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By J. L. Hoffman, F. W. Wood, R. A. Beall, W. E. Anable

For melting and purifying reactive and refractory metals , two electronbeam furnaces have been constructed and operated on the principle of highpowered vacuum diodes . It was necessary to design the vacuum and electrical systems , mechanical features , and operating procedures to cope with dynamic conditions . Vacuums of 10-5 torr , tens of kilowatts of power at 5 to 10 kilovolts , and the evolution of impurities at thousands of liters per minute constitute a challenging combination . The furnaces have been used to melt either button specimens weighing several hundred grams or , by feeding material as a consumable electrode , small ingots weighing several kilograms . Hafnium is among the metals that can be purified . For example , hafnium starting material with Rhn 94B was softened to Rhn 70B after 2 hours of melting under a 25 - kw electron beam , and impurity levels were reduced as follows : Oxygen , from 700 to 350 ppm ; nitrogen , from 71 to 20 ppm ; hydrogen , from 6 to 1 ppm ; aluminum from 75 to < 20 ppm ; chromium , from 80 to < 10 ppm ; iron , from 100 to 40 ppm ; and silicon , from 40 to < 20 ppm .

Jan 1, 1963

By Henry E. Blake

Defluorination studies on refractory fluoride - bearing compounds and minerals , particularly on partly defluorinated residues from high - temperature pyrohydrolysis , required a dependable and reasonably accurate analyticalcontrol method for the analysis of fluorine . The difficulty in liberating fluorine from the fluorides of metallic elements such as aluminum, zirconium , and rare earths by steam- distillation can be largely overcome if the distillation is made from a sulfuric - phosphoric acid solution of a sodium carbonate fusion of the sample material and if the distillation temperature is maintained at about 155 ° C. The data presented in this paper show that liberation of fluorine by this method is more complete and proceeds more rapidly than by usual distillations from perchloric or sulfuric acid alone or a mixture of phosphoric and perchloric acids . Fluorine in amounts ranging up to about 140 mg can be recovered by collecting only about 300 ml of distillate . Determination of fluoride in the distillate is made by the usual thorium nitrate titration .

Jan 1, 1963

By L. G. Trudell, J. W. Smith, K. E. Stanfield

Representation of actual oil yields from sections of the Green River formation oil shales by two types of drill - cutting samples was evaluated . Average oil yields of single sets of mud cuttings from hydraulic rotary drilling in Colorado and gas cuttings from pneumatic rotary drilling in Utah were compared statistically with yields of core samples taken from adjacent holes . Oil yields from gas cuttings were identical to oil yields of core samples . Mud cuttings appeared to represent a section of the formation conservatively , the deficiencies increasing with increasing richness of sample . Because a large amount of the oil - yield data currently available for the Green River formation is based on mud- cutting samples , development of a valid correction method by additional testing is needed .

Jan 1, 1963

By D. W. Bridges, L. Crocker, R. O. Dannenberg

About 95 pct of the beryllium was dissolved from most ore samples by agitation leaching with 600 lb of H2SO4 per ton of ore for 24 hours at 65 ° C and 35 pct solids . Leach slurries generally were viscous , and the limiting pulp density for thorough mixing was about 35 pct solids . Settling of the leached pulp required 0.6 to 0.8 lb of a polyacrylic flocculant per ton of ore leached with 600 lb of H2SO4 per ton , whereas ore leached with 800 lb of H2SO4 per ton required only 0.2 to 0.3 lb of flocculant per ton . Terminal densities of the settled pulps were about 28 and 35 pct solids , respectively , from leaches using 600 and 800 lb of H2SO4 per ton . Vacuum filtration of settled pulps at 15 in . Hg resulted in a filter cake containing 50 to 59 pct solids . Roasting the ore at 500 ° C before leaching increased the limiting pulp density for effective mixing to 50 pct solids . Acid requirements , however , were not diminished , although leaching roasted ore with 600 lb of H2SO4 per ton resulted in densification of settled pulps to about 40 pct solids . Filter cake from leaching preroasted ore contained about 20 pct less water than that from unroasted ore .

Jan 1, 1963

By R. P. Adams, R. A. Beall

The Bureau of Mines developed a method to melt and cast specimens of hafnium- carbon alloy and studied their properties . A rotating - ladle vacuum or inert atmosphere arc furnace was designed , special electrodes and molds were developed , and operating procedures were worked out for casting small shapes . The cast specimens were evaluated according to their carbon content for melting point , density , microhardness , electrical resistivity , and oxidation resistance . Lattice dimensions were determined , and metallographic specimens were prepared . Photomicrographs were taken of specimens containing 2.72 , 5.50 , 6.47 , 9.97 , 12.8 , and 15.7 weight - percent carbon , and their grain structures were compared .

Jan 1, 1963

By R. V. Higgins, A. J. Leighton

A computer program has been devised to calculate the reservoir performance of water floods of complicated well - spacing patterns . The method and program have been tested by calculating the waterflood performance of fivespot patterns using oils of different viscosities and the performance calculations agreed closely with laboratory results . The program on a high - speed digital computer will process the performance prediction in about 1 minute , which is very rapid for a prediction using so much fluid mechanics and nonlinear geometry . The program has been presented in such a way that one may use it as given and save the time required to write and " debug " one of his own . gram processes a complex reservoir analysis , many of the complicated steps are explained in detail , both for the fluid mechanics and the directions for the computer . The subtle features that originally delayed the application of the program to unusual combinations of permeability and viscosity relationships are incorporated and explained

Jan 1, 1963

By B. B. Letson, D. F. Smith, T. E. Gardner, A. R. Taylor

Low- temperature heat capacities of strontium chloride (7° - 300° K) and strontium fluoride ( 11 ° - 300 ° K) were measured with an adiabatic calorimeter . Smooth values of heat capacity , entropy , enthalpy function , and free - energy function were calculated from the heat - capacity data . The smooth values are reported at 10 ° K intervals and at 273.15 ° and 298.15 ° K.

Jan 1, 1963

By F. W. Hoertel

The Bureau of Mines investigated the use of depleted uranium as a sacrificial anode for the cathodic protection of submerged and underground structures of iron , steel , and copper . Uranium-metal couples were tested in simulated marine environments of varying oxygen contents at pH values between 5.5 and 8.5 and under simulated boiler service condition in Rolla , Mo. , city water . Similar couples were tested in samples of Missouri soils to simulate underground service . Uranium remained anodic to iron , steel , and copper in the simulated marine environments and under simulated boiler service if the electrolyte was oxygen- free city water . Uranium appeared to offer limited protection to iron , low- carbon steel , stainless steel , copper , and zinc in the simulated underground tests . Uranium anodes offer a space advantage because 1 cubic inch of uranium gives approximately the same protection as 2 cubic inches of magnesium or 1-1 /2 cubic inches of zinc .

Jan 1, 1963

By NIOSH NIOSH

This work explores application of a double alkaline leach method to extraction of alumina from Oregon ferruginous bauxitic materials. The process recovers a greater proportion of alumina from high-silica ores than is possible by a conventional single-leach method. This recovery is accomplished by calcining the ore, removing reactive silica in a preliminary dilute caustic soda leach, and then applying a second leach to dissolve alumina. Ores containing up to 15 percent Si~) 35 percent AI;:) Os, and 30 percent Os were examined. Under conditions of treatment established by experimentation, more than BO-percent alumina extraction was demonstrated. When and if conditions demand the use of low-grade materials, the double-leach process is capable of providing millions of tons of alumina from Oregon ferruginous bauxite.

Jan 1, 1963

By A. J. Forney

The hot-gas-recycle process, for the hydrogenation of carbon monoxide, was investigated in a 12-inch-diameter reactor. Initially because the distribution of gas was poor, hotspots developed in the catalyst bed. After the velocity profile of the gas flowing through the bed was studied, the method of packing the catalyst was altered. Because this change improved the distribution of gas, temperature control was excellent. The l2-inch-diameter reactor was operated successfully in the synthesis of gaseous and liquid fuels. When high-Btu gas was synthesized in two stages, parallel-plate assemblies of Raney nickel were almost as active as granular Raney nickel in the second reactor. The pressure drop through the second reactor, however, was reduced 90 percent by the use of these assemblies.

Jan 1, 1962

By P. S. Jacobsen

In 1960 over 93 percent of the coal cleaned mechanically in the United States was cleaned in processes that utilized water or dense-medium suspensions of fine solids in water. Thus, in the process of removing deleterious ash-forming and sulfur-bearing minerals, another deleterious substance--water-- is added to the coal. The subsequent removal of the water from the coal, and the concomitant recovery of the coal from the water, is not troublesome in the sizes coarser than 1/4-inch. In the finer sizes, however, it is a difficult procedure that often costs more than the original washing operation. Because of the importance of liquid-solids separation in coal preparation, the Bureau of Mines has a continuing program of research in this field. The objective is to make available information on the performance characteristics of various types of equipment available for liquid-solids separations, thus promoting the wise selection of equipment for specific applications, and, thereby, more effective processing of coal. Results of work on flocculation as an aid to filtration5 and the sieve bend screen6 have been published. The present investigation of the screw-type classifier operating in combination with the cyclone was undertaken primarily because such classifiers are comparatively new to coal preparation and information on their performance is not available. The cyclone has become well-known since its introduction in this country by the Bureau of Mines in 1948.7 Use of the cyclone in conjunction with the screw-type classifier represents an attempt to provide the maximum recovery of solids at minimum moisture content.

Jan 1, 1962

By Alfred V. C. Meyer

A Blastcorder4 was calibrated on the Bureau of Mines shaking table in the frequency range of 12 to 40 c.p.s. and in the amplitude range&apos; of 0.25 to 1.0 g. The results of this calibration study show that in the frequency range of 12 to 30 c.p.s. the average accuracy of the Blastcorder is approximately ± 0.1 g.

Jan 1, 1962

By W. A. Calhoun

A method for concentration of the nickel-cobalt-bearing mineral, siegenite, from a table middling has been developed by the Bureau of Mines at Rolla, Mo. The table middling is composed of a complex series of sulfide minerals, occurring in mill operations in the southeast Missouri "lead belt." In these operations the siegenite is lost as a separate concentrate, being diverted to other products. The procedure also includes recovering commercial-grade concentrates of copper and lead. A low-grade zinc concentrate, a potential coproduct, was also made.

Jan 1, 1962

By Francis J. Kelly

This Bureau of Mines study was made to obtain and present facts concerning the production and marketing of rare-earth metals and thorium in the Central and Southern Rocky Mountains (Arizona, Colorado, New Mexico, Utah, and Wyoming, referred to in this report as the region) and to review the current demand for these elements in the United States. Little or no published information was available on the marketing practices for these commodities. As a result of many inquiries from industry, potential prospectors, and the general public, the various factors of resources, production (present and potential), marketing, and consumption have been investigated, and the results are set forth in this report. Material concerning occurrences and deposits is from published references detailed in the bibliography.

Jan 1, 1962

By W. L. Dare

Tri-axial strains in pillars, created by pillar robbing, were measured in an experiment at the Dysart No. 1 uranium mine near Grants) New Mexico. At this mine, room-and-pillar stoping is used on the advance, and pillars are recovered on the retreat. The are deposit is, for all practical purposes, horizontal. Measuring devices were installed in pillars approximately 90 to 200 feet from the break line, and strains were recorded over a 4-to 6-week period. The measurements indicate that, in general, the algebraic magnitude of vertical strains increased, and the horizontal strains decreased, in turn, indicating that vertical (or near vertical) loads on the instrumented pillars lessened as pillars were recovered.

Jan 1, 1962

By A. A. Cochran

The purpose of this Bureau of Mines research was to investigate the theoretical and practical aspects of using ionizing radiation to promote chemical reactions that are of interest to metallurgists, and to carry out a radiation study of a suitable reaction. The effect of 44,000 roentgens per hour of 120,000-volt X-rays on the chlorination of highly pure mixtures of rutile, carbon, and various catalysts at temperatures up to 540° C. is described. At these low temperatures, recoveries were very low; however, in the eight different systems studied, an increase in yield due to X-rays was statistically significant in two instances and was of borderline significance in a third instance. In the other five systems, the differences in yield were not significant. Impurities and added catalysts caused relatively large variations in the yield of TiC14 from the reaction. Although the catalysts employed were reported in the literature as positive catalysts for the reaction, most of them were negative catalysts for the highly pure system studied. With only one exception, each increase in the purity of the charge resulted in a decreased yield of TiCl4. The experimental results indicate that many substances catalyze the reaction studied and suggest that the differences in reactivity of the charge stocks may be due to their various contents of positive and negative catalysts.

Jan 1, 1962

By Roy F. Waters

An inventory was made by the Bureau of Mines of wastes of mineral origin, water requirements, treatment of wastes, and water treatment practice of 163 industrial installations in the Lower Missouri River Basin. This is the second and concluding report on the survey, conducted in cooperation with the Missouri Basin Field Committee of the Department of the Interior as part of the Missouri Basin project. Principal industries covered by this second report are: Sand and gravel, coal, meat, ice, brewing, paint, petroleum, chemical, fabricated metals, and a number of industries having either no waterborne wastes, or none of mineral origin. Gravel, sand, and silt from 47 producers are the major wastes, totaling 6 million tons annually, Coal mine wastes in the form of slurried solids from washing crude coal are second in volume, totaling 100,000 tons per year. They contain an average of about 40 percent coal. Salt is the third largest waste, amounting to 28,000 tons per year, Next is calcium carbonate, most of which is formed in water treatments, Because of its high unit value, chromic acid is important, although the waste quantity is much smaller; cyanide wastes are also significant because large quantities of sodium hydroxide and chlorine are consumed in their treatments prior to disposal. The various industries discharging wastes use 38 billion gallons of water annually; the recirculation rate is 109 billion gallons per year. The plants discharging no waterborne mineral wastes use 2 billion gallons of water per year and recirculate more than 1 billion gallons. Sand and gravel plants use 13.5 billion gallons; petroleum refineries use 10 billion gallons in direct use and recirculate 82 billion gallons per year.

Jan 1, 1962

By K. E. Tame

The Bureau of Mines is studying possible modifications in conventional ore-processing methods that will confine and permit controlled disposal of radioactive liquid wastes. Stream and ground water pollution from radio-active nuclides, principally radium 226 and thorium 230, in liquid wastes from uranium mills can be minimized by reusing the waste solution within the mill. Such reuse of waste solution in an acid leach-resin-in-pulp flowsheet was investigated in the laboratory. The process consists of acid leaching for dissolution of the uranium, sand-slime separation and countercurrent decantation washing for recovery of a pregnant slime slurry, and the use of ion-exchange resin for recovery of uranium from the slurry. Reuse of clarified barren effluent for washing in the simulated mill circuit was carried through 55 cycles. Dissolution of uranium from the ore averaged 97.5 percent. Washing efficiency of 99.9 percent was attained when using 4.35 volume tons4 of combined barren effluent and makeup water per ton of ore. Absorption of uranium from the pregnant slime slurry by an ion-exchange resin averaged over 99.9 percent.

Jan 1, 1962

By J. Robert Wells

The Bureau of Mines has developed a spectrochemical procedure for determining 19 impurity elements in high-purity titanium metal, titanium oxides, and titanium halides in which all samples are converted to titanium dioxide. Determination of these impurities was studied in the general concentration range of 0 to 1,000 p.p.m., but different determination limits were found for the various elements. The procedure is quantitative for 18 elements but semi-quantitative3 for beryllium and has an overall relative standard deviation of 15.8 percent. Two mixtures were used, one composed of graphite and lithium carbonate plus gallium oxide and the other of graphite and lithium carbonate plus germanium dioxide. Each mixture was blended mechanically with an equal weight of titanium dioxide. Lithium carbonate served as buffer-diluent. Gallium was the internal standard for 1 impurity element, germanium for 7, and titanium for the remaining 11.

Jan 1, 1962

By W. A. Calhoun

This report gives results of metallurgical investigations performed by the Bureau of Mines on mineral samples taken during April 1959, from Hawaiian bauxite deposits on the islands of Kauai, Maui, and Hawaii. The bauxite samples were tested at the Bureau&apos;s Rolla Metallurgy Research Center, Rolla, Mo., to determine if alumina could be extracted. The results were encouraging. Extraction of the alumina by the American Bayer type digest of crude ore samples from Kauai, Maui, and Hawaii recovered 78.8, 73.1, and 70.0 percent, of the total alumina, respectively. These recoveries were increased to 82.8, 85.5, and 79.5 percent by modifying the treatment, which consisted essentially of calcination and weak caustic desilication to provide a residue. The residue was then treated with calcium oxide and digested in a strong caustic solution to extract the alumina.

Jan 1, 1962