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By H. J. Coleman

Knowledge of the types of naturally occurring sulfur compounds in petroleum is of both theoretical and practical interest to petroleum chemists and geologists. This knowledge has been extended by the identification of 77 sulfur compounds, including 36 thiols, 23 chain sulfides, and 18 cyclic sulfides in a 111° to 150° C boiling range distillate of Wasson, Texas, crude oil. The characterization procedure used in separating and identifying these compounds included isothermal distillation, vacuum fractionation, liquid-solid chromatography (alumina adsorption), chemical treatment, gas-liquid chromatography, microdesulfurization, and infrared analysis. The procedural steps described represent a systematic method of sulfur compound analysis considered applicable for determining the nature and concentration of the sulfur constituents present in any straight-run petroleum distillate of the above-boiling range.

Jan 1, 1966

By Thomas C. Atchison, Joseph M. Pugliese

Six explosives were compared by measuring their strain- producing abilities in limestone . Peak strain , e , varied with scaled distance , R/Ro , according to the following equation : € = Kc (R /R 。)- ". The distance exponent , n , was a constant of the rock and did not depend upon explosive . The strain intercept , Ke , increased with increasing detonation pressure of the explosive . The strain intercept also depended upon the explosive- to - rock impedance ratio . For impedance ratios from 0.53 to 1.38 , the strain intercept was approximately proportional to the medium stress , Pn , as calculated from the explosive detonation pressure , P , and the explosive - torock impedence ratio , Z , by the simple elastic theory relation : P = 2P / ( 1 + Z ) . PD However , the data indicated that , at lower values of impedance ratio , the strain intercept is relatively larger than would be expected from the simple elastic theory . The results presented provide a simple method for predicting the relative effectiveness of different explosives in breaking limestone from the detonation pressures and characteristic impedances of the explosives .

Jan 1, 1964

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 D. D. Hamilton

The ISMS program provided for the development and demonstration of equipment modifications for improved safety in both conventional and continuous coal mining systems. This report documents the success of the program in identifying accident hazards in underground coal mines with 4-to 8-foot seam heights, in designing modifications to reduce the hazards, and in demonstrating improved safety through extended underground use of the ISMS equipment.

Jan 1, 1977

By R. O. Dannenberg

The Bureau of Mines investigations described in this report were undertaken to devise a process to economically recover precious metals and copper from low-grade, complex electronic scrap generated in large quantities by military and civilian electronic operations. Leaching with various media is applicable to certain selected items of electronic scrap but cannot be practically applied to complex mixtures of scrap. A process comprising incineration, caustic leaching to remove aluminum, smelting with a siliceous slag, and electrolysis recovered 99.9-percent-pure copper metal and anode slimes assaying more than 7,000 ounces per ton of combined precious metals. Silver, gold, and copper recoveries were 93, 95, and 87 percent, respectively. Cost analysis indicated that an alternative process using direct smelting of the scrap to make assayable products for sale to a custom smelter would provide better overall financial returns.

Jan 1, 1972

By F. G. Horino

The Bureau of Mines conducted compressive strength tests on model pillars of selected rock types with each pillar containing a critically oriented plane of weakness. The objective of these tests was to determine if a significant increase in the strength of the model pillar could be obtained by either (1) installing tensioned rock bolts through the pillar and normal to the plane of weakness, or (2) wrapping tensioned steel wire ropes around the pillar at uniformly spaced intervals along the pillar. Equations based on Coulomb's failure criterion are developed to predict uniaxial compressive strength of model pillars that are either rock-bolted or wire-roped. Laboratory compressive strength tests on unbolted and bolted model pillars of sandstone, marble, Indiana limestone, and oil shale containing a plane of weakness oriented at 45° showed that the bolted pillars are stronger than the unbolted pillars by 84, 31, 52, and 28 pct, respectively. Laboratory compres-sive strength tests on nonroped and roped model pillars of Texas limestone, sandstone, and granite containing planes of weakness showed that the roped pillars were stronger than the nonroped pillars by factors ranging from 1.01 to 2.41, depending upon the angle of the plane of weakness and the rock type. Rocks with a low Young's modulus benefited most by the wire-roping technique.

Jan 1, 1971

By R. S. Dean

The principle of explosive crushing depends upon the fact that an expandable substance contained within the pores of a solid body will disrupt such a body upon expansion. Such expansion may be obtained by the detonation of an explosive or by the sudden release of pressure of a superheated liquid. That this principle of disruption may be applied to minerals rests on the fact that cracks, cleavage planes, and pores exist in all mineral to an extent hardly conceived possible heretofore. Crushing by this method takes advantage of force applied from within the mineral rather than from forces applied from without. The application of a force from within would appear to be more effective. A consideration of the possibilities of such a method for crushing led to some experimental work of a preliminary nature, the results of which are embodied in this paper. No systematic program was followed in the work and the results are, therefore, not final and far from complete. The success attained so far, with the mediocre apparatus available seems to warrant a preliminary report, with the expressed hope that the work may be carried on as well-outline program covering such phases as have been impossible to investigate at this time.

Jan 1, 1931

By F. E. Block

The metallic reduction of vanadium chlorides was investigated by the Federal Bureau of Mines as a possible new route for preparing vanadium metal in an effort to develop a production process that would be adaptable to large-scale plant production and would yield metal of uniformly high quality. Vanadium tetrachloride was usually prepared by chlorinating vanadium pentoxide in the presence of carbon. Although oxygen-?free tetrachloride was difficult to prepare this way, it could be prepared by the direct chlorination of vanadium carbide. Lower valent vanadium trichloride was prepared by the thermal decomposition of vanadium tetrachloride. Vanadium dichloride was also prepared by the thermal disproportionation of vanadium trichloride.

Jan 1, 1961

By Philip C. Good

Preliminary studies showed that direct hydrolysis of H2SiF6 to SiO2 and HF at elevated temperatures was subject to many mechanical difficulties, and that corrosion of construction materials was a serious problem. Elimination of SiO2 from the HF product was generally poor. An alternative procedure, hydrolysis of lime-neutralized H2SiF6 by steam at 950° to 1,100° C, yielded a product very low in SiO2. Condensates containing up to 300 g/1 HF were prepared.

Jan 1, 1968

By A. S. Moore

The Bureau of Mines is doing research and development work on removing acid-gas impurities from synthesis gas made directly from coal. Since conventional gas scrubbers, packed towers and bubble-cap columns, are expensive to construct and difficult to operate with viscous solutions, one aspect of the work was developing a compact, agitated, gas-liquid contactor for use with concentrated absorbents. The efficacy of the agitated contactor for absorbing carbon dioxide in diethanolamine increased with increasing solution rate, turbine speed, diethanolamine concentration, and carbon dioxide concentration in feed gas, and with decreasing liquid-gas ratio. It was unaffected by pressure between 200 and 300 p.s.i.g. and little affected by temperature between 115 and 190° F.

Jan 1, 1961

By C. R. McCann

The Bureau of Mines conducted an experimental study of conditions needed to produce flames of pulverized coal when the heat needed for ignition is sup-plied only from the flame and hot furnace refractory. An electrically heated furnace which burned about 1 pound of coal per hour was designed and fabricated. A sheath of air, surrounding the primary coal and air stream, was used to prevent entry of hot gases from recirculating combustion products. Furnace temperatures needed for ignition ranged from about 1,8300 F for an Illinois coal to 2,250° F for a Beckley seam coal. Apparent flame velocities were about 2 to 5 feet per second, increasing with volatile content of the coal and with distance from the burner mouth to the flame. The time required for ignition, approximately 0.02 to 0.07 sec, was a better measure of flame behavior than was velocity.

Jan 1, 1969

By K. K. Kershner

Nickel having a purity of more than 99.99 percent with reference to metallic impurities was electrodeposited at the Rolla Metallurgy Research Center of the Federal Bureau of Mines. The production of high-purity nickel is in keeping with the current trend in technologies for producing metals with lower and lower percentages of impurities. To understand more fully the role to be played by nickel by itself and as a component in many alloys, the element must be in a state of high purity. Procedures are outlined for purifying nickel solutions by precipitating and filtering off impurities. Details are given for using the purified solutions as electrolytes in depositing high-purity nickel. The elecneleposited nickel contained 0.0005 to 0.002 percent each of cobalt, copper, aid iron together with spectrographically detectable traces of aluminum, magnesium, and silicon. The deposits were smooth and dense; the crystalline structure was typical of an electrodeposited metal. Some preliminary experiments for purifying nickel solutions by liquid-liquid extraction are also described in this report. Tests of this type were limited since more encouraging results were obtained by other methods of purification.

Jan 1, 1961

By V. T. Dow

In April 1957 the Bureau of Mines instituted a reconnaissance of titanium-and zirconium-bearing heavy sandstone deposits in the Four-State area of Utah, Wyoming, New Mexico, and Colorado. This report summarizes the study. Eighty-two deposits or groups of deposits, containing an estimated 27,920,000 tons of titaniferous sandstone, were examined in the Four-State area; 16 in southern Utah, 19 in Wyoming, 33 in New Mexico, and 14 in southwestern Colorado. The 16 deposits examined in Utah contain an estimated 1,043,000 tons with an average grade of 17.98 percent TiO2, 5.67 percent ZrO2, 20.98 percent Fe, and 0.09 percent equivalent Th02. The 19 deposits investigated in Wyoming are estimated to contain 21,873,000 tons of titaniferous sandstone having a weighted grade of 5.22 percent 702, 0.55 percent ZrO2, 24.8 percent Fe, and 0.01 percent equivalent Th02.

Jan 1, 1961

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 Michael G. Zabetakis

Investigation of gas explosions usually reveals that the combustible gases have come from transmission and storage facilities or from natural gas or oil wells. However, combustible gases such as methane and hydrogen can derive from biological processes. Hazardous situations have been created in the past by the use of abandoned mines for the disposal of sewage and rainwater, by the interconnection of storm and sanitary sewers, by sealing the openings in manhole covers when repaving the roadway over a sanitary sewer, and by the construction of buildings over or near garbage fill areas without adequately providing for the release of combustible gases.

Jan 1, 1962

By Jack E. Fraley

In this Bureau of Mines study, sealants containing mineral wool, cement, etc, were sprayed through dry-process equipment that propels dry material pneumatically to the water-adding nozzle. Advantages over slurry applications include no mixing, no extensive cleanup, and freedom from hardened cement in equipment should power be lost. Sealants with large mineral wool nodules (>l-inch) were sprayable at rates to 900 square feet per hour for 1/2-inch thickness with little dust and smooth material flow through equipment, but they were weak for mine use, Materials containing small wool nodules (1/4-inch) were stronger but tended to plug lines because the nodules were inadequately separated in the shredder. Increasing the dedusting oil also increased line plugging by holding the nodules together in larger lumps. Best results were obtained using a 3/4-inch-nodule wool with cement binder, which provided both smooth flow through the machine and adequate strength.

Jan 1, 1977

By W. D. Mcmillan

The Dempsey tract in Washington County, Mo., had a small production of lead-zinc ore from shallow workings. Old dumps from early-day lead mining contain about 25,000 tons of ore averaging about 3 percent combined zinc and lead. Because of the urgent war requirements for lead and zinc, the Dempsey property was examined by Otto Ruhl, formerly an engineer of the Bureau of Mines in August 1942 and selected for further investigation by churn drilling twenty holes totaling 1,309 feet were bored in the fall of 1943. The results of the work are presented in this paper.

Jan 1, 1948

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 D. A. Reynolds, C. R. Holmes

The Bureau of Mines - American Gas Association ( EM - AGA) carbonization test has been used to determine the carbonizing properties of 66 American coals and a larger number of coal blends . A summary of the results obtained for the first 30 coals , including 6 blends , has been published ,4/ and results for individual coals have been reported as the investigations were completed . A bibliography of all publications pertaining to this work has been issued recently . Many of the coals were carbonized at 800 ° and 900° C. in two sizes of retorts ( 13- and 18 - inch diameters ) ; and , because the quality of coke is affected by changing the size of the retort , this report has been prepared to show the average physical properties of coke from the two sizes . This report also purposes to extend the correlation of the physical properties of coke with the rank of coal made by Fieldner and Davis in their summary of the EM-AGA tests on the first 30 coals .

Jun 1, 1942

By R. J. Leary

Significant improvements in surface conditions or mechanical properties of steels have been attributed by several investigators to ladle additions of small quantities of rare-earth metals or their oxides. To investigate systematically these effects in wrought and in cast plain carbon and alloy mechanical steels containing approximately 0.35 percent carbon, heats of four representative compositions were melted by the Bureau of Mines in a 4-ton open-hearth furnace. Each heat was cast into three sets of ingots to exemplify respectively, treatments with (1) rare-earth metals, (2) rare-earth metal oxides, and (3) an untreated set as a control. The development of melting, casting and rolling practices is described and discussed. Lance injection of oxygen shortly after melt raised the temperature of the metal immediately as much as 500° F., principally because mechanical agitation exposed the high-carbon metal to the flame and furnace root. An exceptional degree of superheat in the metal at the termination of the refining period was attributed to oxygen injection during the refining period. Bath temperatures higher than industrial practice were permitted by the all-basic furnace lining. Rates of carbon elimination as high as 0.036 percent carbon per minute were achieved by oxygen injections.

Jan 1, 1961