5.8 34.0 52.0 8.2 2.01 12669 6.0 6.2 32.7 52.4 8.7 2.49 12497 5.5 7.7 31.8 54.1 6.4 0.63 12622 4.5 7.4 31.2 55.5 5.9 0.69 12781 4.5 7.9 32.1 53.8 6.2 0.82 12658 5.5 7.5 31.9 54.2 6.4 0.93 12719 5.0 5.5 30.6 54.1 9.8 1.07 12397 5.0 8.4 30.3 54.7 6.6 0.74 12562 5.5 8.3 30.1 52.8 8.8 0.78 12215 5.0 8.6 31.5 52.6 7.3 1.30 12365 5.5 14.4 30.9 47.9 6.8 0.55 11505 4.0 13.5 31.9 48.1 6.5 0.62 11601 5.5 68 ILLINOIS COAL FOR METALLURGICAL COKE Table 31. — Part A. — (Concluded) Lab. No. Coal Mois- ture % Volatile matter % Fixed carbon % Ash % Total sulfur % B.t.u. per lb. F.S.I. C-2936 Wharton C-3790 Wharton C-3508 Wheelwright Egg (4" x 2" Raw) C-3533 Wheelwright Egg (4" x 2" Raw) C-3554 Wheelwright Egg (4" x 2" Raw) C-3573 Wheelwright Egg (4" x 2" Raw) C-3631 Wheelwright Egg (4" x 2" Raw) C-3706 Wheelwright Egg (4" x 2" Raw) C-3777 Wheelwright Egg (4" x 2" Raw) C-3941 Wheelwright Egg (4" x 2" Raw) C-3439 Wheelwright Slack (2" x Raw) C-3450 Wheelwright Slack (2" x Raw) C-3497 Wheelwright Slack (2" x Raw) C-3523 Wheelwright Slack (2" x Raw) C-3555 Wheelwright Slack (2" x Raw) C-3565 Wheelwright Slack (2" x Raw) C-3577 Wheelwright Slack (2" x Raw) C-3623 Wheelwright Slack (2" x Raw) C-3636 Wheelwright Slack (2" x Raw) C-3705 Wheelwright Slack (2" x Raw) C-3711 Wheelwright Slack (2"xORaw) C-3739 Wheelwright Slack (2" x Raw) C-3776 Wheelwright Slack (2" x Raw) C-3802 Wheelwright Slack (2" x Raw) C-3847 Wheelwright Slack (2" x Raw) C-3861 Wheelwright Slack (2" x Raw. Heat Dried) C-3943 Wheelwright Slack (2"x0 Raw) C-3012 Zeigler No. 1 and 2 (3" x 2" Washed) C-3230 Zeigler No. 1 and 2 (3" x 2" Washed) C-4016 Zeigler No. 1 and 2 (Wx%" Washed) C-4026 Zeigler No. 1 and 2 W x K" Washed) 2.0 3.3 4.1 35.1 32.8 35.6 56.4 57.8 57.7 6.5 6.1 2.6 0.88 0.84 0.67 13952 14165 6.6 5.5 3.0 36.3 58.3 2.4 0.73 14327 5.0 4.4 34.8 57.3 3.5 0.84 13927 5.0 3.5 34.8 58.5 3.2 0.78 13904 5.0 4.7 34.8 57.0 3.5 0.81 13919 6.0 4.3 34.1 58.8 2.8 0.81 14109 6.0 4.4 34.8 57.9 2.9 0.71 14099 5.0 3.4 36.3 57.5 2.8 0.79 14248 5.5 5.8 32.0 56.5 5.7 0.86 13306 5.0 4.5 33.5 55.1 6.9 0.96 13356 5.0 4.7 33.3 55.4 6.6 0.88 13376 5.0 5.4 31.8 55.8 7.0 0.81 13126 4.5 4.3 32.5 55.5 7.7 0.92 13192 4.5 5.8 31.3 55.7 7.2 0.94 13096 5.0 6.5 31.2 55.5 6.8 0.82 13042 5.0 3.6 33.8 57.6 5.0 0.79 13805 5.0 6.3 31.9 55.3 6.5 - 0.82 13132 4.5 4.2 31.6 57 2 7.0 0.94 13382 5.5 3.4 32.9 56.5 7.2 0.90 13454 5.5 5.2 32.7 56.4 5.7 0.79 13487 6.0 5.1 31.2 56.8 6.9 0.80 13298 5.0 4.7 32.4 56.5 6.4 0.94 13416 4.5 3.1 33.0 60.0 3.9 0.85 14060 5.0 2.7 34.3 59.9 3.1 0.71 14307 5.0 3.2 36.2 56.8 3.9 0.82 14094 5.0 9.6 32.5 50.1 7.8 0.79 12078 3.5 8.7 31.5 53.0 6.8 0.73 12256 4.5 8.3 31.9 52.5 7.3 0.97 12207 5.0 8.1 32.0 53.0 6.9 0.82 12304 5.0 APPENDIX A 69 Table 31. — Analyses of Coals and Coal Blends Part B. Coals — Ultimate Analyses (On the "moisture and ash free" basis) Lab. No. Coal Hydrogen % Carbon % Nitrogen % Oxygen % Sulfur % C-3585 Amherst Eagle 5.62 86.47 1.58 5.55 0.78 C-4032 Buccaneer 5.39 87.30 1.43 4.15 1.73 C-4151 Buckhorn {W *%" Washed) 5.98 79.29 1.73 9.26 3.74 C-3833 Eccles (^"xO Washed) 4.92 90.58 1.63 2.01 0.86 C-3532 Glen Rogers (Mine^Run— Raw) 4.89 89.17 1.60 3.24 1.10 C-3532 Glen Rogers (Mine Run— Washed) 4.76 89.70 1.64 3.07 0.83 C-4175 Harco No. 47 (3" x 2" Washed) 5.80 81.42 2.05 8.60 2.13 C-4139 Jefferson No. 20 (lH*xM ff Raw) 5.57 81.84 1.89 9.30 1.40 C-3986 Kentucky White Ash (Brazil Lower Block — Raw) 5.96 80.77 1.71 10.84 0.72 C-3775 Madison County (3" x \y 2 " Raw) 5.48 80.40 1.59 10.81 1.72 C-4182 Majestic No. 14 (3; r x 2 "Washed) 6.01 79.40 1.83 11.24 1.52 C-3498 Medium- Volatile Pocahontas (Slack— Raw) 5.27 89.86 1.31 2.88 0.68 C-3886 Mid vale 5.91 85.74 1.66 5.88 0.81 C-4051 Minonk (4" x 2Y 2 " Hand Picked, Crushed and Screened to 1 " x %") 5.97 80.92 1.49 9.89 1.73 C-4086 Old Ben No. 14 (3" x 2" Washed) 5.68 81.43 1.78 9.95 1.16 C-3441 Orient No. 1 W *%" Washed) 5.63 81.92 1.79 9.72 0.94 C-3778 Orient No. 2 (2" x %" Washed) 5.52 81.87 1.86 9.50 1.25 C-3440 Pocahontas-Inland Steel 4.86 90.64 1.21 2.63 0.66 C-3513 Pocahontas-Carswell 4.74 90.87 1.40 2.27 0.72 C-3400 Sahara No. 4 and 5 (3" x \y 2 " Washed) 5.51 82.24 1.96 8.32 1.97 C-3399 Sahara No. 16 (3" xl" Washed) 5.50 82.95 2.00 8.59 0.96 C-3515 Sahara No. 16 (6" x 28 mesh Washed) 5.61 82.72 1.99 8.60 1.08 C-3724 Saxton (2"xlM' / Raw) 5.65 81.40 1.84 10.41 0.70 C-3533 Wheelwright Egg (4" x 2" Raw) 5.70 85.02 1.64 6.87 0.77 C-3439 Wheelwright Slack 5.66 84.74 1.56 7.07 0.97 C-4016 Zeigler No. 1 and 2 (1^'xM" Washed) 5.71 81.12 1.82 10.20 1.15 70 ILLINOIS COAL FOR METALLURGICAL COKE Table 31. — Analyses of Coals and Coal Blends Part C. Coal Blends— Proximate Analyses (On the "as received" basis) Run No. Mois- Volatile Fixed Ash % Total Coal blend ture matter carbon sulfur % % % % B.t.u. per lb. F.S.I. 1 and 2 70% Wharton 30% Pocahontas-Carswell 3 70% Zeigler No. 1 and 2 (3" x 2" Washed) 30% Pocahontas-Carswell 4 60% Zeigler No. 1 and 2 (3"x2" Washed) 40% Pocahontas-Carswell 5 50% Zeigler No. 1 and 2 (3" x 2" Washed) 50% Pocahontas-Carswell 6 60% Energy No. 5 (3" x 2" Raw) 40% Pocahontas-Carswell 7 60% Energy No. 5 (IK" x^" Washed) 40% Pocahontas-Carswell 8 60% Energy No. 5 (IK" x Vs" Washed) 40% Pocahontas-Carswell 9 60% Orient No. 1 (IK" xM" Washed) 40% Pocahontas-Carswell 10 60% Orient No. 1 (2" x IK" Washed) 40% Pocahontas-Carswell 11 60% Orient No. 1 (6" x 3" Washed) 40% Pocahontas-Carswell 12 55% Orient No. 1 (IK" xM" Washed) 45% Pocahontas-Carswell 13 60% Energy No. 5 (IK " *¥*" Washed) 40% Pocahontas-Carswell 14 60% Energy No. 5 (IK" *%" Washed) 40% Pocahontas-Carswell 15 60% Energy No. 5 (IK" x^" Washed) 40% Pocahontas-Carswell 16 50% Energy No. 5 (IK" x^" Washed) 30% Wharton 20% Pocahontas-Carswell 17 60% Orient No. 1 (^"x0 Air Cleaned) 40% Pocahontas-Carswell 2.6 30.3 60.7 6.4 0.97 14063 6.0 7.7 27.5 57.3 7.5 0.88 12566 3.0 6.7 26.0 60.7 6.6 0.77 13011 2.5 5.7 24.1 63.7 6.5 0.74 13319 3.0 5.3 26.3 60.7 7.7 0.64 13109 3.0 5.8 26.6 60.9 6.7 0.70 13150 2.5 4.7 6.3 25.7 62.0 6.0 0.69 13220 3.5 6.4 26.3 60.4 6.9 0.70 13046 3.5 6.6 27.2 59.2 7.0 0.76 13010 3.0 7.0 25.5 60.0 7.5 0.74 12899 3.0 6.1 24.8 60.7 6.7 0.64 12830 3.0 5.5 26.0 61.8 6.7 0.65 13214 3.0 5.4 28.3 60.4 5.9 0.78 13405 5.0 6.2 25.4 60.4 8.0 0.83 12871 3.0 APPENDIX A 71 Table 31. — Part C. — (Continued) Run No. Coal blend Mois- ture % Volatile matter % Fixed carbon % Ash % Total sulfur % B.t.u. per lb. 1 -S.I. 90% Orient No. 1 (1 ^"Washed) 10% Petroleum Coke 19 80% Orient No. 1 (1^'xr Washed) 20% Petroleum Coke 20 85% Orient No. 1 d^xM" Washed) 15% Petroleum Coke 21 80% Orient No. 1 (W *%» Washed) 20% Petroleum Coke 22 80% Orient No. 1 (IWxW Washed) 20% Petroleum Coke 23 20% Wheelwright Egg 45% Wheelwright Slack 35% Pocahontas-Inland Steel 24 20% Wheelwright Egg 45% Wheelwright Slack 35% Pocahontas-Inland Steel 25 60% Orient No. 1 CWxM" Washed) 40% Pocahontas-Carswell 26 60% Orient No. 1 W xM" Washed) 20% Wharton 20% Petroleum Coke 27 60% Orient No. 1 W *%" Washed) 20% Pocahontas-Carswell 20% Petroleum Coke 28 80% Zeigler No. 1 and 2 (3" x 2 "Washed) 20% Pocahontas-Carswell 29 100% Zeigler No. 1 and 2 (3" x 2" Washed) 30 20% Wheelwright Egg 50% Wheelwright Slack 30% Pocahontas-Inland Steel 31 20% Wheelwright Egg 50% Wheelwright Slack 30% Pocahontas-Inland Steel 32 60% Orient No. 1 (W *%" Washed) 40% Pocahontas-Carswell (V 8 of 1% oil added) 33 60% Orient No. 1 (W x H" Washed) 40% Pocahontas-Carswell (No oil added) 8.0 30.4 55.5 6.1 1.14 12567 4.5 8.4 27.9 57.9 5.8 1.23 12651 3.5 7.7 30.0 56.2 6.1 1.10 12701 4.0 7.9 28.2 58.6 5.3 1.13 12853 3.5 8.2 27.7 58.4 5.7 1.12 12772 3.0 3.8 28.5 62.0 5.7 0.71 13927 6.0 2.5 28.4 63.9 5.2 0.64 14148 6.0 6,0 25.9 61.6 6.5 0.72 13120 3.0 5.7 29.1 59.3 5.9 1.13 13198 3.5 6.0 25.5 62.9 5.6 1.11 13249 2.0 7.5 28.8 57.0 6.7 0.70 12657 4.0 9.0 31.1 53.0 6.9 0.55 12188 3.0 2.7 29.5 61.7 6.1 0.80 13904 5.0 3.0 7.1 26.4 59.6 6.9 0.80 12933 2.5 5.5 25.6 62.2 6.7 0.70 13138 3.0 72 ILLINOIS COAL FOR METALLURGICAL COKE Table 31. — Part C. — (Continued) Run No. Coal blend Mois- ture % Volatile matter % Fixed carbon % Ash % Total sulfur % B.t.u. per lb. F.S.I. 34 75% Corban 25% Pocahontas-Inland DPC 3.5 28.1 60.3 8.1 0.76 13388 4.0 35 75% Corban 25% Pocahontas-Inland DPC 3.8 .... ... .... 36 70% Energy No. 5 {\y 2 " x %" Raw) 30% Pocahontas-Carswell 6.6 27.7 58.1 7.6 0.76 12757 3.5 37 70% Energy No. 5 i\W xV 8 " Raw) 30% Pocahontas-Carswell 7.0 26.6 58.5 7.9 0.78 12586 3.0 38 75% Corban 25% Pocahontas-Inland DPC 3.9 31.0 58.4 6.7 0.84 13513 4.5 39 75% Corban 25% Pocahontas-Inland DPC 2.8 .... .... ... .... ... 40 80% Orient No. 1 5.9 27.9 60.4 5.8 1.15 13012 2.0 dH' *%" Washed) 20% Petroleum Coke 41 70% Sahara No. 16 (6"xl" Raw, Hand Picked) 30% Pocahontas-Carswell 42 70% Sahara No. 16 (3" xl" Washed) 30% Pocahontas-Carswell 43 80% Sahara No. 16 (3* xl" Washed) 20% Petroleum Coke 44 80% Sahara No. 16 (3" x 1" Washed) 20% Pocahontas-Carswell 45 80% Corban 20% Pocahontas-Inland DPC 46 80% Corban 20% Pocahontas-Inland DPC (Blend reground) 47 90% Sahara No. 16 (6"x 1" Raw, Hand Picked) 10% Pocahontas-Carswell 48 90% Sahara No. 16 (3"xl" Washed) 10% Pocahontas-Carswell 49 60% Sahara No. 16 (3"x 1" Washed) 40% Pocahontas-Carswell 50 40% Orient No. 1 (WxM" Washed) 25% Wheelwright Slack 35% Pocahontas-Inland Steel 51 40% Orient No. 1 W x%" Washed) 30% Wheelwright Slack 30% Pocahontas-Inland Steel 5.8 27.2 60.9 6.1 0.63 13204 3.5 5.0 27.4 62.0 5.6 0.72 13369 3.5 6.1 27.6 61.2 5.1 1.07 13292 3.0 6.2 28.5 59.4 5.9 0.86 13113 4.5 3.2 29.9 58.7 8.2 1.08 13376 3.0 2.9 30.5 58.1 8.5 1.06 13337 3.5 6.0 30.4 57.1 6.5 0.78 12837 3.5 6.8 30.1 57.1 6.0 0.78 12915 3.5 5.4 26.1 62.7 5.8 0.74 13419 3.5 5.2 27.5 59.6 7.7 0.78 13109 3.0 4.8 28.3 59.5 7.4 0.81 13209 3.5 APPENDIX A 73 Table 31. — Part C. — (Continued) Run No. Coal blend Mois- ture % Volatile matter % Fixed carbon % Ash % Total sulfur % B.t.u. per lb. F.S.I. 52 53 20% Orient No. 1 (134" xM" Washed) 50% Wheelwright Slack 30% Pocahontas- Inland Steel 20% Orient No. 1 (W x %" Washed) 45% Wheelwright Slack 35% Pocahontas-Inland Steel 4.1 4.3 28.9 27.9 60.1 60.4 6.9 7.4 0.85 0.80 13454 13450 4 3.5 54 70% Sahara No. 4 and 5 (3" x 134" Washed) 30% Pocahontas-Carswell 55 25% Sahara No. 4 and 5 (3"x \y 2 " Washed) 40% Orient No. 1 (134" x %" Washed) 35% Pocahontas-Inland Steel 56 25% Sahara No. 4 and 5 (3" x 134" Washed) 40% Wheelwright Slack 35% Pocahontas-Inland Steel 57 25% Orient No. 1 (Wx%" Washed) 40% Wheelwright Slack 35% Medium-Volatile Pocahon- tas 58 25% Wheelwright Egg 40% Wheelwright Slack 35% Medium- Volatile Pocahon- tas 59 65% Sahara No. 16 (6" x 28 mesh, Washed) 35% Pocahontas-Carswell 60 80% Sahara No. 16 (6" x 28 mesh, Washed) 20% Pocahontas-Carswell 61 70% Wheelwright Slack 30% Glen Rogers (Raw) 62 25% Wheelwright Egg 50% Wheelwright Slack 25% Glen Rogers (Washed) 63 25% Orient No. 1 (134" x%" Washed) 45% Wheelwright Slack 30% Glen Rogers (Washed) 64 25% Orient No. 1 (134" x' 50% Wheelwright Slack 25% Glen Rogers (Washed) 4.4 29.5 58.6 7.5 5.7 27.8 58.6 7.9 3.9 27.7 60.9 7.5 4.4 29.5 59.5 6.6 3.0 29.8 62.0 5.2 5.6 26.0 62.0 6.4 6.0 28.9 58.5 6.6 2.9 28.5 60.9 7.7 3.2 29.9 60.7 6.2 5.0 27.9 60.1 7.0 5.2 28.9 59.9 6.0 1.67 13229 4.5 1.01 12890 4.5 1.10 13497 5.0 0.77 13510 6.0 0.66 14093 7.0 0.84 13265 3.0 0.88 13042 4.0 0.86 13589 5.0 0.85 13744 5.0 0.78 13275 3.5 0.80 13377 4.0 74 ILLINOIS COAL FOR METALLURGICAL COKE Table 31. — Part C. — (Continued) Run No. Coal blend Mois- ture % Volatile matter % Fixed carbon % Ash % Total sulfur % B.t.u. per lb. F.S.I. 65 65% Sahara 25% No. 5 (6" x 28 mesh, Washed) 75% No. 16 (6" x 28 mesh, Washed) 35% Pocahontas-Carswell 66 80% Sahara 25% No. 5 (6" x 28 mesh, Washed) 75% No. 16 (6" x 28 mesh, Washed) 20% Pocahontas-Carswell 67 25% Wheelwright Egg 45% Wheelwright Slack 30% Glen Rogers (Washed) 68 25% Orient No. 1 (W>» x%" Washed) 40% Wheelwright Slack 35% Medium- Volatile Pocahon- tas 69 35% Wheelwright Egg 40% Wheelwright Slack 25% Medium- Volatile Pocahon- 6.2 26.0 60.6 7.2 1.04 13018 3.5 7.3 28.0 57.1 7.6 1.21 12675 4.5 3.8 29.0 60.4 6.8 0.83 13584 5.5 4.1 29.5 59.3 7.1 0.79 13466 6.0 3.5 31.4 59.1 6.0 0.82 13811 6.5 70 70% Wheelwright Slack 30% Glen Rogers (1.5 float) 71 25% Wheelwright Egg 40% Wheelwright Slack 35% Medium- Volatile Pocahon- 3.8 27.7 62.2 6.3 0.91 13725 5.5 3.2 30.0 60.6 6.2 0.73 13877 6.5 72 70% Wheelwright Slack 30% Glen Rogers (1.4 float) 73 25% Amherst Eagle 45% Wheelwright Slack 30% Glen Rogers (Washed) 74 25% Wheelwright Egg 55% Wheelwright Slack 20% Glen Rogers (Washed) 75 25% Wheelwright Egg 60% Wheelwright Slack 15% Glen Rogers (Washed) 76 25% Orient No. 1 (\W*W Washed) 45% Wheelwright Slack (Coarse Grind) 30% Glen Rogers (Washed) 4.4 27.2 62.9 5.5 0.78 13781 6.0 3.5 28.4 61.7 6.4 0.74 13757 6.5 3.5 30.1 60.5 5.9 0.81 13728 5.0 3.6 30.3 60.1 6.0 0.82 13703 5.5 3.9 28.7 60.2 7.2 0.78 13439 5.0 APPENDIX A 75 Table 31. — Part C. — (Continued) Run No. Coal blend Mois- ture % Volatile matter % Fixed carbon % Ash % Total sulfur % B.r.u. per lb. K.S.I. 77 -25% Orient No. 1 a; '2 X ^"Washed) 78 79 45% Wheelwright Slack (Fine Grind) 30% Glen Rogers (Washed) 70% Wheelwright Egg 30% Glen Rogers (Washed) 70% Wheelwright Slack 30% Glen Rogers (Washed) 80 80% Orient No. 1 W *%" Washed) 20% Sahara No. 16 (6" x \A" Raw) 81 70% Orient No. 1 (W *.%" Washed) 30% Sahara No. 16 (6" x W Raw) 82 60% Orient No. 1 (W xr Washed) 40% Sahara No. 16 06" x 13^ "Raw) 83 25% Wheelwright Egg 50% Wheelwright Slack 25% Glen Rogers (Washed) 84 25% Wheelwright Egg 50% Wheelwright Slack 25% Glen Rogers (Washed) 85 25% Orient No. 1 216° C. 1 2 27! 2 Y.2 '\'a 3 31.4 "i.i s.b 20.6 1.7 5.5 "?>'.'\ "lA 4 32.0 3.1 7.7 21.2 2.1 5.8 3.3 2.4 5 31.7 2.7 8.1 20.9 1.3 5.7 3.3 2.4 6 31.4 2.8 7.8 20.8 2.1 6.3 4.0 2.3 7 32.5 2.7 8.1 21.7 2.3 6.2 3.7 2.5 8 33.3 3.0 7.3 23.0 2.2 6.7 4.4 2.3 9 32.0 2.9 7.5 21.6 2.2 6.6 4.1 2.5 10 30.4 2.8 8.1 19.5 2.0 6.4 3.9 2.5 11 29.7 2.6 8.1 19.0 1.3 5.3 2.9 2.4 12 31.0 2.8 8.2 20.0 1.9 4.6 2.3 2.3 13 32.4 2.6 8.0 21.8 2.0 5.0 2.8 2.2 14 34.5 2.6 8.1 23.8 2.0 5.7 3.5 2.2 15 32.4 2.3 8.9 21.2 1.9 5.4 3.5 1.9 16 32.2 3.5 7.2 21.5 2.1 5.7 3.5 2.2 17 31.8 2.5 8.4 20.9 2.0 4.3 3.0 1.3 18 30.4 3.1 7.8 19.5 2.0 5.5 3.5 2.0 19 30.5 2.7 7.4 20.4 2.1 5.7 3.6 2.1 20 28.9 2.5 6.6 19.8 1.9 5.6 3.6 2.0 21 29.6 2.6 6.6 20.4 2.8 5.7 3.6 2.1 22 30.6 2.5 7.2 20.9 2.0 5.9 3.7 2.2 23 29.9 2.6 7.4 19.9 1.7 5.1 3.3 1.8 24 31.0 3.7 6.5 20.8 2.3 6.1 3.8 2.3 25 32.0 4.5 4.6 22.9 2.4 10.5 6.2 4.3 26 26.0 2.9 5.1 18.0 2.5 8.6 6.3 2.3 27 27.4 2.9 5.5 19.0 2.6 7.9 5.3 2.6 28 29.7 2.4 6.1 21.2 2.6 9.0 6.2 2.8 29 28.9 3.4 5.0 20.5 3.1 11.8 7.3 4.5 30 28.9 3.7 5.7 19.5 2.4 8.7 6.0 2.7 31 29.9 4.0 5.7 20.2 2.6 7.9 5.2 2.7 32 29.1 3.3 5.9 19.9 3.0 8.8 6.0 2.8 33 30.5 3.4 6.5 20.6 2.5 8.1 5.8 2.3 34 31.0 3.7 6.9 20.4 2.3 8.1 5.6 2.5 35 31.0 3.7 6.9 20.4 2.5 7.4 5.2 2.2 36 30.4 3.6 6.2 20.6 2.5 9.3 6.5 2.8 37 29.2 4.0 4.1 21.1 3.0 11.4 8.1 3.3 38 30.3 3.4 6.1 20.8 2.6 8.3 6.3 2.0 39 30.4 3.6 5.7 21.1 2.4 8.5 6.3 2.2 40 28.6 2.9 6.4 19.3 2.3 7.9 6.0 1.9 41 29.7 2.9 6.3 20.5 2.3 8.4 6.4 2.0 42 31.2 3.2 5.7 22.3 2.7 8.9 6.7 2.2 43 27.8 2.7 5.8 19.3 2.3 9.4 7.0 2.4 44 29.5 3.3 5.7 20.5 2.6 9.1 6.7 2.4 45 32.5 4.0 6.4 22.1 2.3 8.5 6.0 2.4 46 32.4 3.5 6.5 22.4 2.1 7.6 5.7 1.9 47 29.6 3.5 5.6 20.5 2.5 9.5 7.0 2.5 48 28.3 3.8 5.0 19.5 2.7 9.9 7.2 2.7 49 30.9 3.5 6.2 21.2 2.5 9.2 6.7 2.5 50 30.9 3.6 6.3 21.0 2.3 8.0 5.9 2.1 APPENDIX A Table 34. — Part B. — (Continued) 121 Run No. Neutrals Bases Acids Total Light oil CioHs Residue Total Total B.P.< 216° C. B.P.> 216° C. 51 31.9 2.7 6.5 22.7 2.6 8.3 5.9 2.4 52 31.9 3.8 6.4 21.5 2.3 8.3 5.8 2.5 53 Materia lost in laboratory acci dent. 54 32.6 3.2 6.1 23.3 2.5 7.6 5.4 2.2 55 32.9 3.8 5.8 23.3 2.5 6.9 4.9 2.0 56 33.5 3.4 5.9 24.2 2.6 6.1 3.9 2.2 57 30.7 3.7 5.3 21.7 2.1 5.2 2.7 2.5 58 31.2 4.3 5.6 21.3 1.9 5.0 3.1 1.9 59 34.0 3.8 6.6 23.6 2.5 5.6 3.5 2.1 60 31.6 3.4 5.6 22.6 2.5 6.9 4.2 2.7 61 32.4 3.4 6.0 23.0 2.1 5.9 3.3 2.6 62 33.8 3.9 6.1 23.8 2.1 5.7 3.4 2.3 63 34.3 4.3 6.6 23.4 2.1 5.7 3.3 2.4 64 34.1 4.5 6.5 23.1 2.2 5.9 3.2 2.7 65 33.3 3.7 6.9 22.7 2.2 4.5 2.6 1.9 66 33.4 3.9 6.8 22.7 2.5 5.8 3.3 2.5 67 34.8 4.4 6.6 23.8 2.1 5.3 3.0 2.3 68 32.4 3.8 6.2 22.4 2.0 5.1 2.8 2.3 69 32.3 3.7 6.2 22.4 2.0 5.1 2.8 2.3 70 33.3 4.3 6.2 22.8 1.9 4.7 2.7 2.0 71 32.0 4.1 6.1 21.5 1.9 5.1 3.0 2.1 72 33.4 4.1 6.5 22.8 1.9 4.9 2.6 2.3 73 32.8 4.2 6.4 22.2 1.8 4.6 2.6 2.0 74 33.0 4.4 6.4 22.2 2.0 5.2 3.0 2.2 75 33.2 4.2 6.4 22.6 2.0 5.6 3.4 2.2 76 33.8 4.2 6.4 23.2 2.1 6.7 4.3 2.4 77 32.9 4.3 6.2 22.4 2.1 7.2 4.6 2.6 78 32.1 4.2 6.0 21.9 2.1 7.2 4.7 2.5 79 33.0 4.0 6.3 22.7 2.0 6.9 4.7 2.2 80 31.3 4.1 5.5 21.7 2.7 10.0 6.6 3.4 81 31.1 4.1 5.3 21.7 2.7 11.4 7.5 3.9 82 32.1 4.2 5.0 22.9 2.2 12.1 8.1 4.0 83 32.0 4.3 5.5 22.2 2.9 9.9 6.8 3.1 84 32.4 3.9 6.5 22.0 2.1 8.3 5.7 2.6 85 33.8 3.8 6.1 23.9 2.3 8.6 5.5 3.1 86 34.1 3.7 6.7 23.7 2.5 8.1 5.2 2.9 87 32.8 3.8 6.0 23.0 2.3 8.3 5.5 2.8 88 32.8 3.3 6.8 22.7 1.9 6.3 4.2 2.1 89 33.3 3.6 7.0 22.7 2.2 6.7 4.5 2.2 90 33.2 3.4 7.0 22.8 2.3 7.2 4.8 2.4 91 32.0 3.6 7.0 21.4 2.1 6.6 4.6 2.0 92 31.6 3.8 6.2 21.6 2.5 9.0 6.0 3.0 93 31.3 3.5 6.0 21.8 2.5 9.3 6.2 3.1 94 31.2 3.8 5.8 21.6 2.5 9.6 6.8 2.8 95 31.2 3.6 6.0 21.6 2.5 8.9 6.2 2.7 96 31.1 4.2 5.6 21.3 2.6 10.1 6.8 3.3 97 30.9 4.1 5.9 20.9 2.6 10.0 6.8 3.2 98 32.9 4.5 6.8 21.6 2.3 8.0 5.7 2.3 99 32.0 3.8 6.0 22.2 2.2 7.7 5.5 2.2 100 30.1 3.8 5.7 20.6 2.0 7.0 5.0 2.0 122 ILLINOIS COAL FOR METALLURGICAL COKE Table 34. — Part B. — (Continued) Neutrals Bases Acids Run No. Total Light oil Ciori8 Residue Total Total B.P.< 216° C. B.P.> 216° C. 101 32.2 4.0 5.4 22.8 2.6 9.3 6.0 3.3 102 31.6 4.3 5.9 21.4 2.6 9.2 6.3 2.9 103 32.1 4.0 6.2 21.9 2.6 8.9 5.9 3.0 104 33.5 4.1 6.7 22.7 2.4 8.0 5.3 2.7 105 31.2 3.9 6.2 21.1 2.6 9.3 6.4 2.9 106 32.1 3.9 6.3 21.9 2.7 9.4 6.3 3.1 107 32.5 4.1 6.6 21.8 2.6 9.0 6.2 2.8 108 32.0 4.4 6.2 21.4 2.7 9.4 6.6 2.8 109 30.3 3.8 6.3 20.2 2.6 9.4 6.6 2.8 110 32.3 4.2 6.2 21.9 2.4 8.8 6.0 2.8 111 32.6 4.2 6.2 22.2 2.7 10.1 7.1 3.0 112 32.1 4.3 6.4 21 A 2.3 8.4 5.8 2.6 113* 31.3 3.7 6.4 21.2 2.1 6.9 4.6 2.3 H4a 32.8 4.1 5.8 22.9 2.2 7.2 4.5 2.7 115" 32.6 4.2 5.8 22.6 2.2 7.8 5.1 2.7 116* 31.7 3.7 6.3 21.7 2.1 6.8 4.3 2.5 117" 32.1 4.1 6.2 21.8 2.2 6.7 4.4 2.3 118* 31.9 4.0 6.0 21.9 2.2 7.4 4.9 2.5 119 a 32.2 4.1 6.2 21.9 2.1 7.3 4.8 2.5 120 a 31.3 3.9 5.7 21.7 2.3 6.5 4.1 2.4 121 a 31.8 4.2 6.3 21.3 1.9 6.8 4.5 2.3 122* 31.0 4.1 6.1 20.8 2.4 8.2 5.9 2.3 123 a 31.4 3.8 6.3 21.3 2.4 8.3 5.4 2.9 124" 32.4 3.8 6.6 22.0 2.5 7.7 5.9 2.8 125- 31.6 3.4 6.0 22.2 1.9 3.9 1.9 2.0 126* 33.0 3.8 6.2 23.0 2.6 6.3 3.4 2.9 127 32.9 3.6 6.6 22.7 2.6 7.0 4.6 2.4 128 32.2 3.6 6.7 21.9 2.9 7.7 5.1 2.6 129 29.3 3.2 5.8 20.3 2.6 8.0 5.6 2.4 130 32.8 3.7 6.2 22.9 2.8 8.7 5.7 3.0 131 31.8 3.4 6.8 21.6 2.6 8.3 5.6 2.7 132 31.0 3.5 6.8 20.7 2.3 7.3 5.1 2.2 133 30.5 3.6 6.3 20.6 2.1 7.2 4.9 2.3 134 30.5 3.9 6.0 20.6 2.4 8.3 5.4 2.9 135 31.6 3.3 7.0 21.3 2.2 6.6 4.6 2.0 136 31.9 3.7 6.8 21.4 2.0 6.5 4.0 2.5 137 32.0 3.5 6.4 22.1 2.2 6.7 4.3 2.4 138 30.9 3.7 6.1 21.1 2.5 8.2 5.5 2.7 139 31.5 3.8 6.2 21.5 2.6 9.2 6.0 3.2 140 31.4 3.8 6.2 21.4 2.6 9.7 b b b 141 31.6 3.7 6.3 21.6 2.4 9.2 6.2 3.0 142 32.7 3.9 6.7 22.1 2.4 8.4 5.6 2.8 143 31.2 4.0 6.1 21.1 2.4 9.0 6.0 3.0 144 31.5 3.7 6.4 21.4 2.4 8.8 5.9 2.9 145 31.3 3.7 6.4 • 21.2 2.3 8.6 5.8 2.8 146 29.8 3.4 5.8 20.6 2.3 8.0 5.3 2.7 147 29.8 3.1 6.1 20.6 2.3 7.6 5.1 2.5 148 31.5 3.8 5.5 22.2 2.5 9.2 5.8 2.4 149 31.0 3.2 5.9 21.9 2.5 9.1 6.2 2.9 150 30.8 3.3 6.4 21.1 2.2 6.5 4.1 2.4 a Due to operating conditions, results on runs 113 through 126 are less representative than the other runs listed. b Acids lost. Estimation of total acids based on assumption of loss on manipulation of 1.1%. APPENDIX A Table 34. — Part B. — (Concluded) 123 Run No. Neutrals Bases Acids Total Light oil CioHs Residue Total Total B.P.< 216° C. B.l\> 216° C. 151 31.0 3.3 6.3 21.4 2.3 6.8 4.4 2.4 152 32.0 3.6 6.2 22.2 2.6 7.8 4.8 3.0 153 30.2 4.0 5.5 20.7 2.5 8.7 5.7 3.0 154 33.0 4.0 6.1 22.9 2.6 9.3 6.1 3.2 155 31.5 3.9 5.9 21.7 2.6 9.8 6.5 3.3 156 31.9 4.1 5.9 21.9 2.5 9.1 5.9 3.2 157 32.8 4.3 6.1 22.4 2.5 9.2 5.8 3.4 158 30.8 4.2 5.3 21.3 2.5 10.2 6.5 3.7 159 30.4 3.7 5.8 20.9 2.1 9.1 5.7 3.4 160 30.7 4.0 5.6 21.1 2.0 8.4 5.1 3.3 161 31.0 3.7 6.5 20.8 2.0 7.3 4.5 2.8 162 32.5 4.1 6.5 21.9 2.3 8.1 3.4 4.7 163 32.9 3.6 6.6 22.7 2.0 7.5 4.4 3.1 164 33.8 3.8 6.9 23.1 2.2 7.6 4.7 2.9 165 32.1 4.1 6.4 21.6 2.4 9.9 6.2 3.7 166 34.1 3.9 6.2 24.0 2.4 9.7 6.2 3.5 167 32.3 3.9 5.8 22.6 2.4 9.7 6.5 3.2 168 31.5 4.0 5.9 21.6 2.5 9.7 6.5 3.2 169 Coke bui •ned on whai f. 170 32.8 3.9 5.8 23.1 2.4 9.5 6.1 3.4 171 31.9 3.8 5.7 22.4 2.3 9.8 6.6 3.2 172 30.0 4.1 5.6 20.3 2.3 9.8 6.6 3.2 173 31.6 3.7 5.8 22.1 2.5 10.0 6.7 3.3 174 33.8 3.1 6.9 23.8 2.3 7.6 4.7 2.9 175 32.5 3.6 6.0 22.9 2.4 8.6 5.4 3.2 176 32.1 4.6 6.2 21.3 2.2 8.9 5.7 3.2 177 33.8 4.3 6.5 23.0 2.2 8.2 5.2 3.0 178 32.6 3.9 6.1 22.6 2.5 9.8 6.3 3.5 179 32.7 3.5 6.7 22.5 2.6 9.0 6.2 2.8 180 31.9 3.7 6.4 21.8 2.5 8.6 5.8 2.8 181 32.2 3.4 6.4 22.4 2.4 7.8 5.4 2.4 182 32.9 3.6 6.9 22.4 2.6 8.5 5.7 2.8 183 35.8 3.7 7.6 24.5 2.4 6.5 3.9 2.6 124 ILLINOIS COAL FOR METALLURGICAL COKE Table 35. — Phenol and Cresol Content of Tars Values given are percentage by weight of dry tar. They were determined on samples obtained by combining the tar acid fractions from runs listed in the first column. Table 36. — Index to Coals Used in Experi- mental Coking Runs (See bottom of column 1) Coals Proportions blended Coking run numbers Amherst Eagle AE-GR-Ws 25-30-45 73 Run No. Phenol 0- Cresol Cresol P- Cresol Buccaneer Bc-Mn- MVP-PC 5-70-10-15 161 Bc-OBll 20-80 155 3,4,5 0.8 0.4 0.8 0.6 Bc-OBll- 6, 8, 13 0.9 0.4 0.8 0.6 PC 15-70-15 157 9, 10, 11, 12 0.9 0.4 0.9 0.6 Bc-OBll- 14,15 0.8 0.5 0.8 0.6 PC 10-80-10 156 19, 20, 21, 22 0.8 0.4 0.8 0.6 Buckhorn 23,24 0.9 0.4 0.8 0.6 Bh-PC 80-20 176 25 1.3 0.7 1.5 1.3 Bh-PC 60-40 177 29 1.6 0.8 1.6 1.1 Corban 30,31 1.2 0.6 1.2 0.9 C-Ol-PDP 50-25-25 135, 137 32,33 1.8 0.6 1.2 1.0 C-PDP 80-20 45,46 34, 35, 38, 39 1.4 0.3 1.0 0.7 C-PDP 75-25 34, 35, 38, 39, 136 37 2.0 0.9 1.8 1.3 Eccles 41,42 2.3 0.8 1.2 1.0 Ec-Ol 15-85 125 44, 47, 48 1.3 0.6 0.9 0.8 Ec-02-We- 45,46 1.7 0.6 1.2 1.0 Ws 25-25-18-32 110 49,54 1.4 0.7 1.1 1.0 Ec-02-Ws 25-25-50 113,114,115,116, 50, 51, 52 1.7 0.6 1.1 1.0 117 58, 69, 71 0.4 0.4 0.5 0.5 Ec-S16 15-85 128 59, 60, 65 0.6 0.5 0.5 0.5 Ec-We-Ws 25-25-50 112 61, 70, 72, 79 0.7 ( a ) ( a ) ( a ) Ec-Ws 25-75 118, 119, 120, 121 62, 67, 74, 75 0.5 0.4 0.6 0.5 Energy No. 5 63, 64, 76, 77 0.7 0.5 0.8 0.6 E5-PC 70-30 36,37 80, 81, 82 1.7 0.8 1.6 1.1 E5-PC 60-40 6, 7, 8, 13, 14, 15 83,84 1.7 0.7 1.1 0.9 E5-PC-Wn 50-20-30 16 88,91 1.6 0.6 1.1 0.9 Glen Rogers 92,93 1.7 0.6 1.2 1.0 GR-AE-Ws 30-35-45 73 102, 103 1.8 0.7 1.3 0.9 GR-Ol-Ws 30-25-45 63, 76, 77, 85, 104 106, 107, 109 1.9 0.7 1.3 1.0 GR-Ol-Ws 25-25-50 64 108, 138 1.6 0.7 1.2 0.9 GR-02-We- 113, 114, 116 1.0 0.5 0.9 0.8 Ws 25-25-18-32 99 115, 117 1.2 0.6 1.0 0.7 GR-We 30-70 78 118, 119 1.2 0.6 1.0 0.8 GR-We-Ws 30-25-45 67 127, 128, 129 1.1 0.6 1.0 0.8 GR-We-Ws 25-25-50 62, 83, 84 135, 137 1.2 0.5 0.9 0.7 GR-We-Ws 20-25-55 74 152, 153 1.2 0.6 1. 1 0.9 GR-We-Ws 15-25-60 75 154, 158 1.5 0.7 1.3 1.1 GR-Ws 30-70 61, 70, 72, 79 159, 160 1.3 0.5 1.1 0.8 Harco No. 47 H-PC H-PC 80-20 60-40 180 181 a Material lost in lab oratory ac cident Jefferson No. 20 J-MVP-PC 70-15-15 175 J-Ol-PC 40-40-20 179 J-PC 80-20 173, 178 J-PC 60-40 174 Kentucky White Ash Table 36. — Index to Coals Used in Experi- KWA-MVP 75-25 142 mental Coking Runs KWA-Ol- PC 25-65-10 139 Coals are li sted al phabetic ally by name. Madison Under each coa name ( mtry, th e coal b ends in County which it was us >ed are listed bj r abbreviations; MC-MVP- the next column these coals wen gives tl ; blende le perce d, and ntages in which the last column 01 Majestic No. U M-PC 20-20-60 80-20 101 182 gives serial nui nbers o f experimental runs in M-PC 60-40 183 which this blenc was co ked. (Refer to table 30 for abbreviations.) APPENDIX A 125 Table 36. — (Continued) Coals Proportions blended Coking run numbers Coals Proportions blended Coking run numbers Medium- Vola- Old Ben No. 14 tile Pocahon- (Cont'd) tas OB14-PC 60-40 166 MVP-Bc- Orient No. 1 Mn-PC 9^-53^-70-15 161 Ol-C-PDP 25-50-25 135, 137 MVP-J-PC 15-70-15 175 Ol-Ec 85-15 125 MVP-KWA 25-75 142 Ol-GR-Ws 25-30-45 63, 76, 77, 85, 104 MVP-MC- Ol-GR-Ws 25-25-50 64 01 20-20-60 101 Ol-T-PC 40-40-20 179 MVP-Mn 20-80 160 Ol-KWA-PC 65-25-10 139 MVP-01 20-80 94, 141 Ol-MC- MVP-01 15-85 108, 126, 138 MVP 60-20-20 101 MVP-01 10-90 96 Ol-Md-PC 70-15-15 123, 134 MVP-Ol- Ol-Md-PC 65-25-10 122 PC 20-70-10 146 Ol-Md-PC 65-17^-173^ 167, 168 MVP-Ol-PC 20-60-20 147 Ol-Md-PC 65-15-20 170 MVP-Ol-PC 15-70-15 144 Ol-MVP 90-10 96 MVP-Ol-PC 10-80-10 143 Ol-MVP 85-15 108, 126, 138 MVP-Ol-PC 10-70-20 145 Ol-MVP 80-20 94, 141 MVP-01-S5 10-75-15 97 Ol-MVP-PC 80-10-10 143 MVP-01-Ws 35-25-40 57,68 Ol-MVP-PC 70-20-10 146 MVP-Ol-Ws 25-25-50 87 Ol-MVP-PC 70-15-15 144 MVP-02- Ol-MVP-PC 70-10-20 145 We-Ws 35-25-13-27 100 Ol-MVP-PC 60-20-20 147 MVP-OB 11 20-80 158 01-MVP-S5 75-10-15 97 MVP-OB 14 20-80 172 Ol-MVP-Ws 25-35-40 57,68 MVP-OB 14- Ol-MVP-Ws 25-25-50 87 PC 15-70-15 171 Ol-PC 90-10 140 MVP-PC-Z 20-20-60 151 Ol-PC 85-15 124, 130 MVP-PC-Z 20-10-70 150 Ol-PC 75-25 131 MVP-PC-Z 15-15-70 149 Ol-PC 60-40 9, 10, 11, 17, 25, MVP-PC-Z 10-10-80 148 32,33 MVP-S16 15-85 129 Ol-PC 55-45 12 MVP-Sx 20-80 169 Ol-PC-PetC 60-20-20 27 MVP-We- 01-PC-S5 75-10-15 92 Ws 35-25-40 58,71 01-PC-S5 65-10-25 93 MVP-We- 01-PC-S16 70-15-15 111 Ws 25-35-40 69 01-PC-S16 65-10-25 105 MVP-Z 20-80 153 01-PC-S16 60-15-25 109 Midvale 01-PC-S16 50-10-40 106 Md-Ol-PC 25-65-10 122 01-PC-S16 40-20-40 107 Md-Ol-PC 173^-65-17^ 167, 168 Ol-PC-Wn 75-10-15 95, 102, 103 Md-Ol-PC 15-70-15 123, 134 Ol-PetC 90-10 18 Md-Ol-PC 15-65-20 170 Ol-PetC 85-15 20 Minonk Ol-PetC 80-20 19, 21, 22, 40 Mn-Bc- Ol-PetC-Wn 60-20-20 26 MVP-PC 70-53^-93^-15 161 01-PI-S5 40-35-25 55 Mn-MVP 80-20 160 Ol-PI-Ws 40-35-25 50,90 Mn-PC 80-20 159 Ol-PI-Ws 40-30-30 51 Mn-PC 60-40 163 Ol-PI-Ws 25-35-40 89 Old Ben No. 11 Ol-PI-Ws 20-35-45 53 OBll-Bc 80-20 155 Ol-PI-Ws 20-30-50 52 OBll-Bc-PC 80-10-10 156 01-S16 80-20 80 OBI 1-Bc-PC 70-15-15 157 01-S16 70-30 81 OB11-MVP 80-20 158 01-S16 60-40 82 OB11-PC 80-20 154 Orient No. 2 OB11-PC 60-40 164 02-Ec-We- Old Ben No. 14 Ws 25-25-18-32 110 OB14-MVP 80-20 172 02-Ec-Ws 25-25-50 113, 114, 115, 116, OB14-MVP- 117 PC 70-15-15 171 02-GR-We- OB14-PC 80-20 165 Ws 25-25-18-32 99 126 ILLINOIS COAL FOR METALLURGICAL COKE Table 36.— (Continued) Coals Proportions blended Coking run numbers Coals Proportions blended Coking run numbers Orient No. 2 Pocahontas- (Cont'd) Carswell 02-MVP- (Cont'd) We-Ws 25-35-13-27 100 PC-01-S16 15-60-25 109 02-PI-We- PC-01-S16 10-65-25 105 Ws 25-35-13-27 98 PC-01-S16 10-50-40 106 Petroleum Coke PC-Ol-Wn 10-75-15 95, 102, 103 PetC-Ol 20-80 19, 21, 22, 40 PC-OB 11 40-60 164 PetC-Ol 15-85 20 PC-OB 11 20-80 154 PetC-Ol 10-90 18 PC-OB 14 40-60 166 PetC-Ol-PC 20-60-20 27 PC-OB 14 20-80 165 PetC-Ol-Wn 20-60-20 26 PC-S5 30-70 54 PetC-S16 20-80 43 PC-SI 6 40-60 49 Pocahontas- PC-SI 6 35-65 59 Carswell PC-SI 6 30-70 41,42 PC-Bc- PC-S16 20-80 44, 60 MVP-Mn 15-53^-9^-70 161 PC-S16 15-85 127 PC-Bc-OBll 15-15-70 157 PC-SI 6 10-90 47,48 PC-Bc-OBll 10-10-80 156 PC-S516 35-65 65 PC-Bh 40-60 177 PC-S516 20-80 66 PC-Bh 20-80 176 PC-Sx 35-65 86 PC-E5 40-60 6, 7, 8, 13, 14, 15 PC-Sx 20-80 162 PC-E5 30-70 36,37 PC-Wn 30-70 1,2 PC-E5-Wn 20-50-30 16 PC-Z 50-50 5 PC-H 40-60 181 PC-Z 40-60 4 PC-H 20-80 180 PC-Z 30-70 3 PC-J 40-60 174 PC-Z 20-80 28, 152 PC-J 20-80 173, 178 Pocahontas- PC-J-Ol 20-40-40 179 Inland PC-KWA- Steel 01 10-25-65 139 P1-01-S5 35-40-25 55 PC-M 40-60 183 PI-Ol-Ws 35-40-25 50,90 PC-M 20-80 182 PI-Ol-Ws 35-25-40 89 PC-Md-01 20-15-65 170 PI-Ol-Ws 35-20-45 53 PC-Md-Ol 173^-173^-65 167, 168 PI-Ol-Ws 30-40-30 51 PC-Md-01 15-15-70 123, 134 PI-Ol-Ws 30-20-50 52 PC-Md-Ol 10-25-65 122 PI-02-We- PC-Mn 40-60 163 Ws 35-25-13-27 98 PC-Mn 20-80 159 PI-S5-Ws 35-25-40 56 PC-MVP-J 15-15-70 175 Pl-We-Ws 35-25-40 91, 132, 133 PC-MVP-Ol 20-20-60 147 Pl-We-Ws 35-20-45 23, 24, 88 PC-MVP-Ol 20-10-70 145 Pl-We-Ws 30-20-50 30,31 PC-MVP-Ol 15-15-70 144 Pocahontas- PC-MVP-Ol 10-20-70 146 Inland PC-MVP-Ol 10-10-80 143 Steel, De- PC-MVP- fense Plant OB14 15-15-70 171 Corp. PC-MVP-Z 20-20-60 151 PDP-C 25-75 34, 35, 38, 39, 136 PC-MVP-Z 15-15-70 149 PDP-C 20-80 45,46 PC-MVP-Z 10-20-70 150 PDP-C-Ol 25-50-25 135, 137 PC-MVP-Z 10-10-80 148 Sahara No. 5 PC-Ol 45-55 12 (and No. 4 PC-Ol 40-60 9, 10, 11, 17, 25, + No. 5) 32,33 S5-MVP-01 15-10-75 97 PC-Ol 25-75 131 S5-01-PC 25-65-10 93 PC-Ol 15-85 124, 130 S5-01-PC 15-75-10 92 PC-Ol 10-90 140 S5-01-PI 25-40-35 55 PC-Ol-PetC 20-60-20 27 S5-PC 70-30 54 PC-01-S5 10-75-15 92 S5-PI-Ws 25-35-40 56 PC-01-S5 10-65-25 93 Sahara No. 16 PC-01-S16 20-40-40 107 S16-Ec 85-15 128 PC-01-S16 15-70-15 111 S16-MVP 85-15 129 APPENDIX A 127 Table 36. — (Concluded) Coals Proportions Coking run Coals Proportions Coking run blended numbers blended numbers Sahara No. 16 Wheelwright (Cont'd) (slack) S16-01 40-60 82 Ws-AE-GR 45-25-30 73 SI 6-01 30-70 81 Ws-Ec 75-25 118, 119, 120, 121 S16-01 20-80 80 Ws-Ec-02 50-25-25 113, 114, 115, 116 S16-01-PC 40-50-10 106 117 SI 6-01 -PC 40-40-20 107 Ws-Ec-02- S16-01-PC 25-65-10 105 We 32-25-25-18 110 S16-01-PC 25-60-15 109 Ws-Ec-W 7 e 50-25-25 112 S16-01-PC 15-70-15 111 Ws-GR 70-30 61, 70, 72, 79 S16-PC 90-10 47,48 Ws-GR-Ol 50-25-25 64 S16-PC 85-15 127 Ws-GR-Ol 45-30-25 63, 76, 77, 85, 104 S16-PC 80-20 44,60 Ws-GR-02- S16-PC 70-30 41,42 We 32-25-25-18 99 S16-PC 65-35 59 Ws-GR-We 60-15-25 75 S16-PC 60-40 49 Ws-GR-We 55-20-25 74 S16-PetC 80-20 43 Ws-GR-We 50-25-25 62, 83, 84 Sahara No. 5 + Ws-GR-We 45-30-25 67 No. 16 Ws-MVP-01 50-25-25 87 S516-PC 80-20 66 Ws-MVP-01 40-35-25 57,68 S516-PC 65-35 65 Ws-MVP- Saxton 02-We 27-35-25-13 100 Sx-MVP 80-20 169 Ws-MVP- Sx-PC 80-20 162 We 40-35-25 58,71 Sx-PC 65-35 86 Ws-MVP- Wharton We 40-25-35 69 Wn-E5-PC 30-50-20 16 Ws-Ol-PI 50-20-30 52 Wn-01-PC 15-75-10 95, 102, 103 Ws-Ol-PI 45-20-35 53 Wn-Ol-PetC 20-60-20 26 Ws-Ol-PI 40-25-35 89 Wn-PC 70-30 1,2 Ws-Ol-PI 30-40-30 51 Wheelwright Ws-Ol-PI 25-40-35 50,90 (egg) Ws-02-PI- We-Ec-02- We 27-25-35-13 98 Ws 18-25-25-32 110 WVPI-S5 40-35-25 56 We-Ec-Ws 25-25-50 112 Ws-PI-We 50-30-20 30,31 We-GR 70-30 78 Ws-PI-We 45-35-20 23, 24, 88 We-GR-02- Ws-PI-We 40-35-25 91, 132, 133 Ws 18-25-25-32 99 ZeiglerNo. 1 + We-GR-Ws 25-30-45 67 No. 2 We-GR-Ws 25-25-50 62, 83, 84 Z 100 29 We-GR-Ws 25-20-55 74 Z-MVP 80-20 153 We-GR-Ws 25-15-60 75 Z-MVP-PC 80-10-10 148 We-MVP- Z-MVP-PC 70-20-10 150 02-Ws 13-35-25-27 100 Z-MVP-PC 70-15-15 149 We-MVP- Z-MVP-PC 60-20-20 151 Ws 35-25-40 69 Z-PC 80-20 28, 152 We-MVP- Z-PC 70-30 3 Ws 25-35-40 58,71 Z-PC 60-40 4 We-02-PI- Z-PC 50-50 5 Ws 13-25-35-27 98 We-PI-Ws 25-35-40 91, 132, 133 We-Pl-Ws 20-35-45 23, 24, 88 We-PI-Ws 20-30-50 30,31 APPENDIX B Laboratory Procedures for Tar Analysis DRYING (Note 1) Approximately 2500 grams of wet tar and 170 grams of toluene (Note 2) are accurately weighed into a tared three-liter flask. The mix- ture is heated to boiling and the vapors are refluxed past a water trap (Note 3). The water is withdrawn continuously until the drying is completed (Note 4). The dried mixture is weighed to check the loss in weight against the weight of water removed (Note 5). Notes 1. This procedure was used on all tars. 2. Toluene is added to reduce the amount of foaming and spattering of the tar when it is heated to boiling. 3. The water trap is filled with a known weight of water before the drying is begun. When the drying is completed, the water layer remaining in the trap is withdrawn and the organic layer returned to the pot. 4. The water is withdrawn at such a rate that the organic layer continuously returns to the pot. This has been found necessary to pre- vent excessive foaming and spattering of the boiling tar. 5. The loss in weight of the tar is usually two or three grams more than the weight of water removed. This represents an error of about 0.1 percent. DISTILLATION The dry tar-toluene mixture obtained from the drying procedure is distilled in four separate batches from a one-liter distilling flask through an air-cooled condenser at a rate of about two or three drops per second. The distillate to 350° C. is collected in water-cooled receivers. The original flask plus the remaining tar is weighed again so that the weight of tar and toluene distilled may be calculated. SPECIFIC GRAVITY AND WATER CONTENT (Note 1) Approximately 200 grams of wet tar and 40 grams of toluene are weighed into a tared flask, thoroughly shaken, and brought to 28° C. The specific gravity of the mixture is measured by means of a Westphal balance. The specific gravity of the dry tar (Note 2) and the water content of the wet tar (Note 3) are calculated from these data and data obtained from the drying procedure. Notes 1. On tars 3-13, the standard procedure for measuring the specific gravity of the dry tar S = where: was used. On tars 14-84, a modified procedure was used, similar to the procedure described here in which the measurement was made on a dry-tar toluene mixture. The above procedure was used on tars 85-183. 2. The specific gravity of the dry tar is calculated by the following formula. dxDT (T + t + W) dx — D (tax + Wd) d = specific gravity of toluene at 28° C. x = specific gravity of water at 28° C. (relative to water at 4° C.) D = specific gravity of the wet tar- toluene mixture at 28° C. T = weight of dry tar in the wet tar- toluene mixture. t = weight of toluene added to the wet tar. W = weight of water in the wet tar- toluene mixture. a = .985 = an empirical correction factor to correct for the non- additivity of the volumes of tar and toluene. S = specific gravity of the dry tar at 28° C. The factor 1.00836 is used to convert the specific gravity at 28° C. to the specific gravity at 60° F. The ratio of the weights of dry tar to wet tar, obtained from the drying procedure, is used to calculate the weights of dry tar and water used in the specific gravity measurement. The maximum error in the calculated specific gravity assuming all the errors inherent in the procedure to be acting in the same direction is about ±0.006 _^!l ml. ±0.002 g ms - . ml. 3. The water content is calculated by the formula % H 2 = WS x 100 WS + T where: W = volume of H 2 removed from the wet tar in the drying pro- cedure. S = specific gravity of the dry tar at 28° C. T = weight of dry tar obtained from the drying procedure. The maximum error in the calculated water content is about ±0.2%. The probable error is about [128] APPENDIX B 129 FREE CARBON (Note 1) Wet tar, 5 to 10 grams, is accurately weighed into a 100-ml. beaker and digested with 50 ml. of toluene on a steam cone for 30 minutes. The mixture is filtered through a filter cup (Note 2) and extracted with benzene in a soxhlet extractor until the descending solvent is colorless. The cup and its contents are dried at 105° C. for one hour and then weighed (Note 3). Notes 1. The free carbon determination was car- ried out on the dry tar for runs 3-15, on a dry tar-toluene mixture for runs 16-68, and on the wet tar on runs 69-183. 2. The filter cup is made by folding two 15 cm. filter papers in the form of a thimble and inserting it in a 25 x 80 mm. extraction thimble. The cup is dried at 105° C. for several hours before being used. 3. The ratio of the weights of wet tar to dry tar obtained from the drying procedure is neces- sary to calculate the percentage of free carbon. SEPARATION OF TAR DISTILLATE INTO ACIDIC, BASIC, AND NEUTRAL FRACTIONS The following aqueous solutions are used: 10 percent sodium hydroxide 20 percent sulfuric acid saturated with sodium chloride 25 percent sodium hydroxide 40 percent sulfuric acid saturated sodium chloride saturated sodium bicarbonate-sodium chlo- ride. Approximately 2200 grams (weight known accurately) of dried tar are distilled and the distillate below 350° C. is collected in a water- cooled receiver. After weighing, the distillate is extracted successively with the following solutions (Note 1) : 1. Two 100 cc. portions of 20 percent sulfuric acid and one 50 cc. portion of salt solution. 2. One 700 cc. and three 100 cc. portions of 10 percent sodium hydroxide and one 50 cc. por- tion of salt solution (Note 2). 3. One 500 cc. and two 100 cc. portions of 20 percent sulfuric acid and one 50 cc. portion of salt solution. 4. Three 100 cc. portions of 10 percent sodium hydroxide, and one 50 cc. portion of salt solu- tion. 5. Three 100 cc. portions of 20 percent sul- furic acid and one 50 cc. portion of salt solution. 6. One 200 cc. portion of sodium bicarbonate- sodium chloride solution. The salt wash at the end of each series of extractions is added to the other extracts of that series. After separating extract No. 6, the or- ganic layer (neutrals) is poured into a tared flask. Extracts Nos. 1, 3 and 5 are combined and extracted with two 150 cc. portions of ether to remove trapped tar acids and neutrals. Extracts Nos. 2 and 4 are combined and extracted with three 150 cc. portions of ether to remove tar bases and neutrals. The ether extracts are com- bined to give a solution of tar acids, bases and neutrals in ether. This ether solution is extract- ed with the following solutions: (a) One 100 cc. and two 50 cc. portions of 10 percent sodium hydroxide (b) One 100 cc. and one 50 cc. .portions of 20 percent sulfuric acid (c) One 50 cc. portion of 10 percent sodium hydroxide (d) One 50 cc. portion of salt solution. Extracts (a) and (c) are added to Nos. 2 and 4, extract (b) is added to Nos. 1, 3 and 5, and extract (d) is discarded. The ether solution now contains neutrals alone. Aqueous extract No. 6, containing some suspended neutrals, is extracted twice with ether, and the aqueous layer is dis- carded. The ether solutions of neutrals are com- bined, dried over anhydrous magnesium sulfate, and filtered. Most of the ether is removed by heating on a steam bath, using a one-foot column packed with wire helices. The last traces of ether are removed on a hot plate, using a similar column. (This procedure is followed in all other ether stripping operations.) The residue is added to the main body of the neutrals in the tared flask, which now contains the total neutral fraction plus the toluene added during the dry- ing of the tar. The combined sulfuric acid extracts (Nos. 1, 3, 5 and b) are neutralized with an excess of 25 percent sodium hydroxide to liberate the tar bases. After cooling, the solution is separated in a separatory funnel. The clean aqueous layer is drawn off, and the upper layer (the organic layer plus insoluble fiocculent solid material (Note 3) suspended in water) is filtered through a Biichner funnel (Note 4) to remove the solids, which interfere with the separation during ether extractions. After washing thoroughly with ether and water, the solid material on the filter paper is dried in air and weighed. The filtrate containing the free tar bases and water is separated, and the combined aqueous solutions of tar bases are extracted with four 250 cc. portions of ether. The ether extracts and free bases are combined, dried over anhydrous mag- nesium sulfate, filtered, and the ether distilled off (Note 5). The weight of the residue plus the weight of the insoluble solids (usually 1 to 2 grams) removed by filtration is assumed to give the total weight of tar bases. The combined sodium hydroxide extracts (Nos. 2, 4, a and c) are neutralized with an excess of 40 percent sulfuric acid to liberate the tar acids. The solution is then saturated with salt (most easily done while the solution is still hot from the neutralization). After cool- 130 ILLINOIS COAL FOR METALLURGICAL COKE ing, the organic layer of the tar acids is sepa- rated, and the aqueous layer is extracted with five 300 cc. portions of ether. The tar acids and ether extracts are combined and washed once with 200 cc. salt solution to remove traces of sulfuric acid. No attempt is made to collect and weigh the small amounts ( 1 to 5 grams estimated) of tarry material (Note 2) which usually settles on the walls of the flask or separatory funnel containing the ether solution of tar acids. The salt solution is extracted once with 100 cc. ether which is added to the main ether solution. The ether solution of tar acids is dried over anhydrous magnesium sulfate, filtered, and the ether distilled off. In order to remove the water (1 to 3 grams) not removed from the tar acids by the drying agent, 25 cc. toluene is added to the residue from the ether stripping, and it is given a rough preliminary fractionation through a one-meter column (Note 6), the distillation being carried up to 216° C. The distillate from 145° C. to 216° C. is col- lected and weighed. The static holdup of the column is determined by rinsing the column with ether and distilling the ether off. The total weight of tar acids is the sum of the weights of the distillate from 145° C. to 216° C, plus the holdup, plus the residue in the stillpot. The procedure described above was used in runs 37-183 (Note 7). Prior to run 37, the sodium hydroxide and sulfuric acid extracts were subjected to steam distillation, rather than ether extraction, in order to remove trapped organic material. The results before run 37 are considered less reliable than those since. Notes 1. The procedure employed here is designed for tars containing up to 12 percent acids and 3 percent bases. For tars of higher acid or base content, some changes in the procedure would be necessary. 2. During this and subsequent alkaline ex- tractions, small amounts of flocculent solid ma- terial tend to collect on the walls of the separa- tory funnel in the organic layer. Indications are that care taken to settle as much of this material as possible into the alkaline solution helps to minimize the formation of tarry material during subsequent sulfuric acid extractions. The run- ning of small amounts of the organic layer into the alkaline solution in order to effect this sepa- ration is not objectionable, for the organic ma- terial is recovered later by ether extraction of the aqueous solution. Using this procedure, the tarry material is carried along with the tar acids and finally settles out on the walls of the flask containing the ether solution of tar acids. Because of the difficulty of collecting the tarry material, no attempt is made to weigh it. 3. The insoluble solid material is of un- known composition. It is soluble in mineral acids and insoluble in water, alkali, and ether. It burns in a flame, leaving an inorganic residue. No further investigation has been made. 4. It has been found that less than 1 gram of tar bases is lost by evaporation during this suction filtration. 5. The U.S.P. ether used in the extraction commonly contains about one percent ethanol. This causes no trouble with tar acids or neu- trals, but when stripping ether from the tar bases, it is necessary to continue the stripping until the alcohol (1 to 5 cc.) is removed. 6. The column for the preliminary fractiona- tion is one meter long, 12 mm. i. d., and packed with 3/32 inch Nichrome helices. It has an electrically heated jacket, and the still head has a stopcock take-off. It has a measured efficiency of 25 theoretical plates at total reflux. The frac- tionation is carried out as rapidly as possible without flooding (approximately 200 cc. per hour take-off). The purpose of the distillation is to remove all the phenol and cresols in order that they may be given a more careful fractionation later on. The distillation is carried arbitrarily up to 216° C. to insure that all the cresols are stripped off. Because of the crudeness of this fractionation procedure, too much significance should not be attached to the relative weights of acids below and above 216° C. 7. In four test runs on identical samples using the procedure described here, the per- centages of acids, bases and neutrals checked within ± 0.1 percent of the mean values (based on dry tar). However, the accuracy of the results is considerably poorer than the repro- ducibility, for the sum of the weights of acids, bases and neutrals usually falls short of the weight of the original tar distillate by an amount averaging about 1 percent of the dry tar. This discrepancy cannot be explained by the loss of tar bases during suction filtration (Note 4). Furthermore, the ether stripping procedure is considered efficient enough so that no appreciable amounts of tar components are lost during the ether removal. Possible explanations for this loss are: (a) the original tar distillate contains a small amount of water (caused by cracking during the distillation) which is not removed but is weighed along with the distillate; (b) the tarry material (Note 2) formed during the extraction procedure is not weighed; (c) tar bases and acids (especially the latter) may not be completely extracted by ether from the aque- ous liquors. DETERMINATION OF PHENOL AND CRESOLS IN TAR ACIDS To approximately 200 grams tar acids boiling below 216° C. (Note 1) is added 5 cc. of toluene (to aid in removing the last traces of water) and the mixture is fractionated through a two- meter column (Note 2). The reflux rate is main- tained just below the flood point (estimated at APPENDIX B 131 4-00 cc. per hour) and, unless otherwise noted, the take-off rate is approximately 16 cc. per hour. The following fractions are collected : Fl. Forerun of toluene and water. — This fraction is collected up to 145° C. and is as- sumed to contain no tar acids. F2. Forerun of phenol. — This fraction is col- lected from 145° C. to the b.p. of phenol. The weight of this fraction (about 2 grams) is as- sumed to represent pure phenol, although it contains traces of toluene and water. F3. Main phenol fraction. — This fraction is collected until the temperature has risen at least 2° above the phenol b.p. The phenol percentage is determined from the freezing point, ls (see References to Publications, p. 62) and the re- mainder is assumed to be o-cresol. F4. Phenol and o-cresol. — This fraction is collected until the o-cresol b.p. is reached. The cut should be made as soon as the o-cresol b.p. is reached in order to leave sufficient o-cresol for the next fraction. The o-cresol percentage is determined by the cineol method, 1 ' and the remainder is assumed to be phenol. F5. o-, m-, and p-cresols. — This fraction is collected until a fairly constant plateau is reached, about 10° above the o-cresol b.p. The o-cresol percentage is determined by the cineol method, and the remainder is assumed to be m- and />-cresol. The ratio of /n-cresol to p- cresol in this fraction, as well as in F7, is assumed to be the same as the ratio determined in F6. F6. m- and p-cresol. This fraction is col- lected only on the plateau, during which there is a gradual rise in temperature of 1.5° - 2.0°. The fraction is collected over a range of not more than 2°, and it should be cut as soon as a rise in temperature slightly sharper than the gradual rise is observed. The m-cresol percent- age is determined by the Raschig nitration method, 20 and the remainder is assumed to be p- cresol. F7. m- and p-cresol and higher tar acids. — The take-off rate is reduced to 8 cc. per hour for more efficient fractionation, the distillate is collected in a small graduate, and readings of the volume of distillate vs. temperature are taken until the next plateau is reached, about 7-8° above the ra-/>-cresol b.p. The midpoint of the break is assumed to indicate the amount of m-/>-cresols in the distillate. The weights of phenol, o-cresol, m-cresol and />-cresol are calculated for each of the fractions F2 to F7 and added up to give the total weights of each component present. The above procedure was used on all runs (Note 3). Notes 1. The procedure described here is satisfac- tory for mixtures containing at least 25 grams each of phenol and the cresols. Much smaller quantities cannot be satisfactorily separated by the column used here. For this reason it is usually necessary to combine the tar acids from two or more similar runs in order to obtain sufficient quantities of acids for the fractiona- tion. 2. The fractionating column used here is two meters long, 9 mm. i.d., and packed with 3/32 inch Nichrome helices. It has an electrically heated jacket, and the still head has an inter- mittent take-oif valve operated by an adjust- able automatic timer. It has a measured effi- ciency of 40 theoretical plates at total reflux. 3. On two test fractionations of a sample of tar acids, the percentages of phenol and the cresols checked within 0.05 percent or less (based on dry tar). But while the fractionation pro- cedure may give accurate values for the phenol and cresol content of the tar acid samples, these values probably do not furnish a completely accurate measure of the composition of the tar itself, as an appreciable quantity of tar acids is probably lost during the extraction procedure. ANALYSIS OF THE NEUTRAL FRACTION (Note 1) Approximately 400 grams of the neutral frac- tion is fractionated through a one-meter column (Note 2). The following fractions are col- lected : Fl. Toluene. — ^his fraction contains all the toluene that was added to the tar in the drying procedure. The fraction is cut when the calcu- lated weight of toluene, in the 400 gram portion of neutrals and toluene, has been collected. F2. Light oil. — This fraction is collected at total take-off from the boiling point of toluene to 190° C. It is then fractionated from 190° to 195° C. with intermittent take-off. F3. Mixture of light oil and naphthalene. — This fraction is collected at total take-off from 195° C. to the boiling point of naphthalene, suffi- cient material being collected on the naphthalene plateau to give a satisfactory freezing point (Note 3). The naphthalene content of this fraction is determined by the freezing point (Note 4) and the difference is assumed to be light oil. F4. Mixture of naphthalene and compounds boiling above naphthalene. — This fraction is collected as total take-off until the temperature begins to rise from the naphthalene plateau. It is then collected at intermittent take-off to 230° C. The naphthalene content is determined from the freezing point (Note 4) and the difference is assigned to the residue. F5. Residue. — The residue includes the com- bined weights of material remaining in the stillpot plus the holdup of the column. The weight of each fraction is converted to the weight of that fraction in the total neutrals and the percentages calculated. The percentages of light oil, naphthalene, and residue are summed up for each of the fractions F2 to F5 to give the total percentage of each component present. 132 ILLINOIS COAL FOR METALLURGICAL COKE Notes 1. Only one naphthalene fraction, 205-225° C, was cut on neutrals obtained from tars 3-62. The naphthalene content in this case was determined by the freezing point and the differ- ence assigned to the residue. Approximately 0.6 percent naphthalene remained in the light oil. 2. The fractionation column used here is one meter long, 10 mm. i.d., and packed with 3/32 inch Nichrome helices. It has an electrically heated jacket and a still head with a stopcock take-off. It is rated at about 25 theoretical plates at total reflux. 3. Because the light oil composition may vary and thus affect the accuracy of the freezing point chart, it was thought desirable to have the naphthalene percentage relatively high in this fraction in order to minimize such errors. Freez- ing points obtained for this fraction were usu- ally in the range of 67-75° C, corresponding to 72.5 to 90 percent naphthalene. 4. The percentage naphthalene is determined from a graph in which the freezing points of naphthalene-naphthalene oil mixtures are plot- ted against the percent naphthalene. This graph was obtained from the Inland Steel Company. Illinois State Geological Survey Bulletin No. 71 1947 UNIVERSITY OF ILLINOIS-URBANA 3 0112 109141298