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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 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 Charles K. Rose

This paper presents some research studies of the rotary drilling of oil shale at the Bureau of Mines Oil-Shale Mine, Rifle, Colo. The experimental procedures and the rotary drill test equipment are described. Theories of rock drillability, rotary bit cutting action, and bit design are presented and discussed. The actions of various bit designs are analyzed and compared with the observed results of actual drilling tests. A cost estimate is made for drilling Colorado oil shale.

Jan 1, 1955

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 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 J. D. McLenegan

The purpose of this investigation was to prepare a market survey of the refractories industry in California and Nevada (referred to in subsequent paragraphs as the region), and to determine the degree of self-sufficiency and the potential capacity for anticipated growth. The report includes estimates of the total annual refractories consumption, the quantity of refractories imported into the region, the tonnage of raw materials required for their manufacture, and the resources of fire clay and high-alumina minerals in the region.

Jan 1, 1956

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 David Schlain

The galvanic corrosion properties of titanium in contact with commercially pure aluminum, copper, or type 302 stainless steel in some of the common organic acids were investigated. Acids used in these experiments were 10 percent formic, acetic, lactic, citric; 1 percent oxalic and tartaric; and 9 percent oxalic. Electrode-potential measurements and several types of galvanic couple experiments were carried out. Solutions were aerated by three methods: Flow of air, flow of helium, and natural aeration. Work was done at 35° C. with couples consisting of equal areas of the 2 metals. Titanium was resistant to corrosion in most of the organic acids studied, whether alone or in contact with a dissimilar metal. However, titanium coupled with aluminum did corrode in 1- and 9-percent oxalic acid solutions. Contact with titanium usually caused aluminum to corrode by galvanic action. Copper was subject to galvanic attack in 10-percent acetic acid with a flow of air. Contact with aluminum to some solutions in which titanium is ordinarily inert and noble with respect to aluminum caused titanium to corrode

Jan 1, 1956

By H. Kenworthy

[Experimental studies were made to develop a laboratory technique for direct removal of cadmium and germanium from sphalerite concentrates. Cadmium- and germanium-bearing concentrates from the Illinois-Kentucky fluorspar field were sound to be, amenable to an inert atmosphere fuming process for removing these two moats in the form of gaseous sulfides. Treating the condensed fume by pyrometallurgical methods upgraded the material end provided a means of partly separating the constituents. Cadmium was concentrated about 35:1 arid germanium about 300:1. The extractive investigations were supplemented by vapor-pressure studies on the sulfides of germanium to obtain fundamental data for larger scale laboratory conditioning and control when treating the zinc concentrates. Vapor-pressure curves were developed for synthesized monosulfide and disulfide The results of these- investigations indicate the possibility of significantly increasing the recovery of cadmium from zinc concentrates. Comparison with present recovery of germanium cannot be made, since commercial recovery data arc not available.]

Jan 1, 1956

By R. J. Campbell

[The steady increase of aluminum production means a corresponding increase of carbon consumption in the alumina-reduction cells. Improved petroleum techniques constantly reduce the amount of byproduct petroleum-coke production. These, trends threaten the alumina-reduction works with possible shortages of carbon, which must be supplied from some other source. In anticipation of this shortages, an investigation into the possibility of using coal as an alternative source of carbon was begun at the Northwest Experiment Station of the Federal Bureau of Mines. The investigation lit has developed bench-scale methods that produce carbon of higher purity than is required by specifications for anode carbon. Additional work will b required to bring these processes to pilot-plant seals and to prove the suitability of the carbons, produced or aluminum-anode consumption.]

Jan 1, 1956

By S. S. Todd

[The purpose of this investigation was to obtain, heat-of-formation values a four Common titanates and, to conjunction with other requisite data, to derive free-energy-of-formation values In tem peratures in the range of 1,600°-1,800° K. T ht four titanites are tricalcium ?ditanite !['a¬spheremr?raritanar( rint-tir.rniurn rill( 1 This rc rr,rt sul,rlc?nu?nIs :r },r; vinu~ hul,lrc.irse,n3i n wlti h eht-rmnnIN-ti i n c {ar.a ai?rc? pu -,csseeri (or, 11 in(c-rnxiLIic co mrc+unrls conraininL~ rir:,niurrl. 'f Lac? !1~:)mc? c?xpcrirnc'ntnl n-ut rhod w,i. rna~loycul. lic?.ats of for rn:ltion of rlre comi?c,unr4~ it 29S.N. ut re mca,urc?,l by tioItl[ion e':iIorrr)utrv, using a ctrneaR }ryrlrc,fllanric-hY rir~chlorie- ,aci l mixttrrt .is rhr c-zle~rinrrrric- fluid and rc.actic~n rtu,liura}.]

Jan 1, 1956

By L. R. Willmott

An ethanolamine purification unit for removing carbon dioxide and hydrogen sulfide from Firscher-Tropsch synthesis gas was installed at the Bureau of Mines synthetic liquid fuels demonstration plant at Louisiana, Mo. The unit was a surplus Radford Girbotol unit from the Missouri Ordnance Works modified for a capacity of 90,000 std. cu. ft per hour of synthesis gas at 450 p.s.i.g., operating pressure. The hydrogen sulfide loading of the feed gas was specified at 500 grains per 100 cu. Ft. The unit was designed by the Girdler Corp. and installed by the Koppers Co. Initial operations were conducted far 11 days in May 1951. Thereafter 7 additional runs were made, varying lo duration from 8 to 54 days. The last run was terminated on May 29, 1953, the total time the Plant wars in operation being 219 days.

Jan 1, 1956

By T. C. Atchison

This report describes a mobile laboratory designed and constructed by the Bureau of Mines in 1950 to meet the needs of an experimental blasting research program. The laboratory has facilities for making; film recordings of 16 simultaneous transient electrical signals over a broad range of amplitude, frequency, and duration. The signals are recorded with specially designed oscilloscopes and high-speed drum cameras. Each of the 16 channels records on a separate strip of 35-millimeter film by using interchangeable input units, transducers having different sensitivities and output impedances can be accommodated. The laboratory can be used to record both steady-state and transient phenomena originating as electrical voltages or capable of being converted to electrical voltages by appropriate transducers. Thus, the laboratory can, be used in studying various types of vibration problems or high-speed phenomena, such as ground and building vibrations, machinery vibrations, airborne vibrations, electrical-circuit switching phenomena, millisecond timing, and seismic phenomena occurring when rock is broken by explosives.

Jan 1, 1956