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By P. R. Perry

This publication is a compilation of tested methods for the analyses of titanium tetrachloride, titanium sponge, and various intermediate materials and products. They are presented in concise form without the detail usually found in publication of new methods because many of them are modifications of well known procedures. The Electrometallurgical Experiment Station, Boulder City, Nev., has been developing titanium production methods since 1945. Most of this development was on a modified Kroll Process but also included work on sodium reduction and electrolytic methods. During these years a large variety of samples were analyzed. Most of the analytical problems were solved using published methods or modifications of the same. At the start, there were no published procedures for analyzing titanium sponge using spectrochemical methods. A great deal of study was given to testing several of the well known techniques, and some of them, such as direct sparking of the metal, proved to be completely unsatisfactory. Solution-spark techniques were finally tried, and satisfactory procedures were developed for some of the more common impurities. These spectrochemical methods were then put into routine use for several months before their publication.2/ Some new modifications have been made, and techniques have been developed to determine other impurities found in titanium sponge and tetrachloride. All spectrochemical methods used in 1954 are included in this publication.

Jan 1, 1955

By J. H. Bilbrey

A recording thermobalance ,vas used to determine the rates of oxidation of mol-ten tin over the temperature range 550°-900° C. Oxidation rates were found to vary widely for a given temperature, as previously reported by other investigators. 1 X-ray diffraction data indicated that the probable cause of these variations was the development of preferred orientations in the crystals forming the oxide film. No reasons for the differences in degree of preferred orientation were discovered. For relating the weight of the oxide formed (w) to the time of oxidation (t) an equation of the form wn = kt was found to best represent the experimental data. INTRODUCTION In the course of conducting investigations on the feasibility of using selective oxidation techniques for the purification of various metals in the molten state it was soon discovered that data on the oxidation of molten metals and alloys were very scarce. In contrast to the many hundreds of publications on the oxidation of metals in the solid state there are relatively few articles on the rates of molten-metal oxidation. In view of this scarcity of data, it was decided to institute a series of investigations into the oxidation processes of molten nonferrous metals and alloys with the expectation that the information derived could be put to practical use in developing and improving refining processes based on selective oxidation. This report is the first of a series in which oxidation data for molten nonferrous metals and alloys are presented.

Jan 1, 1955

By Lloyd Williams

1. The investigation shows that the Sewanee bed is the only bed of major importance in Marion County, 97 percent of the coal mined in the county having come from this bed. There are coal reserves in minor quantity in the Battle Creek bed, and production from this bed depends on a few small truck mines. The Richland bed, or Lower Sewanee, has been mined in the past, but no coal has been produced from it in late years. There are no production records of any other beds in the county, although same coal has been produced from them. 2. Known measured and indicated reserves in all beds, based on a minimum thickness of 14 inches and on 1,800 tons per acre-foot of coal in place, are estimated to be 61 million short tons as of January 1, 1953. Of this total, 55 million short tons is in beds 28 inches and more thick. Areas in each bed were omitted from the estimate where available data relative to the bed characteristics are too meager to permit making an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, such reserves should be added to the total estimated reserves.

Jan 1, 1955

By O. C. Baptist

This report presents results of an investigation undertaken by the Bureau of Mines to determine the clay content of typical petroleum reservoir sands in Wyoming and the effect of clay content on the permeability behavior of the sands. These results should have significance in determining the feasibility of injecting water into the sands for secondary recovery and in estimating the probable damage incurred by these sands if invaded with filtrates from water-base drilling muds. The results of air-, brine-, and water-permeability determinations are given for reservoir sands in three Wyoming fields. The amounts of materials of "fine silt and clay size" (Wentworth scale) in the sands and the types of clay minerals present, as identified by X-ray diffraction methods, are also presented and discussed.

Jan 1, 1955

By F. W. Wood

The method described may be used to delineate irregularities, inclusions, porosity, or shrink holes in ingots up to 43 inches in length. Rou¬tine testing does not require technical personnel, and the equipment is easily maintained. INTRODUCTION For a number of years, the Northwest Electrodevelopment Laboratory of the Bureau of Mines, Albany, Oreg., under contract with the Atomic Energy Commission and the Naval Reactors Division of the Bureau of Ships, has studied the production of zirconium and has adopted the Kroll magnesium-reduction process3/ as the, most economical means of producing high-purity zirconium sponge in quantities commensurate with demand. Consumable-electrode arc melting4/ provides a practical means of melting the sponge without increasing the impurity content. The ultimate application for which the metal is intended requires that strict specifications be met to insure workability and maintain the nuclear properties and corrosion resistance. The control measures employed to satisfy these specifications include chemical, spectrographic, and metallographic analyses, mechanical and corrosion tests, and ultrasonic inspection of the finished ingot. The primary purpose of ultrasonic inspection is to augment the other control measures by checking the soundness of each ingot leaving the laboratory. An incidental but important function has been the revelation of information leading to better understanding of the arc-melting process. For example, information obtained through ultrasonic inspection relative to the occurrence and distribution of porosity in ingots has resulted in a. modification of melting practices that minimizes the occurrence.

Jan 1, 1955

By Charles K. Rose

This paper presents some research studies of the rotary drilling of oil shale at the Bureau of Mines Oil-Shale Mine, Rifle, Colo. The experimental procedures and the rotary drill test equipment are described. Theories of rock drillability, rotary bit cutting action, and bit design are presented and discussed. The actions of various bit designs are analyzed and compared with the observed results of actual drilling tests. A cost estimate is made for drilling Colorado oil shale.

Jan 1, 1955

By R. C. Ellman

This report presents results of a series of tests on grindability of lignites and factors that influence grindability determination. All grindability tests in this investigation were made in the standard Hardgrove test apparatus. In addition to tests on standard samples of equilibrium moisture content, grindability determinations were made on air-and oven-dried samples of lignite representing the complete range of moisture content from normal bed moisture to nearly moisture-free conditions. Grindability index for all tests was calculated both by standard method and by an alternate or "corrected" method of calculation based on directly measured weight of fine-particle material produced in the grindability test. The second method of calculation allows more satisfactorily for loss of moisture during testing of high-moisture samples.

Jan 1, 1955

By J. J. Wallace

1. The Pittsburgh is the most important bed in Greene 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 6,011 million short tons as of January 1, 1954. Of this total, 5,967 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 to make an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, such reserves should be added to the total estimated reserves.

Jan 1, 1955

By 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 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 L. A. Stewart

"SUMMARYThis paper describes most of the chrysotile-asbestos deposits of Arizona. Mining methods are discussed briefly and asbestos-mill flowsheets are incorporated. Arizona asbestos mines are the only sources on the American continents of naturally iron-free chrysotile spinning fiber that is so urgently needed for electric-cable coverings, especially on warships.Asbestos was first recorded and recognized in Arizona in 1872, and a minor amount was produced from a deposit in the Grand Canyon in 1900. The discovery of a deposit in the Salt River district in 1912 initiated intensive prospecting, and deposits soon were developed. The total Arizona production of all grades of asbestos through 1953 is estimated at 30,000 to 35,000 tons.The deposits of the Central Arizona region, which are discussed in this paper, are scattered over nearly 2,000 square miles. The annual output is relatively small, because the asbestos occurs in thin, discontinuous veins and only in areas where intrusions of diabase are adjacent to or crosscut certain favorable units of the pre-Cambrian Mescal limestone. This stratigraphic limitation, combined with other essential geologic conditions, tends to restrict the size of the deposits.Virtually all of the deposits are in rugged, mountainous country, and many of the mines are on steep canyon walls. In the average mine, production of 1 ton of commercial asbestos requires removal of 30 to 40 tons of waste rock. Mining and transportation costs consequently are high.Several deposits of chrysotile that is somewhat harsh and of moderate tensile strength have been known for years but were not worked because of the former exacting demands of industry for high-strength, soft asbestos. However, improve¬ments in asbestos fiberization and spinning technique, combined with the urgent need for asbestos, have made this so-called semisoft fiber desirable, and deposits of this type now are being exploited."

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 John P. Walsted

Because of the absence of an iron-producing industry, the Pacific Northwest is working under an economic handicap. This is particularly apparent in the gray-iron-foundry industry because of the high price of pig iron imported from foreign sources or shipped in from producing ?areas within the United States. The high prices and sometimes short supply of ferrous metal products has put a brake on industrialization, which has been only partly compensated by the availability of cheap electric power. The economic condition of the gray-iron-foundry industry could be improved by establishing a small iron-producing industry based on the locally available ores. Moreover, establishing a local iron smelter would create a market for resources now dormant. Low-grade ores of manganese, chromium, and nickel would become usable in industry when combined with the iron ore from Scappoose. Pig iron produced in even limited quantities would level out the fluctuation in supply. The ore deposits, being small, would not supply enough pig iron to satisfy the entire demand. This condition necessitates designing special pig irons that will carry abnormally high proportions of scrap in the cupola charge.

Jan 1, 1955

By J. A. Rowland

Manganese-copper alloys containing 60 percent or more electrolytic manganese exhibit an unusual combination of high vibration damping capacity with good strength properties. Properties of the pure alloys were first studied in the laboratories of the Federal Bureau of Mines and have been described in a series of technical papers1/ published from 1941-49. The unusual characteristics of these manganese-copper alloys attracted the attention of research metallurgists and several additional investigations have also been reported in the literature.2/ The engineer, also, was attracted by the combination of high strength and high vibrational damping capacity possessed by these alloys. A wide field of application in structural and machine design was obvious. However, serious difficulties encountered in commercial fabrication of structural or machine components from the alloys retarded attempts at their practical utilization. For this reason the Federal Bureau of Mines, in cooperation with the United States Navy, Bureau of Ships, undertook a program designed to develop practical methods for fabricating a selected group of the high-damping alloys. It is the purpose of this paper to summarize a part of that investigation in a form suitable for use by the metallurgist interested in commercial fabrication of the alloys.

Jan 1, 1955

By A. Matzick

In its work under the Synthetic Liquid Fuels Program the Bureau of Mines has developed on a 6-ton-a-day-pilot-plant scale a continuous, gravity-feed retort far distilling oil from oil shale. The development work covered by this report was done from January 27, 1950, to January 26, 1952, at the ail-Shale Experiment Station near Rifle, Colo. Over 300 pilot-plant tests were made during the investigation. The basic retort developed has been named the Gas-Combustion retort. In this process, part of the heat for retorting of the shale is generated by burning recycled product gas in a combustion zone within the descending shale bad in the retort. Additional heat is supplied by combustion of the carbonaceous residue remaining in the spent shale after the oil has been distilled. Air for combustion is admitted through an air distributor in the center of the bed at about the mid-point of the retort. Hot gas rising from the combustion zone heats countercurrently the descending raw shale and liberated shale oil by pyrolysis of the shale. After passing through and exchanging heat with the incoming raw shale, the oil is condensed as a fog or mist in the gas, which is withdrawn at the tip of the retort. The cool gas is then piped to an oil-recovery system where the oil is separated from the gas in centrifugal separators or other types of mechanical or electrostatic separators. The hot, spent shale below the combustion zone is cooled by heat exchange with recycle gas, which is a portion of the effluent gas from the oil-recovery system.

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 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 J. W. Miller

Depletion of coals most suitable for metallurgical fuel has made necessary a general survey of coking coal reserves in the United States. These investigations were begunn 1948 at the joint request of the Munitions Board, Department of Defense, and a number of coal companies. This report, which is one in a series, by counties, describes the preparation characteristics of the coals of Harlan County, Ky. From these data it is possible to determine: (a) Which coals, either as mined or after beneficiation by conventional preparation, are chemically suitable under present standards for producing metallurgical coke, (b) Which coals require special and more intensive treatment in preparation than is now practiced; and (c) Which coals cannot be considered to be potential sources of metallurgical fuel regardless of preparation.

Jan 1, 1955

The first metal-mine accident-prevention course was prepared and published in 1942-45 as a series of seven miners' circulars (Nos. 51-57). The scope of the course has been broadened, revised, and brought up to date, and it is being published as a similar series of seven miners' circulars (Nos. 51-57, revised) on accident prevention in metal and nonmetallic mines. These circulars are: Accident Statistics (Miners' Circular 51), dealing with general statistics on accidents and injuries at metal and nonmetallic mines, including causes, costs, and the uses of investigations and reports of all accidents.

Jan 1, 1955

By S. T. Reese

STATISTICS of injuries in the quarrying and related industries in the United States first became available when the Bureau of Mines collected reports from the operating companies for the calendar year 1911. Since then reports have been collected annually. The present bulletin, covering the calendar year 1952, is the 33d publication containing statistical data on injuries at quarries and related plants, and it is the first to be published since 1944. The last publication was Bulletin 458, Quarry Accidents in the United States during the Calendar Year 1942. The unpublished statistics for 1942-51 may be found in the Appendix of this bulletin. The Bureau of Mines is authorized to collect data on injuries at quarries, but there is no Federal law that compels operators to supply such data, and the reports received from operators are voluntary responses to the Bureau's requests for information. Although the figures presented herein may not be complete for the entire industry, every effort has been exerted to make them so, and the figures given are believed to be thoroughly representative of the hazards to which quarry workers are exposed. Moreover, the figures are com¬parable as between States -which is significant in view of the lack of uniformity among the States as regards classes of plants covered by State laws, classes of injuries covered by State reports, and other factors that tend to make it impracticable or impossible to compare the injury experience of one State with that of another or to comprehend the relative importance of the various causes of injuries in the industry as a whole.

Jan 1, 1955