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By A. Y. Lee

Prior work at the Bureau of Mines resulted in the successful development of a bench-scale, combination electrorefining-electrowinning method for recycling the lead from scrap batteries using waste fluosilicic acid (H2SiF6) as electrolyte. This paper describes larger scale experiments. Anodes cast from scrap battery lead were electrorefined in a 20-L multielectrode cell for 3 to 7 days. The anodes, containing 2 to 2.5 pct antimony, were ideal for obtaining firm and adherent slime blankets. Cathode deposits, assaying 99.99 pct Pb, were obtained, with current efficiencies near 99 pct. Sludge leaching was done in 100-L tanks followed by filtering in 61 cm square vacuum pan filtersu Lead of greater than 99.99-pct purity was recovered from the filtrate by electrowinning in a 20-L multielectrode cell using insoluble Pb02-Ti (lead dioxide-coated titanium) anodes and pure lead cathodes. The fluo-silicic acid electrolyte depleted in lead was repeatedly recycled to leach more sludge, and there was no problem with impurity buildup. The amount of Pb02 formed on the anodes during electrowinning was less than 1 pct of the total lead deposited on the cathodes, as long as the phosphorus concentration in the electrolyte was greater than 1.3 giL. Emissions of lead in air were less than 10 ~g/m3, well below the proposed OSHA limit of 50 ~g/m3.

Jan 1, 1984

By W. E. Webb

This report describes a method the Bureau of Mines devised for measuring the dielectric constant and loss tangent of low-loss minerals at microwave frequencies. Determina-tion of these properties makes it possible to predict the effects of using microwave heating in potential mineral processing applications. The method uses a test cell and radio-frequency (RF) impedance analyzer with automated data acquisition and analysis. In this initial phase of microwave heating research, the Bureau measured dielectric constants and loss tangents at frequencies between 100 MHz and 1 GHz. The objective was to establish a reliable data base for use in predicting the effects of microwave heating on minerals. Comparison with previously measured data showed the Bureau's measurement method to be accurate to within ± 3 pct. This report describes the method and discusses the preliminary results of the Bureau's investigations. Typical comparative data are included.

Jan 1, 1986

By D. P. Schlick

As of June 30, 1970, Federal regulations required the operator of each underground coal mine to maintain the average concentration of respirable dust below legislative standards. As of March 1, 1971, over 152,000 respirable dust samples have been processed by the Bureau of Mines. Approximately 75 percent of underground working sections are being sampled in accordance with Federal regulations. Results indicate that 72 percent of the sections which have completed at least one basic sampling cycle are below 3.0 mg/m3, the standard in effect under the Federal Coal Mine Health and Safety Act of 1969 (P.L. 91-173). Notices of Violation were issued on 1,670 underground mines for failure to begin a sampling program; Withdrawal Orders were issued in 64 of these instances. Notices of Violation were issued on 1,121 sections where applicable dust levels were exceeded; Withdrawal Orders were issued in seven of these instances. There are 381 mining sections currently operating on permit; from the interim Compliance Panel.

Jan 1, 1971

By S. E. Khalafalla

The Bureau of Mines investigated variations in the activation energy for the carbon monoxide reduction of magnetite and ferrous oxide with respect to the state of aggregation of the oxide material. Reduction phenomena can only be satisfactorily explained by including an adsorption step in the reduction process. Summation of the values of the exothermic heat of chemisorption and the variable apparent activation energy for reduction yields a nearly constant value of about 50 kcal for either ferrous oxide or magnetite regardless of whether they are aggregated in pelletized form or coarsely crystalline particles.

Jan 1, 1965

By William J. Campbell

The columbite-tantalite mineral series was studied by various instrumental techniques to establish the relationship of density to composition. The samples used were carefully selected to obtain a mineralogical purity of at least 98 percent. Impurities were determined by optical microscopy, X-ray diffraction, and optical and X-ray spectroscopy. Each sample was analyzed by fluorescent X-ray spectroscopy for iron, manganese, columbium (niobium), and tantalum. The existence of a unique relationship in this isomorphous series permits a simple correlation of the intensity of a spectral line with the concentration of the analytical element.

Jan 1, 1955

By Jr. Koch

As a means of investigating the distribution and variability of gold in ore from the Homestake mine, Lead, S. Dak., the Bureau of Mines performed a designed sampling experiment, and assay results were statistically interpreted. Fifty-six feet of diamond-drill core from five boreholes was sawed into l-inch-long cylinders, which were sampled randomly and were assayed. Analyses of variance of the assay results were used to compare and assess the different types of variation: within drill holes, among paired drill holes, among unpaired drill holes, and among furnace runs. The extreme variability in gold mineralization found is the natural variability on the smallest scale that can be detected by fire assay; most of the variability is associated with among-feet rather than within-feet sample intervals. Because of the extreme variability, one-half of the gold is in 3 percent of the samples.

Jan 1, 1967

By Wing G. Agnew

[This report presents the results of tests made by the Mining Division, Bureau of Mines, on the relative durability of manganese-steel drill rods and carbon-steel drill rods for use with the detachable bolts]

Jan 1, 1941

By R. D. Berkenkotter

This report describes a weighted method for evaluating the mean and variance of assay data from samples of different length . The method , which produces unbiased estimates from which valid confidence limits can be computed , is appropriate for bedded deposits of variable bed thickness and for vein deposits of variable vein width . Assay data from the bedded Florida phosphate deposit is used to illustrate the procedure .

Jan 1, 1964

As part of a continuing program of evaluating the Nation's crude-oil resource, this report presents information pertaining to resource, primary reserve, and potential waterflood reserve for 3,209 selected reservoirs contained in 24 oil-producing States, as of January 1, 1968. To that date the selected reservoirs had not been subjected to pressure-maintenance or secondary-recovery operations. These reservoirs also met the following parameters: (1) a minimum of five oil-producing wells on January 1, 1968, (2) a minimum of 50 acres areal extent, (3) a minimum of 50,000 bbl of oil ultimate primary recovery, and (4) the principal reservoir energy was other than active water encroachment. The selected 3,209 reservoirs produced 527 million bbl of oil in 1967, about 17 pct of U.S, total production. Primary oil reserve was 4,983 million stb; in addition, there was 6,043 million stb of potential water- flood oil reserve. Oil resource in the selected reservoirs was 59,547 million stb. A brief history and outlook of waterflooding are presented for each State. Depth and producing rate statistics and geologic distributions of production, resource, reserve, and potential waterflood reserve for the selected reservoirs are presented by States in the appendix. Also included in the appendix are description, history, and technique modifications of waterflooding, and a preliminary cost estimate of a closed-system water-injection project.

Jan 1, 1970

By Joe B. Rosenbaum

New applications and concepts of solvent extraction as a unit operation in extractive metallurgy have been developed in the last decade. Wider use is being made of established solvent extraction techniques in processing spent nuclear fuel elements and in winning columbium-tantalum, hafnium-zirconium, thorium, tungsten, uranium, and vanadium. Commercial application has been extended to recovery of beryllium, boron, bromine, copper, molybdenum, phosphorus, rare-earth metals, and rhenium. Systems in use and proposed typically extract metals or salts as anion, cation, or neutral species from aqueous media by reaction with a recycleable organic reagent.

Jan 1, 1971

By Linneas W. Laage

Coal production from underground coal mines has been important to the development of the industrial economy of the United States. Environmental problems have developed from some abandoned operations. These problems include: mine and refuse pile drainage, subsidence, unsafe mine openings and to a lesser extent mine gases, slope stabilities, mine and refuse pile fires and abandoned equipment and structures. Field investigations in three eastern coal mining districts, two in Ohio and one in Illinois, were performed to document the mine closure procedures used and subsequent problems that developed. The purpose was to identify, evaluate, and rank the seriousness of these problems. Based upon this evaluation, the undesirable present day situations could have been avoided or at least minimized by varying certain mining practices or mine closure procedures. It was found that federal regulations address all of these problems during the pre mining, active mining and post mining phases except for abandoned equipment which is the least threatening problem category. Ideally current practice would prevent future problems. However, the extensive and complicated nature of the legislation, environment and mining practices will necessitate adjustments to the law. The investigator recommends the following: 1) Goal oriented legislation encouraging complete resource extraction, standardization and compilation of mining generated hydrological data, periodic review of the coal mining regulations, and improved communication and cooperation between coal interests, regulators and the public. 2) Permitting effluent limitations to accurately reflect natural conditions. 3) Solidly back filling shafts and individual assessment of sealing or capping requirements. 4) Installing shaft vent pipes into the fill material to intercept and vent methane.

Jan 1, 1982

By N. A. Eilertsen

This report describes field investigations conducted in 1953 of two occurrences of manganese and a separate magnetic anomaly in the Southern manganese district of Aroostook County, vicinity of Houlton, Maine -the Pierce deposits, in Hammond Plantation Township; the Burnham anomaly, also in Hammond Plantation; and the Nickerson-Farm prospect in Hodgdon Township. The manganese occurs in a thinly laminated sedimentary rock containing manganiferous carbonate interlayered with fine-grained metamorphosed sediment, rich in chlorite or hematite. The surrounding rocks are mostly dark gray-green slates. Samples composited for metallurgical testing from the Pierce deposits and the Nickerson-Farm prospect assayed 9.0 to 12.3 percent of manganese. More than 90 percent of the manganese could be extracted with sulfuric acid, but in most instances 30 to 40 percent of the iron was also extracted. Leaching tests indicated that, after being reduced in a hydrogen stmosphere at 600° C., about 85 percent of the manganese could be selectively extracted by a solution of ammonia-ammonium carbonate with iron extraction of only 14 percent.

Jan 1, 1958

By D. W. Butner

This Information Circular , one of a series published by the Bureau of Mines , reports on the methods and costs of mining and concentrating zinclead ore at the Highland Surprise mine in the Pine Creek area of the Coeur d'Alene region of Idaho . The mine is owned and operated by the Highland Surprise Consolidated Mining Co. , which supervises operations of the Nevada Stewart group of claims , which is adjacent on the northwest . These properties are at the extreme eastern end of a zone of fracturing that strikes northwest across the Pine Creek area . In fractures along this zone are the principal Pine Creek mines ; these are the Highland Surprise , Nevada Stewart , Sidney , Denver , V and Idaho , Liberal King , and Northern Light . Country rock at the Highland Surprise is argillite of the Prichard formation (Belt series ) . Fracturing has permitted the movement of mineral- izing agents that have replaced adjacent walls and crushed country rock with sulfides . Ore minerals are sphalerite and galena with accessory pyrite , chalcopyrite , pyrrhotite , and siderite . Three principal ore shoots were found on the Highland Surprise property . The Highland ore shoot was mined from outcrop to the 400 level . The Surprise ore body has been developed to a depth of 1,400 feet on the dip of the vein . The outcrop of the Surprise ore shoot was 150 feet long and 2 to 4 feet thick ; on the 1,150 ( lowest ) level , the ore shoot is 320 feet long and 10 to 17 feet thick , with good zinc content . Surprise ore shoot No. 2 occurs 250 feet west of No. 1 and has been mined from the 500 to the 1,000 level . From 353,000 tons of ore mined between 1910 and 1948 , the property has a recorded production of 256,000 ounces of silver , 7,500 tons of lead , 24,000 tons of zinc , and 412 tons of copper . Both shrinkage and cut and fill stoping methods are used at the Highland Surprise , but shrinkage is unsuitable for mining below the 700 level , because faulting has weakened the walls . Development of the Surprise ore , as well as exploration laterally and along the strike , is prosecuted steadily . A prospect heading is being pushed westward toward Nevada Stewart ground from the 700 level . The mill has a rated capacity of 275 tons per day and operates near capacity . Selective flotation makes zinc concentrate that is shipped to the Anaconda smelter and lead concentrate that is trucked to the Bunker Hill smelter at Kellogg .

Mar 1, 1950

By C. H. Johnson

This paper on the out-and-fill method of mining is one of a series on mining methods published by the United States Bureau of Mines. It has been compiled chiefly from recent publications of the bureau describing in detail mining methods and costs at various mines. Other sources of information were the technical press, the Transactions of the American Institute of Mining and Metallurgical Engineers, the Mines Haudbook, and company reports. References other than those mentioned in Table 1, which lists the mines entering into this discussion and gives general data regarding them, are given in the body of the paper. The authors wish to acknowledge the kind assistance of many operating officials, either through correspondence or in the course of numerous visits to their mines. DEFINITION OF CUT-AND-FILL STOPING The out-and-fill method of stoping is that method in which relatively small sections or slices are taken successively from the lower surface of a block of ground by open-stoping methods, the broken ore being removed and each section filled with waste material before the next is mined. This definition excludes shrinkage stoping, even with subsequent filling; it excludes square-set and fill methods; it excludes the Mitchell slice method, which may be classed as underhand square-setting; it excludes the systematic use of stull sets and filling, which is a variation of square-setting; it excludes any method involving the caving of the ore, walls, or overburden during the process of extraction, although caving may be allowed to take place when the waste fill is withdrawn for use in other stopes; and it excludes any open-stope method without filling. Through variations, which will be discussed later, the cut-and-fill method merges into shrinkage stoping, open stoping, or square-setting. The use of casual timber support, such as props, stulls, or timber cribs for holding up weak portions of the back does not constitute a change from cut-and-fill to square-set mining.

Jan 1, 1933

By W. C. Holliman

This second of a series of reports on the characteristics of commercial aviation gasolines presents inspection test data furni8hed on their products by 15 manufacturers of commercial grades of aviation gasoline and special data obtained in Bureau of Mines laboratories on samples of these gasolines. Data on 18 grade-80, 20 grade-91/98, 20 grade-100/130, and 9 grade-115/145 aviation fuels are presented. These gasolines represent July 1947 production.

Jan 1, 1948

By P. A. Bloom

Bureau of Mines research was conducted to develop effective separation methods that might be used in exploiting substantial tonnages of complex barite-fluorspar ores in Arizona. The exploitable reserves now may be increased as recent batch and continuous flotation tests demonstrated that a complex barite?-fluorspar ore from the Red Chief deposit, Yuma County, Ariz., could be selectively treated to concurrently produce (1) fluorspar and (2) a barite byproduct of marketable grade. The sample contained 24.8 percent CaF2 and 24.3 percent BaS04. Processing comprised production of a fluorspar product containing 97 percent CaF2 with an 82 percent recovery, using a sodium fluoride-lignin sulfonate-fatty acid reagent combination. Concurrent retreatment of the fluorspar tailing, using sodium cetyl sulfate as a collector, yielded a barite product of 94 percent BaS04 grade with a 71-percent recovery. The products met specifications for acid-grade fluorspar and drilling mud-type barite.

Jan 1, 1963

By J. L. Eakin

A method was developed by the Bureau of Mines in the laboratory and in the field to relieve capillary waterblocks in gas wells. Impaired gas permeability was improved by this inexpensive chemical treatment which lowers the surface tension of the water held in the capillaries of the formation. Effectiveness of the alcohol-surfactant treatment was tested with a variety of chemicals and with sandstone cores cut from rocks having relatively low permeability. Field tests on 20 gas-producing and storage wells demonstrated the effectiveness and limitations of the method. The productive capacity of some wells was doubled by the treatment. The final test was evaluated by the neutron logging technique for measuring changes in apparent liquid saturation. Maximum apparent liquid saturation was reduced by 52 percent; gas production rate increased from 2.3 to 3.5 MMcfd (million cubic feet per day).

Jan 1, 1965

By Ellis S. Hertzog

The material published in this report is part of a special study of some of the chemical and physical properties of Alabama coals. The complete study included friability and grindability determinations, high and low temperature assay distillation tests, and ash fusion-temperature determinations. Proximate and ultimate analyses and. calorific values of the coal samples also were obtained. This paper is concerned only with grindabilities, although proximate analyses have been included to give a better picture of the problem as a whole. The growing interest in grindabilities of coals is a result of the increase in use of pulverized fuel in rescent years. The tenative ball-mill grindability method D408-35T4/ was used in making all the determinations. The method of sampling and the technic of the testing procedure is described in Considerable detail in this report because the procedure was established quite recently. The ball-mill grindability index is a measure of the ease with which coal may be ground, which may be an important factor in estimating pulverizing costs. Up to the present time few data on the grindability of Alabama coals have been published. The data in this paper show that the Warrior and Cahaba fields exhibit a wide range of grindability in their coals. The mines tested are well distributed throughout the productive areas of these fields, and it is possible to make rough estimates of the grindabilities of coals not listed in this report from the data given for mines situated in the same vicinity.

Jan 1, 1938

By N. S. Dalal, Xianglin Shi

"Electron spin resonance (ESR) measurements provide direct evidence for the involvement of Cr(V) in the reduction of Cr(VI)· by NAD(P)H. Addition of hydrogen peroxide (H2 O 2) to NAD(P)H-Cr(VI) reaction mixtures suppresses the Cr(V) signal and generates hydroxyl (·OH) radicals (as detected via spin trapping), suggesting that Cr(V) reacts with H2O 2 to generate the ·OH radicals. Reaction between H2O 2 and a Cr(V)·glutathione complex, and between H2O 2 and several Cr(V)-carboxylato complexes also produces ·OH radicals. These results suggest that Cr(V) complexes catalyze the generation of ·OH radicals from H2O 2, and that ·OH radicals might play a significant role in the mechanism of Cr(VI) cytotoxicity. KEY WORDS: ESR. spin trapping, Cr(VI) reduction, Cr(V), hydrogen peroxide, free radicals.INTRODUCTIONThis communication reports an ESR spin trapping detection of hydroxyl ( OH) radicals.in reactions between some Cr(V) complexes containing biologically important ligands and hydrogen peroxide (H2O 2 ). This work was undertaken because while the reduction of Cr(VI) to lower oxidation states has been suggested as a key step in the mechanism of Cr(VI) toxicity, the reaction· mechanism is not yet clear. 1 Mutagencity has been well documented for Cr(VI) via various bacterial assays, while Cr(III) has been shown not to be mutagenic.2 • 3 Since it has been reported that compounds containing Cr(VI) do not react with isolated DNA,4 the reduction of Cr(VI) by other cellular constituents has been thought to be important in the mechanism of Cr(VI) induced DNA alteration.1·4 • 5 For cellular systems earlier studies include those on the reduction of C~(VI) by microsomes,6-8 rat liver DT-diaphorase,9 and aldehyde oxidase. 10 Regarding the reduction mechanism, Jennette used ESR spectroscopy to show that a long-lived Cr(V) complex is formed as an intermediate in the microsomal reduction of Cr(VI) in the presence of NADPH.8 She postulated that Cr(V) is the ""ultimate"" carcinogenic form of chromium compounds. This conclusion has led to many further investigations of the formation of Cr(V) in the reduction of Cr(VI) under biologically relevant conditions.11 - 19 More recently, however, it has been suggested that oxygen-derived radicals generated during the Cr(VI) reduction are the species responsible for the DNA alteration.20.2• To the best of our knowledge, however, no information is available on the generation of such radicals in the reduction of Cr(VI) under biologically relevant conditions, except some preliminary results on the glutathionyl (GS·) radical formation in the reduction of Cr(VI) by glutathione (GSH). 11 - 19 We, therefore, undertook a systematic investigation of the reaction of Cr(VI) with NAD(P)H, GSH, ix-hydroxycarboxylic acids, and H2O 2 • NADPH was chosen as a model reductant because of its ubiquitous existence inside the cells, its critical role in the enzymatic Cr(VI) reduction,1·6-9 its representation of important cellular Cr(VI) reductants, and its ability to reduce other metal ions.22 GSH was chosen as another model Cr(VI) reductant because GSH also exists inside cells, it represents another important category of cellular Cr(VI) reductants, the thiols, and it also plays an important role in the Cr(VI) toxicity .1• 1 ""- 19.i3.i4 For further clarification, we also studied the reaction of Cr(VI) with several '1'.-hydroxycarboxylic acids in the presence of H2O 2 since these acids are definitively known to reduce Cr(VJ) to form stable, isolable Cr(V).25 .2 6 The results obtained indicate that Cr(V) complexes, produced in the reduction of Cr(VJ) by cellular reductants, react with H2 O 2 to generate ·OH radicals, which might be the initiators of primary events in Cr(VI) carcinogenicity."

Jan 1, 1990

By M. Orchin

THIS PAPER is concerned with two aspects of the behavior of coal: (1) Dispersion by solvents atmospheric pressure and high temperature and (2) the destruction and regeneration of the coking properties of coal. Several pure polycyclic compounds and a coal-tar fraction were found to extract 95 percent of the organic material of a bituminous coal. About 20 percent of the extract was soluble in benzene, and this fraction contained the ?coking principle? of the coal. From an extensive chemical spectroscopic, and x-ray study of the benzene-soluble material, some conclusions could be drawn concerning the composition and structure of this fraction of coal. A possible commercial application of the extraction technique is in the preparation of low-ash carbonaceous material for the manufacture of electrode carbon.

Jan 1, 1951