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By P. R. Perry

This publication is a compilation of tested methods for the analyses of titanium tetrachloride, titanium sponge, and various intermediate materials and products. They are presented in concise form without the detail usually found in publication of new methods because many of them are modifications of well known procedures. The Electrometallurgical Experiment Station, Boulder City, Nev., has been developing titanium production methods since 1945. Most of this development was on a modified Kroll Process but also included work on sodium reduction and electrolytic methods. During these years a large variety of samples were analyzed. Most of the analytical problems were solved using published methods or modifications of the same. At the start, there were no published procedures for analyzing titanium sponge using spectrochemical methods. A great deal of study was given to testing several of the well known techniques, and some of them, such as direct sparking of the metal, proved to be completely unsatisfactory. Solution-spark techniques were finally tried, and satisfactory procedures were developed for some of the more common impurities. These spectrochemical methods were then put into routine use for several months before their publication.2/ Some new modifications have been made, and techniques have been developed to determine other impurities found in titanium sponge and tetrachloride. All spectrochemical methods used in 1954 are included in this publication.

Jan 1, 1955

By H. P. Holmes

Tonnage quantities of hafnium metal have been prepared in Kroll-process equipment designed for producing zirconium. Some slight process modifications have been necessary, but overall operation is the same as for zirconium. Hafnium oxide is chlorinated in the presence of carbon and the resultant hafnium tetrachloride reduced by magnesium metal. Byproduct magnesium chloride is removed in a high-vacuum distillation step and the hafnium sponge metal crushed for further use. Arc-melted metal can be forged and rolled to sheet, but the best material produced to date would not be considered cold ductile. INTRODUCTION This investigation is part of the program for the production of pure metals from domestic and foreign ores that has been underway at the Bureau of Mines for several years. It was done in cooperation with the Atomic Energy Commission and the Bureau of Ships.

Jan 1, 1955

By L. H. Banning

Recent dry-top electric smelting tests at the Northwest Electrodevelopment Experiment Station, Albany, Oreg., indicate that a high-titanium slag and a good grade of pig iron can be produced from alluvial Idaho ilmenite. A total of 120 tons of concentrates were smelted during this investigation, to yield an average of 0.5 ton of slag and 0.3 ton of pig iron per ton of ilmenite. Power consumption averaged 1,400 kv.-hr. per ton of ilmenite, at a feed rate of 400 to 500 pounds per hour, when operating at an electrical energy input of 290 to 370 kilowatts. The optimum operating voltage appeared to be 110 volts, phase-to-phase. Graphite electrode consumption averaged 15.6 pounds per ton of ilmenite smelted. Magnesite furnace refractory withstood the corrosive action of the hot metal and slag better than carbon refractory.

Jan 1, 1955

By J. J. Dowd

1. The Pittsburgh bed is the most important bed in Ohio County, and virtually the entire production of coal in the county comes from this bed. 2. Known measured and indicated reserves in all beds, based on a minimum thickness of 14 inches and 1,800 tons per acre-foot of-coal in place, are estimated at 365 million short tons as of January 1, 1954. Of this total, 356 million short tons is in beds 28 inches and more thick. Areas in each bed were omitted from the estimate because available data relative to the bed characteristics are too meager to make an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, such reserves should be added to the total estimated reserves.

Jan 1, 1955

By A. L. Engel

Production of chromite in California has been from many small, high-grade mines. The opening of the Purchase Depot at Grants Pass, Oreg., in 1951 has stimulated chromite mining in California, and a large number of properties are being reexamined as there is a possibility that some low-grade ores from many of these properties can be beneficiated to meet the purchasing schedule. The Bureau of Mines in its program of conservation is continuing ore-dressing tests on chromite ores to better evaluate their potential. This report is a compilation of preliminary concentration tests on samples from five different properties in California. The concentration tests were made on ores from the David mine, Butte County, the Seiad Creek mine, Siskiyou County, the High Plateau mine, Del Norte County, Bud's mine, Tuolumne County, and tailings from the Miller concentration plant in San Luis Obispo County, Calif., to determine the possibility of beneficiating these ores so that they will meet the specifications for the Government stockpile.

Jan 1, 1956

By J. S. McNabb

"A search for manganese ore by core-drill exploration was carried out by the Bureau of Mines in the Philipsburg mining district in Granite County, Mont., in 1939 and 1940. This work was based on detailed studies of the manganese ore bodies of the district previously made by the Geological Survey.In 1949 further search for manganese in the district was deemed advisable. Diamond drilling was begun the following year as a joint program by the Geological Survey and the Bureau of Mines with the primary purposes of probing ore-leasing structures and extending the limits of known ore bodies. A secondary objective was to test a geologic theory based on a new conception of manganese-ore localization. The exploration targets were designated and the drilling results interpreted by the Geological Survey, and the Bureau of Mines was responsible for the drilling, sampling, and core handling. Improved drilling equipment and methods were utilized in an effort to obtain better core recoveries than resulted from the earlier drilling campaign.The Philipsburg mining district, Granite County, Mont., is 27 miles south of Drurrnnond, about 45 miles airline northwest of Butte, and 1 mile east of Philipsburg. During the course of the investigation patented lode-mining claims owned by the American Machine & Metals, Inc., the Contact Mines, Inc., and the Moorlight Mining Co. were diamond drilled.The district has been an important source of domestic manganese dioxide ore since local recognition of the mineral's importance during World War I. Peak annual output in 1918 of about 127,000 tons of manganese ore was utilized principally by the steel industry. A small but relatively steady output has persisted to the present to satisfy demands by battery manufacturers for battery-grade manganese dioxide.The known manganese deposits of the district are in sedimentary rocks of Paleozoic age. These rocks lie along a north-trending anticline traversed by a series of east-west tension veins. The east flank of the anticline terminates at a steep-dipping fault contact against a small granodiorite batholith.Replacement deposits of manganese oxides and carbonates occur locally in or closely associated with tension veins cutting calcareous rocks, or adjacent to the intrusive. Rhodochrosite has been a common accessory mineral in deposits valuable chiefly for lead, zinc, and silver. Some of the replacement deposits characteristically are irr2gular in outline, whereas others have fairly regular walls marking the limits of favorable beds."

Dec 1, 1955

By K. K. Kershner

To meet an increasing demand for high-purity cobalt, the Bureau of Mines has conducted investigations for producing this metal. Cobalt having a purity of 99.95 percent or higher is needed to determine heats of formation, corrosion resistances, phase diagrams, and other basic properties of the element and its compounds. This grade of cobalt may be used for preparing radioactive metal. As a result of its investigations a detailed procedure, which is of practical significance to the production of high-purity cobalt, has been developed by the Bureau for purifying cobalt solutions and for electrolytic deposition of the metal. Cobalt metal, which had a purity of 99.99 percent with reference to metallic contaminations, was deposited electrolytically. Qualitative spectrographic analysis showed only traces of calcium, copper, iron, magnesium, nickel, and zinc.

Jan 1, 1956

By J. B. Gayle

Both immediate and long-range economic factors are associated with blending anthrafines to produce metallurgical cokes, and they warrant careful consideration of the technology of carbonization of blends containing significant proportions of inert substances in general and anthrafines in particular. This situation has resulted in numerous publications dealing with various phases of the overall problem, particular emphasis being placed on the effects of inert substances on the yields and quality of cokes produced. Because relatively little attention has been given to the expansion behavior of coal blends containing inert substances, an investigation of this problem was undertaken using the Bureau of Mines sole-heated oven. Since experiments in the sole-heated oven do not measure wall pressures directly, a new method of interpretation of sole-heated oven data, which permits estimates of wall pressures, has been proposed.

Jan 1, 1955

By W. A. Grosh

In 1951 the Federal Bureau of Mines became interested in the reports of copper-nickel mineralization in northern Minnesota. Several outcrops on the north side of the Duluth gabbro in the Kawishiwi River area were sampled by the Federal Bureau of Mines and George M. Schwartz of the Minnesota Geological Survey. Because these samples showed appreciable amounts of copper and nickel, a 100-pound sample of an un-altered outcrop was obtained for metallurgical testing. Results from this preliminary work were all favorable; therefore, in the fall of 1953 the Bureau of Mines diamond-drilled three holes near the outcrop of the con-tact between the Duluth gabbro and the Algoma granite. A total of 686 feet of NX size hole was drilled, and 100 percent of the core was recovered. Each hole intersected the contact, and the strike and dip for that locality were established. The core was split, and half was used for analyses and further metallurgical tests; the remainder was retained for permanent record in the Bureau of Mines core-storage warehouse.

Jan 1, 1955

By J. C. Barrett

Bureau of Mines research on the arc welding characteristics of titanium was initiated in 1948. Little was known about the art except that the easily contaminated metal required more protection from the atmosphere during welding than most other metals. Chambers were designed and built within which titanium could be welded with adequate inert gas protection. Welds were made and their properties studied, and prototype items were made successfully. This report, presenting a resume of the titanium arc-welding experiments undertaken by the Bureau of Mines, demonstrates that the process is successful if conducted under proper conditions and describes the welding of prototypes. INTRODUCTION The Bureau of Mines' first report on methods of joining titanium covered the subject of spot welding,4/ outlining the conditions necessary for producing spot welds in ductile titanium consolidated by powder metallurgy methods and describing the characteristics of such welds. This report embraces the field of fusion weld-ing of titanium and traces the development of suitable methods and equipment for producing such welds.

Jan 1, 1956

By R. W. Huber

The successful development of a titanium prototype of the 81-mm. mortar base plate for the Army Ordnance Corps is outlined in this report. Information is presented dealing with forming, forging, and machining, welding and assembly techniques, and design changes relative to this prototype. INTRODUCTION The work of the Federal Bureau of Mines in making ductile titanium available2/ has resulted in the establishment of a new industry. Owing to its strategic importance and the combination of low density and high strength, titanium has received considerable attention as a structural metal. Titanium's favorable strength-to-weight ratio is of particular importance to the Army Ordnance for equipment that is transported by airplane or by foot soldiers.

Jan 1, 1956

By O. C. Baptist

This report presents results of an investigation undertaken by the Bureau of Mines to determine the clay content of typical petroleum reservoir sands in Wyoming and the effect of clay content on the permeability behavior of the sands. These results should have significance in determining the feasibility of injecting water into the sands for secondary recovery and in estimating the probable damage incurred by these sands if invaded with filtrates from water-base drilling muds. The results of air-, brine-, and water-permeability determinations are given for reservoir sands in three Wyoming fields. The amounts of materials of "fine silt and clay size" (Wentworth scale) in the sands and the types of clay minerals present, as identified by X-ray diffraction methods, are also presented and discussed.

Jan 1, 1955

By J. H. Bilbrey

A recording thermobalance ,vas used to determine the rates of oxidation of mol-ten tin over the temperature range 550°-900° C. Oxidation rates were found to vary widely for a given temperature, as previously reported by other investigators. 1 X-ray diffraction data indicated that the probable cause of these variations was the development of preferred orientations in the crystals forming the oxide film. No reasons for the differences in degree of preferred orientation were discovered. For relating the weight of the oxide formed (w) to the time of oxidation (t) an equation of the form wn = kt was found to best represent the experimental data. INTRODUCTION In the course of conducting investigations on the feasibility of using selective oxidation techniques for the purification of various metals in the molten state it was soon discovered that data on the oxidation of molten metals and alloys were very scarce. In contrast to the many hundreds of publications on the oxidation of metals in the solid state there are relatively few articles on the rates of molten-metal oxidation. In view of this scarcity of data, it was decided to institute a series of investigations into the oxidation processes of molten nonferrous metals and alloys with the expectation that the information derived could be put to practical use in developing and improving refining processes based on selective oxidation. This report is the first of a series in which oxidation data for molten nonferrous metals and alloys are presented.

Jan 1, 1955

By W. J. Crawford, P. M. Gruzensky

"Several experiments have been carried out in efforts to evaluate qualitatively a variety of electrolytes for refining bismuth. Most extensive work was done with the basic tartrate, hydrochloric acid, and hydrofluosilicic acid electrolytes. Deposits that are smooth and adherent can be obtained from these three electrolytes if low cathode current densities are employed. All three electrolytes were effective in purifying crude bismuth considerably, with additional purification indicated in each instance by a reelectrolysis step.With the basic tartrate electrolyte best results were obtained when the electrolyte was at 40° C. and contained at least 100 grams of bismuth per liter. An apparent disadvantage was depletion of bismuth from this electrolyte, causing the deposits to become spongy and nonadherent.The hydrochloric acid electrolyte had the greatest tendency to yield rough, dendritic deposits. Best deposits were obtained at cathode-current densities below 2 amperes per square decimeter. A small amount of glycerin helped to produce a smoother deposit, and adding sulfuric acid or methyl sulfuric acid retarded the deposition of impurities. Very good results were obtained in electrowinning bismuth from a bismuth trichloride-hydrochloric acid electrolyte.Smooth and adherent deposits were obtained from a hydrofluosilicic acid electrolyte, with very good refining as regards lead and silver impurities; however, higher reagent costs and slow decomposition of the electrolyte have discouraged its use.INTRODUCTIONMethods of recovering bismuth from ores and byproducts were underdeveloped for many years because of the limited uses for bismuth, the pharmaceutical industry being the chief consumer. In the past decade or so additional uses for bismuth, particularly in the metallurgical field, have brought about increased demand for the metal with the result that bismuth is being recovered from byproducts that were once discarded. In addition to such uses as low-melting alloys, solders, bearings, die setting, etc., some interest has been indicated in bismuth as a possible coolant for nuclear reactors. The advent of ductile bismuth and bismuth-alloy thermocouple wire has contributed greatly to temperature measurement, particularly in the below-zero range."

Jan 1, 1956

By P. M. Gruzensky

Several experiments have been carried out in efforts to evaluate qualitatively a variety of electrolytes for refining bismuth. Most extensive work was done with the basic tartrate, hydrochloric acid, and hydrofluosilicic acid electrolytes. Deposits that are smooth and adherent can be obtained from these three electrolytes if low cathode current densities are employed. All three electrolytes were effective in purifying crude bismuth considerably, with additional purification indicated in each instance by a reelectrolysis step. With the basic tartrate electrolyte best results were obtained when the electrolyte was at 40° C, and contained at least 100 grams of bismuth per liter, An apparent disadvantage was depletion of bismuth from this electrolyte, causing the deposits to become spongy and nonadherent.

Jan 1, 1956

By E. R. Palowitch

Coal wasted with mine refuse represents losses in overall recovery of merchantable coal to the mine operator and a concomitant reduction in domestic reserves of available coal. Fraser, Kelley, and Graham3/ in studying the available coal in mine refuse in the Pittsburgh district of western Pennsylvania have estimated that at least 1 ton of mine refuse is produced for each 10 tons of merchantable coal and that 20 percent of this mine refuse might be recovered as salable coal by mechanical cleaning. SUMMARY This investigation dealt with the mechanical recovery of coal from wine refuse by a dense-medium washery employing pulverized mine rock as the dense medium and operating at a rate of 175 tons per hour. Two types of mint refuse were tested: Freshly mined and that .which had been mined 2 years before and piled on a waste dump.

Jan 1, 1955

By Lloyd Williams

1. The investigation shows that the Pewee, Big Mary, and Windrock are the most important beds in Anderson County. About 73 percent of the known recoverable reserves of coal in the county are in these beds, and from them comes 94 percent of the production. The remaining reserves tabulated in this report are in the Joyner, Jellico, Coal Creek, and Poplar Creek beds, and 6 percent of the county production comes from these beds. No production is being reported at present from the Jellico bed, although it was mined years ago. 2. Known measured and indicated reserves in all beds, bared on a minimum thickness of 1/4 inches and on 1,800 short tons put acre-foot of coal in place, are estimated to be 170 million torts as of January 1, 1953 Of this total, 155 million tons is in beds 2S inches and more thick. Areas in each bed were omitted from the estimate because available data relative to the bed characteristics are too meager to permit making an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, such reserves should be added to they total estimated reserves.

Jan 1, 1955

By John B. Gayle

[The coking time exerts a Considerable influence on the throughout of a coke oven, and for this reason a large number of papers dealing with the relation between coking tine and the different operating variables have been published. Although all of the factors known to ink influence the coking time have been studied, agreement leas not boon reached on several questions, 3/4/ and it appears worthwhile to evaluate any data that become available during investigations of the carbonizing properties of various oafs and coat blends, this report, therefore, includes a Study of the relation between coking lime and flue temperature and represents the second phase of overall investigation ion of factors influencing the coking time in slot-type ovens.]

Jan 1, 1956

By R. J. Hundhausen

The Takilma-Waldo copper district in Josephine County, Oreg., was studied by the Bureau of Mines from September 1950 to April 1.951 and from December 1953 to April 1954. Funds for the investigation were provided by the Bureau of Mines and the California-Oregon Power Co., Medford, Oreg., on a cooperative basis. The copper mines in the district are credited with a total production of ore worth $1,700,000. Since 1933 the mines have been unproductive and, except for minor exploration, largely inactive. The history of the district indicates that the copper deposits were mined principally during periods of high metal prices.

Jan 1, 1956

By A. B. Needham

This report describes the exploration work done in 1941 in connection with the search for strategic minerals as authorized by the Strategic Materials Act approved by the President on June 7, 1939. It deals with the various manganese deposits and showings in the Tombstone mining district of Cochise County, Ariz. The exploration project comprised a study of the geology, mapping of the areas, and exploration of various mines and deposits by sampling old drifts, crosscuts, and scopes, supplemented by diamond drilling from underground stations. The Federal Government's manganese-purchasing programs have revived interest in occurrences such as the scattered deposits near Tombstone. Because of this, the Bureau of Mines project report on the Tombstone district, prepared originally in 1941 but not published, has been revised and now is being made public.

Jan 1, 1956