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By Earl T. Hayes, W. M. Sternberg, F. P. Williams

"INTRODUCTION The limited domestic demands for lithium salts and metal before the war were met readily by the use of minerals particularly lepidolite (lithium mica) and amblygonite (a lithium phosphate), from which lithium can be recovered relatively easily. New wartime uses, however, created such a demand that it became necessary to turn to spodumene (a lithium feldspar) as the principal source of supply. Although very large deposits of spodumene occur in South Dakota and in North Carolina, it much more difficult to extract lithium from spodumene than from lepidolite or amblygonite.During the spring and summer of 1942 a study was made in Salt Lake City laboratory of the Bureau of Mines on the recovery of lithium from spodumede. Preliminary tests were made on two processes - roasting with potassium sulfate 4/ 5/ and roasting with calcium chloride and calcium carbonate 6/ -,which appeared to be the most promising of the various processes that had been proposed. By roasting spodumene with approximately its own weight of potassium sulfate at 1,050º C. and leaching the product with water, about 70 percent of the lithium could be extracted. Consumption of the relatively expensive potassium sulfate, however, was high; much of the potassium was found in the insoluble leach residue, end large amounts were lost by volatilization and dusting. By roasting the spodumene with calcium chloride and calcium carbonate, nearly 90 percent of the lithium was chloridized temperatures of 850° to 1,050° C. Much of the lithium could be extracted from the calcine by leaching with water after roasting at the lower temperatures, but volatilization of lithium chloride was appreciable, amounting to 20 to 25 percent in a direct gas-fired furnace at temperatures of 800° to 850° C. At 1,000° to 1,050° C., volatilization was far from complete. Thus, it would be necessary to use both fume collection and leaching of the calcine, unless the roasting temperatures were sufficiently high to volatilize all the lithium chloride. Because of the well-known difficulties of collecting chloride fumes, it was decided to search for a better process."

Mar 1, 1946

By B. J. Scheiner

Extraction of silver from silver mill tailings by an electrolytic oxidation procedure was investigated by the Bureau of Mines. Various parameters affecting silver extraction, such as electrolysis time, particle size, and dissolution of the silver as the tetrachloro or cyanide complex, were studied at 30° C with an electrolyte concentration of 20 weight-percent sodium chloride. Resulting silver extractions ranged from 77 to 90 percent, depending on the tailings being treated. Concomitant extraction of mercury ranged between 90 and 95 percent. Power consumption was 52 to 90 kilowatt-hours per ton for the tailings investigated. Comparative experiments using direct cyanidation resulted in extraction of 46 to 82 percent of the silver and 20 percent of the mercury. Cyanide consumption ranged from 3.3 to 9.4 pounds per ton of tailings, depending on the tailings being treated. Silver and mercury were recovered from leach solutions by precipitation on iron powder, followed by conventional distillation and fire refining steps.

Jan 1, 1972

By J. F. Smith

A series of studies of emissions from large coal-fired steam generators have included measurements of the concentrations of oxides of sulfur and oxides of notrogen. The sampling equipment, method of sampling, and analytical techniques used for processing of these samples are detailed. A method based on the precipitation of benzidine sulfate was developed for determining both SO3 and total oxides of sulfur in the presence of interfering acidic components in the stack gases. In addition, difficulties encountered with sampling and analytical techniques are also described.

Jan 1, 1968

By P. T. Brooks

Semipilot scale tests were made to demonstrate a newly developed electrorefining process which could be extrapolated to commercial scale in producing high-purity nickel and cobalt from crude nickel metal and high-grade ferronickel. The new process comprises application of solvent extraction techniques to remove and separate cobalt and iron from nickel and the electrodeposition in diaphragm cells of pure nickel and cobalt from chloride-based purified electrolyte. Using water insoluble organic amines, the solvent extraction operations enabled production of commercial-sized nickel and cobalt cathodes of higher purity than that of commercial electrolytic metals. The solvent extraction operation for separation of cobalt from nickel was made simpler than the conventional method. Furthermore, the solvent. extraction operation for iron removal made possible the electrorefining of ferronickel without the prohibitive loss of nickel resulting from the method ordinarily used for iron removal.

Jan 1, 1970

By Robert T. MacMillan

An essentially chemical technique has been developed on a small scale for the efficient utilization of certain domestic titaniferous iron ores. Three main steps are involved: (1) Sintering the ore at 1,050° C. with carbon and soda ash to reduce the iron to metal powder, retaining the titania in the slag, (2) separating the powdered iron from the slag, after wet grinding, by magnetic or gravity methods, and (3) sulfuric-acid decomposition of the titania fraction to produce pigment and certain byproducts. The technique was first applied to the tailings from the Bureau of Mines bauxite-concentrating plant at Bauxite, Ark. A good grade of powdered iron was produced from this material. Subsequently, the work was diverted to the study of the titaniferous magnetite from the MacIntyre Mine at Tahawus, N.Y., because of the potentially higher recoveries of iron, titanium and vanadium. Ninety percent of the iron in this ore has been recovered as an iron powder analyzing 90 percent metallic iron and containing 2 to 3 percent TiO2. The remaining titania was found in the slag and was recovered as pigment-grade TiO2 by application of a suitable technique. The vanadium was distributed between the TiO2 fraction and the alkaline liquor resulting from the wet-grinding and magnetic-separation operations, with only a minor proportion retained by the metallic iron.

Jan 1, 1950

By William H. Lyon

In 1950 the Program Staff of the Department of the Interior undertook an exploratory study in the projection of energy requirements of the nation. This work was reported in Bureau of Mines Information Circular 7582 by H. J. Barnett. In that preliminary study Mr. Barnett, after exploring the nature of the energy economy in some detail, evolved a method for estimating how much energy will be required in the future, based on estimates of trends in efficiency of energy utilization in specific applications, the physical output of specific energy-consuming industries, size of the population, productivity advances in the economy at large, consumer preferences, and other factors. Considerable new information was developed regarding the nature of energy demands and the possible levels of requirements for each fuel under various assumed business conditions. The study analyzed the interrelationships, including substitutions, among the fuels and emphasized the need for viewing the energy economy as an integrated albeit complex whole. This exploratory study showed a need for a single comprehensive statistical re-port that would assemble and show in a uniform manner the diverse published statistical data on energy commodities now scattered through many publications. A particularly important need was for a set of historical statistics showing the production and consumption of all energy on a B.t.u. basis. As the prospective size and nature of the future energy requirements of the nation are matters of continuing importance, this report was prepared to assist further investigations of the subject. In this report the authors undertake to assemble and present in tabular form, on a uniform basis, the production and use of each of the fuels and electric energy in the United states for three census years -1929, 1939, and 1947. The year 1947, rather than a later year, was selected because it is the most recent year for which census data are available showing the consumption of fuel by each of the manufacturing industries. It is hoped that making data for these 3 years available in one re-port will provide the needed statistical background for further studies of fuel requirements and supplies.

Jan 1, 1951

By B. J. Scheiner

The Federal Bureau of Mines has successfully demonstrated an electrooxidation-solvent extraction-carbon adsorption process for recovering molybdenum and rhenium from offgrade concentrates. The flow sequence consists of dissolution of metal values by electrooxidation, liquid-solid separation by thickening, acidification and chlorate ion removal by sulfur dioxide treatment, solvent extraction to concentrate the molybdenum and rhenium, separation of molybdenum and rhenium by carbon adsorption, and metal recovery by crystallization. Molybdenum and rhenium were recovered as ammonium paramolybdate and ammonium perrhenate. Electrolysis of brine-concentrate pulps to generate a hypochlorite oxidizing agent in situ resulted in the dissolution of 98.9 and 99.1 pct of the molybdenum and rhenium, respectively, at an energy consumption of 13.7 kwhr/lb of molybdenum extracted.

Jan 1, 1976

By Gerald W. Elger

This report describes development of the fusion-leach crystallization precipitation process for producing a hafnium content feed material for hafnium-zirconium separation plants. Mixtures of zircon, potassium silicofluoride, and potassium carbonate (or potassium chloride) were fused to prepare soluble potassium zirconium hexafluoride-potassium hafnium hexafluoride salts. High extraction of these salts was obtained by countercurrent leaching the fused material in dilute hydrofluoric acid. About one-half of the hafnium was recovered in hafnium-enriched mother liquor by cooling clarified lead: liquor to crystallize most of the zirconium salt. Additional hafnium was recovered from the primary crystals in a multiple dissolution-recrystallization step. Hafnium-enriched oxides having a hafnium-zirconium ratio of more than three times that of zircon were precipitated from the combined mother liquors. The hafnium and zirconium recoveries in the precipitate were 83 and 24 percent, respectively. About 71 percent of the zirconium and the remainder of the hafnium were recovered in potassium zirconium hexafluoride crystals of low-hafnium content.

Jan 1, 1966

By D. J. Parker

State governments are increasing their efforts each year toward promoting the safety of miners .. Accidents underground are being avoided and mines made safer by means of revising and adding to their mining laws , by enforcing them through mine inspection departments , and by hearty co - operation with other agencies working miners ' safety . The U. S. Bureau of Mines is glad to testify to the co -operation that it receives from State mining departments in its safety work ; reports of the field mining engineers of the Bureau bear witness almost daily to the efforts of the States toward safety in mining . * This Through the courtesy of Mr. William Ogilvie , District State Wine Inspector of District No. 2 , with headquarters at "cAlester , Oklahoma, the Bureau has been furnished with a copy of a letter sent to various mining companies of Mr. Ogilvie's district in Oklahoma, relative to safety in Oklahoma mines . letter shows both the vigorous efforts which the State of Oklahoma is making toward increased safety in mines , and the recognized value of the types of electric cap lamps approved by the U. S. Bureau of Mines as " permissible " for use in gaseous mines ; it is accordingly reproduced in part : "hen during my first inspections of several coal mines in the district I found gas , or fire- darp being given off more or less constantly from the freshly cut coal at numerous points throughout the mines , I became uneasy relative to safety conditions , and am still considering your safety from many angles , but I am more concerned about the gas given off and the coal dust produced daily, than any other factor at the present time .

Jun 1, 1922

By Edmund S. Leaver, Charles E. Van Barneveld

In response to numerous requests from metallurgists and operators for information regarding the status of the sulphur dioxide leaching process , developed at the Southwest experiment station of the U. S. Bureau of Mines , Tucson , Ariz . , the following statement has been prepared . A more complete report is now in course of publication and will appear as Technical Paper 312. This process was devised to provide a cheap and efficient method for treating the so- called "porphyry " copper ores of the Southwest which generally contain both " sulphide " and "nonsulphide " copper minerals , mixed in such proportions that they can only be satisfactorily treated by a method which will concurrently recover both the sulphide copper and the nonsulphide copper . The latter term has been adopted to include all the minerals commonly referred to in operating phraseology in the mills of the Southwest as " oxidized" , " oxide " , or " soluble " copper . confident that the sulphide dioxide leaching process , as developed by us with the cooperation of the Miami Copper Co. and the Arizona Copper Co. , is suitable and commercially available for a wide range of ores .

May 1, 1922

By Benjamin W. Haynes

The Bureau of Mines conducted research to provide technical information needed to devise waste management plans for the processing of manganese nodules. Studies included summary descriptions of Pacific manganese nodules, process options and flowsheets, methods for characterizing nodules and their tailings, and results of analyses of laboratory and pilot-plant generated tailings. This information is the result of a cooperative research effort of the Bureau of Mines and the National Oceanic and Atmospheric Administration (NOAA), with NOAA providing funding and the Bureau conducting the research. A summary of the extensive literature review is provided for manganese nodule mineralogy, chemistry, processing techniques, and methods of analyses. Characterizations and analyses of laboratory-generated tailings and slags are given, as well as the results of the leaching studies on these waste materials. Leachability was determined by three standard leachate tests- the Environmental Protection Agency (EPA) extraction procedure (EP) toxicity test, the American Society for Testing and Materials shake extraction test, and the U.S. Army Corps of Engineers-EPA seawater elutriant test. While the wastes generated in the laboratory may not be entirely representative of those to be generated in full-scale plants, results of these studies provide a positive indication that commercial recovery of cobalt, copper, manganese, and nickel from manganese nodules would be environmentally acceptable.

Jan 1, 1985

By R. E. Lindstrom

A study of ion-exchange resin crosslinkage and eluant flow rate, resin-bed shape, and addition of separating ions to feed stock was undertaken to determine their effect on the separation efficiency of ion-exchange on bastna-site-rare-earth elements. Results show that 12-percent divinylbenzene (DVB) crosslinkage resin is detrimental to separation efficiency at flow rates over 2 to 5 ml./min./sq. cm.; whereas, separation with 4-percent DVB crosslinkage resin is relatively unaffected by flow rates between 2 and 10 m1./min./sq.cm.

Jan 1, 1959

By Oliver Bowles

"A New Mica Company in China A report has been received from the American Consulate at Chungking, China, to the affect that a new company has been organized to operate a mica mine north of Ta-chien-lu, in the province of Ssu-Chuan. The company, which is entirely under Chinese management and control, has a working capital of $10,000. While comparatively new, the mine has been worked before, and apparently with some success. The mica is said to be of good quality. It is claimed that the deposit will supply a limited amount of mica that will cut in pieces a foot square or over, and larger quantities of smaller sizes. The chief difficulty is transportation, for it is reported that a ten days' journey, part of it over mountain trails, will be necessary to transport the mica from the mine to Yachow, the nearest practical waterway. It is probable, therefore, that the output of the mine will be limited.Necessity for Careful Trimming and Grading of MicaA recent report to the Department of Trade and Commerce, Ottawa, Canada, by Acting Trade Commissioner C. G. Venus, London, England, contains information which is of vital interest to mica producers in the United States. It is pointed out that mica exports from Canada to England show a gradual decline dur¬ing recent years, the figures being as follows: 1913- 1,383 cwt: 1914 - 1,225 cwt: 1915 - 1,864 cwt: 1S16 - 879 cwt: 1917 444 cwt: 1918 - 480 cwt. Shipments from India to England, on the other hand, show a steady increase from 40,178 cwt. in 1913 to 66,401 cwt, in 1918."

Jan 1, 1920

By Richard P. Cislo

The evaluation of the effectiveness of the time domain Coal Interface Detector developed by the General Electric Company under contract H0155120 is the subject of this report. The sensor utilizes differences in the time characteristics of shearer vibrations as sensed by an accelerometer mounted on the ranging arm to discriminate the cutting of coal and rock. Pour identical time domain sensors were supplied by the Bureau for field evaluation. The performance of the time domain sensor was evaluated by an extensive field test and data collection program that included four longwall mines and a total of nine mine visits. The intent was to determine the sensor's applicability to a wide range of mining conditions and to document its limitations. Results of the extensive field tests indicate that shearer vibration data processed by GE's time domain signal processing algorithm cannot be used to reliably detect when the cutting drum crossed the coal/rock interface.

Jan 1, 1987

By E. J. Schneider

In view of the growing commercial interest In the higher boiling fractions of low-temperature tar, a study of the literature has been undertaken to obtain as many data as possible regarding the properties of possible pure constituents. The following substances have been studied: THREE-ORTHO-XYLENOL (1, 2-DIMETHYL-3-HYDROXYBENZENE) Detection By the isolation of the silver salt of 1, 2-dimethyl-3-phenoxyacetic acid.

Jan 1, 1930

By George T. Motock

In Germany the extraction of lithium and its salts has been handled mainly by units of the two major concerns - Metallgesellschaft A, G. and Deutsche Gold und Silber Scheide Anstalt, both with headquarters in Frankfurt. Zinnwaldite, which belongs to the mica group, is the major source of the lithium-containing raw material in Germany. Lepidolite and amblygonite also are used when available, but they are imported, as there are no major deposits of these two minerals in Germany.

Jan 1, 1946

By R. Hogg, S. Chander

"INTRODUCTION The behavior of particulate systems in general is determined by the properties of the solid and fluid phases and of the interfaces between them. As particle size is reduced, the inter facial effects become increasingly important until, in colloidal systems, they become completely dominant. Interfacial phenomena are especially important in coal processing for a variety of reasons. Because coal is naturally hydrophobic and its density is low, surface forces begin to dominate over gravity at relatively coarse sizes. Coal is thermodynamically unstable in the presence of air, so that surface oxidation occurs readily leading to important variations in surface properties with time and environment. These effects are further compounded by the inherent heterogeneity of the material.Surface characteristics and properties play a significant role in most aspects of coal processing. Comminution, for example, is a process of creating new surface, while agglomeration involves the reduction of surface area and is usually controlled by surface forces. Both solid-solid and solid-liquid separations are influenced by interracial phenomena, Gravity separations are usually performed in a liquid phase and are affected by the wetting characteristics of the various solids present and by the need to ensure proper dispersion of the individual particles. Froth notation, of course, separates particles on the basis of differences in surface characteristics. Chemical processes such as leaching generally involve interfacial reactions whose rates depend on surface area and may be influenced by electrochemical effects in the electrical double layer at the solid-liquid interface, or by adsorption of reactant and/or product species from solution. Solid-liquid separations and associated processes such as flocculation are strongly dependent on the nature and properties of the solid-liquid interface.In characterizing solid surfaces, it is important to consider first the surface area, since this determines the relative importance of the interfacial effects. The structure and chemical composition of the surface may depend on the distribution of different petrographic constituents and impurities such as finely disseminated mineral matter, on the extent of surface oxidation, and on adsorption from the environment. These, in turn, will generally determine the surface properties which define particle behavior. Since the relationships between structure etc. , and properties are not generally known, it is usually necessary to measure properties such as wettability and electrical charge directly."

Jan 1, 1989

By K. O. Bennington

Thermodynamic properties were determined by the Federal Bureau of Mines for lithium metasilicate (Li2Si03) and lithium disilicate (Li2Si205). Their enthalpies of formation were investigated by hydrofluoric acid solution calorimetry. The standard values are ?Hf°298 -393.8 ± 0.8 kcal/mole for Li2Si03, and ?Hf°298 -611.8 ± 1.0 kcal/mole for LiSi205. Enthalpy increments above 298 K were measured by copper-block drop calorimetry from 298 to 1,404 K for Li2Si03, and from 298 to 1,281 K for Li2Si205. Low-temperature heat capacities were determined adiabatically from 6 to 305 K for Li2Si205 only. The derived standard entropy is S°298 = 29.20 ± 0.10 cal/deg-mole. The various experimental data were combined with other data from the literature, and resulting properties of ?Hf°, ?Gf°, and log Kf were tabulated as a function of temperature.

Jan 1, 1976

By F. W. Lane

Some months ago the Bureau of Mines began research of a fundamental character on sulphur in petroleum. In the course of this work, the usual qualitative test for sulphur in organic compounds1 was applied to certain oils that were believed to contain approximately 0.5 percent sulphur. No sulphur was found, and, as a check on the qualitative test, the oils were subjected to quantitative determination of this element by the oxygen-bomb method.2 The sulphur content of the oils ranged from 0.10 per cent to 0.50 per cent. This experience led to further trial of the qualitative test for organic sulphur, both on the oils mentioned above, and on common sulphur-containing organic substances. No difficulty was experienced in detecting the element in the latter, but with the petroleum oils the test, as usually performed, could not be relied upon to detect less than 0.60 per cent of sulphur consistently. The use of mechanically polished pure sheet copper for the detection of free sulphur, hydrogen sulphide, and perhaps other sulphur compounds has been recommended.3

Jan 1, 1927

By R. H. Jefferson

This Bureau of Mines report describes a series of rapid wet chemical methods for the analysis of blast furnace slags. A "complete" analysis for total iron, manganese, silica, lime (calcium oxide), magnesia (magnesium oxide), sulfur, and mixed oxides (R203) can be routinely performed in less than 3 hours. These methods were employed as the analytical control procedures for the Bureau's experimental blast furnace operations and have been satisfactorily applied to the analysis of other slags and calcareous materials.

Jan 1, 1974