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By R. V. Lundquist

This report describes results of tests on the desilication of solutions resulting from the leaching of lime-soda sinters. Desilication was accomplished by heating the solutions in an autoclave. A liquor relatively free of silica was obtained after 30 minutes of heating at 200 p.s.i.g. in the presence of lime. The addition of lime improved desilication, but the rate and efficiency of desilication was effected by the quality of lime used. The optimum quantity of lime for effective desilication was about 6 grams per liter. A lesser quantity gave poorer desilication, and a greater quantity increased the alumina loss without improving desilication. The alumina loss was approximately proportional to the lime added. A complex structure, called artificial noselite in this report, was the only silica bearing compound detected in the desilication precipitate. Other compounds present were Ca(OH)2 (calcium hydroxide), CaCO3 (calcium carbonate), and Ca [A1(OH)6]2 (hydrated tricalcium aluminate). Sodium carbonate in the leach liquor retarded the formation of the calcium aluminate; hence it decreased the alumina lost to the precipitate. The extraction of alumina from aluminum silicate materials by the limestone soda-sinter process has been investigated by the Bureau of Mines for many years. The process consists of the following major operations: Blending the aluminum silicate with limestone and soda ash in such proportions that dicalcium silicate and sodium aluminate are formed on sintering; leaching the sinter in a carbonated caustic solution to extract the soluble alumina; purifying the leach liquor by the precipitation of soluble silica (this precipitate is designated desilication precipitate in this paper); precipitating alumina trihydrate from the purified liquors by carbonating with carbon dioxide gas; and calcining the trihydrate to alumina. Commercial grades of

Jan 1, 1962

By E. C. Perkins

Preliminary experiments are reported utilizing bacteria to leach manganese from a variety of domestic low grade manganiferous materials. In two large leaches manganese extraction ranged from 71.7 to 92.5 percent, and the products analyzed over 48 percent manganese. Nutrient requirements and leaching time experiments were made. The mechanism of leaching is not understood, but is different than the mechanism encountered in the microorganism accelerated leaching of copper in the presence of sulfide minerals.

Jan 1, 1962

By W. W. Agey

This report summarizes results of bench-scale metallurgical studies by the Federal Bureau of Mines on three composite samples representative of the low-grade manganese ores purchased by the General Services Administration (GSA) and stockpiled at Deming, N. Mex., and Wenden, Ariz. Bench-scale flotation tests at the Salt Lake City Metallurgy Research Center showed that all three composites could be beneficiated by flotation to recover 88 to 90 percent of the manganese in concentrates that assayed from 38.5 to 39.0 percent Mn, 10 to 12 percent insoluble, 5 percent CaO, 3 to 5 percent Fe, and 1.3 to 1.7 percent combined Pb plus Zn plus Cu, Sintering studies indicated that specification-grade material could be made from these concentrates by sintering above 1,000° C, and adding either sodium or calcium chloride to the charge to insure removal of enough lead and zinc to meet the specifications.

Jan 1, 1962

By D. W. Frommer

Composite samples of nonmagnetic taconite from the western Mesabi range were evaluated by reductive roasting, fine grinding, and magnetic separation to determine potential sources of concentratable material. Although large tonnages of nonmagnetic taconite are known to occur in the western Mesabi district, these materials are not as yet a commercial source of iron ore. The technique employed permits the evaluation of individual composites and blocks of composites in terms of responsiveness to a process of potential commercial significance. The 159 composites, from open-pit mines located between Grand Rapids and Chisholm, Minn., were evaluated in the following sequence: 1. Minus 8-mesh material was roasted at 500° C. in hydrogen. 2. The roasted are was ground to one or more sizes in the minus 100-to minus 400-mesh range. 3. The roasted ground ore was magnetically separated in a Davis tube. 4. Composites were classified according to degree of grinding required to produce minimal concentrates. (Minimal concentrates are herein defined as those containing less than 10 percent silica, and responsive composites as those yielding minimal concentrates.)

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 R. C. Bates

Uranium mine workers? daily exposure to radon daughters was estimated by two methods of sampling, detailed and spot-check. Both methods involve time- weighting measured exposure levels to arrive at an average exposure figure. Random sampling, or sampling without regard for the duration of exposure, has proved inadequate for estimating average exposure levels. During the first phase of the study, the breathing zones of eight workmen in three underground uranium mines were sampled for an entire shift; 20 to 36 radon-daughter samples were collected per man-shift, Analysis of these data indicated that a suitably accurate estimate of the full-shift exposure could be made by time weighting a considerable lesser number of representative radon-daughter samples. This analysis led to the spot-check method of estimating full-shift exposures to radon daughters. Additional detailed studies were made in seven mines to Learn more about the full-shift radon-daughter exposures and to test the spot-check method, In all, 617 radon-daughter samples were taken in 10 underground uranium mines during 26 man-shifts, and the spot-check method was tested 35 times.

Jan 1, 1962

By A. G. Starliper

The report covers studies by the Bureau of Mines on the removal of metallic values in two waste products from the Longhorn tin smelter at Texas City, Tex. One product was a slag that contained tin, tungsten, iron, tantalum, and columbium. The other product was a spent acid solution that contained tin, tungsten, iron, lead, copper, zinc, and silver and that came from presmelting treatment of impure tin concentrates. Molten slag was treated with sulfur or sulfur compounds and with coke, calcium carbide, or gaseous reductants to form tin sulfide that volatilized from the charge and to reduce tungsten along with iron and silicon to form a carbon-bearing metallic layer. The metallic layer was treated by an oxidizing alkali roast and then was water-leached to extract the tungsten. The waste acid was used in other experiments to dissolve an iron-tin- tungsten alloy (hardhead) obtained by direct reduction of the slag. An insoluble fraction containing tungsten, silver, silicon, columbium, and tantalum was removed, and copper was cemented on metallic iron, Tin was recovered by cementation on zinc plates, and lead was precipitated by adding sulfate ion. Iron was precipitated by increasing the pH which left a solution containing principally zinc. Slabs of hardhead were electrolyzed in an electrolyte consisting of waste acid to plate out groups of metals at different pH?s. The time did not permit thorough exploration of this method of treatment.

Jan 1, 1962

By R. W. Lewis

Spectrochemical procedures were developed using dc arc excitation for the determination, in parts per million, of 18 impurity elements in electrorefined beryllium and high-purity beryllium oxide. The metal samples were dissolved in dilute hydrochloric acid, evaporated to dryness, and converted to the oxide in a muffle furnace at 900° C. Germanium oxide was added as an internal standard for the determination of 15 of the elements, copper oxide for boron and molybdenum, and neodymium oxide for calcium. The average coefficient of variation was 11 percent with the exception of copper, which averaged about 43 percent.

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 Leonard Obert

Between 1927 and 1957, sodium borate minerals were mined by underground methods in the Kramer District, Kern County, Calif. In 1957, surface mining methods were initiated, and during the next two or more decades it is probable that most of the production from the district will be obtained from open pits. However, part of this borate deposit is sufficiently deep that surface mining may not be economical and, hence, at some future date underground methods may again be employed. This report was prepared to document the underground mining methods employed in the district before 1957. The general geology of the district and the detailed geology of each of four mine sites are presented, together with a mineral and mechanical description of the ore and enveloping rock. The report also describes the stoping, extraction, pillar support, methods of artificial support, and other factors that affect the structural characteristics of these mines.

Jan 1, 1962

By J. D. Brown

The electron optics, vacuum system, and sample stage assembly for the Bureau of Mines? electron probe X-ray spectrograph were purchased. Four scanning curved-crystal spectrometers, two reflection- and two transmission-type, were designed and constructed by the authors. The reflection spectrometers are placed in a vacuum chamber for measurement of long-wave-length X-radiation. Detection, pulse-amplitude discrimination, and recording circuits are provided for the simultaneous measurement of four X-ray spectral lines. Minimum spot size is approximately 2 microns in diameter at 30 kilovolts and a sample-to-ground current of 5 x 10-8 ampere. At this voltage and current the limit of detection with reflection spectrometers is less than 0.05 weight-percent for most elements. The limit of detection for elements determined by transmission-type spectrometers, evaluated at 35 kilovolts and 5 x 10-8 ampere, is approximately 0.1 weight--percent for all elements having excitation voltages below 20 kilovolts. In general, reflection spectrometers exhibited satisfactory but poorer resolution than the transmission type, resolution of the spectrometers being limited primarily by crystal imperfections, with greater mosaic structure being introduced by the grinding process for the reflection crystals. Several applications of the electron probe X-ray spectrograph are described. Analysis of a uranium-steel is discussed in detail to illustrate calculation of composition from measured X-ray intensities.

Jan 1, 1962

By Michael G. Zabetakis

The autoignition temperatures (A.I.T.'s) of natural and synthetic lubricants in air were generally found to decrease with increasing pressure. Of the two types of fluids, synthetic and natural, studied in some detail, the phosphate esters had higher A.I.T.'s at any pressure between 1 and 200 atmospheres than the mineral oils. Most of the A.I.T. data obtained in this study obeyed the relationship predicted by Semenov's theory of ignition.

Jan 1, 1962

By F. E. Brantley

Blister copper was successfully deoxidized with any of a variety of reducing gases; lancing techniques or a vertical-column furnace were used to contact the copper and gases. Of the gases tested, butane, when used to lance molten copper at about 1,200° C, reaction temperature, was slightly more effective than propane, natural gas, carbon monoxide, or reformed gas for deoxidizing copper from about 1.0 to less than 0.1 percent oxygen content, Laboratory-scale tests revealed that the vertical furnace, composed of a heated column packed with silicon carbide chips or hollow carbon cylinders, was significantly faster and more efficient than the lancing technique for deoxidizing molten copper with any of the gases tested. Comparison of the gaseous-reduction method with the conventional poling method suggests that the gaseous method has important technical and economic advantages for deoxidizing blister copper to any readily controlled amount of residual oxygen content.

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 William J. Campbell

Evaluation by the Bureau of Mines of published expansion values for magnesium oxide shows significant variation in values, which may be attributed to sample variables, experimental errors, or systematic differences between measuring techniques. To eliminate the sample variable in measuring expansion, thermal expansion characteristics of a high-purity polycrystalline magnesium oxide were determined by 21 cooperating laboratories using one or more of the following techniques; X-ray camera, X-ray diffractometer, dilatometer, interferometer, and telemicroscope. All expansion values were corrected by the author to a single reference temperature of 25° C. Linear expansion was expressed as a power series in the form of the following equation. Expansion (percent) = [[ A + B (?t) + C (?t)2] ?t 104] The constants, A, B, and C, were determined by least square techniques for X-ray camera, X-ray diffractometer, and dilatometer data separately, and for combined data of all five techniques. Expansion values are tabulated from 26° C. to 1,400° C. in 2° C. intervals using constants derived from X-ray camera data. Below approximately 500° C., expansion values obtained by dilatometric and interferometric methods are significantly lower than those by X-ray methods; above 500° C., this bias decreases rapidly. Comparison of results within methods showed the least variance for X-ray camera results; dilatometer and X-ray diffractometer results have about the same variance. The average deviations, in percent, between observed and calculated expansion values among methods were approximately 10 percent from 100°C. to 300°C., 5 percent from 300°C. to 500°C., and 2 percent from 500°C. to 1,400°C. Maximum deviations were approximately twice as large in most instances.

Jan 1, 1962

By D. F. Walsh

A study of damping capacity was made on a number of magnesium-base alloys, commercial types and experimental compositions. Hardness and tensile properties were determined, and the microstructure of each alloy was examined. Alloys of low yield strength, in general, possessed high damping ability. A correlation was established between damping capacity and composition.

Jan 1, 1962

By Robert Hall

The Lynch Creek beryllium-tungsten prospect was investigated as part of the domestic beryllium resource studies by the Bureau of Mines. This prospect is in the Birch Creek mining district, Lander County, Nev., 9 airline miles south of Austin. A tungsten mine was operated intermittently from 1952 to 1957. Beryl was identified in the pegmatite dikes in 1960, and the lode claims were relocated. No beryl has been produced. Rocks in the area are Paleozoic sediments2 cut by pegmatite and aplite dikes and quartz stringers. Beryl occurs in random pockets, as disseminations throughout the dikes, and in occasional pockets in the quartz stringers.

Jan 1, 1962

By Kenneth M. Earl

This report describes the results of a field study conducted by the Bureau of Mines during 1956 and 1957 on manganese-and iron-bearing mineral deposits in the southern district of Aroostook County, Maine. The work was undertaken to determine the extent of deposits largely concealed under glacial drift and to obtain subsurface samples for manganese mineral identification and research in ore dressing and extractive metallurgy. The investigation was confined to the Westford Hill-Daggett Hill area in Hodgdon Township and to the Stewart prospects and vicinity in Linneus Township. Over 50 magnetic anomalies were mapped by magnetometric surveys in the Westford Hill-Daggett Hill area, Hodgdon Township. The largest anomaly, as outlined by the 1,000-gamma contour, indicates a deposit 3,200 feet long with a maximum width of 350 feet. The smallest anomaly measures about 10 feet wide by 25 feet long.

Jan 1, 1962

By F. B. Petermann

The Bureau of Mines conducted electric furnace smelting tests on sintered flotation concentrate and siliceous log-washed are. The flotation concentrate was derived from the Maggie Canyon deposit of the Artillery Mountains area, Mohave County, Ariz., and contained, before sintering, 35.6 percent Mil and 19.4 percent Si02 + A1203. The log-washed ore was from the McGregor deposit of the Artillery Mountains area, Mohave County, Ariz., and contained 31.2 to 33.6 percent Mil, 19.5 to 27.6 percent Si02 + A1203, and 2.5 percent Pb. This work was undertaken to determine the most effective smelting technique for producing standard products from such nonspecification ore and concentrates. The objective was to collect data, using a small furnace, which would be reasonably accurate and permit extrapolation to large-scale practice for comparing with results on specification-grade are.

Jan 1, 1962

By G. V. Sullivan

This report summarizes the results of a preliminary study concerning manganese extraction from low-grade dolomitic materials from the Philipsburg district in Montana by the Dean-Leute ammonium carbamate process. Studies were made to determine the relationship between the variables involved in treating these materials by a roast-leach process and the amount of manganese extracted. The variables studied were the roast temperature, the roast particle size, the molar ratio of NH3 to CO2 in the leach solution, the liquid-solid ratio in leaching, the leach time, and the size of the particles being leached. The roast-leach studies were statistically designed, and the experimental results were evaluated by an analysis of variance.

Jan 1, 1962