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By M. H. Stanczyk

The Bureau of Mines made bench-scale laboratory tests on a sample of typical Florida phosphate slime to determine alumina and phosphate extractions obtainable by agitation leaching, by baking and curing, and by a leach-electrolysis scheme. Recovery of mineral values from leached slime pulps by resin-in-pulp ion exchange contact and the reaction of the leached pulps to filtration, flocculation, and settling were also investigated. The best extractions of alumina and phosphate were obtained by (l) agitation leaching with sulfuric, hydrochloric, or nitric acid at an elevated temperature or (2) curing or baking the slime with sulfuric acid. Alumina extractions ranged from 80.8 to 90.0 percent and phosphate extractions ranged from 93.3 to 98.4 percent when the slime was leached at 90° C with sulfuric, hydrochloric, or nitric acids. Baking the slime with sulfuric acid at 200° C for 4 hours yielded an alumina extraction of 92.3 percent and a phosphate extraction of 97.0 percent, whereas curing with sulfuric acid at 100° C for 24 hours gave slightly higher alumina and phosphate extractions. Flocculation and settling properties of the slime were virtually unaffected in all cases. Filter area requirements, although somewhat improved as compared to untreated slime, remained relatively high. The lowest filter area requirement obtained was 44 square feet per ton of dry solids treated per day. Contacting leached slime pulps with ion exchange resins depleted the leach pulps of solubilized values; however, the filtration and settling properties of the barren pulps were unaffected. A leach-electrolysis scheme resulted in some concentration of solubilized phosphorus, but the method showed little promise of being commercially feasible.

Jan 1, 1966

By H. C. Fuller

A method was devised and developed by the Bureau of Mines for decomposing manganese sulfate at significantly lower temperature than that required by the conventional procedure of using heat alone. This technique, called the partial reduction method, effected decomposition at 700° to 800° C, as compared to 900° 1,000° C normally required. The process consisted of heating, in the absence of oxygen, a mixture of manganese sulfate and a controlled quantity of a reducing agent. The suitability of commercial-type equipment was tested in laboratory-size models of an externally heated rotary kiln, a r bbled muffle-hearth furnace, and a fluidized-bed reactor. The rabbled-hearth furnace gave the best results with the least operating difficulty produced a gas containing more than 80 percent SC and eliminated 96 percent of the sulfur when coal was used as the reductant. Sintering of the powdery decomposition product produced an agglomerate containing, in percent, 63.6 Mn and 0.4 S.

Jan 1, 1966

By Stephen D. Hill

The Bureau of Mines devised and constructed a modified Knudsen effusion apparatus, permitting a constant measure of the weight of effusing vapor, to determine the equilibrium vapor pressure of metal halides at temperatures up to 1,200° K and over the pressure range 10-5 to 10-2 torr. The reliability of the apparatus was established by determining the vapor pressure of potassium chloride. After correcting for partial dimerization of the vapor, data obtained on solid KCl between 750° and 950° K can be expressed by the following equation:

Jan 1, 1966

By Wallace W. Key

This report concerns types, quantities, specifications, and uses of non-metallic minerals as a basis for improving their supply, conservation, and utilization. Supply-demand details concerning mineral fillers, rooting granules, and roofing rock used in asphalt are incorporated in this report, along with highlights on production and sales of rooting, floor tile, and other related asphalt products of California. Comparable data for the United States are included. Although large quantities of commercially prepared mineral fillers are used in asphalt for paving and related applications in other States, addition of commercial fillers for these uses rarely is required in California because of the natural tines available. On the other hand, California manufacturers of asphalt products other than having utilize about 300,000 tons of asbestos, diatomite, limestone, mica, soapstone, and other nonmetallic minerals as filler, mainly for reeling and flooring. Also about 500,000 tons of roofing, granules is produced in California, most of which goes into roofing manufacture in California. In addition. A significantly large and growing tonnage of relatively coarse mineral aggregates Ire used on low-angle, built-up, asphalt roofs to produce in attractive surface and offer protection against the clements. Clearly ill minerals used in asphalt products manufactured in California come from local sources, except asbestos and mica--and there are indications that local deposits of those commodities could be utilized in some use categories.

Jan 1, 1966

By R. F. Abernethy

A modified Unterzaucher method was applied to the direct determination of oxygen in coal. Coal samples were pyrolyzed in a nitrogen atmosphere, and the gaseous oxygen compounds liberated were converted to carbon monoxide by a platinized-carbon catalyst at 9000 C. After passing over heated copper and through a tube containing soda-asbestos and magnesium perchlorate, the purified carbon monoxide was oxidized to carbon dioxide by iodine pentoxide--liberating an equivalent amount of iodine. The iodine was titrated with 0.02 ~ sodium thiosulfate; in a few tests the weight of carbon dioxide produced was determined. Direct oxygen determinations of coal included organic oxygen from the coal substance, plus a small quantity of inorganic oxygen derived principally from carbonate minerals and from combined water of silicates in the mineral matter. The influence of mineral matter on the direct oxygen determination was investigated by testing (1) untreated coal, (2) demineralized coal from which most of the mineral matter except pyrite was removed by treatment with hydrofluoric and hydrochloric acids, and (3) coal samples treated with dilute hydrochloric acid.

Jan 1, 1966

By A. W. Deurbrouck

The Bureau of Mines reviewed available data on the effect of crushing high-sulfur coals for the liberation of impurities in the light of increasingly stringent air pollution regulations. The survey, which provided information on Appalachian region coals only, indicated that such important coal- beds as the Upper and Lower Freeport and the Upper Kittanning show significant sulfur reductions when crushed to 14-mesh top size. For many other coalbeds amenability to sulfur liberation by crushing was indicated, although too few samples were available to draw firm conclusions,

Jan 1, 1966

By K. P. Wang

SIGNIFICANT general developments took place in the Far East during 1964, with far-reaching repercussions on the mineral and industrial economies of individual countries and the region as a whole. Japan, during this, "the Year of the Open Door," ushered in the era of industrial maturity, greater independence in economic policy, and expanded technical assistance to less developed countries. Symbolic of its dynamic economic growth is the fact that Japan out-produced the Federal Republic of Germany in steel during 1964 to take over a third-ranking world position. Mainland China, recovering from the "Leap Forward" debacle, made significant gains in industrial output. Mainland Chinese trade with Japan was on the upswing, and discussions were held between the Chinese and the Soviets for possibly resuming Soviet aid in industrial and mineral development. Meanwhile, United States aid to Taiwan was being phased out because of progress achieved. Rapprochement between South Korea and Japan was imminent late in 1964, a factor which may well affect South Korean mineral development. The Indonesian-Malaysian confrontation created economic difficulties in both countries. The war in Viet-Nam seriously disrupted industrial activities, particularly in the south.

Jan 1, 1966

By M. E. Hawkins

This Bureau of Mines report provides information on all of the 329 proved salt domes in the Gulf Coastal States and offshore area of the United States. It includes specific data related to location, depth to the cap rock and to the salt, storage facilities for LPG, and production of salt, sulfur, petroleum, and rock related to or associated with the dome structure in the subject area. Also included is a brief history of the salt, sulfur, and petroleum industries as related to the salt domes. Gulf Coast salt domes were the scene of the first discovery of a large deposit of rock salt in North America, the birthplace of the Frasch sulfur industry, and the location of the first large oil gushers that ushered in the modern liquid fuel age.

Jan 1, 1966

By Eliot J. White

The Bureau of Mines tested cores from 35 wells from 14 oil-producing zones in southern Illinois, southern Indiana, and western Kentucky to determine why rates of water injection were apparently low in some zones. Since these zones contain only minor amounts of clay minerals, it is concluded that permeability reduction results from movement of dislodged silica particles and other material, including the clays, that lines the pores. Both single-phase and two-phase permeability measurements, however, indicated that most samples had only low to moderate water sensitivity, so that permeability reduction due to such particle movement should usually not be of practical significance. The effective permeability to water was considerably lower than the effective permeability to oil during two-phase flow measurements, as is typical of most reservoir rocks. It can be concluded, therefore, that relatively high injection pressures will be required in waterflooding thin zones or zones having low permeabilities.

Jan 1, 1966

By Kenneth R. Farley

The Bureau of Mines developed a rapid and accurate flame photometric procedure for determining cesium and rubidium in ores and in products associated with the extractive metallurgy of these elements. The effect of associated ions is neutralized by addition of buffer solution; alkali metal effects are neutralized by parallel analyses made on standard solutions similar in composition to the sample being studied. The overall accuracy of the method is within 2.5 pct of the amount of cesium or rubidium present; the range from 1 to 25 pct is the most accurate.

Jan 1, 1966

By C. Ortuglio

The Bureau of Mines developed equations to determine the relationship of yields and products obtained from BM-AGA carbonization in 13-and l8-inch-diameter retorts. The developed equations indicate that results of carbonization in l8-inch-diameter retorts can be predicted from results obtained with l3-inch-diameter retorts.

Jan 1, 1966

By R. H. Schutz

TO ASSIST users in the selection of reliable and satisfactory respiratory protective devices, the Bureau of Mines bas established five schedules of minimum performance requirements for the approval of respirators. The current revisions of these schedules3 include 13D for self-contained breathing apparatus, 141F for gas masks, 19B and the amendments to 19B for supplied- air respirators, 21B for dust, fume, and mist respirators, and 23B for chemical cartridge respirators. Copies of these schedules may be obtained from the Bureau of Mines, Publications Distribution Section, 4800 Forbes Avenue, Pittsburgh, Pa., 15213. Approval tests on respirators are performed only at the request of the manufacturer4 of the respirator and at his expense. If the device meets the approval requirements, a certificate of approval is granted on the complete respirator. This certificate states that as long as the respirator is manufactured as originally approved, or in accordance with any changes covered by an extension of the original approval, the manufacturer may advertise and sell his respirator as being approved by the Bureau of Mines. Many industries and regulatory agencies require that respirators approved by the Bureau of Mines he used where respiratory protection is needed. The Bureau of Mines, however, has no regulatory power over the use of the respirators that it approves. It acts as an impartial testing agency to insure the availability of suitable and safe respirators.

Jan 1, 1966

By Gerald W. Elger

This report describes development of the fusion-leach crystallization precipitation process for producing a hafnium content feed material for hafnium-zirconium separation plants. Mixtures of zircon, potassium silicofluoride, and potassium carbonate (or potassium chloride) were fused to prepare soluble potassium zirconium hexafluoride-potassium hafnium hexafluoride salts. High extraction of these salts was obtained by countercurrent leaching the fused material in dilute hydrofluoric acid. About one-half of the hafnium was recovered in hafnium-enriched mother liquor by cooling clarified lead: liquor to crystallize most of the zirconium salt. Additional hafnium was recovered from the primary crystals in a multiple dissolution-recrystallization step. Hafnium-enriched oxides having a hafnium-zirconium ratio of more than three times that of zircon were precipitated from the combined mother liquors. The hafnium and zirconium recoveries in the precipitate were 83 and 24 percent, respectively. About 71 percent of the zirconium and the remainder of the hafnium were recovered in potassium zirconium hexafluoride crystals of low-hafnium content.

Jan 1, 1966

By Kenneth H. Johnston

This publication describes a thermal-recovery project and two waterflood projects in Carter, Garvin, and Stephens Counties, Okla., that will be visited during the 1966 annual tour by the Bureau of Mines in cooperation with the Kansas-Oklahoma Waterflood Association. Among the unique features of the projects arc (1) the movement of heavy (15° to 28° API gravity) crude oil through the reservoir and into the well bore with energy furnished by burning a portion of the crude oil therein; (2) the use of an inverted nine-spot pattern with dually completed injection wells, to produce oil from deep (8,200 to 10,200 feet) reservoirs; and (3) the flooding of five sand lenses separately by using controlled water injections through multizone completed injection wells. Discussion of the individual projects includes information on their early history, method of completing and operating wells, source and treatment of injection fluids, oil production decline curves, and the results obtained from the development.

Jan 1, 1966

By Lars Osen

The Bureau of Mines investigated (1) the effect of torsion on yield and ultimate strengths of bolts when the torsion is applied first and tensile load is applied independently of torsion and (2) various methods of increasing the tension-torque ratio and/or narrowing the data spread of the tension-torque relationship. A special torsional attachment was fabricated to attach to a universal testing machine to independently subject rock bolts to combined tensile and torsional loads. It was found that initially installed torsion is nullified during tensile loading and the tensile yield and ultimate strengths are not significantly reduced. Lubricating various components of a bolt assembly or using hardened washers will improve the tension-torque relationship during conventional installation; however, the torsional load is not nullified during this type of loading. Hence, a bolt is subjected to a combined stress throughout the loading cycle; the yield point will thus be lowered compared with the pure tensile yield if care is not taken during installation to stay below the torsional yield.

Jan 1, 1966

By Arnold M. Lansche

Domestic Production.-Domestic production of white arsenic, AS,03, was derived entirely as a byproduct of smelting arsenic-containing copper ores by The Anaconda Company at Anaconda, Mont., and American Smelting and Refining Company at Tacoma, Wash. The Anaconda Company discontinued production of white arsenic in 1965. Arsenic metal was not produced. Consumption and Uses.-Most of the white arsenic produced in 1965 was consumed in manufacturing lead and calcium arsenate insecticides.

Jan 1, 1966

By E. S. Shedd

The Bureau of Mines investigated electrowinning and tapping lanthanum metal from lanthanum oxide in a fluoride bath. The electrolyte was composed of LaF3, BaF2, and LiF. Metal containing 0.2 percent impurities was produced at a rate of over 2 pounds per hour. Principal impurities were carbon, aluminum, and silicon. Low-carbon metal was produced by continually discharging the carbon oxide gases and maintaining 0.1-atmosphere pressure. Anode reactions and cell design were found to be important factors in cell operation. Both frozen electrolyte skulls and tungsten metal crucibles proved satisfactory for collecting the metal and did not react with the molten lanthanum.

Jan 1, 1966

By William E. Young

There are many large rhodunite-bearing veins containing manganese in the Eureka-Animas Forks area of the San Juan Mountains in Colorado. The Sunnyside vein is the largest known vein in the area. As observed on the surface, the vein is mineralized over 8,000 feet and attains a maximum width of 200 feet. The average width of the vein and its branches and ramifications is 58 feet in the area that was mapped in detail. The weighted-average analysis of surface and underground samples from the northeastern extension of the Sunnyside vein is 8 percent manganese. Most other known veins in the area have a similar manganese content. The Hidden Treasure vein lies southeast of the Sunnyside-No Name-Mastadon vein. The weighted average of the analyses of surface and underground samples from this vein is 13 percent manganese. Exposures of the Scotia-Silver Chord vein are visible over a strike length of 4,000 feet on Treasure Mountain. Diamond-drill holes show that the vein contains 10 percent or more manganese to a depth of 400 feet. The vein has an average width of 28 feet. The Independence vein is exposed on the surface for a distance of 600 feet and has an average width of 6 feet. Three cut samples taken across the vein had an average content of 20.7 percent manganese. Sampling of the outcrops of eight veins in the Placer Gulch area also indicates manganese. Numerous other veins cropping out in the surrounding area are similar to the outcrop of the. Sunnyside vein system mineralogically and are worth investigating.

Jan 1, 1966

By Albert W. Deurbrouck

The preparation characteristics of the coals of Buchanan County, Va., are described in this Bureau of Mines report. Twenty-one samples ,,,ere collected from 9 coalbeds in the county. Of these samples 13 were of metallurgical quality as received, and 8 required some upgrading to provide acceptable products. In general, the coals were of low to medium ash and sulfur content, and ranked as medium-to high-volatile bituminous. In 1963, production in the county was in excess of 13 million tons, of which 2.2 million tons were mechanically cleaned.

Jan 1, 1966

By W. L. Acherman

Molybdenum, tungsten, and vanadium were found by the Bureau of Mines to possess generally superior chemical and galvanic corrosion properties in many aqueous corrosive media at temperatures up to the boiling point. The corrosion resistance of vanadium in certain solutions was further improved by alloying it with such metals as columbium, tantalum, and titanium. was susceptible to a type of crevice corrosion in mercuric chloride solutions, but no other instances of crevice corrosion were encountered. With few exceptions, molybdenum, tungsten, and vanadium were not adversely affected when coupled with dissimilar metals in galvanic corrosion experiments; in some cases one or both members of a couple were protected by contact. When exposed to aqueous ammonia spray at 60° C, all three metals were attacked, but they were moderately resistant in spray environments of substitute ocean water and ammonium dihydrogen phosphate.

Jan 1, 1966