Search Documents

By F. P. Haver

A method to recover copper and elemental sulfur from chalcopyrite concen¬trate, using a ferric chloride leach, CuFeS2 + 3FeCl3 ? CuCl + 4FeCl2 + 2S, was reported by the Federal Bureau of Mines in 1971 (Report of Investigations 7474). Since that time, additional work has been done to improve certain steps in the procedure; that is, the recovery of sulfur from the leach residue, the recovery of copper and iron from the leach solution, and the regeneration of the leach solution. It was determined that over 99 pct of the elemental sulfur in the leach residue could be extracted at ambient temperature with an ammonium sulfide solution. Heating the pregnant solution precipitated crystals of rhombic sulfur (99.5 pct purity) and liberated ammonia and hydrogen sulfide for recycle. Copper with a purity in excess of 99 pct was obtained from the leach solution by electrolysis, using a diaphragm cell, with an energy requirement of less than 0.7 kW-hr/lb. Metal was deposited as a weakly adherent powder that could be easily dislodged from the cathode and withdrawn continuously from the cell in the form of a slurry. During electrolysis, part of the Fe(II) was oxidized to Fe (III) at the anode so there was no chlorine evolution. The leach solution was regenerated by direct oxidation of the spent electrolyte with air or oxygen in a turboaerator at 80° C. This precipitated the iron dissolved during leaching in an easily filterable form, Fe203.xH20, and converted the remaining Fe(II) to Fe(III).

Jan 1, 1975

By V. H. Gottschalk

Among the procedures developed by the Germans for providing the tonnage of iron powder needed to make rotating bands for artillery shells is the use of a ceramic tunnel kiln, not only for finishing the reduction of centrifugal powders but also for making so-called "brickyard sponge iron," which, after crushing and grinding, seems to yield a product suitable for powder-metallur- gical purposes. The final report issued jointly by the German Powder-Metallurgical Society (DPG) and the Chemical-Metallurgical Branch of the Research Depart- ment of the Metallgesellschaft, Inc. (ZFC of MG) gives the available details of this procedure, which may be regarded as a further development of the process in commercial use since 1911 at a ceramic plant in Hoeganaes, Sweden. The Bureau of Mines' wartime development of the Hoeganaes process also cul- minated in the adaptation of ceramic tunnel kilns for carrying out the solid- carbon reduction of iron ores, and comparison with the German technique should further advance the art. This information circular is issued as a supplement to Bureau of Mines reports of investigations Nos. 3819,2 3822, 3841,2 and 4271, on brick- yard sponge iron and is based on four German reports entitled "Making Iron. Powder in the Tunnel Kiln," translated from FIAT microfilm reel H-46, frames 9190-9209, 9280-9299, 9339-9357, and 9377-9384 (PB L 70042), which represent the four original research reports, Nos. 2005, 2008, 2010, and 2012, respec- tively, of the Metallgesellschaft, Inc.

Aug 1, 1948

By E. G. King

Strontium sulfide and barium sulfide occur as intermediates in commercial treatments of the impure natural sulfates to produce pure strontium and barium chemicals. Thermodynamic considerations involving these sulfides have been hampered by lack of basic data, such as the entropies at 298.15°K. This paper reports the results of heat capacity measurements of strontium sulfide and barium sulfide in the temperature range 50°-298°K. The entropies at 298.15°K. were derived from the heat capacity values. Free energies of formation at 298.15°k. were computed from the entropies and literature values of the heats of formation. Strontium sulfide and barium sulfide are thermo-dynamically less stable than calcium sulfide, but more stable than magnesium sulfide.

Jan 1, 1960

By A. F. Baker

Laboratory flotation of synthetic coal-pyrite mixtures and high-pyritic-sulfur coal indicated that ferric chloride (FeCl3), aluminum chloride (AIC13), chromium chloride (CrCl3), and cupric sulfate (CuSO4) are potential pyrite depressants. For each metal salt there appeared to be a range of pH values and optimum concentration for selectively depressing pyrite in coal flotation. Pyrite was depressed in the pH range from 4.5 to 7.0 with ferric chloride, from 5.8 to 7.0 with aluminum chloride, from 6.4 to 7.1 with chromium chloride, and from 6.4 to 7.4 with cupric sulfate. Best separation of pyrite from coal was achieved in flotation solutions containing from 2 X 10-5 to 5 x 10-5 mole/ liter of each salt. In solutions containing excess salt concentrations, coal was also depressed. These Bureau of Mines tests demonstrated on a laboratory scale that, in solutions containing 4 X 10-5 mole/liter ferric chloride and from 1 x 10-4 to 2 x 10-4 mole/liter sodium hydroxide, the pyritic sulfur content of a Lower Freeport bed coal sample could be reduced from about 2.51 percent to less than 0.60 percent with recoveries of over 83 percent. The depression of pyrite appears to be due to the adsorption of positively charged colloidal metal hydroxide at the pyrite-solution interface. This hypothesis is supported by zeta potential determinations which showed that suspended coal and pyrite particles in solutions containing metal salts are positively charged in the pH range where depression occurs.

Jan 1, 1971

By Scott Turner

Within recent years , people have begun to realize the importance and significance of the mining and allied industries . The leading part the engineer plays in civilization is becoming recognized . However , accurate quantitative knowledge of the industrial importance of mining is still seldom possessed except by those close to this business . It is true that there are a few who go to the extreme and represent the whole progress of civilization as a reflection of man's gradual mastery of mineral utilization , but on the whole , the magnitude of the industry is underestimated . The uncertainties of mining , as evidenced by the variable results of prospecting on surface or underground , in an unknown new field or from the bottom levels of a mature mine , the ins and outs of tonnages and metal contents , the possibility of a widespread or even a sudden change between cost and realization-price , add to its picturesqueness and make mining attractive to some . To many , the fact that results are generally more uncertain and less predictable than in other industries lends added charm . The following pages may serve to call attention briefly to the importance of mining relative to other industries in the United States , in Canada , and in the world . Ordinarily , the annual primary mineral production of the United States amounts to about 5 billion dollars . The average for the last five years has been a little over 5 billion dollars . Last year , sadly enough , it was less than 34 billions . Just now , we are on the decline , and have been for the past two years . In Canada , the 5-year average was about 268 million dollars . Last year it was 227 million . Due in part to gold output ( in 1930 , for the first time , Canada's gold production exceeded that of the United States ) , the Canadian average is holding up better than ours . It has been estimated that the average world mineral production over the past five years has amounted to about 12 billion dollars , while in 1931 it was less than 8 billions . The mineral industries are as indispensable for the conduct of modern society as are those of agriculture , but , in the United States at least , they receive far less recognition from the Government . With us , agriculture is fostered by a great department that is maintained by enormous appropriations , while the mineral industries get but little financial support . In the United States , in the calendar year 1930 , the value of production by these two industries were as follows : to 1 . Agriculture ( inclusive of forestry ) 9.9 billion dollars ; mining 4.8 billions ; ratio 2 Direct appropriations by our Federal Government were 109 million dollars to agriculture and 2.8 million to mining , a ratio of 39 to 1. Obviously this is out of balance to the extent of 19 to 1 in favor of agriculture .

Jun 1, 1932

By Robert K. Koch

The Bureau of Mines investigated separating HF from HF-SiF4-H2O mixtures by passing the mixed gases through a sodium fluoride slurry in an airlift scrubber and forming a mixed precipitate of NaHF2 and Na2SiF6. The oven-dried precipitate was thermally dissociated in two stages. The first stage was carried out at 400° C and dissociated NaHF2 to NaF and HF. Condensation and analysis of the evolved HF proved it to be 97 to 99 weight-percent HF containing 0.79 to 0.99 weight-percent H2O and 10 to 93 ppm silicon. The second stage was carried out at 700° C and dissociated Na2SiF6 to NaF (for recycle) and SiF4. The quantity of HF recovered from gaseous HF-H2O-air mixtures decreased with increasing relative H2O concentrations. Air was beneficial when scrubbing extremely dilute wet HF gases. At HF partial pressures of 0.24 and 0.013 mm Hg in the scrubber entrance gases, HF partial pressures of 6.2 x 10-4 and 9 x 10-6 mm Hg were obtained, respectively, in the scrubber exit gases. Scrubber efficiencies were 99.7 and 99.3 percent.

Jan 1, 1966

By D. E. Wolfson

As part of its overall program of coal-carbonization research, the Bureau of Mines is studying the coking properties of coals from various fields of this country. Few of the coals included in this survey are used for the manufacture of metallurgical coke, although some well-known coking coals necessarily are tested to provide comparative data, particularly on blending properties. The overall objectives of the study were given in detail in a previous report.3/ The inherent suitability of coal for metallurgical purposes, as distinguished from economic considerations, depends primarily on (1) the available reserves, (2) chemical composition, (3) preparation characteristics, and (4) carbonization behavior. These items are considered in selecting coal for carbonization tests.

Jan 1, 1956

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 J. B. Zink

The Bureau of Mines developed a spectrochemical method to determine six constituents in coal ash in the following concentration ranges: silica 9 to 63 percent, alumina 7.5 to 35 percent, ferric oxide 2 to 30 percent, calcium oxide 1 to 29 percent, magnesium oxide 0.5 to 6 percent, and titanium oxide 0.5 to 4 percent. Samples of coal ash are fused with a mixture of lithium tetraborate and vanadium pentoxide. The resulting beads are crushed, mixed with powdered graphite, and briquetted. The pellets are analyzed spectrographically, using controlled high-voltage spark excitation. Vanadium serves as the internal standard. Effects due to matrix variations are minimized by fusion with lithium tetraborate. Intensity ratios of selected analytical lines are determined photometrically, Concentrations are read from analytical curves, prepared from synthetic standards, relating log intensity ratios to log concentration. A combustion procedure is used to determine sulfur tri-oxide. The method is most useful when large numbers of coal ashes must be analyzed but a high degree of accuracy is not essential.

Jan 1, 1967

By R. V. Lundquist

Aeration in water slurries and controlled drying of manganous hydroxide produced from dithionate leaching of Artillery Peak manganese ores from Arizona were investigated by the Bureau of Mines at its Electrometallurgical Experiment Station, Boulder City, Nev., to determine whether a simple process could be developed for converting this product into a battery-grade manganese dioxide. The properties of manganese dioxide prepared by the thermal decomposition of manganous nitrate were investigated also. Manganese dioxide suitable for use in batteries was not obtained from the dithionate leach product, but some of the factors controlling its oxidation were isolated. Aging of manganous hydroxide was of major importance in retarding its oxidation by aeration. Sodium hydroxide and sodium silicate promoted oxidation by drying. Optimum quantities were about 0.85 mol of sodium hydroxide and 0.2 mol of sodium silicate per mol of manganese, and drying temperatures of 200° C. produced yields of manganese dioxide up to 90 percent of the manganese present. Higher temperatures and concentrations of reagents carried oxidation of manganese beyond its tetravalent state.

Jan 1, 1957

By M. P. Dalton

This paper which describes the milling practice at the Morning concentrator of the Federal Mining and Smelting Co., Mullan, Idaho, is one of a series being prepared by the Bureau of Mines. ACKNOWLEDGMENT The author wishes to acknowledge the assistance given by H. G. Washburn, general manager of the Federal Mining and Smelting Co., and by C. S. Price, assistant mill superintendent, in the preparation of this paper.

Jan 1, 1932

By J. E. Matta

The methane gas emitted from coal samples collected from the conveyor belts dumping into silos was measured by the Bureau of Mines. Approximately 50 pct of the total gas desorbed into a sealed can within 1 week was released during the first 24 hours. No simple correlation between the gassiness of the coal stored and the methane concentration in the silo open space above the coal was found. This was probably because the gassier coals were stored in open-top Silos, which were better ventilated. Although the methane concentration in the open space above the coal pile was less than 1 pct for all 34 silos investigated, a methane measurement in the coal pile showed that high methane concentrations can exist. The methane released in the pile appears to accumulate and not liberate freely into the open space above the coal pile. Probably this gas is released during reclaiming operations, but further research is required to substantiate this claim.

Jan 1, 1978

By James Noll

Total carbon (TC) is sometimes used to measure or characterize diesel particulate matter (DPM) in occupational settings such as underground mines. DPM samples are collected on quartz fiber filters. When using quartz fiber ?lters, adsorption of gas phase organic carbon (OC) has been reported, causing a positive bias in the particulate TC results (adsorption artifact). Most of the data on the sampling artifacts and corrections apply to environmental air sampling, where samples are collected at a much higher filter face velocity and the OC concentrations are generally much lower relative to occupational sampling. In this study, we investigated the effects of adsorption artifact on samples from occupational settings. Samples were collected with and without denuders to determine the amount of gas phase OC collected and the accuracy of certain corrections. In underground stone mines, the adsorption artifact was found to positively bias the particulate TC by greater than 20% for filter loadings below 25 µg/cm2 TC (8-h time weighted average) 262 µg/m3). The tandem ?lter correction reduced the effect of the artifact, as high as 60% of the TC value, to less than 11% for laboratory data. It also significantly reduced the effect of the artifact obtained for field samples.

Jan 1, 2008

By Jr. Hazen

Relationships that may exist between assays and sample interval lengths when using unequal sample intervals in mine sampling have been investigated as part of the larger research problem of adapting statistical methods to the analysis of weighted average grades. The theoretical relationship between the amount of difference in the weighted and unweighted average grade of ore and the size of the correlation coefficient between assay value and sample interval length was found to be linear. Numerous examples of actual field sample and assay data, which have been obtained by using unequal sample intervals, are documented, and the differences between weighted and unweighted average grades of ore and the correlation coefficients between assays and sample interval lengths have been computed and plotted on graphs. Differences between these actual field data and the expected theoretical linear relationship are examined. It is hypothesized that the use of unequal sample intervals in mine sampling is, in fact, stratified sampling in a statistical context. The sampler establishes stratification by selecting unequal sample intervals on the basis of differences in lithology, changes in rock type, characteristics of mineralization, or differences in metal content. Statistically} methods currently used in mine sampling, involving unequal sample intervals, fail to consider differences in the inherent variances in grade of ore within the various strata established by using unequal sample intervals. Consequently the strata are sampled with different precision. This difference in precision of sampling between strata may account for much of the deviation between the plotted points representing actual field sampling data and the theoretical linear relationship between the amount of the difference between weighted and unweighted average grade of ore and the size of correlation coefficient between assays and sample interval lengths.

Jan 1, 1966

By Albert J. Forney

Extensive studies have been made of the various effluents found in the Synthane coal-to-gas process. Analyses have been made of the waters, gases, and trace elements present in some of the streams. Results of analyses show the water effluents are the area where extensive research is needed.

Jan 1, 1974

By G. L. Oldright

In the previous study that has been made by the authors on smelting in the lead blast furnace,4 the furnace examined was one that operated under conditions that have been considered as more or less normal up to the present time. That is, although the furnace had in its charge a large portion of sinter, it also handled considerable quantities of naturally oxidized direct-smelting ore. Other ingredients, such as the limestone, were also added as fairly coarse material. The charges contained only about 24 per cent of lead. Until the changes incident to modern flotation began to take effect, many lead plants doing semicustom smelting in districts where competition was keen and much of the bonanza ore was exhausted were faced with the difficulty of obtaining enough lead to get a sufficient "lead fall" in the blast furnaces to clean the slag thoroughly and to separate it from the lead. A charge containing 24 per cent of lead would have been considered a very rich one by such smelters.

Jan 1, 1931

By G. L. Oldright

In the previous study that has been made by the authors on smelting in the lead blast furnace, the furnace examined was one that operated under conditions that have been considered as more or less normal up to the present time. That is although the furnace had in its charge a large portion of sinter, it also handled considerable quantities of naturally oxidized direct-smelting ore. Other ingredients, such as the limestone, were also added as fairly coarse material. The charges contained only about 24 per cent of lead. Until the changes incident to modern flotation began to take effect, many lead plants doing semicustom smelting in districts where competition was keen and much of the bonanza ore was exhausted were faced with the difficulty of obtaining enough lead to get a sufficient "lead fall" in the blast furnaces to clean the slag thoroughly and to separate it from the lead. A charge containing 24 per cent of lead would have been considered a very rich one by such smelters.

Jan 1, 1931

By Agnes Y. Lee

The Bureau of Mines has developed an effective hydrometallurgical method to recover high-purity Pb metal and elemental S from concentrates. This low-temperature process eliminates S gases and Pb emissions, in contrast to the current high-temperature smelting technology. The method consists of (1) oxidative leaching with H202, Pb02, and waste fluosilicic acid at 95° C to produce a solution of PbSiF6 and a residue containing elemental S, (2) electrowinning the PbSiF6 solution at 35° C to produce 99.99 pct Pb metal and H2SiF6, and (3) solvent extraction to recover S, leaving a residue containing Cu, Ag, and other metal values. Spent electrolyte was recycled repeatedly, with impurity buildup controlled by controlling the leach parameters.

Jan 1, 1986

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 Frank C. Morris

This report presents the results of a Bureau of Mines study to identify clays found in several petroleum-reservoir rocks in the Tejon-Grapevine area, Kern County, Calif., and to determine the effect of water sensitivity of the clays on the permeability of the reservoir rocks. The clays in the porous rocks were examined in detail, and the clay-mineral types were identified by differential thermal analysis, X-ray diffraction, and optical and dye-staining methods. Fresh-water damage to the permeability of the oil-reservoir rocks was indicated by a study of 125 core samples from productive formations. The study indicated that, although clays were generally less than 5 percent of the reservoir rocks, they swelled in water, particularly fresh water, and nearly blocked the flow channels through which oil flows to the well, effectively reducing the permeability of the formations. The average permeability of rock decreased from 1,600 millidarcys in air to 620 millidarcys in salt water and 120 millidarcys in fresh water. The dominant clays in the oil-bearing sandstones were members of the montmorillonite group. They were associated with smaller quantities of clays found to be in the mica or illite group. None of the cores appeared to contain clays of the kaolinite group. In the lower section of the J.V. sandstone indications of what appeared to be the mineral sepiolite were noted.

Jan 1, 1959