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By Harry Freund

Gallic acid is a sensitive, stable, colorimetric reagent for the determination of tantalum in the range of 2 to 40 µg.Ta/ml. The method consists of the fusion of tantalum oxide with potassium pyrosulfate and solution of the cooled melt in satu-rated ammonium oxalate, followed by development of a yellow complex with an ethanolic solution of gallic acid. The tantalum-gallic acid complex absorbs over a broad region in the blue and near ultraviolet. Adverse effects due to interfering ions and solution conditions, such as oxalate concentration and pH, can be minimized by a suitable choice of wave length. A new and sensitive colorimetric method is provided that has been used successfully at the Northwest Electrodevelopment Laboratory of the Federal Bureau of Mines for determining minor amounts of tantalum.

Jan 1, 1956

By E. G. Erspamer

Laboratory investigations were made by the Bureau of Mines on ore containing the sulfides of both mercury and antimony to develop a method or methods for the economic recovery of mercury metal and the concurrent recovery of antimony as metal or salts,. If standard mercury-recovery techniques are applied to such ores, the antimony content interferes with the effective production of mercury metal; further-more, the antimony is lost. This report presents the results of tests on a sample of cinnabar-stibnite ore from the Red Devil mine near Sleitmute, Alaska. Red Devil ore was chosen for the investigation because it is purported to be typical of ores of the Kuskokwim River area, which, in their aggregate, constitute large potential reserves of mercury and antimony. Studies included petrographic, spectrographic, and chemical analyses, gravity-separation tests, bulk flotation of mercury and antimony sulfides, differential flotation, leaching, and furnacing of crude ore and of flotation concentrate.

Jan 1, 1956

By B. E. Blair

The physical properties and related geological and petrographic data for 81 rock types obtained from operating mines or selected test sites are presented in this report. Most of these rock data were obtained to supplement structural studies in underground mines; however, the data may be equally applicable to other problems where the physical properties of rock are an important factor. Stress-strain curves are presented, where available, and free medium velocities from laboratory and field measurements are compared for several rock types. Rock-type, geographical, and geo-logical indexes are included for reference relative to physical property data in this and previously published Bureau of Mines physical property reports. INTRODUCTION This report presents the physical properties of 81 rock types from 16 different projects (sections 53-68). Three previous physical property reports2 3 4/ (herein after referred to as parts I, II, and III) presented data on 244 rock types from 52 project areas. (Part I included sections 1-25, part II sections 26-36, and part III sections 37-52).

Jan 1, 1956

By R. R. Wells

This report summarizes the results of preliminary mineral-dressing studies by the Bureau of Mines on five samples of copper-bearing ore from various Alaska de-posits. The work on each sample was not extensive enough to warrant individual publication. The results, however, indicate the possibilities and limitations of concentration of the respective ores. The information therefore may be helpful in future development of these ore bodies. Four of the five samples tested were submitted to the laboratory by engineers of the Bureau of Mines as part of the examinations and survey investigations of strategic-mineral deposits in Alaska. This program is conducted to assist development of mineral resources in the Territory and particularly to aid economic exploitation of marginal or complex ores. The fifth sample was submitted by engineers of the Defense Minerals Exploration Administration.

Jan 1, 1956

By D. W. Frommer

The investigation reported in this paper is one of several included in a broad program of developing new or improved concentration processes for the oxidized and partly oxidized deposits of lead and zinc, A sample from the Playter lease, Newton County, Mo., containing pyromorphite was successfully concentrated by fatty acid flotation to a grade of over 62 percent lead. Owing to the presence of a high content of slime-size values, the overall recovery of lead at that grade was limited to 44 percent. DESCRIPTION AND HISTORY OF PROPERTY The mineral pyromorphite is a chlorophosphate of lead containing 76.4 percent lead, and, although it occurs frequently in association with other lead minerals, it is considered a minor ore mineral of lead. The manner of occurrence of oxidized lead minerals, including pyromorphite, which frequently are no larger in grain size than the clay with which they are found, militates both against development of a simple beneficiation process and high recovery. The profitable exploitation of such deposits depends not only on a successful treatment procedure but a highly favorable metal market as well. For these, and perhaps other reasons, very little research has been done on the recovery of pyromorphite from its deposits.

Jan 1, 1956

By R. A. Beall

Consumable-electrode arc melting is now accepted throughout the industry as the best method for producing ingots of zirconium, titanium, molybdenum, and their alloys. In addition, the technique is widely used in laboratories for fusing samples of such metals as hafnium, chromium, tantalum, columbium, and thorium. The production of consumable electrodes from these metals presents some rather difficult problems, the accepted industrial solution being the use of heavy powder-metallurgy-type presses. This paper summarizes information on fabrication of consumable electrodes by this and alternative means, such as sintering, nippling, and welding lightly pressed compacts of scrap metal. A possible saving of considerable capital investment is shown in the case of sintered compacts. The electrical circuit components of a pilot sintering unit are analyzed. INTRODUCTION The consumable-electrode arc-melting process has been accepted by most of the industry as the best method at present for producing high-quality pure or alloy in-got from sponge titanium or zirconium. This technique is not particularly new, having been patented by Von Bolton (l)3/ in 1909 for melting tantalum. However, it has been applied to industrial-scale operation only in the last few years. Among the important contributions to this technique are the work of Kroll (2) and Parke and Ham (3) and the work reported by the Office of Naval Research (4). The Bureau of Mines-has added considerably to the knowledge of this process (5-9).

Jan 1, 1956

By C. T. Baroch

This report summarizes cost data accumulated during 15 months of sustained operation of the Bureau of Mines Boulder City (Nev.) titanium plant, which had a capacity of about 1,350 pounds of titanium sponge per day. The plant was constructed during the 1952 fiscal year with funds supplied by the Ordnance Corps, Department of the Army. Its original purpose was to engage in process development work as a continuing phase of the Bureau of Mines policy to seek improvements in producing titanium metal. In early 1953 the Defense Materials Procurement Agency contracted with the Bureau of Mines for producing approximately one-half million pounds of usable ductile titanium sponge. Production began in May 1953, ended in September 1954, and yielded 492,503 pounds of acceptable metal. Operating costs covering this period of operation, with suggested depreciation and administrative costs, are given, as well as outlines of building and equipment capital costs. In addition, miscellaneous economic considerations are discussed, including labor and operating-time schedules.

Jan 1, 1956

By E. L. Garton

Bureau of Mines routine crude-oil analyses of 88 samples from 60 fields are presented in this report. Similar analyses from other fields in California have been published in previous reports listed in the appendix, page 52. Yearly production of crude oil in California and the percentage of United States production represented by California production for 1948-54 are given in table 1. [ ] Analyses in this report are of samples from the fields listed in table 2, with production data for 1953, cumulative production through 1953, and year of discovery of each field. Information regarding the source and general characteristics of the samples is included in table 3 with a summary of analytical and computed data.

Jan 1, 1956

By J. A. Rowland

Magnesium alloys containing nickel, nickel and manganese, lithium, lithium and manganese, and lithium and aluminum were investigated. Melting, casting, and mechanical working techniques and the heat treatment of various compositions were studied. Amenability to cold and hot working was shown for many compositions. The magnesium-nickel and magnesium-nickel-manganese alloys failed to develop superior mechanical properties and were very low in resistance to corrosion. The magnesium-lithium series, although entirely plastic, had low strength properties. The addition of small amounts of aluminum to the Mg-Li base did not affect greatly either the ductility or the strength; further additions developed increased strength, but only at room temperature, and the alloys became brittle with age. Continued study, concentrating on the ductile lithium-rich beta phase as a base composition for ternary and quaternary systems, is recommended.

Jan 1, 1956

By P. N. Summerfield

This report describes the first phase of a general investigation designed to ascertain whether an electronic roof-testing device can be developed that will improve the ability to detect "loose" or "drummy" roof rock over that possible by striking the roof with a sounding bar and noting the character of the air vibrations with the unaided ear or the rock vibrations with the fingers. The amplitude, frequency content, and duration of the vibrations produced by striking solid and drummy roof rock with a hammer or sounding bar have been measured. Results disclosed that there is a significant difference between the characteristics of the vibrations produced in solid and drummy roof. This difference is such that the design of an electronic device to indicate quantitatively the condition of the roof rock appears possible. INTRODUCTION The conventional method of roof testing consists of striking the roof with a bar2/ and judging its soundness from the character of the air vibrations heard with the ear and/or the rock vibrations felt with the fingers -a procedure that depends upon the experience and the sensory abilities of the observer. Impact testing of a solid roof rock usually produces a sharp ping or click, whereas impact testing of a drummy roof rock produces a dull thud or drummy sound. This method of roof testing is, at most, only a qualitative test, and many roof rocks are difficult to classify as drummy or solid.

Jan 1, 1956

By M. M. Fine

A preliminary mineral-dressing study of five samples of East Texas limonitic brown iron ores was conducted as part of the Bureau of Mines program to develop and extend domestic resources of iron ore. The samples were considered to be typical of ore currently being mined and beneficiated by the Lone Star Steel Co. and Sheffield Steel Co. The objective of the research was to investigate those mineral-dressing unit operations that might recover some of the fine iron lost in current industrial wastes or perhaps improve the recoveries when applied to the ores as well. Since current industrial beneficiation practice yields a washed limonite analyzing 41 to 45 percent iron, higher grade concentrates were not sought in this laboratory study. Laboratory investigation included washing and sizing, reduction roasting, and subsequent magnetic separation of the finely ground roasted materials. The results showed that laboratory recoveries of over 80 percent of the iron were possible, for the ores investigated, at concentrate grades comparable to those expected from cur-rent industrial beneficiation practice. ACKNOWLEDGMENTS Acknowledgment is made to the Lone Star Steel Co. and Sheffield Steel Co. for supplying the brown iron-ore samples on which this research was conducted.

Jan 1, 1956

By C. T. Baroch

As part of a general program for investigating all phases of titanium production, argon was substituted for helium in the reduction step at the Bureau of Mines pilot plant, which employed a modification of the Kroll, or magnesium-reduction, process. Argon was substituted for helium in 108 of the 140 batches of sponge made during 1 month's reduction operations for July 1954. Argon was substituted for helium satisfactorily, with only slight modifications in technique. Metal quality, feed rate of TiC14, magnesium efficiency, and average production per batch were closely comparable with either gas. Argon runs were slightly more troublesome because of the formation of condensable chloride complexes, which tended to plug feed and vent lines and to entrap deposits of lower titanium chlorides on the reactor-pot lids. These lower chlorides were objection-able because they were pyrophoric and created obnoxious fumes when pots were opened. When feed and vent lines became plugged care was required in poking or unplugging these lines to prevent air from entering the reactor. These problems were relatively minor, and continued development of reactors and techniques for the use of argon should further minimize objectionable side reactions obtained when argon is used.

Jan 1, 1956

By M. E. Volin

To extend or delimit the known ore reserves of the Black Wonder manganese de-posit, the Bureau of Mines undertook an exploration project consisting of trenching, underground excavation, long-hole drilling, and sampling. The mineralization is spread over 6 square miles containing numerous small individual manganese deposits. There has been only small production from some of these deposits; however, simultaneous operations from many such small deposits could contribute considerably to the production from the district. A custom mill to treat oxide ore for battery use was built near Patterson in 1942 by the General Dry Batteries Co., Inc. It operated during World War II and was removed in 1944 when the manganese mines ceased operation. Except for some small experimental shipments, there has been no activity in the district since that time.

Jan 1, 1956

By W. A. Stickney

The Bureau of Mines conducted beneficiation and smelting studies on siliceous offgrade manganese samples to indicate effective methods of manufacturing silicomanganese from materials that cannot be economically beneficiated to meet General Services Administration (GSA) specifications for stockpiling. Laboratory and pilot-plant flotation tests were conducted on 2 samples, 1 from the waste-tailings dump of the Domestic Manganese & Development Co , Butte, Mont., and the other from the Nettie mine in the Butte-Philipsburg area. Smelting tests were made on the combined concentrates from the pilot-plant flotation tests and on part of the tailings sample The flotation scheme found to be adequate in laboratory tests and later in the pilot-plant tests consisted of flotation by a fuel oil-tall oil emulsion in an acid circuit (pH )-1-.8 to 5.0). The oil-emulsion reagent flocculated the manganese minerals and selectively floated them from the siliceous gangue, In the pilot-plant flotation test on Butte-mill tailings 90.1 percent of the manganese was recovered in a concentrate that analyzed 32.6 percent Mn, 4.8 percent Fe and 28.1 percent Si02. In the test on Nettie mine ore 90.8 percent of the manganese was recovered in a concentrate that analyzed 36 6 percent Mn, 5.5 percent Fe, and 26-4 percent Si02.

Jan 1, 1956

A spectrochemical procedure applicable to the determination of iron, manganese, and magnesium in titanium metal and to the determination of alloying constituents in three types of titanium alloys is presented. Acid solutions of samples and standards are excited with a spark-type discharge and porous-cup electrode arrangement. The method is particularly applicable for analyzing samples for which a self-electrode method cannot be used. Calibrations are accomplished with synthetic standard solutions, resulting in a primary method that makes calibrations based upon results of other analytical methods unnecessary. Replicate determinations are reproduced to within 5 percent, and the average percentage deviations from reliable chemical values are less than 6 percent. The method can be extended readily to determine additional elements that are similarly soluble and have similar spectral sensitivities. It also can be used as a starting point to establish standards for a direct sparking procedure for analyzing titanium alloys. In view of the absence of established reliable analytical methods in the titanium industry, the spectrochemical method described here should prove to be a timely contribution.

Jan 1, 1956

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 The inherent suitability of coal for metallurgical purposes depends primarily on (1) chemical composition, (2) preparation characteristics, and (3) carbonization behavior. The first two factors, Be well as the amount of available reserves, are considered in selecting coals for carbonization tests. The selection of coal beds in Harlan County, Ky., for coking tests was based, in part, on recent studies of coal reserves by Wallace,3/ who estimated the recoverable reserves in beds 28 inches or more thick, in tons, as follows:

Jan 1, 1956

By Lloyd Williams

1. The investigation shows that the Coal Creek has been the most productive, bed in Campbell County and contains the largest recoverable reserves of coal. The Pewee, Red Ash, and Jullico have been relatively productive beds and contain appreciable recoverable reserves of coal. The Blue Gem also has been productive in the past, but available information indicates that most of the remaining coal is Less than 28 inches thick. The Big Mary has relatively large reserves over 28 inches thick, but the coal is high in ash and sulfur. Thick partings in the Windrock bed have discouraged mining in that bed. The Poplar Creek and Rex beds generally are below drainage, and large areas have been excluded from the reserve estimate, Reserves in the Walnut Mountain bed will be difficult to mine due to the irregu¬lar thickness and lack of continuity of the bed. Estimated coal reserves are- small in the remaining five beds. 2. Known measured and indicated reserves of coal, based on a minimum bed thickness of 14 inches and on 1,800 short tons per acre-Foot of coal in place, are estimated to be 398 million tons as of January 1, 1953, o? this total, 267 million 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, these should be added to the total estimated reserves.

Jan 1, 1956

By William H. Tavenner

1. The 1952 Annual Report of the West Virginia Department of Mines lists nine beds that arc being mined in Logan County, of which the Cedar Grove and Chilton are the most important. The Cedar Grove group, No. 2 Gas, and Alma beds have the largest remaining reserves, in the order given. 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 5,411 million tons as of January 1, 1954. Of this total, 3,939 million 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 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 estimate reserves.

Jan 1, 1956

By J. J. Hoeppner

Lignite samples were collected so as to be widely representative of the extensive deposits in the western north-central area. These were carbonized at temperatures ranging from 450° to 550° C., according, to a standardized procedure. In general, product yields varied; extremes obtained on selected samples show char recoveries on the moisture- and ash-free basis as 56.7 percent for slack lignite or "leonardite" to 80.8 percent for a concentrate of the fusain component from a typical face sample; normal lignite samples averaged approximately 70 percent. Tar-plus-light-oil yields ranged from 3.3 percent for the fusain concentrate to 11.0 percent for a normal sample, averaging approximately 8 percent; gas recoveries varied more widely both in yield and in composition, ranging, from 10.0 percent to 27.7 percent, the latter being from leonardite and quite high in carbon dioxide. Sampling was conducted with the view of representing, as nearly as possible, all beds delineated by Brant (2);4/ many are necessarily missing since collection was confined largely to worked deposits. Data presented in this report indicate a general uniformity of North-Central lignite in respect to low-temperature carbonization, with a few possible exceptions of a local nature. When processed according to the indicated conditions, maximum tar yield may be realized with minimum loss of recoverable heating value of the original coal. Natural weathering of lignite, however, does affect tar yield adversely and should be held to a practical minimum in any commercial operation.

Jan 1, 1956

By J. E. Shelton

Flotation tests are described on samples of two lowgrade nickeliferous ores of Oregon and Washington. The sample from the Congress mine, Ferry County, Wash., contained 1.2 percent Ni, occurring chiefly as millerite. The sample from the Shamrock mine, Jackson County, Oreg., contained 2.20 percent Ni and 0.78 percent Cu occurring chiefly as pentlandite, nickeliferous pyrrhotite, and chalcopyrite. The millerite in the Congress ore was concentrated by flotatioin with aulfydric collectors in a series of locked tests to recover 73 percent of the nickel as a 7 percent bulk concentrate. By successively regrinding and floating the bulk concentrate, it was further concentrated to 12.4 percent Ni at a recovery of 59 percent and 21.8 percent Ni at a recovery of 50 percent. Attempts at selective concentration of the copper-nickel Shamrock ore were only partly successful because of the intimate association of pentlandite and chalcopyrite. The nickel concentrate, which contained 86 percent of the nickel, had an analysis of 4.42 percent Ni and 1.03 percent Cu. The copper concentrate had an analysis of 18.8 percent Cu and 1.96 percent Ni and contained 48.5 percent of the copper. A bulk sulfide concentrate contained 92 percent of the copper and 01 per¬cent of the nickel and had an analysis of 4.17 percent Ni and 1.63 percent Cu.

Jan 1, 1956