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By J. M. Kuchta

Concentrated hydrogen peroxide (H202) is a highly reactive oxidizing agent that liberates heat when it decomposes. The heat liberated may be sufficient to ignite combustibles with which the peroxide comes in contact. For this reason, concentrated hydrogen peroxide should be handled only by personnel familiar with its many unique properties.6 Hydrogen peroxide is used as a bleaching agent in the manufacture of textiles; this is its major single use in the United States. It is also employed as a reagent in chemical synthesis, as a source of free radicals to start polymerization, as a foaming agent in the manufacture of porous substances, and for its effect on biological processes. Moreover, highly concentrated hydrogen peroxide is a compact source of energy that can be utilized both as a monopropellant and as the oxidizer in a bipropellant system, During World War II, large quantities of highly concentrated hydro- gen peroxide were used as propellants, particularly in Germany. Since then, production of the peroxide has increased rapidly; in the United States alone it has more than doubled since 1950.7 Because of its widespread use, increasing interest has been shown in the hazards of handling the high- strength peroxide.

Jan 1, 1961

By D. H. Baker

These investigations were conducted to determine the feasibility of molten salt electrorefining of zirconium scrap, offgrade sponge, and alloys under contract number AT(11-1)-475 between the Atomic Energy Commission and the Federal Bureau of Mines. Offgrade zirconium sponge having a Brinell hardness of 169 can be refined by this technique to produce metal having, consistently, a Brinell hardness of less than 90. Also, zirconium alloy scrap, approximating zircaloy-2 in composition, can be refined to recover zirconium metal with a Brinell hardness of less than 100 that is essentially free of the major alloying elements. Analysis showed that the quantities of these elements were decreased as follows: iron from 0.27 to 0.002, tin from 1.36 to 0.001, nickel from 0.02 to 0.001, and chromium from 0.12 to 0.002 percent.

Jan 1, 1961

By T. A. Henrie

One objective of Project Gnome is to study the feasibility of a phase of the Plowshare program recovering thermal energy from an underground nuclear explosion. The test will be conducted in an underground salt deposit. It is anticipated that some of the energy thus released will be stored as thermal energy in molten salt. This report describes the pre-Gnome experiments conducted at the Federal Bureau of Mines Metallurgy Research Laboratory, Boulder City, Nev. The objectives of this study were to determine the problems involved in the recovery of thermal energy from molten salts to assist in planning the experimental program for the Gnome project.

Jan 1, 1961

By M. D. Carver

This investigation was undertaken by the Bureau of Nines to determine the effects of impurity levels on the mechanical properties of columbium at low temperatures. High-purity, electron-bombardment-melted columbium was purchased and used as a basis material. Variations in impurity levels were obtained by arc-melting charges containing definite amounts of added impurities. Tensile tests were conducted at low temperatures. Results showed the almost pure basis metal to be ductile at minus 194° C., the lower limit of the range used, Ductility of less pure columbium appeared to depend on interstitial element content. The ductile-to-brittle transition temperature appeared to be raised by increasing carbon content in the range of 50 to 730 parts per million, nitrogen content in the range of 50 to 200 parts per million, or total interstitial element content in the range of 240 to 1,380 parts per million. Some evidence was obtained indicating that decreasing cold work also raised the transition temperature, but recrystallization appeared to have no effect on it. Variations in interstitial element levels appeared to have little or no effect on ultimate strength of columbim in the range of room temperature to minus 194° C, Physical metallurgy studies of massive arc-melted and electron-bombardment- melted columbium were included in the columbium-tantalum research work assigned to the Albany Metallurgy Research Center in fiscal year 1959.

Jan 1, 1961

By John P. Capp

The feasibility of simultaneously burning several paths through a coalbed to develop a multiple path underground gasification system was investigated by the Bureau of Mines during two experiments, Boreholes were drilled through the overburden and into the coal and arranged in a circle approximately 50 feet from a central borehole. In the first experiment, in an area which had previously been hydraulically fractured,5 air was injected at the center borehole. The coal was ignited at the other boreholes and the fire fronts traveled toward the center, counter to the flow of air, to backward burn paths through the coalbed. Two paths were linked during the first 5 days of operation. The outlets of these two paths were throttled and air pressure was increased to maintain the flow of air, but no other linkages were made. Fourteen days after the two linkages these two paths were opened and gasification was carried on for 10 days, but with only moderate success. In an effort to overcome operating difficulties air was injected at the peripheral boreholes, and the gases were drawn off at the center borehole. Reversed flow operations continued for 12 days and two more paths linked. The heating value of the gas generally was higher than 100 British thermal units per standard cubic foot (B.t.u. per std. c.f.). Because only four of seven paths linked, however, the entire system could not be evaluated with respect to product-gas output and recovery of energy.

Jan 1, 1961

By J. W. Davis

The storage stability characteristics of a diesel type fuel were determined to evaluate the effect of the polar compounds in the fuel. These compounds, comprising most of the nitrogen and oxygen containing compounds and many sulfur containing compounds, were separated from the fuel with a chromatographic column. This fraction was further separated into three polar extracts by graded elution through the column. Each extract was characterized. A storage program using the depolarized fuel, the fuel as received, and blends of the extracts with both fuels, was conducted. Results showed that the removal of the more polar components stabilized the fuel. Blending the polar extracts with the original fuel and with the depolarized fuel in the same ratio as they existed originally and at two and three times the original ratio increased the amount of gum present before storage, but had little effect on the formation of additional gum during storage. Distillate fuels produced by commercial refining of petroleum contain traces of organic nitrogen, sulfur, and oxygen compounds that are more polar4 than the remainder of the fuel. Recent laboratory studies by the Federal Bureau of Mines (1),6 in which these compounds were removed from a fuel, have shown that they influence its storage stability. The objective of this work was to determine the amount of these compounds present in a fuel and their effect upon its stability in storage. To evaluate the role of these polar compounds, it is necessary to remove them from the distillate fuel. Many can be removed by chemical treatment (2), but such treatment precludes reblending the polar components to approximate the original fuel composition. Solvent extraction is free of some of the criticism of chemical treatment, but it is more difficult because of the complex mixture from which compounds must be removed.

Jan 1, 1961

By E. C. Perkins

The purpose of the research described in this report was to develop techniques for using ilmenite from domestic deposits for the production of titanium tetrachloride. The research was done by the Federal Bureau of Mines in cooperation with the General Services Administration under contract DMP-116, Utilization of Domestic Ilmenite. Bench-scale continuous chlorination of an Idaho ilmenite containing 27.9 percent titanium and 35.6 percent iron yielded a crude titanium tetrachloride suitable for purification and for the production of titanium metal and pigment. A summary of the results of 380 hours of operation showed that 82.4 percent of the titanium was chlorinated, with 92.5 percent utilization of chlorine. The construction- of a. quartz tube chlorinator 4-inches in diameter and 24 inches long is described with the necessary details of operation.

Jan 1, 1961

By A. D. Hahn

The Federal Bureau of Mines examined ilmenite-bearing sands in southern Texas as part of a program to discover sources of supply for the domestic titanium industry. Deposits were examined from May 1956 through January 1959 in the outcrops of sandstone beds in the Jackson group of Eocene formations in Lee, Burleson, Fayette, and Starr Counties on the Gulf Coastal Plain; in alluvial valley fill in Brewster County in southwest Texas; in the sand beaches of Matagorda Peninsula and the Galveston, Padre, and Brazos Islands--part of the offshore chain of barrier islands along the Texas coast; and in unconsolidated sediments in Willacy County on the Rio Grande delta in the southeast Texas.

Jan 1, 1961

By J. L. Konchesky

In gasifying pulverized coal with steam and oxygen, the particle size of the coal fed to a gasifier should be as small as economically possible. A potential way to achieve this advantage is to reduce the particle size of the coal by passing the coal-steam mixture at high velocity through a heated tube coil before the mixture enters the gasifier. To evaluate this method the Federal Bureau of Mines flashed coal-water slurries in externally heated metallic tube coils to determine the extent of size reduction. The first of two different laboratory-scale apparatus reduced the average particle diameter of subbituminous C coal from 190 to 110 microns at an outlet velocity of 330 feet per second (f.p.s.). At the same outlet velocity, a second apparatus reduced the average particle diameter from 250 to 140 microns. An increase in velocity produced more finely divided coal, but variation in temperature and pressure had no effect except as they affected velocity. Virtually the same size reduction was noted for five ranks of coal at equal velocities. The rate of increase in particle-size reduction with increase in velocity decreased with a decrease in particle size. The pulverizing mechanism was concluded to be abrasion of the particles with each other and with the tube wall.

Jan 1, 1961

By Eugene T. Sheridan

The Bureau of Mines annually canvasses the peat producers in the United states and publishes economic data on the peat industry, based upon reports submitted by producers. This publication lists all producers that reported commercial production to the Bureau for 1960 and presents data on individual plants. The companies named herein represent virtually all commercial producers, although a few small companies may not have been canvassed as the industry has many small operations that operate intermittently. Output of the various companies listed ranged from a few tons to more than 50,000 tons. Peat is included in the Bureau's annual surveys of the mineral industries because peat is classified as a mineral fuel. Although none is used for fuel in the United States, peat is a potential source of energy and ranks as one of our large mineral resources. The domestic peat industry sells peat, chiefly, for use as a soil amendment for general soil-improvement purposes. During the past decade the industry has expanded rapidly with operations increasing from 45 in 1947-494/ to 115 in 1960. Output during this period has more than tripled, increasing from 131,782 short tons to 470,889 short tons.

Jan 1, 1961

By Benjamin Petkof

Production quarry blasts in three rock types were photographed with a high-speed camera. Analysis of the films showed that step increases sometimes occur in the horizontal velocity of the broken rock. These step velocity increases were observed only in the first foot or so of rock movement. This observation indicates that the gaseous products of the explosion do additional work on the rock after it is crushed and cracked by the initial compressive-stress pulse and the reflected tensile-stress pulse. The observed initial fly-rock velocity is compared with the calculated fly-rock velocity for reflection spalling. A mechanism possibly causing the velocity increases is discussed. INTRODUCTION When a small concentrated charge of explosive is detonated at the bottom of a drill hole near a free surface, two modes of rock failure have been observed; both are associated with the stress pulse generated in the rock by the detonating explosive. The first mode of failure is the crushing and radial tensile cracking associated with the initial passage of the compressive-stress pulse as it propagates outward from the explosion. This type of rock failure is usually confined to the immediate vicinity of the charge hole. The second mode of failure is the tangential and radial tensile cracking associated with the tensile-stress pulse that is reflected from the free surface. This mode of failure is commonly called scabbing or spalling and has been shown to be a primary cause of rock failure in crater formation at one free surface. (3).4

Jan 1, 1961

By Ronald M. Lewis

Quadratic functions, Q(hkl), are given to six places in increments of 0.01° for 2? from 00 to 90° for FeKa and from 25° to 180° for FeKa1. The wavelengths used for Fe in the computation are those agreed upon by the Editorial Commission of the International Tables for X-ray Crystallography (1950): FeKa1 1.93597 A.; Feka2 1.93991 A. INTRODUCTION At the Federal Bureau of Mines laboratory, Norris, Tenn. X-ray diffraction crystallography using tubes with iron targets revealed a need for a handy reference for the quadratic functions of iron radiation. The tables presented here were prepared to satisfy that need. The quadratic form Q(hkl) may be expressed in terms of the Bragg diffraction angle 2? and of the wavelength ? as

Jan 1, 1961

By P. C. Good

Tungsten metal in fused form and of high purity was prepared by reducing tungstic oxide with redistilled calcium metal in a heavy-walled sealed reactor. Alloys of tungsten with vanadium, molybdenum) chromium, columbium, and tantalum were prepared by coreduction of mixed metal oxides in the same manner. This work was undertaken by the Bureau of Mines to investigate new approaches for preparing tungsten and its alloys in high-purity form. The standard method of producing tungsten metal has been the reduction of tungstic oxides by hydrogen. The resulting metal powder is compacted, sintered, and fabricated by powder metallurgy methods. Long experience in this field has resulted in the development of a technology that (by careful control of the variables such as metal composition, particle size, and sinterng technique) is well adapted to producing wire and the small shapes usually prepared from tungsten metal.

Jan 1, 1961

By Joseph A. DeCarlo

This information circular presents data for 1960 on individual coke plants in the United States. All oven-coke plants in existence, whether active or idle at the close of the year, are listed in this report. With two exceptions, only beehive plants on which reports were submitted to the Bureau of Mines are included. Although the Bureau was unable to obtain reports from these two active plants in 1960, the number of ovens and annual coke capacity are estimates, based on previous reports filed with the Bureau of Mines. Accordingly, there were 73 oven-coke plants in existence at the end of 1960 of which 70 were active. Reports were received on 44 beehive plants of which only 13 were in operation at year end. Oven-coke plants are listed alphabetically by States in table 1 which shows the name and address of the company, location of plant, classification or type of ownership, number and type of ovens, annual coke capacity, and coal-chemical materials produced. The terms "furnace" and "merchant" plants used in this and all other reports of the Bureau of Mines designate the type of ownership. Furnace plants are those owned by iron and steel companies whose main business is production of coke for use in their own blast furnaces. Merchant plants are those associated with chemical companies, gas utilities, as well as those that produce for sale on the open market metallurgical, industrial, and residential-heating grades of coke and coal-chemical materials. The annual coke capacity shown for each plant in this table is based on the minimum coking time necessary to produce coke with qualities suitable for its intended use. Therefore, the annual capacity of a plant may change from year to year, depending on age and condition of ovens, the character and quality of coal carbonized, the grade of coke required, and other factors. For example, annual coke capacity of a coke plant primarily making foundry coke with longer coking cycles would be lower than one making blast-furnace coke. Also some ovens must be operated at slightly lower than normal flue temperature because of the condition of the refractories and maximum capacity would be somewhat lower than designed capacity. For this reason, the capacity reported to the Bureau of Mines may differ from the designed or rated capacity estimated by the coke-oven builders at the time of construction. For example, if the generally accepted standard coking rate of one inch per hour were used on all ovens to calculate total annual capacity, it would have been 80.4 million tons or 2 percent higher than the capacity reported to the Bureau. Because of the factors mentioned above, the annual coke capacity shown in this table is believed to be a reliable measure of the practical operating capacity of the industry.

Jan 1, 1961

By P. M. Sullivan

The principles and application of amalgam electrolysis to the recovery of zinc and tin from secondary products were studied; this Bureau of Mines project was one phase of investigating the development of more efficient methods for processing iron-bearing zinc and tin to produce both base metals of high purity. Zinc of 99-99-percent purity was recovered from galvanizer's dross with recovery efficiency of 98 percent. Tin of 99.9-to 99.99-percent purity was recovered from hardhead with recovery efficiency of 81 percent. Both materials were treated by the same method in separate systems. Mercury was used to leach zinc from dross and tin from hardhead to form amalgams of each metal, both of which were subsequently refined electrolytically to produce high-purity metal. Impurities that were contained in both secondary products behaved as theoretically predicted; impurities that were insoluble in mercury remained as sludge in the leaching column. Except for lead, the readily amalgamated impurities were prevented from fouling the electrolyte by the blocking action of the amalgam electrode. Lead impurity in the tin-refining system dissolved and immediately precipitated as the sulfate. The primary advantage of the amalgam refining method lies in direct recovery of the extremely pure base metal from highly contaminated secondary material.

Jan 1, 1961

By Mah Alla D.

Previously existing heat-of-formation values for the oxides of vanadium were rudimentary. They were subject to uncertainties of 1 to 5 kilocalories per gram-atom of contained oxygen. This fact has been the only adverse influence on the accuracy of thermodynamic calculations involving these substances, as the requisite entropy and high-temperature heat-content data are known with reasonable accuracy. This report presents new heat-of-formation data for four oxides of vanadium (VO, V203, V02, and V205), obtained by combustion calorimetry. It is believed that the uncertainties have been reduced to 0.1 to 0.3 kilocalorie per gram-atom of contained oxygen. The new heat-of-formation data were combined with existing entropy and high-temperature heat-content values to obtain free energies of formation of the four oxides at temperatures up to 2,000° K.

Jan 1, 1961

By E. R. Palowitch

This report stems from a study by the Bureau of Mines of the possibility of reducing coal filter-cake moisture by applying radiant heat directly to the filter cake while under vacuum during the drying phase of the filter cycle. One disk of a 4-foot-diameter vacuum filter was equipped with gas-fired radiant-heat generators and the effect of radiant heating on the moisture content of a variety of filter cakes was studied. The results of this investigation show that this process can best be described as a filter aid capable of increasing the effectiveness of conventional filtration approximately 6 percentage points of moisture. The operating cost of removing water by this method is somewhat lower than the average operating cost of thermal drying and is considerably cheaper when the total cost is considered. Removal of water from coal that has been wet-cleaned is an important part of the overall coal preparation process. Water is a contaminant, and it is foolish to wash coal to reduce its ash content and add inert water in the process. In some instances the removal of water is actually more important than the removal of ash-forming minerals; its weight adds to the cost of transportation, and its evaporation during burning or carbonizing absorbs useful heat. Fine coal that contains more than about 10 percent moisture is notoriously difficult to handle. A problem thus exists for which there are sound practical and economic reasons to seek a solution.

Jan 1, 1961

By R. L. Grant

The principal official test performed by the Bureau of Mines to determine the permissibility of coal-mine explosives, commonly referred to as the gallery test, has been in use at the Bruceton station for many years (2, 16).4/ In this test the explosive under study is loaded into the borehole of a steel cannon and fired into a flammable mixture of natural gas and air or natural gas, air, and coal dust. To meet the requirements for permissibility, the explosive must not ignite the gas mixture under the conditions of the test. There is little doubt that these tests have succeeded in the main objective, namely, to screen the relatively safe from the relatively hazardous explosives. It has been generally conceded that adoption of permissible explosives by the coal-mining industry in the United States has substantially reduced the frequency of disastrous underground explosions caused by blasting. In recent years, however, research workers planning programs for improving the safety of coal-mine explosives have felt the growing need of a more quantitative method for measuring the incendivity of explosives based on a better understanding of the role of the important variables in the gallery tests, Accordingly, it was decided to apply certain statistical methods and techniques to the gallery test to develop it into a more precise tool for evaluating permissible explosives. One of the first and more important methods applied for this purpose was the up-and-down technique (6,7,17), It was demonstrated (14,15) that the weight of the explosive charge directly affects the ignition probability of the natural gas-air atmosphere and that the curve of ignition probability versus charge weight is a cumulative normal curve. Following these experiments, a program, still in progress, was set up to study how the addition of sodium chloride to various permissible-type ex-plosives affects their incendivity. This program resulted in 3,294 shots,

Jan 1, 1961

By W. M. Dressel

The Federal Bureau of Mines has obtained data by differential thermal analysis of the various minerals that represent the nation's resources in manganese. These data are supported by X-ray diffraction analysis, chemical analysis, mineralography, and optical mineralogy, and provide fundamental information on the response of each mineral to thermal treatment in oxidizing, reducing, and neutral atmospheres. The information can be applied advantage¬ously in the identification of manganese minerals. Its greatest potential value, however, lies in the application of the quantitative data on the reaction temperatures, rates, and products to the more efficient extraction of manganese from U.S. ores. Thermal analysis curves are presented for certain manganese minerals, namely hausmannite, bixbyite, braunite, pyrolusite, lithiophorite, cryptomelane, hollandite, manganite, rhodochrosite, and rhodonite. The original minerals and the products of their thermal decomposition were identified by X-ray diffraction analysis, supplemented by chemical analysis and mineralogical identification.

Jan 1, 1961

By T. E. Gray

This report describes the preparation characteristics of the signifi¬cant coalbeds in Preston County, W. Va. It is one in a series of reports planned to determine coals suitable for the production of metallurgical coke, either as mined or after beneficiation. Over 2 million tons of coal was produced in Preston County, W. Va. in 190, none of which was cleaned mechanically. Estimates as of January 1, 1959, indicate that more than 3 billion tons of coal remained in the county in beds 12 inches or more thick. The Bakerstown, Mahoning, Upper Freeport, and Upper Kittanning beds were selected by the Bureau of Mines for study based on current production and estimated minable reserves. Sample locations were selected after study of the literature, conferences with mining engineers and mining company offi¬cials in the field, and examination of available sites. Four samples were collected from the Bakerstown and Upper Freeport beds and one each from the Mahoning and Upper Kittanning beds.

Jan 1, 1961