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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 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 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 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 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 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