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By Donald R. Johnson

Apparatus developed by the Bureau of Mines for thermal analysis of oil shale was used to determine the thermal properties of shortite. Dissociation of shortite near 470° C occurs as an endothermic reaction that could consume significant quantities of heat in the oil-shale retorting process that produces shale oil. The shortite dissociation products undergo other thermal reactions that would not affect the retorting process. These reactions include crystal inversions near 365° C and 425° C and melting and decomposition endotherms above 500° C. Two separate reaction route for fusion and decomposition of the shortite decomposition products are dictated by the presence or absence of CO2 around the sample.

Jan 1, 1974

By William C. Larson

A study was conducted by the Bureau of Mines to provide quarry operators with information regarding (1) the effects of jointing and bedding on rock fragmentation when bench blasting in two small-scale (2.5-ft) limestone benches, and (2) the successful use of inexpensive equipment and field techniques to determine the orientation and spacing of joints and bedding separations within the quarry. Using inexpensive equipment, such as a pocket transit and steel and paper tapes, joint and bedding separations were mapped and their frequencies measured. Results from two small-scale bench blasts in the Stewartville member of the Galena limestone formation showed that when the row of vertical blast-holes was oblique to the vertical joint orientations, the backface expression was outlined by two relatively large triangular protrusions (joint surfaces). In this blast, part of the rock burden was unbroken. When the line of vertical blastholes paralleled a predominant joint set, all of the rock burden was broken and displaced. The thickness of fragments that had been displaced by a blast correlated with the observed bedding thickness in the bench.

Jan 1, 1974

By A. R. Rule

A flotation process was developed by the Bureau of Mines for separation of carbonate and phosphate minerals occurring in unaltered phosphate ores of the Phosphoria formation. The process involves depression of phosphate minerals with fluosilicic acid and flotation of carbonate minerals with fatty acid emulsions. In individual laboratory tests, selective removal of carbonates was achieved with phosphate recoveries ranging from 60 to 80 pct P205. In continuous-circuit testing, sizing and separate treatment of coarse and fine fractions was necessary to achieve 65-pct P205 recovery. Concentrate grade ranged from 26 to 33 pct P205. The flotation tailings containing primarily carbonate and phosphate minerals is a potential fertilizer material. When reacted with H3P04, concentrated superphosphate containing approximately 40 pct available P205 was obtained.

Jan 1, 1974

By Warren W. Krech

Rock property data is needed over a wide range of parameters for the optimum execution of rapid excavation research. Eight rock types were chosen by the Bureau of Mines for a standard rock suite for such research. Large rock blocks were quarried and the standard physical and mechanical properties measured and documented. The eight rock types that comprise the rock suite are Barre Granite, Berea Sandstone, Dresser basalt, Holston Limestone, Salem Lime-stone, Sioux Quartzite, St. Cloud Gray Granodiorite, and Westerly Granite. Geologic, petrographic, physical-property, and mechanical-property test data are reported for each rock type. The information is the first step in the building of a comprehensive property listing for the eight rock types. A limited number of rock cubes are available from the Bureau of Mines Twin Cities Mining Research Center for use by researchers to broaden the information available on the suite.

Jan 1, 1974

By A. R. Rule

This report describes preliminary studies by the Bureau of Mines to develop a procedure for extracting the fluorine from low-grade fluorspar ores in which the CaF2 particles are finely locked in the calcite matrix. A combination of flotation beneficiation and pyrohydrolysis is applied to recover and to liberate the fluorine. Flotation of a finely locked high-calcite fluorspar ore containing only 11.7 pct CaF2 recovered over 92 pct of the fluorspar at a grade of 51 to 52 pct CaF2. Pyrohydrolysis of the flotation concentrate liberated nearly 90 pct of the fluorine as aqueous HF. By this procedure over 80 pct of the fluorine contained in the original ore was extracted.

Jan 1, 1974

By R. F. Chaiken

The Bureau of Mines has carried out experimental and theoretical studies with prilled and pulverized ammonium nitrate-fuel oil (AN-FO) mixtures containing varying amounts of fuel oil in an attempt to quantify the effects of stoichiometric composition, nonideal detonation behavior, and expansion volume on the production of CO, NO, and N02 fumes. Experimental fume measurements were obtained in the Bureau's large closed gallery facility (7.2 X 104 liter expansion chamber) and in the standard Crawshaw-Jones apparatus (90--liter expansion shamber) using a prepackaged charge configuration containing about 450 g of explosive.4 The theoretical calculation of toxic fumes was achieved with an equilibrium detonation code called "TIGER,," Contrary to initial expectations, the NOx (= NO + N02) fumes from the large gallery test were found to be in essential agreement with the Crawshaw-Jones results. It was also concluded that (1) "TIGER" calculations offer a good approach to the prediction of toxic fumes; (2) there is a basic problem in extrapolating laboratory measurements of CO fumes to mine conditions--this being due to postdetonation oxidation of CO to CO2; and (3) the detonation velocity decay rate of an explosive is a useful experimental parameter for correlating toxic fumes production with nonideal detonation behavior.

Jan 1, 1974

By Jack C. White

The purpose of this Bureau of Mines work was to develop information useful in improving copper recovery during copper milling operations. Eleven copper mill tailings from the Western United States were subjected to froth flotation and cyanide leaching to provide an experimental basis for comparing their beneficiation response. Recoveries in flotation concentrates made from mill tailings ranged from 65 to 15 percent, at copper grades of 13 and 2.2 percent, respectively. Liberated copper sulfide minerals present in two samples were readily recovered by laboratory froth flotation. Nine of the samples were less amenable to froth flotation because of physical locking between copper sulfide minerals and gangue. Correlations among tailings indicated that recovery of sulfide copper by flotation was directly related to the sulfide copper content. Empirical equations derived from flotation data provided average values for unrecoverable copper and for recovery efficiency. Flotation response of copper mill tailings may be predicted from the equations. Data from cyanide leaching provides an equation describing the limiting high values for removal of copper by this method.

Jan 1, 1974

By C. H. Elder

An analysis of the geologic structure of an area of Buchanan County, Va., was made by the Bureau of Mines using imagery from an airborne AN/APQ-97 side-looking radar system to evaluate that mapping technique for delineating structural features that may cause mining problems. Side-looking airborne radar (SLAR) was found to be a useful remote sensing tool for geologic structural analysis, Fault and joint systems identified by lineaments and linear patterns in the imagery were verified by surface and in-mine observations. Little Paw Paw fault was extended 10 miles by SLAR lineament analysis. A 22-mile fault, here named the Bishop-Bradshaw Creek fault, was mapped by lineament analysis and verified by observation of the fault on the Bishop Coal Co. mine map and on offset patterns of commercial gas production along the fault and surface observation of lineament along the fault. Three major super-imposed joint sets and several fault or fractured zones were identified by SLAR lineament analysis, showing more complex structure than earlier mapping indicated. SLAR imagery accurately delineated structural features that are known to affect gas migration and accumulation and that weaken the rock forming the immediate roof to mine workings, causing mining problems and potentially hazardous environment in the mines.

Jan 1, 1974

By R. B. Schluter

The objective of this Bureau of Mines investigation was to determine the effects of adding manganese compounds and ores to iron ore pellets. Manganese dioxide, carbonate, sulfate and chloride, plus six manganiferous ores from the Minnesota Cuyuna Range were tested as additives to increase the manganese content of iron ore pellets. One to 5 percent manganese, as a compound or ore, was added to five magnetite concentrates and one hematite concentrate. These concentrates were ballad, indurated (1,300° C), and tested for reducibility. Manganese sulfate and chloride were unsatisfactory additives causing cracking and degradation of the pellets during reduction. Manganese dioxide, carbonate, and the ores were satisfactory additives. The additives increased pellet compression strengths with a corresponding loss of reducibility, as compared to the pellets without manganese additions. The changes in compression strengths and reducibility were caused by the formation of Jacobite spinel and slag within the pellets. However, when the induration temperature was lowered from 1,300° to 1,200° C the reducibility and compression strengths were comparable to the pellets without manganese additions indurated at 1,300° C.

Jan 1, 1974

By Phillip N. Yasnowsky

The thrust of this Bureau of Mines report is to relate the size of automobiles to the price of gasoline, and the use of minerals in automobile manufacture to the size of automobiles. Only one of the many plausible scenarios of public reaction to higher gasoline prices, a switch to economy size automobiles, is developed. No account is taken of other potential impacts such as improvements in public transportation or increased occupancy per vehicle. Furthermore, a gasoline price increase is the only incentive to the greater utilization of economy cars that is considered. A gasoline price increase to $0.60 per gallon would reduce the amount of minerals required to produce the automobiles sold in the United States by an estimated 15 percent. Gasoline prices of $0.80 and $1 per gallon would cause declines in mineral requirements for U.S. automobile sales estimated at 26 percent and 35 percent, respectively.

Jan 1, 1974

By Arthur M. Hartstein

The Bureau of Mines, through contract with Ultrasystems, Inc., obtained data on the oxidative degradative behavior of a number of materials used in coal mines. Tests were performed using a stagnation burner arrangement. Materials examined included those used in typical coal mining operations such as (1) polyvinyl chloride-containing materials. (2) neoprene compositions, (3) rigid foams (urethanes/isocyanates), (4) miscellaneous materials (including jute, fiber glass, and polyethylene), (5) coal, (6) fluids (phosphate esters, organic esters, oil-water emulsions), and (7) composites. The composite comprised a mixture of a phosphate ester fluid with (1) coal, (2) a representative polyvinyl chloride sample, or (3) a neoprene-type composition. A number of decomposition products are identified that could represent a potential health hazard to miners including HC1, CO, SO2 and H2S, if they were generated to exceed toxic levels.

Jan 1, 1974

By P. B. Lorenz

Wettability measurements and laboratory waterflood tests were compared under a wide variety of conditions. Experiments were conducted with synthetic and natural crude oils, treated and untreated outcrop and oilfield sandstone cores, and synthetic brines with and without caustic, detergent, or phosphate additives. Measurements were made on equilibrated and unequilibrated systems at 77° and 150° F. Wettability was evaluated by the Bureau of Mines method from capillary pressure curves determined with a centrifuge. The waterflood data were fitted by empirical curves; the parameters of the curves characterize primary and subordinate production and also give the ultimate oil recovery. Results showed that wettability measurements at 77° F were useful predictors of recovery efficiency in waterflood tests run at both temperatures. Oil recovery in the early stages of waterflooding increased with increasing water wettability; however, the ultimate recovery was highest at a slightly oil-wet condition. The oil displaced at highest speed in the centrifuge was correlated with ultimate recovery in waterflood tests. Chemical additives to the brine sometimes lowered wettability and also sometimes improved waterflood recovery, but wettability and recovery were not correlated with additives present. The effect of additives on recovery in waterflooding was best seen in water-oil ratio curves.

Jan 1, 1974

By J. S. Miller

This report presents a complete coverage of results from Bureau of Mines preliminary research and the field application of explosive fracturing techniques to prepare oil shale for in situ recovery of shale oil. Small-scale surface tests were conducted to determine the feasibility of using a nitroglycerin-base explosive for creating rock fractures. Prior to underground testing, surface and near-surface tests with liquid explosives showed that explosions in sheetlike layers simulating underground fractures would propagate effectively. Successful surface experiments were conducted using layers of explosive placed between glass plates and explosive-saturated sand confined in small-diameter metal tubes. The tests in glass-plate reservoirs and metal tubes demonstrated that nitroglycerin would detonate and the explosion would propagate in cracks as thin as 1/32 inch and through distances up to 12 feet. In a shallow field test, nitroglycerin was detonated in a vertical crack in limestone and produced extensive fracturing. Explosive fracturing tests were performed in oil shale formations on seven sites near Rock Springs, Wyo. The procedures included (1) displacing and detonating nitroglycerin in natural or hydraulically induced fracture systems; (2) detonating nitroglycerin in wellbore shots; (3) displacing and detonating nitroglycerin in induced fractures followed by wellbore shots using pelletized TNT; and (4) detonating wellbore charges using pelletized TNT. The research on oil shale formations demonstrated that nitroglycerin displaced in a natural or hydraulically induced fracture would detonate, and the explosion would propagate through the explosive-filled fracture. Shooting a pattern of wells in oil shale at 100-foot depth with wellbore charges of pelletized TNT developed a satisfactory interwell fragmented zone. Tests performed on other sites at depths to 385 feet caused fragmentation of rock around the wellbore and provided interwell communication. Fourteen methods used to evaluate the extent and degree of fragmentation in the explosive fractured oil shale are discussed.

Jan 1, 1974

By D. E. Hirsch

The Bureau of Mines, as a part of American Petroleum Institute Research Project 60, Characterization of the Heavy Ends of Petroleum, has made extensive use of gel permeation chromatography (GPC). Data developed in this study were used to develop several correlations that greatly expanded the usefulness of GPC and the data have been used as an aid in the interpretation of mass spectra (MS). GPC retention volume data on pure compounds were used with molecular structure to develop correlations that can be used to accurately predict retention volumes, molecular volumes, densities, chain lengths, and ring numbers of many components of petroleum without resorting to further laboratory experimentation. Conversely, the correlation can be used to select or reject some compounds from several possible compounds that are indicated on the basis of MS analysis. The utility of these correlations in compound type characterization is demonstrated by showing their application to 330° to 550° C fractions from a low-sulfur and a high-sulfur crude oil.

Jan 1, 1974

By Kenneth C. Stewart

Eight brands (three samples of each kind) of commercially available audio-dosimeters were performance-tested. Each unit was placed in an anechoic chamber and subjected to various acoustic signals to measure its A-weighting response and overall integration accuracy. All units met the A-weighting tolerance for type II sould level meters, and six brands were within the Bureau I s overall accuracy requirements of ±2 dbA referred to input.

Jan 1, 1974

By Andrew A. Cochran

Laboratory-scale research was conducted by the Bureau of Mines to develop a new process for treating electroplating and other wastes. Various acid and alkaline cyanide wastes were combined under controlled conditions to neutralize the wastes and to almost completely precipitate the metals and cyanides. The metals were subsequently recovered for recycling; the cyanides can also be easily recycled. The process was successfully used to treat the major types of electroplating and etching wastes, containing Cd, Cr, Cu, Ni, and Zn, and to treat both concentrated and dilute wastes. The economic aspects of treating concentrated electroplating, etching, and anodizing wastes are especially attractive because of the low cost of mixing two wastes, the high value of the recovered metals, and the simplicity of the recovery procedures. The filtrates from the waste-plus-waste step were relatively harmless compared with the original wastes and met Public Health Service standards for free cyanide content. Free cyanide ions were not detected in most of the filtrates; the limit of detection was 0.03 ppm. Only small amounts of HCN were produced during the neutralization; the HCN was collected and neutralized.

Jan 1, 1974

By Harold E. Marr

Energy dispersion X-ray analysis was evaluated for possible application in the secondary metals industries for the rapid analysis and identification of copper-base alloys. Laboratory investigations of standard brass and bronze samples indicate that X-ray methods are capable of separating standard alloys into 10 general classes with analytical times of less than 3 seconds per sample for clean, flat samples. A radioactive source of americium 241 with a secondary fluorescer was used as an excitation source, and a lithium-drifted silicon semiconductor detector was utilized for energy discrimination of X-rays.

Jan 1, 1974

By C. B. Daellenbach

A prototype particulate size analyzer system was developed that would rapidly determine size distributions of homogeneous and two-mineral materials in the 74-micrometer (200-mesh) to 7-micrometer size range. The system sizes particles in a series of hydrocyclone elutriation steps and senses the weight of the five sized fractions by nuclear attenuation techniques. Size distribution of materials was determined from experimentally developed mathematical relationships that existed between particulate weight and the measured transmittance of gamma rays from an Americium-241 source. In the developmental phases, size distributions of three minerals (quartz, magnetite, and hematite) and a laboratory prepared two-mineral mixture of quartz and magnetite were accurately determined by the prototype system. In later stages of the investigation, semiconcentrates, an intermediate magnetic product from a taconite plant, were evaluated. Using 25-gram feed samples of this industrial material, the analyzer system was found to predict weight percentages for individual size fractions with an accuracy of ±0.85 percent or better at a 95-percent confidence level.

Jan 1, 1974

By H. H. Fukubayashi

This Bureau of Mines report describes the development of a pyrometallurgical process for the recovery of the zinc and lead contained in brass smelter flue dusts, which constitute a recycling or disposal problem. Tests on brass flue dust from several sources were made in a quartz tube, heated by an electric furnace to temperatures as high as 1,050° C. The dusts were mixed with carbon and heated in an oxygen-free atmosphere. It was demonstrated that 98 pct of the zinc and 12 to 25 pct of the lead, both in the metallic state, could readily be removed from the dusts. It was also found that 75 pct of the zinc could be recovered, with less than 0.1 pct of the lead, in the absence of chlorides. Pelletization techniques were investigated and 0.6 inch pellets were found to be optimal. Pelletizing results in a tenfold reduction in volume.

Jan 1, 1974

By Parviz F. Rad

The Bureau of Mines conducted groove cutting experiments in marble, lime-stone, granite, and quartzite with a 7-inch disk cutter under a normal thrust of 7,000 lb. The values of muck weight per unit length, specific energy, cutting coefficient, and groove depth for each of these rocks were determined for groove spacings ranging from 0.1 to 4 inches, and from these results the values of optimum and critical spacing were computed" The results indicate that compressive strength may be used to predict some of the cutting characteristics of the independent grooves. Considering all the cutting characteristics, particularly those for the interacting grooves, Shore hardness, coefficient of rock strength, and torsional velocity correlate with cutting characteristics better than do other physical properties. Some of the field applications of the principles established in this report are identified.

Jan 1, 1974