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By Joan T. May

The Bureau of Mines conducted laboratory tests to evaluate the production of high-purity H3P04 by HCl digestion and solvent extraction. Both batch and bench-scale continuous tests were made. Western phosphate rock concentrates were acidulated with HCI, and the digestion liquors were processed by solvent extraction. Phosphoric acid was extracted with isoamyl alcohol and recovered from the organic extract by contact with an NH4F solution. This solution was fractionally distilled to yield high-purity H3P04. The raffinate from solvent extraction was treated with lime to precipitate CaF2, which was subjected to steam pyrolysis to generate HF. This method was successful in recovering 95 pet of the phosphate and 80 pct of the fluoride contained in the concentrates.

Jan 1, 1976

By K. C. Dean

Time and motion studies were made by the Federal Bureau of Mines on the hand and machine dismantling of scrapped auto starter motors, generators, and alternators for recovery of copper, aluminum, and iron. The studies showed that an individual with power handtools and convenient access to a hydraulic press, power bandsaw, acetylene torch, and power lathe could, in an 8-hour day, disassemble about 100 starters, or 150 generators, or 30 alternators. The scrap copper yield would be 280, 390, and 45 pounds, respectively, and the iron yield would be about seven times the copper weight. About 100 pounds of aluminum would be obtained from the alternators.

Jan 1, 1976

By L. W. Higley

Electrowinning metals from solutions leached from low-grade ores is becoming an increasingly important extraction method as the metal industry turns to pollution-free recovery processes. Lead-alloy anodes are used industrially in the electrolytic recovery of zinc and copper. However, associated with the use of these anodes are the inherent problems of stability and lead contamination of the cathode. In an effort to eliminate these problems, the Bureau of Mines has developed a relatively inexpensive lead dioxide anode for electrowinning metals from strong acid solutions. The anode was prepared by depositing Pb02 directly on a titanium blank in a strong HN03-Pb(N03)2 solution at 2.15 to 6.45 A/dm2 and 60° C. This anode was tested in zinc and copper electrowinning cells containing 200 gpl H2S04 and 35 to 100 gpl metal ions at the current density of 3.23 to 6.45 A/dm2. Contamination of the cathode by lead was =0.005 pet. A 30-day test at 6.45 to 12.90 A/dm2 in an electrolyte containing 200 gpl H2S04 and no metal ions resulted in a slight change in surface morphology of the Pb02 anode but no measurable change in anode weight or dimensions.

Jan 1, 1976

By Noel N. Moebs

Valley Camp No. 3 mine was the scene of an experimental shortwall introduced in 1973 in an attempt to improve the recovery from the Pittsburgh coalbed in the Ohio Valley area where adverse ground conditions have imposed partial extraction methods with only 40 to 55 percent recovery of the valuable resource. The Bureau of Mines, under a cooperative agreement with Valley Camp Coal Co., monitored ground pressures and caving in the shortwall section in an effort to determine whether the roof strata, notably the limestone main roof, will cave to the extent that roof pressures at the face are relieved and whether the powered roof supports can sustain the roof load. The Bureau's efforts included mapping of clay veins, instrumentation of chain pillars and shortwall panels with encapsulated pressure cells, recording hydraulic pressures in the legs of the shortwall chocks, and core drilling underground and from the :surface. The experimental shortwall was a qualified success. Recovery increased 5.4 percent compared with partial extraction. Pressures in chain pillars and the abutment zone were not excessive. Hydraulic pressures in the chock legs did not approach the yielding pressure. Apparently, the limestone strata caved and the roof pressure at the face was relieved.

Jan 1, 1976

By P. T. Brooks

Electrochemical machining sludge, a troublesome fluid waste product, was dewatered on a bench-scale basis by three alternative methods tested by the Federal Bureau of Mines. These methods would enable recycling 89 percent or more of the liquid content of the sludge and allow the dewatered solids to be dumped as landfill or processed further to recover contained nickel. Dewatering by vacuum precoat filtration was estimated to be the least expensive. Based on treating 20,000 gallons per day of sludge, precoat filtration costs were estimated as totaling 1.96 cents per gallon of sludge. Two options of an alternative method, comprised of acidification, reprecipitation, thickening, and filtration, were estimated to cost either 3.41 or 3.60 cents per gallon of sludge.

Jan 1, 1976

By Philip E. Sanker

The Bureau of Mines conducted small-scale batch and semicontinuous tests on the reduction of zinc sulfide with iron according to the reaction ZnS + Fe ? FeS + Zn to determine reaction kinetics in the temperature range 1,000° to 1,400° C and to investigate the potential use of a scrap iron reductant. Batch tests indicated that a temperature of at least 1,300° C with a 1:1 mole ratio of Fe to ZnS is needed for good zinc recovery. Semicontinuous tests were conducted, using four zinc concentrate samples, containing various percentages of copper, cadmium, and lead, which were reacted with iron and iron contaminated with iron oxide and tin in an externally heated graphite furnace. Analysis of the zinc metal and FeS matte reaction products showed cadmium to be entirely in the zinc metal, copper to be in the FeS matte, and lead to be about 60 pct in the zinc metal and 40 pct in the matte. Tin reported to the matte, and none was detected above the O.OS-pct level in the zinc. Sulfur dioxide was not detected in the offgas when up to 20 pct of the iron was replaced by Fe203.

Jan 1, 1976

By J. B. Janus

This report, the 25th in a series, lists analytical data of coal samples collected by the Bureau of Mines in connection with the purchase of several million tons of coal for various Government agencies during fiscal year 1975. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. Ultimate analyses are given for these coalbeds only. The delivered coal was sampled at destination in accordance with instructions furnished by the Bureau of Mines, and all samples were analyzed in the Bureau laboratory at Pittsburgh.

Jan 1, 1976

By J. R. White, S. W. Lambert, C. M. McCulloch

Examination of several coalbeds in Walker County, Ala., Cambria, Greene, and Fayette Counties, Pa., and Raleigh and Wyoming Counties, W. Va., indicates that cleat orientations are similar throughout a vertical sequence of strata. Studies of cleat orientation were carried out in underground mines that are operating in separate coalbeds vertically above one another. The data show that over a vertical separation of 100 to 400 feet, the average difference in coal cleat orientation between mines is 04° for the face and 08" for the butt cleat. Variations of coal cleat direction between coalbeds examined in strip-mined areas show similar values. Cleat orientations measured at outcrops agree well with the directions measured underground, suggesting that the amount of vertical separation between coalbeds has little effect on the resulting differences in cleat directions. The largest variation of cleat directions between adjacent coalbeds occurs where a large horizontal distance separates two sample locations. Cleat orientations for deeper coalbeds are most reliable where the data are taken from directly above.

Jan 1, 1976

By C. M. McCulloch

Examination of several coalbeds in Walker County, Ala., Cambria, Greene, and Fayette Counties, Pa., and Raleigh and Wyoming Counties, W. Va., indicates that cleat orientations are similar throughout a vertical sequence of strata. Studies of cleat orientation were carried out in underground mines that are operating in separate coalbeds vertically above one another. The data show that over a vertical separation of 100 to 400 feet, the average difference in coal cleat orientation between mines is 04° for the face and 08° for the butt cleat. Variations of coal cleat direction between coalbeds examined in strip-mined areas show similar values. Cleat orientations measured at outcrops agree well with the directions measured underground, suggesting that the amount of vertical separation between coalbeds has little effect on the resulting differences in cleat directions. The largest variation of cleat directions between adjacent coalbeds occurs where a large horizontal distance separates two sample locations. Cleat orientations for deeper coalbeds are most reliable where the data are taken from directly above.

Jan 1, 1976

By G. W. Murrie, W. P. Diamond, C. M. McCulloch

It is estimated that more than 1 trillion cubic feet of methane is contained within the coals of the Mary Lee group in Jefferson, eastern Tuscaloosa, and southern Walker Counties, Ala. Most of this methane will be encountered by mining. Coals of the Mary Lee group are presently being mined at depths exceeding 1,000 feet and will in the near future be mined at even greater depths, where the problem of methane gas affecting the mining operations will be acute. It is calculated that approximately 90 pct of the methane is at depths greater than 1,000 feet, and over half of the gas is contained within only 12 pct of the study area which is under more than 1,500 feet of over- burden. Degasification in advance of mining will increase mine safety, reduce ventilation expenditures, increase productivity, provide an additional energy source, and make it possible to mine parts of deep coalbeds that probably could not otherwise be mined.

Jan 1, 1976

By W. P. Diamond

It is estimated that more than 1 trillion cubic feet of methane is contained within the coals of the Mary Lee group in Jefferson, eastern Tuscaloosa, and southern Walker Counties, Ala. Most of this methane will be encountered by mining. Coals of the Mary Lee group are presently being mined at depths exceeding 1,000 feet and will in the near future be mined at even greater depths, where the problem of methane gas affecting the mining operations will be acute. It is calculated that approximately 90 pct of the methane is at depths greater than 1,000 feet, and over half of the gas is contained within only 12 pct of the study area which is under more than 1,500 feet of over-burden. Degasification in advance of mining will increase mine safety, reduce ventilation expenditures, increase productivity, provide an additional energy source, and make it possible to mine parts of deep coalbeds that probably could not otherwise be mined.

Jan 1, 1976

By Cavallaro. J. A.

This report presents the results of a washability study of 455 raw coal channel samples with special emphasis on sulfur reduction. These raw coals contained on the average 14.0 percent ash, 1.91 percent pyritic sulfur, and 3.02 percent total sulfur. The complete washability data are presented for each sample processed. A statistical evaluation is included for the coalbeds from which more than 10 samples were collected and for the geographical coal producing regions. A graphical summation is presented for the coal producing regions and selected coalbeds. Finally a similar statistical evaluation is included showing composited data interpolated at Btu recovery levels of 50, 60, 70, 80, 90, and 100 percent. Graphical summations are presented for the various coal producing regions. Generally, significant sulfur reduction is achieved if the coals are crushed to a finer size and the higher specific gravity increments are removed. If a 50-percent Btu recovery was acceptable, then 32 percent of the samples tested could be upgraded to meet the current Environmental Protection Agency (EPA) standard of 1.2 pounds of S02 emission per million (MM) Btu when crushed to 14-mesh top size and separated gravimetrically.

Jan 1, 1976

By David E. Emerson

The Bureau of Mines has developed a mass spectrometer method for deter-mining the helium-3 content of high-purity helium. The work was performed to evaluate experimental methods for removing helium-3 from high-purity helium and to better determine the composition of pure helium used in research. This was accomplished by increasing the inlet sample pressure, ionizing current, and amplification of the current produced by the ions collected on a conventional mass spectrometer that had been modified. With these modifications, the helium-3 content was determined in the parts-per-million and parts-per-billion range in helium-4.

Jan 1, 1976

By W. P. Diamond, B. M. Bench, C. M. McCulloch

Coalbeds exhibit a directional permeability, with the maximum permeability oriented parallel to the face cleat. Thus, the most efficient pattern of vertical degasification holes for a coalbed is dependent upon cleat orientation. Surface joints, infrared photolinears, and Ronchi grating photolinears were investigated as potential estimators of subsurface cleat orientation. Cleat orientations were masured in 18 mines, in the Pittsburgh coalbed in southwestern Pennsylvania and northern West Virginia to be used as a standard against which prediction techniques would be evaluated. Two cleat systems with a strong geographic segregation were measured in the study area: N 67° W - N 28° E (95° separation) for the north, and N 76° W - N 17° E (93° separation) for the south. Directional data obtained from the three techniques investigated yielded satisfactory regional predictions of cleat orientation. Analysis of surface joints was the only technique considered sufficiently reliable on a local basis. Prediction of cleat orientation is based on the pairing of the principal directional sets into all reasonable combinations of fundamental systems. The system or systems composed of the most dominant sets nearest to 90° separation are likely to be a reliable prediction of cleat orientation. The most dominant set of the system selected is likely to be the face cleat.

Jan 1, 1976

By W. P. Diamond

Coalbeds exhibit a directional permeability, with the maximum permeability oriented parallel to the face cleat. Thus, the most efficient pattern of vertical degasification holes for a coalbed is dependent upon cleat orientation. Surface joints, infrared photolinears, and Ronchi grating photolinears were investigated as potential estimators of subsurface cleat orientation. Cleat orientations were measured in 18 mines, in the Pittsburgh coalbed in southwestern Pennsylvania and northern West Virginia to be used as a standard against which prediction techniques would be evaluated. Two cleat systems with a strong geographic segregation were measured in the study area: N 670 W -N 280 E (950 separation) for the north, and N 76° W -N 17° E (930 separation) for the south. Directional data obtained from the three techniques investigated yielded satisfactory regional predictions of cleat orientation. Analysis of surface joints was the only technique considered sufficiently reliable on a local basis. Prediction of cleat orientation is based on the pairing of the principal directional sets into all reasonable combinations of fundamental systems. The system or systems composed of the most dominant sets nearest to 90° separation are likely to be a reliable prediction of cleat orientation. The most dominant set of the system selected is likely to be the face cleat.

Jan 1, 1976

By Paul Biggs

This report presents information on 77 waterflood projects in 31 Montana oilfields. The study shows the locations of the projects, the sources and amounts of injection water, and the results in oil produced. Waterflooding, a secondary recovery technique, began in Montana about 40 years after the initial oil discovery in 1920. Often, the difference between water disposal by injection and pressure maintenance operations is not clear. Water injected at the projects in 1973 was 157.7 million barrels. In 1973, the 31 fields having waterflood projects produced 28.3 million barrels of oil valued at $88.4 million. Both in volume and value, this represents over 80 percent of the State's 1973 oil output. The projects are making possible the recovery of additional oil, thus contributing to the conservation of oil and lessening the impact of the current oil shortage.

Jan 1, 1976

By Donald P. Blasko

The Bureau of Mines investigated two areas of the Alaska Peninsula (Iniskin Peninsula and Becharof Lake) where oil and gas seeps were known to occur in an attempt to determine (1) whether the seeps are still active and (2) the amount of bitumen contained in the drainage leaving the seeps. The oil, water, oil-water, and gas were sampled and analyzed. Five oil samples were taken at four separate oil seeps. The API gravity of the oil ranged from 8.90 to 21.4° and the sulfur content was from 0.12 percent to 0.59 percent. Four of the seven gas samples obtained revealed fair high caloric values, ranging from 746 to 924 Btu/cu ft, and averaging 844 Btu/cu ft. A total of 44 water samples were obtained. Bitumen content of the water was as high as 9,773 mg/l at one seep, but averaged less than I mg/l where the seep-drainage water entered the Gulf of Alaska.

Jan 1, 1976

By D. A. Wilson

A laboratory method for processing lead battery scrap has been developed that eliminates virtually all of the S02 emission that normally is produced when a reverberatory or blast furnace is used. The method employs a hydrometallurgical step to convert the PbS04 to PbO and CaS04 by mixing the battery scrap with a slurry of Ca(OH)2. The reaction is exothermic and goes to completion in 2 to 5 minutes at room temperature. The dried product is mixed with a KC1-NaC1 flux and carbon and reduced at 6500 C. A minimum charge ratio of 3 parts of carbon to 100 parts of battery scrap is required for reduction. The process produces lead reductions and recoveries as high as 97.0 and 94.9 percent, respectively. The KCI-NaCl flux is recovered using a standard counter-current water leach followed by evaporation.

Jan 1, 1976

By G. M. Martinez

A cell concept adaptable to large-scale electrowinning of zirconium metal from zirconium tetrachloride was investigated by the Federal Bureau of Mines. Tests were made in twin cells, each 12 inches in diameter by 33 inches long. Electrowinning was performed in one chamber from which the electrolyte was transferred after electrolysis to the other chamber where it was renewed by the introduction of ZrC14 by direct sublimation. The formation of a salt plug in the connecting pipe provided a seal between the chambers. Optimum electrolyte composition, with respect to quality of the metal product (91 pct meeting ASTM standards except for the oxygen content) and current-carrying capability (about 350 amp) was determined to be 16.7 wt-pct NaF-83.3 wt-pct NaCl mixture plus ZrC14 equal to about 3 wt-pct zirconium. A twin-cell design incorporating the unit operations covered by this investigation is proposed.

Jan 1, 1976

By Lewis M. McNay

The strength characteristics of hydraulic sandfill modified by varying quantities of type III portland cement and two flocculants were investigated by the Bureau of Mines. Three different sand-cement ratios were examined using different percentages of flocculant. Two other experimental variables were curing time and weight-percent solids for hydraulic mixture. Results of unconfined compression tests with strain are discussed. Maximum strength was achieved with 0.5 weight-percent of ferric sulfate per ton of solids when the slurry mixture was 75 weight-percent solids. The bearing capacity of hydraulic sandfill is reduced by increasing the water content and decreasing the amount of cement mixed with sandfill.

Jan 1, 1976