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By R. R. Wells

This report summarizes the results of laboratory testing of copper-bearing magnetite ore from the Poorman, Bush & Brown, and Copper Center deposits, Kasaan Peninsula, Prince of Wales Island, southeastern Alaska. The ores contain minor amounts of chalcopyrite and pyrite. Intimate association of these sulfides with magnetite necessitates fine grinding for adequate liberation and rejection of copper and sulfur and for the production of high-grade iron concentrate low in objectionable impurities. Laboratory tests indicated that the optimum results can be obtained by flotation of ore ground to minus-100-mesh, with subsequent wet magnetic separation treatment of the flotation tailing. A summary of results obtained by this treatment of the three samples tested is shown in table 1.

Jan 1, 1957

By D. E. Wolfson

As a part of its overall program of coal carbonization, the Bureau of Mines is studying the coking properties of coals that may be used for metallurgical purposes. The objectives of this study were given in detail in a previous report.2/ The inherent suitability of coal for metallurgical use depends primarily on (1) chemical composition, (2) preparation characteristics, and (3) carbonization behavior. The first two factors, as well as the available reserves, are considered in selecting coals for carbonization tests.

Jan 1, 1957

By J. R. Nettle

A method has been developed in the laboratory for successfully electro-refining titanium metal. Refining is accomplished in e fused-salt electrolyte using offgrade metal as the anode and collecting the purified metal at the cathode. The characteristics and requirements of the various alkali chlorides tested as electrolytes are discussed in relation to relative ease of purification and serviceability. The various types of cells designed and tested for electrorefining are illustrated and their method of operation discussed. The individual advantage of each cell and the purpose for which it was designed are reviewed. The magnitude of the cathode current density was found to depend largely upon the quantity of soluble titanium chloride in the electrolyte. The physical condition of the anode also greatly affected the cathode current density.

Jan 1, 1957

By Alla D. Mah

Titanium forms several compounds with oxygen and also is able to dissolve interstitially about 33 atomic percent of oxygen. Starting with titanium dioxide, reduction becomes increasingly difficult as oxygen is removed; and the final step, be reduction of the titanium-oxygen interstitial solutions, is by far the most difficult. The possibility of reducing titanium oxide, or of purifying titanium containing oxygen, by treatment with certain more volatile metals has been a subject of considerable interest. Theoretical appraisal of the limitations of this possibility, however, has been hampered by lack of adequate information on the thermodynamic properties of the titanium-oxygen solutions. The purpose of the present work was to remedy this difficulty by expanding the thermodynamic knowledge regarding these solutions. The experimental work involved three types of calorimetry and furnished the following information: (1) Heats of formation of 11 titanium-oxygen solutions, in the range of 0 to 10 wt.-percent oxygen, were determined at 298.15° K. As a byproduct, an improved value of the heat of formation of rutile was obtained, which, in turn, led to improved values of the heats of formation of the lower titanium-oxygen compounds. (2) Low-temperature heat-capacity data and entropies at 298.15°K in were determined for 2 representative titanium-oxygen interstitial solutions. (3) High-temperature heat-content data were obtained for 2 titanium-oxygen interstitial solutions to about 1,600° K.

Jan 1, 1957

By J. P. Powell

The importance of recovering more oil from known petroleum reserves has placed increasing emphasis on the application of secondary producing methods. One of the most successful of these has been the injection of water into depleted oil reservoirs. Water flooding is now recognized as a valuable conservation measure that not only prevents the premature abandonment of stripper leases but also is credited with reviving operations in many oil-producing areas previously abandoned. The injection of water into an oil-producing zone as a method of stimulating oil production was legalized in Kansas in 1935. Although water flooding had been attempted previously in other parts of the State, 1935 marked its introduction into the shallow stripper area of eastern Kansas. Two years later flooding was begun in the five-county area that is described in this report. Figure 1 is a map showing the water-flood areas in Allen, Bourbon, Crawford, Labette, and Neosho Counties, Kans. To July 1, 1955, the 77 projects in the oil fields of these 5 counties are credited with recovering an estimated 12.3 million barrels of oil that would not have been produced by methods used previously. These projects are expected ultimately to cover 10,700 acres, of which only 5,400 has been flooded to date.

Jan 1, 1957

By Clyde L. Brown

Recent developments in portable communication equipment for use in emergency recovery work following mine fires and explosions have wade possible a convenient and dependable means of directing rescue teams working under hazardous conditions. INTRODUCTION Mine rescue and recovery operations following; fires and explosions are frequently conducted under adverse conditions that require the use of oxygen breathing apparatus by members of a 5- or 6-man team. Conventional apparatus used for this purpose for many years was equipped with an oxygen supply adequate for at least 2 hours. The design of the apparatus is such that the nose passages are closed with a clamp, and breathing is accomplished through a mouthpiece connected to the apparatus by tubes and arranged to prevent inhaling air or gases from outside sources. The use of the mouthpiece has presented difficulties in the development of telephone communication because of the wearer's inability to speak while wearing the mouthpiece. The method of conducting operations of rescue teams requires a person to direct operations at a fresh-air base as close to the rescue team as possible. At least one standby rescue team and 2 or 3 other persons assigned to various tasks are stationed at the fresh-air base. An efficient and reliable means of communication between the director of operations and the rescue team is necessary for reasonably safe and efficient work in hazardous areas.

Jan 1, 1957

By Miro Mihelich

The mines and prospects in the vicinity of Landlocked Bay, 25 miles southwest of Valdez, Alaska (fig. 1), were examined, mapped, and sampled in July and August 1955 as part of a comprehensive investigation by the Bureau of Mines of ore deposits adjacent to Prince William Sound. The purpose of the investigation is to establish and record the location, nature, extent, and metallurgical characteristics of copper and associated metallization in the Prince William Sound district and to indicate, if possible, those areas in which additional exploration and development may be justified. Of particular interest are the possibly numerous deposits of massive iron sulfides that were neglected during early mining operations. These deposits may constitute important reserves of sulfur and iron. At Landlocked Bay deposits of copper-bearing iron sulfide minerals have been mined or partly explored through mine workings, which are in a zone about 1 mile wide along the western side of a large overthrust fault known as the Landlock Overthrust. Eight of the principal mines along this zone were examined end sampled. Although only three of the mines have a recorded production of shipping-grade copper ore, all have deposits of copper-bearing iron sulfide minerals that are similar in occurrence. The deposits occur as lenticular masses and disseminations of chalcopyrite, pyrite, and pyrrhotite which replace crushed rock or fill cavities along shear zones in greenstones and in sedimentary rocks that are exposed between sea level and an altitude of 2,500 feet. These lenticular masses of sulfide minerals range in size from small pods to ore bodies that have been stoped to maximum widths of 9 feet, strike lengths up to 70 feet, and dip lengths as much as 350 feet. Where accessible for sampling,, the copper content of the deposits ranged from a few hundredths of a percent to over S percent; zinc, gold, and silver are present in negligible amounts. Flotation tests of a sample composited to represent typical mine-run ore indicate that 81 percent of the copper is recoverable in a product assaying 28 percent copper at a concentration ratio of 17.5 : 1. INTRODUCTION Statistical records indicate that approximately 110,000 tons of metallic copper (about 16 percent of total Alaskan production) was produced from mines adjacent to Prince William Sound during the 40-year period ended in 1938. Although the principal production was from a large-scale mining and milling operation on Latouche Island (Kennecott Copper Corp., Beatson mine), a substantial amount of the total copper was derived from direct-shipping ores selectively mined or hand-sorted from numerous other deposits in the district. No production has been made since 1938; many of the claims have long been abandoned, and mine workings are either caved or deteriorating rapidly.

Jan 1, 1957

By K. E. Stanfield

The Bureau of Mines oil-shale program, initiated in April 1944, is concerned with the future utilization of oil shale in the United States as a source of liquid fuel. One phase of this program is the accumulation of information on the location, extent, and richness of oil-shale deposits that may be suitable for processing to oil and related products. A previous publication5/ presented, by means of logs, the oil yields of sections of the largest known oil-shale deposit in this country -the shales of the Green River formation occurring in adjoining portions of the states of Colorado, Utah, and Wyoming. This present supplementary report presents the oil yields of cores from 48 holes drilled during 1952 to 1954 in the Green River formation of Colorado, which is distributed over an area of more than 1,000 square miles. The oil yields of the 48 oil-shale sections, involving the assay of 9,651 samples, representing 22,451 feet of core, are presented by means of logs. In addition, the oil yields of samples comprising the maximum sections of 15 gallon-per-ton shale are tabulated for these cores and for the 28 cores from Colorado which were logged in the previous report.

Jan 1, 1957

By J. B. Rosenbaum

This report presents new findings and consolidates previously published data to provide a single reference containing a concise and comprehensive description of the Bureau's work on electrolytic chromium. Two separate systems for electrolytic-chromium recovery were developed, one designated as the oxidized system the other as the reduced system. The electrowinning of chromium metal follows the dissolution of chromium from the ore or from ferrochrome and its separation from gangue and metallic impurities. Chromite was first solubilized by pressure digestion at slightly elevated temperatures in an oxidized acid solution using Na2Cr2O7 as an oxidizing agent. Later it was found that a sodium-free electrolyte was preferable, using return-cell anolyte containing H2SO4 and Cr03 as the oxidizing agent. Gangue materials were separated from the soluble metallics by filtration; and, after the Cr+3 had been stabilized, the metallic impurities were separated as crystalline ammonium salts by vacuum crystallization.

Jan 1, 1957

By F. N. Bender

Percolation leaching of wad-type manganese ores was investigated, using a novel system of alternate upward passage of sulfur dioxide gas through moistened ore and downward percolation of wash solutions to extract solubilized manganese. Bench and large-scale tests designed to simulate vat and heap leaching were made on four wad ores from Arizona and Nevada and on a pailomelane ore from Arizona. Three of the wad ores required prebaking at 500° to 600° C. to produce a permeable agglomerate that would not slake during percolation washing. The hard-type ore and one of the wad ores that contained a large amount of granular gangue did not require prior roasting. The deportment of the different ores toward leaching and percolation was studied with particular reference to the influence of the sulfur dioxide - oxygen ratio and the effect of gas dilution on the rate of manganese dissolution, dithionate formation, and acid production. Crushed charges of the ores, as coarse as 1 inch and as fine as 1/4 inch, were treated for periods of 5 to 11 days. Percolation of the gas and leach solutions through the charges was achieved without difficulty. The manganese extractions varied between 78 and 97 percent and depended upon the size and type of ore leached. The average quantity of sulfur dioxide required in the larger scale tests was about 2.6 pounds per pound of manganese recovered. The dithionate formation varied from 0.35 to 0.9 pound per pound of manganese extracted depending upon the strength of leaching gas.

Jan 1, 1957

By T. A. Evans

The Bureau of Mines conducted a Laboratory and pilot-plant investigation of the flotation of iron sulfides from zinc-lead mill tailings near Platteville, in south-western Wisconsin, at the North Central Experiment Station, Minneapolis, Minn. The procedures used and the results obtained in this investigation are described in this report. Samples for laboratory tests were obtained from each mill in the district, namely, Calumet & Hecla, Inc., Eagle-Picher Co., Vinegar Hill Zinc Co., and Tri-State Zinc, Inc. The sample fat pilot-plant work was obtained from the Davis Mining Enterprises mill.

Jan 1, 1957

By Wilbur A. Haley

One of the purposes of the investigation was to determine and report on how coal augers are used to mine bituminous coal that is near outcrops and may not be mined otherwise by any other present-day method. Such increased overall recovery results in the conservation of coal resources. Other reasons for the investigation were to determine and report the production rates of such operations and the types of equipment used. Auger mining of coal as a means of coal recovery supplementary to strip mining has been introduced and developed since World War II. This type of coal mining has grown rapidly, and bituminous-coal production by auger mining has been estimated at 6,000,000 tons in 1955. Mines were selected for study to give reasonably representative information on auger mining in different types and thicknesses of coal beds in different geographic areas and on different types and sizes of equipment operated under various conditions. This report is based on field studies of 8 auger-miming operations in Pennsylvania, West Virginia, and Ohio and in 5 different coal beds. Operations were observed in active strip mines, in strip mines reopened for auger mining, and along benched coal-bed outcrops. At the time of this study, no augers were reported to be operating in underground mines. The diameters of holes drilled ranged from 26 to 52 inches, and the lengths of holes ranged up to 208 feet. At some operations auger holes often penetrated abandoned underground mine workings.

Jan 1, 1957

By Effie T. Kurt, Jack Wright, J. W. Watkins, Cynthia Pearson

"The analysis of water produced with crude petroleum has interested oil producers since inception of the industry. Records of the first analysis of mineralized water produced from an oil-productive formation are obscure, and references to the first use of brine analyses to assist in solving problems of petroleum production are not available in the technical literature. However, many early reports of the Federal Bureau of Mines 5-8/ and. Federal Geological Survey, 9-11/ as well as articles in engineering and geological placed special emphasis on journals ,12-l4/ the importance, interpretation, and application of water analyses.One of the earliest applications of water analyses, and still a major one today, is for identification of intrusive waters in oil wells. This may be done by comparing the chemical constituents of a sample of water indigenous to the oil-productive formation with those of samples from upper, water-bearing formations within the same general area. Some earlier investigators recognized the need for analyzing samples of all waters encountered in drilling operations. Ambrose15/ stated, in part, ""In wells being drilled, the engineer should grasp every opportunity to get a true sample of water from each sand. . .,"" and, ""The waters of each oil field are chemically different from those of another field."" The validity of the latter observation and the importance of the former one have been borne out by comparing the results of analyses of many samples and noting the differences in relative concentrations of like constituents of waters from the same geological formation in different localities or oil pools."

Apr 1, 1957

By Jack Wright

The analysis of water produced with crude petroleum has interested oil producers since inception of the industry. Records of the first analysis of mineralized water produced from an oil-productive formation are obscure, and references to the first use of brine analyses to assist in solving problems of petroleum production are not available in the technical literature. However, many early reports of the Federal Bureau of Mines5-8 and Federal Geological Survey,9-11/ as well as articles in engineer and geological journals12-14/ placed special emphasis on the importance, interpretation, and application of water analyses. One of the earliest applications of water analyses, and still a major one today, is for identification of intrusive waters in oil wells. This may be done by comparing the chemical constituents of a sample of water indigenous to the oil-productive formation with those of samples from upper, water-bearing formations within the same general area. Some earlier investigators recognized the need for Analyzing samples of all waters encountered in drilling operations. Ambrose15/ stated, in part, "In wells being drilled, the engineer should grasp every opportunity to get a true sample of water from each sand. . .," and, "The waters of each oil field are chemically different from those of another field." The validity of the latter observation and the importance of the former one have been borne out by comparing the results of analyses of many samples and noting the differences in relative concentrations of like constituents of waters from the a geological formation in different localities or oil pools.

Jan 1, 1957

By H. Kenworthy

The investigations described in this report were undertaken to demonstrate, on a laboratory scale, the possibility of recovering several million pounds of tin plus tungsten contained in stockpiled and currently rejected slags from the Longhorn tin smelter at Texas City, Tex. At the same time, it was anticipated that the treatment procedures developed might be applicable to slags from other tin-smelting operations. Results of the laboratory work show that it is possible, by pyrometallurgical means, to separate the tin and tungsten into products of intermediate grade that may be returned to the smelter circuits for further upgrading. Several methods of treatment were investigated. The methods that proved effective were: Fusion reduction, chloride volatilization, sulfide volatilization, and carbide formation. Over 90 percent of the tin and tungsten could be removed from the slat by any of these methods. Each type of treatment has advantages and disadvantages, and it could not be determined from the small-scale work which method was the more meritorious. Tungsten and (in some types of treatment) tin-bearing products were diluted by iron, the separation of which will require additional studies. Prevention of a portion of the iron from reporting with the tin or tungsten is a distinct advantage and possibility that will require inure laboratory work to develop the needed techniques for its accomplishment. Tin products from single treatments of stag ranged up to 75 percent in tin content but were more generally under 35 percent. Tungsten products were usually under 15 percent; but segregated portions could be selected, at a sacrifice in recovery, that contained up to 50 percent tungstic oxide equivalent.

Jan 1, 1957

By H. E. Peterson

A study was undertaken by the Bureau of Mines to develop a simple, reliable test for field detection of selenium in rocks and soils. Two methods are described for qualitative detection of selenium, dependent upon its form of occurrence and the presence of interfering constituents in the sample. Both methods involve fusion of the sample in a test tube to form elemental selenium that will volatilize and condense as a red deposit on the cooler upper portion of the test tube. The methods are sensitive to 10 parts per million, (p.p.m.) equivalent to 0.001 percent, and can be made semiquantitative by using suitable standard samples. INTRODUCTION Although selenium is widely distributed in the United States, the known deposits are either so small or so low grade that they cannot be processed economically for selenium alone-4/ At present, commercial production is a byproduct of the smelting and refining of base-metal ores, particularly copper.5/ About 0.75 pound of selenium is recovered per ton of electrolytic copper, and small amounts are recovered by special treatment of assorted smelter dusts and fume products. Since selenium is a strategic metal in short supply, new sources are being sought by both Government and private interests.

Jan 1, 1957

By R. A. Meyer

A table that greatly simplifies determination of metastable transitions in mass spectra has been prepared. All the mathematically possible metastable transitions of any compound whose molecular weight lies between 26 and 150 can be determined from the table without calculation. The method of utilizing the table is described, using selected peaks from the spectrum of normal butane for illustration. In the mass spectrometer, ions are formed in the isatron and accelerated through a series of slits. Most of these ions reach the collector without further change, but a few dissociate in transit to form new ions. These ions appear in the mass spectrum at neither the mass--to-charge ratio (m/e) of the original ion nor that of the new ion. A formula that relates the appearance of these new ions to the ion from which they were formed is: [ ]

Jan 1, 1957

By Oren C. Baptist

[Several new oilfields have been developed in northwestern Wyoming during the past 10 years, production is obtained from discontinuous, permeable sands enclosed within impermeable shales. The energy to drive the oil to producing wells in supplied by gas in solution in the oil. Most of the wells had high-initial potentials, but rates of oil production have steadily declined, indicating a dissipation of the driving energy and the possibility that large volumes of oil will remain unrecovered in the reservoirs. The studies reported in this paper were undertaken to develop laboratory data of the type most likely to be needed by persons studying the susceptibility of the Newcastle sand reservoir to secondary-recovery methods.]

Jan 1, 1957

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions4/ issued by the Bureau of Mines, the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1957

By Frank C. Morris

It is generally recognized that the productivity and ultimate recovery of an oil well may be reduced as a result of reduction in permeability of the sand at the well bore by invasion of filtrates and clay particles from drilling fluids. As a means of determining whether a sand has been "damaged" from these sources, several investigators2 3 4 5/ have developed methods of analysis based on the rate of increase in bottom-hole pressure while a well is shut in. Because of growing recognition of the importance of completion practices as related to the quantity of oil that may be recovered from wells, the Bureau of Mines has studied completion practices in California and the Midcontinent area. Well-interference and pressure-buildup tests were completed Ear seven wells in the Scurry Reef field to determine the effective permeability in the reservoir.6/ Also, a study was made of the pressure-decline curves obtained from 35 water-input wells in 5 different production areas of northeastern Oklahoma and eastern Kansas.7/

Jan 1, 1957