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By C. C. Merrill

Columbium, tantalum, titanium, and zirconium are present in solid waste products generated by the chlorination of rutile used for production of titanium tetrachloride (TiC14). The columbium and tantalum were separated from titanium and zirconium by liquid-liquid extraction techniques using a secondary amine. Salts of these elements are in a leach liquor produced by water leaching of mineral waste from the chlorination of rutile. This waste, produced at the rate of approximately 50,000 tons per year, is about 40 wt pct water soluble. Leach liquors, separated by filtration, were further separated into a solid fraction and a liquid fraction by pressure hydrolysis, The solid fraction containing Cb, Ta, Ti, and Zr was dissolved in HC1-HF and used as a feed solution. Columbium and tantalum were removed from the organic extractant with 1 [N] HC1. A miniature 10-stage reactor showed that the columbium and tantalum present in solution could be separated with a continuous flow.

Jan 1, 1972

By F. H. Gibson

An investigation was made by the Federal Bureau of Mines of methods for determining phosphorus in coal, coal ash, and coke ash. Several of these methods are being considered for international standardization. As might be expected, methods and proposals from other countries for determining phosphorus differ considerably from those accepted an standard in the United States. Some of the methods differ fundamentally in principle from the American Society for Testing Materials (ASTM) standard used in the United States; others differ only in details of procedure. Because the Bureau considered that certain of the proposed methods might offer advantages in obtaining increased accuracy and precision or in decreasing the time required for making analyses, these methods were investigated, and the results compared with those obtained by the ASTM method. The methods investigated may be grouped into three types--volumetric, colorimetric, and gravimetric. All were about equally accurate and may be used alternatively. From a practical viewpoint, when only a limited number of analyses are made intermittently, the gravimetric procedure probably is the most suitable because no special apparatus or standard solutions are required. The volumetric methods are more rapid when more analyses are made. For mass production, the colorimetric methods, although requiring a suitable photometer or spectrophotometer, are more suitable because a large throughput should be feasible.

Jan 1, 1961

By Helen W. Lang

The Bureau of Mines has developed a very rapid gas chromatographic method for routine determination of oxygen, nitrogen, methane, and carbon dioxide in mine atmosphere samples. Analysis is accomplished in 3 min; readout appears on a single strip chart. The gas sample is split between two columns contained in separate chromatographs. A 5 A molecular sieve column separates oxygen, nitrogen, and methane; a porous polymer column separates carbon dioxide from an air peak. Direct selective analysis of methane from this unresolved air peak is accomplished using a hydrogen flame ionization detector (FID). Carbon dioxide is catalytically converted to methane and detected by FID.

Jan 1, 1972

By R. L. Crosby

The effect of indium on the solid solubility of calcium and of silicon in magnesium was studied using metallographic, X-ray diffraction, and electrical resistivity techniques. The addition of 2 weight-percent or more of indium reduced the solid solubility of calcium in magnesium by forming a compound containing indium and calcium. Indium additions have no perceptible effect on the solid solubility of silicon in magnesium.

Jan 1, 1963

By D. H. Baker

These investigations were conducted to determine the feasibility of molten salt electrorefining of zirconium scrap, offgrade sponge, and alloys under contract number AT(11-1)-475 between the Atomic Energy Commission and the Federal Bureau of Mines. Offgrade zirconium sponge having a Brinell hardness of 169 can be refined by this technique to produce metal having, consistently, a Brinell hardness of less than 90. Also, zirconium alloy scrap, approximating zircaloy-2 in composition, can be refined to recover zirconium metal with a Brinell hardness of less than 100 that is essentially free of the major alloying elements. Analysis showed that the quantities of these elements were decreased as follows: iron from 0.27 to 0.002, tin from 1.36 to 0.001, nickel from 0.02 to 0.001, and chromium from 0.12 to 0.002 percent.

Jan 1, 1961

By M. M. Tilman

The Bureau of Mines conducted research into the dispersion strengthening of lead by the coprecipitation method. Commercially available reagents in water solutions were reacted to form homogeneous precipitates of lead and aluminum compounds. The resulting precipitates were roasted to oxides and reduced in hydrogen to form mixtures of lead powder and alumina. The powders were isostatically pressed into billets which were extruded into rods. The rods were rolled into strip to provide material for testing. Alloys containing 0.5, 1, 2, and 3 nominal volume-percent A1203 were tested in short-time tensile tests and in tensile creep tests. An alloy of Pb-3 volume-percent A1203 exhibited an average tensile strength of 8,570 psi after rolling to 75-percent reduction at 125° C but had no measurable elongation. Alloys of lower A1203 content provided a better compromise between tensile strength and ductility. For example, an alloy of Pb-0.5 volume-percent A1203 had an average tensile strength of 6,590 psi with 9-percent elongation after rolling to 75-percent reduction at 125° C. Creep rates of dispersion-strengthened Pb-A1203 alloys were below 1 percent in 10,000 hours at stresses of 2,000 to 4,000 psi.

Jan 1, 1971

By T. Christos

The explosive oils, nitroglycerin (NG) and ethylene glycol dinitrate (EGDN), were extracted from dynamites by a halocarbon solvent and were then determined by high-pressure liquid chromatography. Separation was achieved by liquid-liquid chromatography on a column packed with Durapak-Carbowax 400/Corasil II and the eluted NG and EGDN were detected with a double-beam ultraviolet detector.

Jan 1, 1973

Objective: To identify and evaluate a durable, flexible, and practical stopping to direct ventilation airflows in large-opening metal/nonmetal mines.

May 1, 2006

By Charles F. Weber

Premature blasts of charges of explosives have caused many deaths in anthracite mines, and the causes of many of the blasts were not determined satisfactorily. Investigators often found fairly high potential differences between such metallic objects as rails, pipes, conveyor lines, or sheet-iron chutes in the working place where an accident had occurred. At one mine where a premature blast occurred in a rock tunnel, one workman was killed and two others were injured, and several days later a potential difference large enough to explode an electric squib was detected between the compressed-air pipe and the track rail; the voltage fluctuated and appeared to change with the movement of a locomotive. At another mine, a. workman was killed when a primed cartridge that he was about to load in a blast hole exploded in his hand. During the investigation, a potential difference was found between the conveyor line and the sheet-iron chute. During a 5-year Period, 61 fatalities and 771 nonfatal injuries were caused by explosives accidents in anthracite mines, and one of the chief causes of these accidents was premature blasts.

Jan 1, 1950

By Árpád B. Palotás, Adel F. Sarofim, John B. Vander Sande, Paolo Ciambelli, Lenore Rainey

"The evolution during oxidation of the internal structure of soot and carbon black particles was studied using high-resolution transmission electron microscopy (HRTEM) and an image analysis system. Increasing ordering to the carbon structure with increasing oxidation is observed. Measures of the increased order are increases in the fractional coverage of a cross section of the particles with a layered structure, a decrease in the mean interlayer spacing, and a decrease in the spread of the interlayer spacing. The changing structure of the carbon black impacts its properties, such as the rate of oxidation.There is considerable interest in the study of the structural changes of carbonaceous materials as a function of oxidation. Davis et al.1 measured the variation of carbon dioxide surface area of various coals as a function of residence time in a flow reactor. HRTEM measurements revealed that crystallite dimensions and interlayer spacings are altered by combustion. Ishiguro et al.2 showed that oxidation alters the structure of diesel soot. The aim of our current research is to develop a better understanding of the microstructural reordering of carbon blacks with implications to their properties. The carbon blacks used in this research have already been studied and their reactivities as a function of oxidation measured.3The methodology used in this work has already been described in detail elsewhere.4 This paper presents an application to quantify the structural changes of carbon black particles as a function of oxidation and graphitization. The technique used is based on the use of HRTEM (high-resolution transmission electron microscopy) and computational image analysis.It is well-known that carbonaceous materials like graphite, soots, coals, chars, etc., possess characteristic structural appearances which can vary from mostly random or amorphous to a perfectly ordered graphitic crystalline structure. The carbon structure has been variously described as turbostratic5 or as crumpled sheets6 to indicate that parallel layering, reminiscent of graphite, is observed over dimensions of nanometers but that these planes or crystallites show disorder over larger scales. The degree of order of such structures is strongly dependent on the thermal treatment of the material as well as the composition of the source of the carbonaceous material. The value of electron micros¬copy in studying the morphology of such materials has been well established,2,7,8 although only a few attempts toward quantification have been made.The sample observed was carbon black CB330 from De¬gussa. One set of carbon black samples were oxidized in a thermo-gravimetric analyzer (TGA) in air at 575 0C, so that the conversion varied from 0 to 96%. Another set of carbon black samples were graphitized (Graphpac-GB by ALLTECH) and then oxidized in the TGA at 680 °C until 92% burnout was reached. The latter samples are called GB 0% and GB 92%, respectively.For the HRTEM observation a small portion of each sample was ultrasonically dispersed in ethanol. The suspension was deposited dropwise on a copper TEM grid coated with a lacey carbon film. The examination of the samples was carried out on areas that extend over the holes in the supporting film in order to avoid interference from the amorphous carbon background film An oriented gold crystal was used as a calibration standard and subjected to the same techniques as the carbon black samples."

Jan 1, 1998

By Robert A. Jankowski

Through laboratory and underground studies, the Bureau of Mines has evaluated the use of passive barriers (dust shields) to help confine dust generated by longwall shearers to the face area. Laboratory studies focused first on selection of the optimum barrier design, which proved to be a simple, gobside barrier (made of conveyor belting), coupled with a headgate splitter arm, which was found necessary to prevent the dust cloud from entering the walkway at the headgate end of the shearer when cutting tail to head. Further laboratory testing was done to determine whether using passive barriers in combination with different water-spray dust-reduction methods, including the shearer-clearer system developed by the Bureau, would improve dust reduction over that from using the water sprays alone. It was found that the combination of gobs ide passive barriers plus the full shearer-clearer system was most effective, and surmised that this would be especially useful in thicker seams. However, underground testing revealed that the shearer-clearer system alone was 35 pct more effective in reducing dust contamination than when used with the gobside passive barriers, and far more effective than using passive barriers with a conventional water spray system. For such an effective system as the shearer-clearer; the reduction in avail-able space over the top of the machine actually impeded system performance; this was shom1 in both eastern and western mines. But when used with comparatively inefficient water spray systems, the passive barriers, used in combination with a headgate splitter arm, provide consider-able help in reducing dust levels in the walkway.

Jan 1, 1986

By Irving Hartmann

The fire end explosion hazard of excessive coal-dust deposits in mines has been recognized for many years, and important measures have been developed for reducing dust formation and to alley loose dust near its source. Nevertheless, in the course of normal mining it has been estimated that 1 to 3 percent (in some thin, friable seams up to 10 percent) of the total coal mined is reduced to dust of through-20-mesh fineness. In highly mechanized, continuous mining operations the production of fines is even greater. Most dust is trapped near its point of origin and removed from the mine, but large quantities are transported by the air current and by haulage into entries, where the greatest proportion settles on the floor and the balance on the rib and roof surfaces. The latter is generally finer in particle size than the floor dust; this, coupled with its more advantageous position for dispersion, makes the rib-roof dust (also to be referred to as overhead dust) a greater potential explosion hazard.

Jan 1, 1954

By D. A. O'Keefe, M. M. Wong

To obtain beryllium metal of higher purity , flakes produced from electrorefining scrap metal were used as cell feed for a second cycle of electrore fining at 500 ° C in an electrolyte composed of 51.7 mole - percent LiCl , 36.9 molepercent KC1 , and 11.4 mole - percent BeC¹ · Metallic impurities in the flakes totaled more than 108 ppm , the metallic impurities in the metal obtained from the two - cycle electrorefining were , with the exception of 35 ppm of calcium , below the spectrographic determination limits .

Jan 1, 1964

By F. H. Nehl

Ion elutriation was used to extract silver cyanide complexes and free cyanide from aqueous streams containing up to 10 ppm silver and 5 ppm free cyanide. Screening tests selected nine of 350 different surfactants for further, larger scale experiments. The screening procedure used 0.1 g of each of the surfactants in 300 mL of synthetic wastewater. Air was sparged into the test cell at 50 cc/min. The foam was refluxed during the tests and was not sampled. Samples of the solution were taken at specified intervals and analyzed by wet chemical methods for free cyanide and by atomic absorption for silver content. The most effective surfactants lowered the silver and free cyanide concentrations to less than 0.5 ppm in 1 h or less. These surfactants were quaternary amine salts with one long chain (C12-C18) organic group and three methyl groups. Experiments using 3 L batches of wastewater or an ion elutriation cell continuously fed with solution draining from an inactive heap leach operation confirmed the results from the screening tests.

Jan 1, 2010

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 John Redington

This paper describing the milling practice at the Coniaurum Mine is one of a series of papers on milling methods, practice, and costs prepared in cooperation with an published by the United States Bureau of Mines. The 500-ton will of the Coniaurum Mines (Ltd.) is located at approximately the center of the company's property and a little more than a mile from the town of Schumacher, Ontario. The main shaft through which all the ore is heisted is adjacent to the mill so that the ore hoisted in a 3-ton skip is dumped directly into a 15-ton bin at the crusher.

Jan 1, 1931

By Loyal Clarke, H. H. Storch

"The discovery of large deposits of polyhalite (K2S04.MgS04.2CaSO4.2H2O) in Texas has led to an investigation of possible industrial proecsses for the extraction of potash from this material. This mineral was first discovored in small quantities in the European potash deposits in or about the year 1800. Chemists fire thought it to be a form of calcium sulphate, but a more accurate analysis by Strohmiyer indicated the composition as given by the above formula.The decomposition of polytalite by aster is very slow and results in the formation of a layer of gypsum at the surface of the polyhalite which retarts the solution of the potaseium and magnesium sulphates. To obtain a substantial yield of K2S04 in solution it is necessary to use large amounts of water at room temperature, for he concentration of K2S04 is limited by the low solubility of syngonite (K2S04.CaS04.H2O) whereas at 100º C. several days boiling are necessary to obtain more than a 6 per cent K2S04 solution even when finely powdered polyhalite is employed.In 1854 H. Rose discovered that calcination, followed by leaching with water, resulted in a larger extraction of the potassium and magnesium sulphates, as compared with leaching without precalcination. During the course of a series of investigations concerning formation of oceanic salt deposits, Van't Hoff and his pupils obtained sufficient data to construct the equilibrium diagram for the system K+Mg+SO4--Ca++.H2O for 25° C. and for 83° C. These data are very well summarized. in the International Critical Tables' and by Boeke and Eitel. From a consideration of the diagrams for 83º C. one would conclude that an extraction of polyhalite with moderate amounts of water at 33º C. would result in a solution whose maximum concentration of K2So4 would be about 3.6 grams per 100 grams of water and of M2SO; about 4.0 grams per 100 grams of water, corresponding to equilibriumwith the solid phases: Polyhalite potassiam-calcium pentasulphate and anhydrite.The fact that it has been found possible to obtain as high as 11.4 grams of K2S04 per 100 grams of water (see table 6) and an equivalent amount of MgSo4 (8.1 grams per 100 grams of water was obtained corresponding to a ratio K2/Mg of 0.98; indicates that the formation of these complex salts is very slow. To be sure, this results was obtained at 100° C. instead of 83º C. However, the work of Anderson and Nestall 9 on the double salts of calcium and potassium sulphates at 100º C. indicates that the diagram at 100º C. C. would not be greatly different from that at 83º C. This slow rate of approach to equilibrium when combined with precalcination of,of polyhzli-,a is the 17,asis of some of the more p:olisinE methods of extracting potash from polyhalite."

Jun 1, 1930

By F. W. Hoertel

Near-optimum parameters were determined by the Bureau of Mines for vapor deposition of rhenium on heated copper substrates by hydrogen reduction of rhenium hexafluoride (ReF6). High-purity deposits of nearly 90-percent theo¬retical density were obtained with the reaction chamber at 250° C, with an H2 to ReF6 volume ratio of 25 to 1, and with an ReF6 flow rate of 5 grams per hour. Some rhenium deposited as a loose, black powder. When the established near-optimum parameters were carefully followed, this could be minimized but never completely avoided. Varying the reaction chamber pressure, both above and below atmospheric, yielded excessive quantities of rhenium powder. Deposition efficiencies, based on only the coherent metal, ranged between 70 and 75 percent. Massive deposits contained only spectrographic traces of impurities. The average microhardness (Knoop, 100-gram load) of vapor-deposited rhenium was 907. Limited research on the deposition of rhenium-tungsten alloys by reduction of the mixed hexafluorides produced deposits in which linear composition gradients were pronounced; this nonhomogeneity was attributed to the wide variation in optimum hydrogen-reduction temperatures of the two hexafluorides (250° C for ReF6 and 550° C for WF6). Using deposition temperatures between 250° and 550° C did not eliminate the composition variations.

Jan 1, 1967

By R. Hogg, E. Kaya

"The presence of agglomerated particles in airborne dust in coal mines has been confirmed by SEM examination of static samples collected on substrates. In addition, the effect of agglomerated particles on the performance of cascade impactors and cyclone-type personal samplers has been studied. Simple procedures have been developed for evaluating the extent of agglomeration in air-borne dust by comparing the observed size-selectivity of the sampling devices with that expected under idealized conditions. Applications of these techniques in the laboratory and in underground mines are discussed.INTRODUCTIONAirborne dust is invariably present in mine atmospheres. Particle size is a primary factor in determining the behavior of the dust, its effects on miners' health and the effectiveness of dust control measures. Obviously, agglomeration of the dust particles can have important effects on: ""natural"" dust removal processes such as settling• the use of water sprays etc., for dust control• pulmonary deposition characteristicsIn addition, the presence of agglomerates could influence the effective toxicity of the dust. For example, ultrafine particles are often thought to be relatively unimportant in the development of respiratory ailments because of their low deposition efficiency. However, the latter could be substantially increased if such particles were present in larger agglomerates. It is by no means obvious that there should be significant agglomeration of the airborne dust in a mine atmosphere. In fact, calculations based on the classical coagulation theories indicate that, at the kinds of dust concentrations that exist even in what would be regarded as “very dusty"" atmospheres, the coagulation half-time* .should be of the order of weeks or even months. On this basis, agglomeration would be expected to be essentially negligible. On the other hand, laboratory experiments (Polat et al., 1991) have revealed very extensive agglomeration in the airborne dust released during the crushing of individual coal and mineral particles. It is postulated that such agglomeration occurs immediately at the point of dust generation. In other words, many of the fine fragments produced on fracture are never completely separated from their neighbors."

Mar 1, 1992

By Richard L. Sayrs

The Idol zinc prospect, formerly known as the Comstock, was examined by Harold B. Ewoldt, a Bureau of Mines' engineer, accompanied by Deane F. Kent of the United States Geological Survey on July 22, 1943. Previous to that time, the Geological Survey had contoured and studied the area. As a part of the war minerals program, further investigation of the area was recommended. The Dalton property, a mile and a half northeast of the Idol property, was examined during the progress of the work at the Idol, and it was decided to include this property also in the project. From February 7, 1944, to May 16, 1944, six holes totaling 2,739 feet were diamond-drilled on the Idol property and eight holes totaling 1,850 feet were diamond-drilled, and three pits channel sampled on the Dalton property. The drilling showed sphalerite to be sparsely distributed through a 100 foot thickness of the Kingsport member of the Knox dolomite.

Jan 1, 1949