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By R. M. Creamer

Attempts have been made to electroplate titanium and zirconium from aqueous, nonaqueous, and fused-salt electrolytes. Metals were produced only in fused-salt electrolytes, the major product being sponge metal. All other electrolytes gave only partial reduction of the metal ions. Fused alkali borate electrolytes containing titanium salts gave titanium boride powders and coatings of poor adherence. Some of the problems encountered in the deposition of these metals and some of the aspects of titanium and zirconium chemistry involved are discussed. INTRODUCTION Titanium and zirconium are both relatively light, noncorrosive metals with both military and civilian uses. This has led to intensive investigations into the metallurgy of these metals. Both metals are high in the Electrochemical Displacement Series and are difficult to prepare in a pure state. At present they are prepared by reducing their chlorides, using magnesium. Electrolytic reductions have resulted in the preparation of fine powders or sponge of variable quality. It is believed that a good process of electroplating these metals on a baser metal would result in a very desirable product. The objective of the research summarized in this report was to investigate methods of electrodepositing these metals, with the idea of producing uniform, coherent plates. Most of the work was concentrated on titanium, the more abundant of the two metals. A system developed for titanium should be applicable to zirconium owing to their chemical similarity. Information gained from these experiments may also be applicable to the electro-winning of the metal.

Jan 1, 1954

By B. K. Shibler, I. S. Solet, H. W. St. Clair

"This study was undertaken to provide a more adequate knowledge of the chemistry of the sulfide volatilization process for recovery of tin from low-grade Bolivian ores. The investigation was partly supported by the Department of State under its program for scientific cooperation with South American republics.The results of this investigation demonstrate the conditions under which cassiterite (Sn02) may be converted to stannous sulfide by reaction with pyrite or sulfur vapor. Quantitative data are given on the rate of sulfidization and on the vapor pressure of stannous sulfide.INTRODUCTIONAlthough the United States is the world's largest consumer of tin, virtually no tin ores occur within our national borders. Most of the world's tin supply comes from alluvial deposits in the Far East and in Africa, The major sources of tin ores are Malaya, Indochina, Bolivia, Belgian Congo, Nigeria, Thailand, Burma, China, and the United Kingdom. Bolivia is the only important source of tin in the western hemisphere. It was the chief source of tin f or the United States during World War II. The Government-owned tin smelter at Texas City, Tex., was built primarily for smelting Bolivian ores and depends largely on Bolivian ores for its operation. Bolivia is the only major tin-producing country in which the tin ores occur as vein or lode deposits requiring underground mining. Most of the tin from the Far East and Africa is mined by dredges from alluvial or placer depos its. It is recovered as a high-grade concentrate of cassiterite relatively free from impurities. The tin minerals in the lode deposits are more intimately associated with other minerals and more difficult to separate into a clean concentrate. Furthermore, a large part of the tin in the original ore is lost during concentration. The ores as mined contain only a few percent of tin, so they must be milled to separate the gangue minerals and produce a concentrate containing 30 to 40 percent tin before they are shipped to the smelter. The losses of tin that occur during milling vary from 18 to 65 percent. The average recovery of tin from Bolivian ores is probably 50 to 60 percent."

Dec 1, 1954

By W. F. Dietrich

1. On St. Thomas and St. Croix, and possibly also on St. John, low-quality red-burning clays probably can be developed to provide the major part of the raw materials for structural clay products and earthenware pottery. 2. The potential sales volume for structural clay products is too small to sustain a plant in the Virgin Islands to manufacture such products in competition with Puerto Rico; however, handmade patio tile might be produced successfully. 3. The market for pottery utility wares in the Virgin Islands is too small to justify a plant devoted solely to the production of such wares; but it may be feasible to evolve a diversified community activity to make jugs, pots, casseroles, bowls, charcoal burners, patio tile, and other items.

Jan 1, 1955

By W. A. Stickney

This report summarizes the results of laboratory tests of five samples of low-grade phosphate ores from Idaho. The laboratory test work has demonstrated that by grinding, desliming, and flotation a portion of the siliceous gangue can be removed. The highly carbonaceous ores responded successfully to treatment after preroasting, to produce a plus-30-percent-P205 product. It has been found that highly siliceous ores, as represented by the samples treated, are more readily amenable to concentration than ores high in calcium carbonate. Of the five samples tested, four were amenable to concentration to a product containing over 30 percent P205. One sample, from the Conda, second bed, was not amenable to mineral-dressing treatment to produce a plus-25-percent-P205 product.

Jan 1, 1955

By W. D. Mcmillan

Important reserves of nickel ore occur in the Levies district in Oriente, Cuba. The area is mountainous and mostly covered by heavy vegetation. The ore bodies comprise surface tracts of nickeliferous laterite underlain with decomposed serpentine of ore grade. The Cuban Nickel Co., a wholly owned United States Government corporation, owns a plant for leaching the nickel from its ores at Nicaro, Oriente, Cuba, Between December 1943 and March 31, 1954, 5,902,225 short tons of ore was treated, with a recovery of 116,206,519 pounds of nickel (52,711 metric tons). In 1953, 1,330, 224 short tons of ore was mined and 27;"3,129 pounds of nickel produced. The Cuban Nickel Co. also owns a townsite, with the necessary facilities, mining equipment, and 11 miles of railroad. Ore for the plant has been produced from the Ocujal-San Juan claims on lends owned by the Nicaro Nickel Co., a sub¬sidiary of Freeport Sulphur Co. The Government enterprise is man-aged by the Nickel Processing Corp. The Cuban Nickel Co. has denounced mineral concessions and has purchased other claims from private owners.

Jan 1, 1955

By N. A. Eilertsen

Eastern Aroostook County, Maine, contains an enormous tonnage of manganese widely distributed in manganiferous sedimentary beds composed of hematitic shale, hematitic slate, and laminated siliceous carbonate rock. The bedded deposits range in thickness from several feet to over 150 feet. Manganese minerals that occur as silicates and carbonate are so minute that they cannot be concentrated by present methods of ore dressing. From a hydrometallurgical standpoint, the deposits can best be classified by amenability to acid leaching. The deposits of Aroostook County are in three geographical groups (see fig. l), designated as the northern, central, and southern districts. At least 13 deposits are known to occur in the latter district, which covers an Ewes about 8 miles wide and 15 miles long. The Littleton Ridge deposit, on the northern boundary of the southern district, previously examined by geologists from the State and Federal Geological Surveys on the farms of Donald H. Haggerty and David A. Abernethy, was pointed out in reports as being possibly the richest and largest in the southern district. The Bureau of Mines sampled this deposit by surface trenching and diamond drilling from May 1 to September 30, 1951. A total of 23 trenches was bulldozed, aggregating 5,355 linear feet, of which 8 trenches were sampled by cutting 185 channel samples over a linear distance of 1,820 feet.

Jan 1, 1955

By R. G. Nelson

This report covers investigations of the Bureau of Mines for the period of June 15, 1952, to June 15, 1953, on a research project for the Materials Laboratory, Wright Patterson Air Force Base, Dayton, Ohio. The primary purpose of this investigation was to make high-purity chromium-base alloys having room-temperature ductility and high-temperature strength. The Nonferrous Metals Branch of the Bureau of Mines, Albany, Oreg., has, during the past 7 years, developed on a laboratory scale a hydrogen treatment method for making high-purity chromium that can be fabricated into thin sheet and wire. This material can be bent at room temperature. The object of this investigation was to use this material to develop improved chromium-rich alloys for high-temperature uses.

Jan 1, 1955

By L. F. Willmott

The production operation of a Kerpely gas producer at Louisiana, Mo., is described. This unit, originally designed for airblown operation was modified to permit using oxygen in the blast in place of air. The first runs J for test purposes, were made in June 1950. After this, seven production runs were made and these are the subject of this report. Total gasification time was 245 days. In each run, Nut or Pea coke or mixtures of both at a rate varying from 1,700 to 2,300 pounds per hour was converted with oxygen and saturated steam to produce synthesis gas - primarily carbon monoxide and hydrogen -approximating a predetermined rate of 80,000 to 95,000 cu. ft. per hour and a predetermined hydrogen-carbon monoxide ratio, The requirements per 1,000 std. cu. ft. of (CO + H2) were 21.6 to 30 pounds of coke, 213 to 267 std. cu. ft. of oxygen, and 3L4 to 47.B pounds of steam.

Jan 1, 1955

By Joseph J. Wallace

1. The Pittsburgh is the most important bed in Washington County from the standpoint of present production and recoverable reserves. 2. Known measured and indicated reserves in all beds, based on a minimum thickness of 14 inches and 1,800 short tons per acre-foot of coal in place, are estimated at 4,181 million short tons as of January 1, 1954. Of this total, 4,132 million short tons is in beds 28 inches and more thick. Areas in some beds were omitted from the estimate because available data relative to the bed characteristics are too meager for 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 the total estimated reserves.

Jan 1, 1955

By J. F. Barkley

The work covered in this report was done to meet the requests from many Government agencies for information on alleviating sludge difficulties in No. 6 (Bunker C) fuel-oil storage tanks. Accumulated sludge at times caused serious loss in tank capacities; pumps became overloaded or lost suction; strainers often required very frequent cleaning; fuel-oil heaters in some instances became fouled and inefficient; and gobs of sludge that passed the strainers interfered with good combustion. The requests also included questions regarding the usefulness in general of oil "additives" for preventing sludge and the relative merits of the many trade-named additives being marketed. Realizing that preventing such difficulties would result in substantial savings to the Government, an investigation was begun with the limited funds avail-able. Although various claims are made for No. 6 fuel-oil additives other than preventing sludge, only an investigation as regards the storage tank-sludge problem has been possible.

Jan 1, 1955

By R. W. Huber, R. C. Wiley, V. C. Petersen

"Three arc- melted ingots, two of a t itanium-7 percent manganese all oy and the third of unalloyed titanium, were forged and rolled into 3/ 4-inch plate; comparative data were obtained on these processes. The finished plate, part of which was used by the Naval Bureau of Ordnance, was tested for mechanical and other properties.These properties were correlated with sponge purity, forging technique, rolling temperature, and cooling rate from the rolling temperature. For the alloy material, transformation data were obtained, and their age-hardening characteristics were studied. The temperature-impact relationship was established for rolled sections from all three ingots.INTRODUCTIONArc -melted ingots of unalloyed titanium and a titanium-manganese alloy were fabricated into plate under closely controlled conditions by personnel of the Metals and Alloys Section, Physical Metallurgy Branch, Bureau of Mines, College Perk, Md. This program was cosponsored by the Naval Bureau of Ordnance. Bureau of Mines interest lay in correlating the processing procedures with the mechanical properties of the finished plate.Considerable data have been published recently on constitution diagrams and properties of titanium-manganese alloys in genera1. 3/ 4/5/6/ However, little if any correlation between processing schedules and end results has been published, particularly with respect to the present commercial production of the proprietary titanium manganese alloys . Several factors in the production of titanium and titanium alloys have a pronounced influence on the physical and mechanical properties of the finished product: (1) The degree and nature of impurities in the base materials, ( 2) the amount of impurities introduced during the melting cycle and their distribution, (3) the homogeneity of the alloy, (4) forging, (5) rolling, and ( 6) final heat-treating cycles. All of these item£ are important from a metallurgical standpoint in producing the desired end properties in the metal."

Mar 1, 1955

By R. W. Huber

Three arc-melted ingots, two of a titanium-7 percent manganese alloy and the third of unalloyed titanium, were forged and rolled into 3/4-inch plate; comparative data were obtained on these processes. The finished plate, part of which was used by the Naval Bureau of Ordnance, was tested for mechanical and other properties. These properties were correlated with sponge purity, forging technique, rolling temperature, and cooling rate from the rolling temperature. For the alloy material, transformation data were obtained, and their age-hardening characteristics were studied. The temperature-impact relationship was established for rolled sections from all three ingots. INTRODUCTION Arc-melted ingots of unalloyed titanium and a titanium-manganese alloy were fabricated into plate under closely controlled conditions by personnel of the Metals and Alloys Section, Physical Metallurgy Branch, Bureau of Mines, College Park, Md. This program was cosponsored by the Naval Bureau of Ordnance. Bureau of Mines interest lay in correlating the processing procedures with the mechanical properties of the finished plate.

Jan 1, 1955

By BUREAU OF MINES

This report is submitted in accordance with provisions of the Synthetic Liquid Fuels Act of April 5, 1944 (30 U. S. C. 321-325, as amended), which require that: "The Secretary of the Interior shall render to Congress on or before the first day of January of each year a report on all operations under this Act." Owing to the broad scope of the content and the diversity of interests represented, the Annual Report for 1954 has been divided into two separate publications. Each is being published by the Bureau of Mines as a Report of Investigations, and the respective titles follow: R. I. 5118, Part I - R. I. 5119, Part II - 011 From Coal. 011 From 011 Shale. The introduction, identical in both reports, summarizes research progress in 1954 under the entire Synthetic Liquid Fuels program. A free copy of either publication may be obtained by writing to the Bureau of Mines, Publications Distribution Sec- tion, 4800 Forbes Street, Pittsburgh 13, Pa. The R. I. number and title of the publication desired should be indicated.

Mar 1, 1955

By BUREAU OF MINES

This report is submitted in accordance with provisions of the Synthetic Liquid Fuels Act of April 5, 1944 (30 U. S. C. 321-325, as amended), which require that: "The Secretary of the Interior shall render to Congress on or before the first day of January of each year a report on all operations under this Act." Owing to the broad scope of the content and the diversity of interests represented, the Annual Report for 1954 has been divided into two separate publications. Each is being published by the Bureau of Mines as a Report of Investigations, and the respective titles follow: R. I. 5118, Part I - R. I. 5119, Part II - 011 From Coal. 011 From 011 Shale. The introduction, identical in both reports, summarizes research progress in 1954 under the entire Synthetic Liquid Fuels program. A free copy of either publication may be obtained by writing to the Bureau of Mines, Publications Distribution Sec- tion, 4800 Forbes Street, Pittsburgh 13, Pa. The R. I. number and title of the publication desired should be indicated.

Mar 1, 1955

By V. F. Parry

The major industrial uses of char or semicoke produced by low-temperature carbonization of coal4/ are as fuel for generating electric power, for blending with metallurgical coking coal as a substitute for low-volatile coals, and for gasification to produce synthesis gas for chemical purposes. This paper discusses various methods for carbonizing coal, emphasizing processing of the noncoking coals to produce char for thermal power-plant fuel and for blending with metallurgical coking coals and tar for chemical use. Low-temperature carbonization is a relatively simple processing step involving heating coal to about 900° to 1,200° F. to decompose the coal into 4 main products: (1) Semicoke or char; (2) complex, partly oxygenated liquid hydrocarbons or tar; (3) fixed gases; and (4) water. If the coal is heated rapidly under conditions that prevent decomposition of the primary products, 68 to 87 percent of the net heat in the raw coal is left in the char and 10 to 23 percent of the potential heat appears in the primary tar. Fixed gases represent approximately 7 percent of the heat and approximately 2 percent is lost or dissipated in the reactions of decomposition. Considering the different ranks of coal in the United States, the yield of tar will vary from about 9 to 44 gallons per ton, therefore it is important that each coal be carefully considered if it is to be carbonized for industrial use.

Jan 1, 1955

By R. August Heindl

A process for recovering manganese from open-hearth steel-plant slags was investigated. The proposed method of accomplishing this is indicated by the flow diagram in figure 1. Mixtures of open-hearth, steel-plant flush slags and limestone, so proportioned as to have molar [CaO -3P205] ratios of approximately 2, were fired at approximately 2,400° F. in an oxidizing atmosphere and then cooled slowly. This treatment produced a clinker consisting principally of two solid phases comprised of (1) various combinations of the oxides of manganese, iron, aluminum, and magnesium, probably in spinel complexes, and (2) a dicalcium silicate phase, which contains the phosphorus. Reduction of these clinkers with hydrogen or with gaseous mixtures containing CO, CH4, and other hydrocarbons at about 1,300° F. formed manganous oxide as well as varying amounts of ferrous oxide and iron. Carbon monoxide and mixtures of hydrogen and carbon monoxide effectively reduced the clinkers but also gave higher proportions of soluble iron when the manganese was extracted from the reduced clinkers by leaching at about 80° F. with ammonium carbonate solutions containing 26 to 28 percent ammonia and 15 to 26 percent carbon dioxide. It is believed that the manganese is in solution as an ammonia-manganese complex. Concentrations of about 90 grams of manganese per liter were obtained by batch countercurrent procedures. By distilling 50 percent of the ammonia, the ammonia-manganese complex was decomposed, and approximately 90 percent of the manganese was precipitated as the carbonate with the simultaneous precipitation of 15 to 30 percent of the iron, the larger amounts of iron precipitating in the continuous tests. The manganese-iron ratio in the product could be increased either by recycling more manganese from the distillation to the extraction or by aerating the liquor to purge it of iron before, rather than after, the distillation step. Calcination of the pelletized manganese carbonate in an oxidizing stmosphere at 2,000° F. or above gave a final product, Mn304, resistant to crushing and apparently possessing the other physical properties essential in a ferromanganese blast-furnace feed.

Jan 1, 1955

By B. W. Gandrud

At the Southern Experiment Station of the Federal Bureau of Mines, reports are prepared from time to time on results of washability studies of commercially important coal beds in the Southern Appalachian region. The investigations that provide the material for these reports are made by the Bureau of Mines, United States Department of the Interior, in cooperation with the University of Alabama and the mine operators. This report records the results obtained on a sample of run-of-mine coal taken in June 1953 from the Pratt bed at the Davidson Coal Co. mine about 1 mile west of Graysville, Ala. One of the main objectives of a washability study is to obtain technically and commercially important data in connection with the best methods for preparing and utilizing the Nation's limited reserves of good coking coal. Such information is important from the standpoint of conservation in that it facilitates selection of preparation methods that will yield an acceptable grade of coking coal with a mini-mum of losses of coal in the rejects. The Pratt bed is one of the main sources of coking coal in the Jefferson County part of the Warrior field. This is the first time, however, that data from a complete washability study of coal have been obtained from this bed in Jefferson County. In the Graysville area, Pratt-bed coal has good coking characteristics and is used for blending with other coals in making metallurgical coal. The extent of its use in such blends is severely limited in this area, however, by the fact that it has a high sulfur content, which has not been reducible to any great extent by washery treatment.

Jan 1, 1955

By Lloyd Williams

1. The investigation shows that the bed identified as Wilder in this report is the only bed in Overton County that has produced commercial coal and is the only bed in which coal reserves were estimated for this report. Three other coal horizons were recognized but lacked enough data for reserve estimates. 2. Known measured and indicated reserves of coal, based on a minimum bed thickness of 14 inches and on 1,800 tons per acre-foot of coal in place, are estimated to be 19 million short tons, as of January 1, 1953. Of this total, 10 million tons represents coal 28 inches and more thick. Areas of the Wilder bed were omitted from the estimate because available data relative to the bed characteristics were too meager for 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 the total estimated reserves.

Jan 1, 1955

By Lloyd Williams

1. This investigation shows that the Sewanee bed is the only coal bed being mined in Sequatchie County. Other coal beds are present, but as they do not contain known recoverable reserves, estimates of reserves were made only for the Sewanee bed. 2. Known measured and indicated reserves in the Sewanee bed, based on a minimum thickness of 14 inches and on 1,800 short tons per acre-foot of coal in place, are estimated to be 76 million short tons as of January 1, 1953. Of this total 62 million short tons represent coal 28 inches and more thick. Areas in the bed were omitted from the estimate because available data relative to the bed characteristics were insufficient to permit making an estimate conforming 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 determined by this investigation.

Jan 1, 1955

By Murray Greyson

A number of tests were made with various methanation catalysts in fixed-bed, conventional fluidized-bed, and multiple-feed, fluidized-bed equipment to develop catalysts and processes for methanation of synthesis gas. The results show: 1. Methanation reactions may be carried out in 1-inch, bench-scale equipment at high synthesis-gas throughputs with good temperature control of the reactions if a multiple-feed type of fluidized-bed design is used. 2. Nickel is superior to iron as a catalyst for the methanation of synthesis gas, unless the process is considered in terms of a combined operation that produces both gaseous and liquid products. 3. Techniques of catalyst preparation determine, to a large extent, the process life of nickel catalysts, and these techniques must be thoroughly investigated before any conclusions can be reached. 4. Enough data are available to indicate that the sulfur concentrations in synthesis gas that is used for methanation are extremely critical, and maximum process limits should be carefully evaluated.

Jan 1, 1955