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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

By M. M. Fine

Small-scale laboratory mineral-dressing studies were made on a total of nine individual or composite samples of manganese-bearing material from the west-central Arkansas, or Mena, district. Of these, only three yielded concentrates that would probably be acceptable for purchases by the Federal Government fur the National Stockpile. Concentrates from some of the other properties, however, contained more than 40 percent Mn and might be merchantable to other purchasers of manganese ore. In most instances, a too-intimate association of manganese oxides and gangue is conducive to low grade, low recovery, or both, so that mechanical concentration processes do not promise much for this district.

Jan 1, 1956

By Robert E. Hershey

1. Estimates of reserves were made for three coal beds in Hamilton County the - Lantana, Sewanee, and Richland. Nine coal beds have been mined at one time or another in the county, but not enough information was available to estimate reserves in any beds other than the three given. 2. Known measured and indicated reserves for all beds, 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 53 million tons as of January 1, 1954. Of this total 35 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 insufficient for making an estimate conforming with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove re-serves in these areas, such reserves should be added to the total estimated reserves determined by this investigation.

Jan 1, 1956

By Irving Hartmann

As part of the continuing effort by the Bureau of Mines to promote mine safety, research work is being conducted at the Experimental coal mine, Bruceton, Pa., on the prevention of coal-mine explosions and on other mine-safety problems. The principal subjects studied during the past 2 years are briefly described in this paper. Although at present these problems are relevant particularly to the mine layout and to high-speed mining practices in numerous American coal mines, it is hoped that the findings will prove interesting and useful also to our European research colleagues. Some of the investigations treated here will be presented in greater detail in forthcoming Bureau of Mines reports. 1. UNDERGROUND STORAGE OF COAL CUTTINGS The seams in mist American bituminous-coal mines are undercut, shear-cut, or top-cut before blasting. The cuttings arc generally loaded out with the balance of the coal. However, in some mines it is not economical to load and remove cuttings from the mine. This applies especially if the cut section of the seam is of appreciably lower grade than the rest of the coal, or if the cut is made partly into an adjacent stratum that is high in incombustible content. In such mines the cuttings are sometimes stored in random heaps in rooms or other areas, along the ribs of mine entries, or in layers on the floor of rooms or entries.

Jan 1, 1956

By R. A. Beall

This paper summarizes the development of a furnace for producing titanium castings. The general problem is outlined and chronological details are given on the construction and operation of four different casting furnaces, all utilizing consumable-electrode arc heating and water-cooled copper crucibles. Of the two methods of pouring, the tilt-pour technique has been more satisfactory than bottom tapping. Mold design, electrode fabrication, and deep-pool production are discussed. INTRODUCTION In the early summer of 1953 the Bureau of Mines was contacted by the Department of the Army through Watertown Arsenal to explore the possibility of conducting research on casting titanium metal. The objective of the program was "to develop a technique for producing formed castings of titanium metal not less than 40 pounds in weight and without introduction of deleterious contamination."

Jan 1, 1956

By Lloyd Williams

1. The investigation shows that the Poplar Creek and Big Mary beds contain the largest known recoverable reserves of coal in Morgan County, Tenn. The Poplar Creek bed has been the most productive. 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 96 million tons, as of January 1, 1954. Of this total, 59 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 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, 1956

By J. M. Provost

1. Estimates have been made for eight coal beds in Marion County, but only the Pittsburgh is important from a production standpoint at this time. The Pittsburgh bed has the largest recoverable reserve, and the Sewickley is second in importance. 2. Known measured and indicated reserves thickness of 14 inches and on 1,800 short tons estimated at 3,141 million tons, as of January lion tons is in beds 28 inches and more thick in all beds, based on a minimum per acre-foot of coal in place, are 1, 1955. Of this total, 2,983 mil-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 estimated reserves.

Jan 1, 1956

By J. P. Walsted

Offgrade chromite concentrate, with a Cr-Fe ratio of 1.3 to 1.4 has been successfully smelted to produce useful ferroalloys. The Cr-Fe ratio is not improved, but the alloys can be used without a too drastic change in normal steel-mill practice. The ordinary high-carbon ferrochrome has been successfully produced by smelting under highly acid smelting conditions. An alloy containing 50 percent chromium was produced at a power consumption of 4,490 kw.-hr. per ton of alloy. Alloys containing 20 percent silicon were made by direct smelting chromite concentrate and silica.

Jan 1, 1956

By D. E. Wolfson

As part of its overall program of coal-carbonization research, the Bureau of Mines is studying the coking properties of coals from various fields of this country. Few of the coals included in this survey are used for the manufacture of metallurgical coke, although some well-known coking coals necessarily are tested to provide comparative data, particularly on blending properties. The overall objectives of the study were given in detail in a previous report.3/ The inherent suitability of coal for metallurgical purposes, as distinguished from economic considerations, depends primarily on (1) the available reserves, (2) chemical composition, (3) preparation characteristics, and (4) carbonization behavior. These items are considered in selecting coal for carbonization tests.

Jan 1, 1956

By M. L. Skow

Large tonnages of the manganese ores found in Aroostook County, Maine, are refractory to conventional mineral-dressing techniques and to the common chemical- extraction procedures. The Maple Mountain-Hovey Mountain ores are typical of this type. Because the most promising method of recovering the manganese from these ores has been a chloridizing roast in which the ground ore is in contact with gaseous hydrogen chloride, preliminary batch tests were made with a fluidized bed. On the basis of these tests, it was concluded that fluidization, with careful control of operating conditions, could be employed for this cloridization and warrants further study. Selective volatilization of the iron at 600° C. was unsuccessful. An operating temperature of approximately 950° C. was necessary for a practicable rate of volatilization of manganese chloride. Hydrogen chloride contents of 10 to 100 percent of the fluidized gas gave essentially equivalent manganese recoveries with an 80- minute retention time, For shorter periods reaction was more complete with the higher hydrogen chloride concentrations. At the 80-minute retention period the lower hydrogen chloride concentrations volatilized somewhat less iron and also improved the physical operation of the process. Fluidization gave results superior to comparable tests on chloridization in a fixed bed.

Jan 1, 1956

By Ralph H. Whaite

To assist the anthracite industry obtain technical data on pneumatic packing, the Federal Bureau of Mines imported a pneumatic packing machine from Germany and installed it in a mine of a cooperating company in the Northern anthracite field of Pennsylvania. This report covers the second in a series of experiments in applying pneumatic packing for controlling strata movement (subsidence) above mine workings in the Pennsylvania anthracite region. The first experiment2/ was begun in January 1950, in a section of the mine where about 50 percent of the original coal remained in the form of pillars; since the company did not plan to mine the pillars in this particular area, pneumatic packing of the chamber voids was done for test purposes only. During this initial test the machine was operated on 204 shifts, and 652,400 cubic feet of breaker refuse material (22,834 tons) was packed into the voids of 16 chambers. The work was completed in December 1951.

Jan 1, 1956

By J. S. Browning

The purpose of this Bureau of Mines project was to develop a method for recovering kyanite and sillimanite from the present zircon-mill tailing of the Jacksonville and Starke, Fla., plants of Humphreys Gold Corp. The kyanite and sillimanite in the ore are not being exploited at present, but procedures for recovering the two minerals were worked out by the Bureau in the interest of conserving natural resources. The current zircon-mill tailing of the Starke plant contains up to 20 percent of a mixture of kyanite and sillimanite. A similar product of the Jacksonville plant contains up to 15 percent kyanite and sillimanite. The average annual production of the tailing now being stockpiled contains several thousand tons of the two minerals. Laboratory batch-flotation tests were made on the materials to determine the feasibility of flotation methods for recovering high-grade concentrates. Various reagents were employed under different conditions to determine the optimum conditions for flotation of kyanite and sillimanite and retardation of the gangue materials. The results of the preliminary flotation tests were encouraging enough to warrant more comprehensive testing of a larger sample of the ore in the laboratory pilot plant.

Jan 1, 1956

By F. E. Block

The reaction between calcined dolomite and ferrosilicon has been studies with the aim of developing a continuous process for magnesium production. Small-scale tests were made in vacuum retorts similar to those used in the vacuum retort process as developed by Pidgeon (1)2/ and operated during the period of World War II in several Government-owned plants. Factors investigated with respect to the silicon efficiency were the reaction temperature, reaction time, amount of excess dolomite in the charge, and effect of adding sodium silicate to the charge to serve as a binder. Additional laboratory tests were made to study the reaction at elevated temperature but at atmospheric pressure. Silicon efficiencies exceeding 80 percent were found to result when operating in the temperature range from 1,750° to 1,800° C. for periods of 20 to 30 minutes.

Jan 1, 1956

By John B. Gayle

The suitability of fluid petroleum coke as a blending agent for producing metallurgical coke has been investigated using the Tuscaloosa and sole-heated experimental ovens. From the results of tests with three representative blends, it has been fond that additions of fluid petroleum coke effect the following changes: (1) Increase in size, resistance to shatter, and apparent specific gravity of cokes produced; (2) little or no change in coke hardness and stability or in the amount of breeze formed; (3) increased charge density; (4) modification of expansion characteristics of blends charged; and (5) decreased ash and increased sulfur contents of blends charged and cokes produced. Substitution of a calcined sample of fluid coke of greatly reduced sulfur content resulted in a coke of inferior physical properties. This effect indicates that additions of the calcined product should probably be limited and that other methods for producing a low sulfur fluid coke should be considered.

Jan 1, 1956

By Manuel Gomez

A lignite from Milam County, Tex., has been oxidized by air at temperatures from about 27° to 300° C. for varying lengths of time. The oxidized coal was carbonized at 500° C. in a laboratory assay unit, and the products of carbonization were measured and analyzed. The data presented suggest that, as lignite is progressively oxidized, tar yields are decreased and gas yields are increased in a ratio approximating 1:1. It is surmised that tar-yielding structures in the nonoxidized coal produce gas, principally, when the coal is oxidized. Char-yielding structures of the nonoxidized coal give rise to additional water of decomposition after oxidation and pyrolysis. As lignite is subjected to greater oxidation, the gaseous product evolved on pyrolysis becomes almost entirely carbon dioxide. Tar yields decrease with an increased degree of oxidation, so that the reduction in tar yield may be used as a qualitative measure of oxidation. Pilot-plant drying and carbonization, where air is used as the transport gas and where some air is included in the drying and carbonizing gases, induces some oxidation of the coal particle. The short residence time in a fluidized system with reference to the oxidation environment limits the oxidation.

Jan 1, 1956