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By H. E. Powell

The mineral dressing research here reported is part of a continuing program by the Bureau of Mines to develop new or improved concentration processes for oxidized or partly oxidized lead and zinc ores. A sample of low-grade sulfide-oxide, lead-zinc ore from Jasper County, Mo., containing galena, cerussite, pyromorphite, hemimorphite, smithsonite, and sphalerite was concentrated by froth flotation and tabling to a grade of 66 percent lead. Because of the presence of a high content of slime-size values, the overall recovery of lead was limited to 64 percent at this grade. Tests to recover the zinc by froth flotation and by gravity concentration did not give satisfactory results. INTRODUCTION Since its establishment, the Rolla Metallurgy Research Center has con-ducted studies of base metals as a part of its overall program (1, 2, 3, 4, 5,6,7).3/ This research has been, and is, directed to beneficiating complex and submarginal ores, to retreating rejects from commercial installations, and to developing fundamental data.

Jan 1, 1960

By P. C. Good

To meet a growing need for thorium metal of high purity and amenability to fabrication, the Bureau of Mines devised a method for preparing thorium metal by the reduction of thorium tetrachloride. Thorium tetrachloride was prepared by chlorinating calcined thorium oxalate with carbon tetrachloride. The crude thorium tetrachloride, containing oxygen-bearing compounds, was purified by a double vacuum distillation at 800 to 900° C., and thorium metal was made in the form of a dense sponge by the reaction of metallic sodium or magnesium with thorium tetrachloride at 800° C. Vacuum arc melting was used to consolidate the sponge metal to ingot form for evaluation of its physical and chemical properties.

Jan 1, 1960

By M. R. Geer

The cleaning of fine coal, particularly for metallurgical use, is receiving greater attention. An increase in the proportion of fine coal in the run-of-mine product has been created by changes in mining practice, and a concur-rent deterioration in the quality of the fines has occurred because of more widespread full-seam mining. These two factors, augmented by the depletion of premium beds of metallurgical coal in some areas and the resulting shift to "dirtier" beds, are providing the impetus for adoption of improved cleaning techniques. For example, froth flotation, which has been used for years in a few preparation plants, now is gaining more rapidly in acceptance. Similarly, the dense-medium cyclone, which is used widely in Europe for making difficult separations, recently has been introduced to the United States. Regardless of the cleaning process employed, the finer sizes of coal can be treated with maximum effectiveness only when they are removed from the run-of-mine product and treated separately. No present process can treat the full range of sizes together with complete effectiveness. Flotation is applicable only to the coal finer than a top size ranging between 14-and 48-mesh, and cyclones require removal of all material finer than 0.5 to 0.3 mm. from the feed. Thus, the trend toward more-effective cleaning of the fine coal imposes the attendant problem of fine screening. Whereas in the past there was little need to screen finer than about l/4-in., present developments indicate that fine screening will become increasingly prevalent.

Jan 1, 1960

By E. G. King

Strontium sulfide and barium sulfide occur as intermediates in commercial treatments of the impure natural sulfates to produce pure strontium and barium chemicals. Thermodynamic considerations involving these sulfides have been hampered by lack of basic data, such as the entropies at 298.15°K. This paper reports the results of heat capacity measurements of strontium sulfide and barium sulfide in the temperature range 50°-298°K. The entropies at 298.15°K. were derived from the heat capacity values. Free energies of formation at 298.15°k. were computed from the entropies and literature values of the heats of formation. Strontium sulfide and barium sulfide are thermo-dynamically less stable than calcium sulfide, but more stable than magnesium sulfide.

Jan 1, 1960

By Charles K. Rose

The Cebolla Creek titaniferous iron deposits near Powderhorn in southern Gunnison County, Colo., were examined by the Federal Bureau of Mines as part of an overall program to investigate the Nation's titanium and iron resources. The deposits occur around the periphery of the Iron Hill stock, which underlies an area of about 12 square miles. Concentrations of magnetite, ilmenite, and perovskite arc localized along fractures in the pyroxenite stock. Mineralogical studies of composite surface samples collected in 1956 showed that most of the iron is present in ilmenite-bearing magnetite. Perovskite is the chief titanium mineral in the magnetite-rich and augite-rich types, and sphene is the principal titanium mineral in the placer material. The mica-rich rock contains approximately equal amounts of perovskite, ilmenite, and sphene.

Jan 1, 1960

By W. H. Oppelt

The Federal Bureau of Mines investigated combustion of lignite in domes-tic heating equipment to obtain information on equipment performance and to evaluate testing procedures. Three types of domestic heating equipment were tested, ranging from a hand-tilled, magazine-type space heater to a ram-type overfeed stoker. Lignite was readily burned in each of the three units under various test conditions. Burnoff rates determined by adding weighed charges to the magazine were found to be in error because of shrinkage of the lignite when only a portion of the magazine capacity was consumed during a test. More reliable burnoff rates could be determined by carbon-nitrogen balances. A hand-fired magazine-type space heater (Booker heater) was operated without the furnace attachment at efficiencies to 75 pct. One test series was run with minimum supervision under conditions encountered in actual household operation. No mechanical trouble was encountered.

Jan 1, 1960

By Warren M. Mahan

A rotary kiln process was developed by the Federal Bureau of Mines to produce consistently an iron product containing 3 to 7 percent nickel. Cuban laterite and serpentine ores were smelted in a gas-fired batch-rotary kiln) 5 feet in diameter and 9 feet long. The metal contained 2 to 4 percent carbon, with little or no silicon, and could be produced on a large scale with modest capital investment. A total of 121 tests was run using this procedure. The tests were conducted with a maximum temperature of 2,625° F., using linings of firebrick containing 40 to 70 percent alumina. Slags in the kiln were acid to neutral. The material in each batch passed through three stages: (1) Sponge metal, (2) carburization, and (3) balling and meltdown. Half the tests were made while firing the kiln with atmospheric-temperature air; the remainder were fired with preheated air. Tests showed that preheated air decreased fuel requirements, dust losses, and reducing agent, and increased the capacity of the kiln.

Jan 1, 1960

By M. G. Zabetakis

This publication describes an investigation conducted by the Federal Bureau of Mines regarding the cause of an explosion of a dephlegmator or fractionating column at the Cities Service Oil Company Refinery, Ponca City, Okla., January 22, 1959. The column was that used with the refinery's No.1 Dubbs Coker. The explosion caused the death of an employee of the refinery and resulted in extensive damage to the refinery and to nearby property. The Bureau's study of the explosion began January 26.

Jan 1, 1960

Although alternating-current (a.-c.) power systems and equipment have been used in coal mining for many years, most mines in the United States are powered mainly by direct current (d.-c.). There are several logical reasons for this, but the use of d.-c, equipment is, in most instances, a direct outgrowth of the original practice of using such power for haulage systems. For traction equipment such as the electric trolley locomotive the d.-c. motor has ideal operating characteristics, and thus it has been widely used for haulage locomotive service. The first efforts at electrification of coal mines started with the haulage system and from there branched out to include the many types of electrically powered mining machinery used in the industry today.

Jan 1, 1960

By F. R. Cattoir

The Federal Bureau of Mines refined chromium from an aqueous electrolytic process in molten sodium chloride-chromium chloride electrolytes. Oxygen and nitrogen contents were reduced by a factor of 10 to 40, but most other impurities were little changed. The product usually contained a little more iron than the feed. Since iron was entering the bath from the iron pot and the graphite liner at a nearly constant rate, contamination of the chromium deposits by it was more serious at low currents and deposition rates. A few runs in an iron cell with a nickel liner yielded chromium containing one half as much iron as the feed, but up to 1.5 pct. nickel. In all cases the anode feed lay in the bottom of the container, which itself was used as the anode connection. With a 12-in. cell, variations in applied voltage from 0.05 to 1.5, in current from less than 10 to over 100 a., and in initial cathode current densities from less than 100 to over 2,000 a./sq.ft. had little or no effect upon the analysis of the metal produced) except for iron content. Changes in bath analysis from 3 to 11 pct. chromium were also without effect. These changes did bring about large differences in the physical forms of the crystals obtained. The thick heavy crystals produced at low voltage and current contained voids which made them difficult to leach free of chlorides. Easiest to leach were the thin leaf-like crystals obtained at around 1 v.

Jan 1, 1960

By Victor Erickson

ECONOMIC recovery, which began in 1958, carried through into 1959 but was somewhat retarded by the 116-day steel strike beginning in July 1959. Recovery and economic growth increased production and consumption of mineral fuels 3 percent above 1958. The increase was accomplished despite a drop of 26 percent in coal exports. Prices remained constant during the year so that the value of production and consumption also increased 3 percent over 1958. Stocks in the hands of producers at yearend were little changed from the supply at the beginning of the year. Employment in the field of mineral fuels decreased 6.4 percent from 1958. Average hourly earnings were up 7 percent, and average hours worked were up 5 percent, with the result that weekly earnings gained 11.8 percent. Internal freight rates were relatively constant, but ocean tanker rates declined both in 1958 and 1959 from the high rates charged during the Suez crisis. The index of major input expenses decreased for anthracite, held constant for bituminous coal, and increased for petroleum. The index of labor cost per dollar of product and per ton of product declined again in 1959 to a new low in anthracite and bituminous-coal mining industries.

Jan 1, 1960

By R. J. Leary

A small electronic digital computer employing punched cards has been used to facilitate the solution of a variety of problems in Bureau of Mines pyrometallurgical research. In this work the computer has been found to be economical for solving both simple problems that occur repeatedly and those involving complex or iterative calculations. Each of these classes of problems and their respective solutions are described. These small computers can be used effectively by researchers when they work in consultation with a computer specialist. Close team work produces the required solutions in less time, and, oftentimes, in a more useful form. Participation in programming by researchers develops in them a skill for evaluating the suitability of problems for electronic computing.

Jan 1, 1960

By J. W. Eckerd

The crushing of chestnut-size (1-5/8 by 13/16 inch) Pennsylvania anthracite in four commercial crushers (impact) jaw) hammer-mill) and gyratory types) was studied by the Bureau of Mines to determine which could produce the largest proportions of buckwheat Nos. 1 and 2 sizes (9/16 by 3/16 inch). Single pass dry and wet crushing techniques and the effect of stage crushing were evaluated. Calculations were made to show the effect of closed-circuit reduction on production rates and yield of the various sizes. The data show that the gyratory crushers produced the greatest percentage of the desired sizes. A ring-type hammer mill produced the greatest tonnage of buckwheat No.1 and rice (14.9 tons per hr.) during dry grinding tests) but the yield of these sizes was only about 55 percent) as compared with 62 to 70 percent for the gyratory crushers. The impact and jaw crushers produced the smallest amount of buckwheat and rice and the largest quantity of oversize material.

Jan 1, 1960

By Joseph A. DeCarlo

This publication presents a tabulation of oven-and beehive-coke plants in the United States as well as pertinent statistical data on the number, capacity, kind, and condition of the ovens. Coke is an essential raw material in pig-iron production and the coal-chemical materials produced during the coking process are used to manufacture fertilizers, paints, plastics, synthetic rubber, explosives, detergents, nylon, pharmaceuticals; dyes, and many other products necessary to the high standard of living in this country. In table 1 the oven-coke plants in the United States on December 31, 1959, are listed. This shows the name and address of the company, location of the plant, classification or type of ownership, number and type of ovens, annual coke capacity, and the coal-chemical materials produced. The "furnace" plants I are those owned by iron and steel companies and most of them are integrated with blast furnaces to facilitate transportation of raw materials for steel making. Furnace plants represented 87 percent of the total coking capacity and their average annual capacity was 1. 3 million tons. The "merchant" plants are those associated with chemical companies, gas utilities, as well as those that produce metallurgical, industrial, and residential-heating grades of coke and coal-chemical materials for sale on the open market. These coke plants are smaller than furnace plants and in 1959 their average coke capacity was only 520 thousand tons annually. On December 3l, 1959, there were 54 furnace and 20 merchant oven-coke plants in existence in the United States.

Jan 1, 1960

By R. V. Lundquist

Lime-soda sinters, made and processed for recovering alumina and soda, consisted of several types of compound structures differing from the ideal dicalcium silicate and sodium aluminate. Many or these compound structures were causes for low alumina recovery and contributed to the relation or leach slurries. Presence or free lime, whether in the sinter or released by hydrolysis of sinter compounds, contributed to relation of leach slurries. Free lime tends to establish the initial viscosity assumed by a leach slurry. Previous investigations by the Bureau of Mines (1, 4)4/ and by other laboratories (5) have demonstrated the technical applicability of the lime-soda sinter process to the recovery of alumina from aluminum silicate materials. The basic concept of the process is sintering aluminum silicate materials with limestone and soda ash for the production of dicalcium silicate and sodium aluminate and then extracting the sodium aluminate by leaching the sinter in causticized liquors. Alumina is precipitated from the pregnant liquors by carbonating with carbon dioxide. Reaction in the sintering operation may be represented by the following simplified equation: A1203?SiO + 2CaCO3 + Na2C03 = 2Ca0?SiO + Na20?Al203 + 3C02

Jan 1, 1960

By T. A. Sullivan

Research undertaken by the Bureau of Mines in 1938 has resulted in the development of titanium from a laboratory curiosity to a commercial metal. Along with processes for producing the metal, it was necessary for the Bureau to develop methods for analyzing the metal, raw materials, and intermediate products. Some of the methods developed have been published.3 4 5/ General Services Administration (GSA) was responsible for purchasing titanium metal under Defense Production Act contracts with commercial producers. GSA designated the Federal Bureau of Mines to analyze this metal and establish its compliance with Government specifications. A substantial quantity of tin was found in some of the samples analyzed, and in July 1957 tin was added to the list of impurity elements to be determined. The specifications limited the amount of tin in titanium sponge to a maximum of 0.10 percent. A program was immediately initiated to investigate methods and techniques for determining tin in the range of 0 to 1.0 percent. A method accurate at the 0.10 percent level was necessary, as this level was the critical range for acceptance or rejection of the metal.

Jan 1, 1960

By E. Morrice

The metallurgical laboratory data developed in this study indicate an improved electrowinning process for producing higher purity cerium ingot. A typical sample of the Reno electrocerium contains 99.9 weight-percent cerium and the following impurities: Total other rare-earth elements, less than 0.04 percent; iron not detected; silicon and aluminum, less than 0.02 percent each; calcium plus magnesium, less than 0.01 percent; carbon, 0.01 percent; oxygen, 0.002 percent; hydrogen, 0.0003 percent; and nitrogen, 0.0015 percent.

Jan 1, 1960

By E. D. Wilson

This is the second of a series of progress reports describing work undertaken at the San Manuel copper mine to study the geologic factors influencing block caving of the deposit. The first report described the work done from April 1954 to March 1956.3/ This report describes the progress from March 1956 through March 1958 and presents additional maps, factural data, inferences, and conclusions resulting from a continuation of the underground geological work. As outlined in these reports, the study thus far has shown that the principal geologic factors affecting block caving are structure, rock types, alteration, mineralization, oxidation, and presence of water. Structure is fundamentally the most important. Systematic fracturing governed the extent and grade of primary ore mineralization and tangibly affects the subsidence or ground movement, which extends from the mine workings to the surface because of the block caving.

Jan 1, 1960

By Walter Kawa

In connection with its research in producing synthetic liquid fuels from coal, the Federal Bureau of Mines studied reactions of iron and iron compounds with hydrogen and hydrogen sulfide in batch autoclaves. The Bureau hoped to gain indirect evidence regarding the chemical changes that iron catalysts undergo when they are used in the hydrogenation of coal. The information obtained may be helpful in identifying the active form or forms of iron catalysts. At 450° C., with hydrogen at hundreds of atmospheres and hydrogen sulfide at 1 or 2 atmospheres, the thermodynamically stable form of iron is ferrous sulfide in the case of the metal, magnetite, ferric oxide, ferrous sulfate, ferrous oxalate, or the chlorides of iron. However, complete conversion to ferrous sulfide was not achieved at temperatures of 400° to 500° C. for kinetic reasons. Extensive sulfiding of iron, magnetite, ferric oxide, and ferrous oxalate occurred below 400° C., and some conversion of ferrous sulfate to ferrous sulfide occurred at 400° C. In the hydrogenation of coal, ferrous sulfide is the form of iron likely to be available for heterogeneous catalysis when starting with the metal, oxide, sulfate, or oxalate.

Jan 1, 1960

By Norwood B. Melcher

This report describes preliminary experiments by the Federal Bureau of Mines on the practicability of adding raw pellets of taconite concentrate to blast furnace feeds. The usual industrial practice is to harden the pellets by heating before they are charged to the furnace. The Bureau research demonstrated that raw pellets could be successfully smelted in an experimental furnace with no significant change in coke consumption and only a moderate increase in dust losses. The dust loss was 43 pounds per ton of metal for an all-pellet charge, compared with 7 pounds per ton for an all-sinter charge. Raw taconite pellets undergo only slight degradation during charging to the furnace if 1 percent bentonite is used as a binder. INTRODUCTION Fines and concentrates must be consolidated or agglomerated into larger masses before they can be smelted in a commercial blast furnace. Such agglomeration is usually done by sintering, pelletizing, nodulizing, or briquetting. Sintering has been the more common practice, but with the advent of taconite concentrates pelletizing is increasing in importance.

Jan 1, 1960