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By J. B. Gayle

Many investigators have reported studies of size distributions for particulate solids ; usually , these have involved the fitting of size distribution data to a particular mathematical function . Such studies are of unquestioned value and have contributed much worthwhile information regarding the breakage mechanisms for a variety of brittle materials . In connection with a Bureau of Mines study of the size distribution of coke , which has been subjected to the standard American Society for Testing Materials (ASTM) tumbler test , attention was focused on the relation between the 1 -inch tumbler index (usually considered to be indicative of the ability of coke to resist degradation by impact ) and the 1 /4 - inch tumbler index ( indicative of the ability to resist degradation by abrasion ) . Specifically , it was noted that for certain sets of data the correlation coefficients denoting the relation between these indexes were positive ; for other sets of data , these coefficients were negative . Preliminary consideration of this problem indicated that the usual interpretation placed on correlation coefficients was erroneous in this particular instance because the variables being correlated were necessarily related . The work described in this report was undertaken to clarify the interpretation of results of correlation studies for variables of this type .

Jul 1, 1960

By Jerome J. Hoeppner, Walter W. Fowkes

The Federal Bureau of Mines has determined the distribution of forms of sulfur for several lignites and gasification chars and noted the changes induced by the gasification process . A method was adopted for quantitatively determining sulfide sulfur that was found to be present in the chars , although absent in the lignites . Changes in the behavior and distribution of sulfur forms were further investigated concerning the ashing of lignites and chars under standard conditions , as well as at various temperatures , and the determination of volatile matter applied to both chars and lignites . The authors concluded that the first and greatest change in the form of sulfur present in natural lignite , upon heat treatment , resulted from the reduction of pyritic and sulfate sulfur to sulfide . Organically - bound sulfur originally present is less reactive , but largely disappears on strong ignition . An appreciable part of the sulfur content of natural lignite is fixed in the char as sulfide and in the ash as water - soluble sulfate and will affect the summation of constituents , to a greater or lesser degree , in reporting the ultimate analysis of a lignite or char .

Jul 1, 1960

By M. Vanpée, H. G. Wolfhard

Jets of hot gases issuing into explosive gaseous mixtures are efficient agents of ignition . The ignition temperature is defined as the temperature of the jet as it enters the cold explosive mixture which is just high enough to produce ignition . Such data have been published recently.5/ The investigators note especially that no correlation seems to exist between hot - gas ignition temperatures and spontaneous ignition temperatures , although there is a rather loose relation with limit flame temperatures . Before a more quantitative theory of the hot - gas ignition process can be attempted effectively , several questions must be answered : ( 1 ) Can the reactions leading to ignition be described by an Arrhenius type activation energy? ( 2 ) Is ignition preceded by an induction period ? ( 3 ) What is the rate - determining process of the ignition ? (4) And how does turbulence affect this type of ignition ?

Jul 1, 1960

By G. W. Birge, D. E. Wolfson, J. H. Lynch

This report by the Federal Bureau of Mines describes the carbonizing properties of coals from the principal beds in Boone County , W. Va . Results are given for samples of coals from No. 5 Block , Stockton - Lewiston , Coalburg , Winifrede , Chilton , Hernshaw , Cedar Grove , Alma , and No. 2 Gas beds . Boone County coals rank as high -volatile A bituminous . Eighteen of the 21 samples tested contained from 3.3 to 7.9 percent ash and 16 of the samples contained from 0.6 to 0.9 percent sulfur . Two samples from the Alma and No. 2 Gas beds , the lowest stratigraphically of the seams tested in Boone County , contained from 1.4 to 2.7 percent sulfur . Most Boone County coals yield

Jul 1, 1960

By Carl Rampacek, W. A. McKinney

The feasibility of leaching calcareous and siliceous oxidized copper ores by downward percolation with dilute acid was investigated in the laboratory and in a small continuous plant operated by the Federal Bureau of Mines . The crushed ore was leached in deep columns with solutions containing 1 or 5 percent sulfuric acid to dissolve the oxidized copper . Bench - scale laboratory tests on two calcareous ores from the same deposit indicated that a maximum copper extraction , about 72 percent , could be expected from heap leaching a feed as coarse as 1 inch . Laboratory tests on a siliceous ore showed that almost 70 percent of the copper could be extracted by leaching a 1 / 4 - inch feed . The bench - scale tests were supplemented by larger continuous runs wherein the copper was recovered from the leach liquors by precipitation on detinned scrap iron . Leaching the calcareous ore for approximately 10 days recovered 62 percent of the total copper . The sulfuric acid consumption was 9.6 pounds per pound of copper recovered . Treatment of the siliceous ore recovered 62.5 percent of the total copper in a 2.5 - day leach and the acid consumption was 3.7 pounds per pound of copper recovered . Cement copper products that assayed over 71 percent copper were obtained from the leach solutions by precipitation on scrap iron . The bench - scale and continuous tests demonstrated that downward percolation leaching of the calcareous ores was technically feasible but not economically practicable because of high acid consumption by the gangue . Leaching of the siliceous ore was rapid and the acid and water requirements were nominal . The downward percolation leach procedure is simple and requires a minimum of plant equipment .

Jul 1, 1960

By F. R. Cattoir, D. H. Baker

Fused - salt electrorefining has been successfully applied to the purification of vanadium metal . The electrolyte used in this refining technique was sodium chloride to which had been added 3 to 6 percent vanadium as vanadium dichloride . The average deposition current efficiency was 91 percent . Oxygen and nitrogen , the impurities in commercially produced vanadium metal , were reduced by two - thirds of the amount contained in the feed material . Hardness of the vanadium- metal product was reduced from an initial 97 Rockwell B ( RB ) to a minimum of 35 Rg . The reduction of these impurities markedly improved the plasticity of the final product obtained by melting the crystalline cell metal into small ingots . These ingots could be given a 99 - percent cold reduction by rolling before edge cracking appeared . Growing interest in high - purity vanadium and the industrial need for purer metals and improved alloys for use under high temperatures and high speeds have demanded the elimination and/or control of impurities . Accordingly, research to eliminate or control the undesirable impurities has been expanded .

Jul 1, 1960

By R. W. Stahl

"This study by the Federal Bureau of Mines was confined to pillaring with continuous mining machines and to mines where total extraction is practiced. Many different conditions and practices in as many coalbeds as possible in Pennsylvania were observed.Pillar extraction or pillaring can be the most productive part of coal mining if done properly; but it also can be the most dangerous if done improperly.Because of the need for more careful planning before and caution during pillaring, many mining companies resort to the undesirable practice of stumping or hogging of pillars with subsequent unnecessary waste of valuable natural resources. Pillaring can be done at reasonable cost and safely, as proven at many mines where complete extraction is practiced and enviable cost and accident records are maintained.Although continuous mining machines are bulky and sometimes difficult to maneuver, they have been used with great success in pillaring. Occasionally, however, a machine is caught, or men are injured by a fall during pillar recovery. This Bureau survey was conducted to ascertain how safe and successful pillaring (especially the removal of final stumps in lifts or the final stump of a pillar), is accomplished in some mines, while others have considerable difficulty under similar conditions.The Bureau hopes the information to be presented in this publication will prove beneficial to those who wish to recover more pillar coal and to improve their accident record during such procedures."

Dec 1, 1959

By Donald W. Mitchell, John Nagy, Edwin M. Murphy

"Investigations in the Federal Bureau of Mines Experimental coal mine near Pittsburgh, Pa., have shown that high-expansion foam containing at least 0.2 ounce of water per cubic foot of volume is effective in controlling exper-imental underground coal, oil, or wood fires. Some of the fires were extinguished, but more of the coal and wood fires were brought under enough control to permit direct attack with water or other extinguishing agent or loading the hot material into cars. The largest controlled experimental fire, which burned about 5 hours before attack, was in a coalbed 5 feet wide, 10 inches thick, and 100 feet long. The greatest distance foam was transported to control a fire was 1,010 feet.An incipient fire should be attacked promptly with water, rock dust, or other approved and readily available extinguishing agents. Where heat, roof falls, and smoke prevent direct approach, the more involved procedure of using foam may be advantageous. The effectiveness of the foam in controlling a deep coated fire of considerable extent H,vet to be proved by actual trials in aSome hydrogen, carbon monoxide, and methane gases are generated when a fire is attacked with foam. Calculations showed that in experimental fire tests an explosive mixture could form; however, this would occur only within a narrow range of combustible gas-air mixtures not likely to be found in practice. The principal explosion hazards are due to generation of gases by the foam, localized build-up of normally liberated methane, and volatiles liberated by the coal during heating. The quantity of combustible gases generated by the action of the foam on the fire is about the same as that when an equivalent amount of water is applied."

Mar 1, 1960

By Gerald W. Elger

The Federal Bureau of Mines developed a modification in the conventional Kroll process for preparing high - purity hafnium metal . This modification involved the partial replacement of magnesium by sodium in the batch reduction of purified hafnium tetrachloride to sponge metal . The raw tetrachloride was purified either by thermal degassing of the volatile contaminants to the atmosphere or by fused- salt treatment . In the fused- salt treatment , the tetrachloride was contacted with molten alkali chlorides to remove the impurities . The reaction byproducts were removed from the metal by heat treatment in an evacuated furnace . The metal sponge was consolidated by melting into buttons or ingots , which were analyzed for impurities . The purity of the metal prepared by the modified process is superior to that of the metal produced by the conventional method . The hafnium metal was comparable to crystal - bar hafnium except for the oxygen content , despite the abnormally high impurity concentrations in the raw tetrachloride . Several ingots were successfully cold - rolled to sheet .

Jul 1, 1960

By P. L. Woolf, J. P. Morris, E. Foerster, G. R. Zellars

Measurements of vapor pressure can be used to determine the thermodynamic activities of the components of metallic solutions . The determination of activity by this method requires accurate values for the vapor pressure of the pure component and for its partial pressure above the alloy solution . This investigation was conducted to measure the vapor pressure of liquid manganese for use in future studies of the activity of manganese in various liquid alloys . In related investigations in the Bureau's Pyrometallurgy Laboratory , vapor pressures of copper , iron and nickel have been measured and activit 4 5 6 have been determined in the iron- copper and iron- nickel systems . Difficulties were experienced with manganese which were not encountered in the previous investigations . Manganese oxidizes readily and greater care was needed to maintain an oxygen- and moisture - free atmosphere in the furnace . In addition , liquid manganese wet the refractories and there was a tendency to foam and splash on introduction of the carrier gas . Because of these difficulties several variations in the experimental procedure were studied . These were first tested with silver which has a vapor pressure of the same order of magnitude as manganese but is relatively inert at high temperatures . Although no significant changes in the original procedure resulted from this work, considerable data were obtained for silver and have been included in this report . Bauer and BBrruunnnneerr7/ have reported the only extensive investigation of the vapor pressure of liquid manganese . However , their results are not consistent with the data obtained by McCabe and Hudson for solid manganese . Measurements of the vapor pressure of silver have been reported by McCabe and Birchenal1,2/ Schadel and Birchenall , 10/ Harteck , 11 / Fischer , 12/ and von Wartenberg.13 / Generally , these investigators conducted their measurements at lower temperatures than were used in this study .

Jul 1, 1960

By Michael G. Zabetakis, Glenn H. Damon, Joseph A. Herickes

The flammability and explosibility of unsymmetrical dimethylhydrazine ( UDMH ) were investigated by the Federal Bureau of Mines to evaluate hazards associated with commercial application of this material as a missile fuel . This program included the following determinations : 1. Temperature limits of flammability in air at one atmosphere pressure ; 2. limits of flammability at selected elevated temperatures and pressures ; 3. 4 . 5. spontaneous ignition temperature in air at one atmosphere and at 200 pressure per square inch gage ( p.s.i.g. ) initial pressure ; spontaneous decomposition temperatures in nitrogen at one atmosphere and at 200 p.s.i.g .; shock sensitivity over a temperature range from about ( ca. ) 25 ° to 50 ° C .; 6. shock sensitivity of reference propellants ( hydrazine , nitromethane , methyl acetylene , etc. ) ; 7 . shock sensitivity of UDMH plus small amounts of selected metal catalysts . Part of the corresponding data was obtained for a mixture of unsymmetrical - dimethylhydrazine and diethylenetriamine ( U - DETA) .

Jul 1, 1960

By Raymond L. Carpenter

In connection with its continuing studies of the characteristics of alloys and alloying elements, the Bureau of Mines investigated the crystal structure of fused boron. This report describes how the structure of fused boron was found to be rhombohedral by the powder method for crystal-structure determinations by X-ray diffraction. The determinations of the crystal structure of boron reported in the literature were made on crystals prepared by various methods such as electrolysis, thermal decomposition of a boride, or by hydrogen reduction of boron tribromide. Table 1 summarizes the data found in the literature on the crystal structure of boron. The information shows the following: (1) Three structures have been reported for boron, (2) boron prepared by different processes--or even by varied conditions of a process--produces crystals of different structure, and (3) no information is given on the crystal structure of fused boron.

Jan 1, 1960

By L. J. Kane

Conventional methods for determining the size of dust suspended in a gas require that agglomerates (clusters of particles) first be broken into particles, but in evaluating industrial dust-removing equipment the size of the agglomerates as they actually exist in the gas stream is far more important. This paper presents results of an investigation by the Federal Bureau of Mines to develop methods for determining the size of dust agglomerates suspended in a gas stream. The studies are part of the Bureau's continuing research on synthetic liquid fuels. The size and size-distribution of agglomerates as they exist when the gas reaches the filter was determined by using a membrane filter in conjunction with a dust count under a microscope. A membrane filter is a cellulosic sheet about 150 microns thick containing millions of holes per square centimeter--holes of uniform diameter that run directly through the sheet without interconnection.

Jan 1, 1960

By Warren M. Mahan

A rotary kiln process was developed by the Federal Bureau of Mines to produce consistently an iron product containing 3 to 7 percent nickel. Cuban laterite and serpentine ores were smelted in a gas-fired batch-rotary kiln) 5 feet in diameter and 9 feet long. The metal contained 2 to 4 percent carbon, with little or no silicon, and could be produced on a large scale with modest capital investment. A total of 121 tests was run using this procedure. The tests were conducted with a maximum temperature of 2,625° F., using linings of firebrick containing 40 to 70 percent alumina. Slags in the kiln were acid to neutral. The material in each batch passed through three stages: (1) Sponge metal, (2) carburization, and (3) balling and meltdown. Half the tests were made while firing the kiln with atmospheric-temperature air; the remainder were fired with preheated air. Tests showed that preheated air decreased fuel requirements, dust losses, and reducing agent, and increased the capacity of the kiln.

Jan 1, 1960

By T. A. Sullivan

Research undertaken by the Bureau of Mines in 1938 has resulted in the development of titanium from a laboratory curiosity to a commercial metal. Along with processes for producing the metal, it was necessary for the Bureau to develop methods for analyzing the metal, raw materials, and intermediate products. Some of the methods developed have been published.3 4 5/ General Services Administration (GSA) was responsible for purchasing titanium metal under Defense Production Act contracts with commercial producers. GSA designated the Federal Bureau of Mines to analyze this metal and establish its compliance with Government specifications. A substantial quantity of tin was found in some of the samples analyzed, and in July 1957 tin was added to the list of impurity elements to be determined. The specifications limited the amount of tin in titanium sponge to a maximum of 0.10 percent. A program was immediately initiated to investigate methods and techniques for determining tin in the range of 0 to 1.0 percent. A method accurate at the 0.10 percent level was necessary, as this level was the critical range for acceptance or rejection of the metal.

Jan 1, 1960

By Norwood B. Melcher

This report describes preliminary experiments by the Federal Bureau of Mines on the practicability of adding raw pellets of taconite concentrate to blast furnace feeds. The usual industrial practice is to harden the pellets by heating before they are charged to the furnace. The Bureau research demonstrated that raw pellets could be successfully smelted in an experimental furnace with no significant change in coke consumption and only a moderate increase in dust losses. The dust loss was 43 pounds per ton of metal for an all-pellet charge, compared with 7 pounds per ton for an all-sinter charge. Raw taconite pellets undergo only slight degradation during charging to the furnace if 1 percent bentonite is used as a binder. INTRODUCTION Fines and concentrates must be consolidated or agglomerated into larger masses before they can be smelted in a commercial blast furnace. Such agglomeration is usually done by sintering, pelletizing, nodulizing, or briquetting. Sintering has been the more common practice, but with the advent of taconite concentrates pelletizing is increasing in importance.

Jan 1, 1960

By A. L. Engel

This publication describes further research by the Federal Bureau of Mines in beneficiating domestic manganese ores. The ores selected for treatment were typical of many manganese deposits in California and Nevada in that they have not been economical to mine because they are low grade or contaminated with siliceous minerals and are not amenable to physical concentration.3 4/ It would be desirable to develop a simple treatment method resulting in nearly complete extraction of manganese from these ores and applicable to small-scale operations. Sulfation reduction appeared to be such a method. The studies reported in this publication were directed toward sawdust or lignin-sulfonates as reducing agents. Sawdust, as waste from lumbering, and lignin-sulfonates, byproducts of woodpulp papermaking, are comparatively cheap and may be available in areas where manganese ores are found. Sugar, oils, and coal were also tried as reducing agents.

Jan 1, 1960

By Oren C. Baptist

Umiat field contains the largest accumulation of oil discovered so far in Naval Petroleum Reserve No. 4 in Arctic Alaska. The Umiat anticline was tested with 11 wells; 6 produced oil in varying quantities. Behavior of the wells during testing was unpredictable. For example, one well was abandoned as a dry hole after all tests failed to recover any oil, yet an offset well, only 200 feet from the dry hole, produced 400 barrels of oil a day. The main oil reservoirs are less than 1,000 feet deep and are in the permanently frozen zone (permafrost). Reservoir pressures are low, and most primary production will be by expansion of gas-in-solution in the oil. Because of the unusual reservoir conditions and the difficulties encountered in drilling and completing the wells, the Department of the Navy asked the Federal Bureau of Mines to make laboratory studies of the reservoir sand to determine the cause of well plugging and to provide laboratory information, to be used as an aid in estimating oil recovery from frozen reservoir rocks under solution-gas expansion from low-saturation pressure conditions.

Jan 1, 1960

By M. M. Gilkey

Pegmatites in Colorado occur for 150 miles along the Front Range (eastern-most range of the Rocky Mountains) from Larimer County on the north to Canon City on the south, and west into the Gunnison area. Many of the deposits have been classified. Minerals found in the various dikes include beryl, scrap and possibly punch mica, lithium-bearing minerals, columbite-tantalite, feldspar, and several rare minerals. Pegmatites are abundant in the Crystal Mountain district in Larimer County. About 5 miles south of the Crystal Mountain district and often identified with that district is the Hyatt pegmatite area. The Hyatt Ranch deposit has attracted particular attention because of the comparatively high beryl con-tent of the upper part exposed in opencut workings.

Jan 1, 1960

By C. G. Kirkland

An apparatus for determining trace impurities in Grade-A helium by mass spectrometer methods was designed and built by the Federal Bureau of Mines. Grade-A is the designation for helium commercially produced by the Bureau. Its nominal purity is 99.995 percent. The device, following a suggestion by Deaton, concentrates the impurities in the helium by freezing them out in a coil-and-trap assembly cooled by liquid helium. A known volume of helium is passed through the trap, the concentration ratio determined, and samples of the concentrated impurities are analyzed by mass spectrometer methods. The apparatus has been in service for approximately 20 months and has satisfactorily met all requirements. Over 200 analyses were made of helium contained in conventional cylinders, obtained from the Amarillo, Exell, Otis, and Navajo Helium Plants, during the 6-month period ending March I, 1959. Total impurity concentrations, in parts per million, were as follows: Amarillo, 19.1; Exell, 17.1; Otis, 11.3; and Navajo, 6.6. Neon and nitrogen were the major impurities. Complete data are shown in table 4 in the body of this report.

Jan 1, 1960