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By W. W. Agey

Past investigations on waterborne impurities in the flotation process have been concerned primarily with the treatment of specific ores with particular local waters. Although some anions and cations present in water are known to react with flotation reagents, a definitive study has not been made on the effect of such common ions upon the flotation process. This report describes the fundamental research undertaken to define and measure the adverse and/or beneficial effects of different concentrations and combinations of several common anions and cations when oleic acid is used to froth-float limestone from a pulp of quartz and limestone. Research on the effect of waterborne impurities upon the flotation process was composed of two equally important phases. The first phase comprised development of a procedure for floating limestone from quartz that would give the same results in test after test. Some difficulty was encountered, but once such a procedure was developed, the second phase, comprising study and measurement of the effect of various ions c on to natural water upon the flotation of limestone, was quickly completed.

Jan 1, 1963

By George H. Johnson

This report describes the procedures and summarizes the results of an investigation of surface subsidence above caving blocks at the San Manuel mine, San Manuel, Ariz., in order to obtain quantitative information on subsidence and ground movement caused by mining large volumes of ore. This investigation is one part of an overall study of rock mechanics being undertaken by the Bureau of Mines. Attention was given to the improvement of a rapid and precise method of surveying a large number of subsidence pins and cracks in the surface terrain. Photogrammetric methods were used as an adjunct to the triangulation subsidence surveying as well as in ordinary topographic work Maps of various kinds were prepared to show the results obtained. The computation of the survey notes was programed for an electronic digital computer at a saving of time and expense over the use of a desk calculator and trigonometric tables.

Jan 1, 1963

By E. C. Pattee

A mobile spectroscopic laboratory was completed by the Bureau of Mines in 195 to provide a rapid, inexpensive means of field testing samples for beryl¬lium and other associated metals of possible commercial importance. Spectro-copes have been used in laboratories for many years in various types of research and routine analyses, but this spectroscope is probably the first mobile unit. The laboratory provides for spectroscopic, radioactivity, fluorescent, and limited chemical tests of samples. The unit has been a valuable reconnaissance tool. It has been used to search for beryllium, cesium, columbium, tantalum, rubidium, and lithium in Idaho, Washington, and Montana. Several very low grade deposits of these elements were found, and occurrences of other important elements were identified; however, none are of economic importance. The spectroscope permits the detection of elements by analysis of visible light produced when elements in a small powdered sample are volatilized in an electric arc., A total of 70 elements can be detected; 29 can be detected at or below 0.01 percent, Electric power for the arc is supplied by a gasoline motor-driven generator, Equipment is housed in an aluminum van, mounted on a 4-wheel-drive vehicle for easy maneuverability on mountain roads, A trailer with crushing, pulverizing, and splitting equipment permits the reduction of samples to a small representative pulp.

Jan 1, 1963

By B. K. Shibler

A highly flexible laboratory-scale fluidized-bed reactor was designed, constructed, and successfully operated continuously at temperatures up to 1,300° C during an investigation of thermal methods for decomposing gypsum. This report discusses briefly the many problems encountered in developing the 10-inch-diameter reactor and describes its design and construction in sufficient detail to enable other research organizations to build a comparable unit. The reactor consists of a 10-inch-inside-diameter vertical tube which can be varied from 6 to 10 feet high; it is formed from 2-and 3-foot sections of silicon carbide pipe. The tube is surrounded by a 3-inch heating space formed by an outer 4.5-inch-thick circular wall of insulating firebrick. A cone-shaped fluidizing chamber is bolted to the bottom of the reactor. Fluidizing gas enters through the bottom of the cone, and ore is introduced by means of a screw feeder connected to an inlet located just above the gas port. A silicon carbide overflow tube of 1.25-inch inside diameter extends upward into the reactor. The depth of the bed is controlled by substituting different lengths of overflow tube. Twin dust-recovery systems, each composed of a cyclone and Fiberglas filter, are attached to two gas outlets at the top of the reactor tube. The reactor is designed for research on both exothermic and highly endothermic reactions. It can be fired externally by means of four natural gas burners that jet tangentially into the annular space at the base of the reactor. Alternatively, it can be fired internally, using a mixture of air or oxygen and natural gas as the fluidizing medium. A separate instrument panel contains flowmeters, manometers, an automatic program controller, and a multiple-point recorder for printing a record of the temperatures measured by thermocouples located at critical points in the reactor.

Jan 1, 1963

By Scott W. Hazen

This Bureau of Mines report presents the results of a study and statistical analysis of part of the initial exploration churn-drill sampling and some of the subsequent underground diamond-drill-core sampling in the North are body at the San Manuel copper mine, Arizona. These data were derived from regular exploration and mine sampling, not from special samples obtained solely for statistical analysis. The study was conducted as part of the Bureau's continuing program on sampling-methods research. The major objective of the study was to investigate the feasibility of using the techniques of statistical analysis in evaluating sample and assay data and computing grade and tonnage of Ore from porphyry-type copper deposits. It was recognized that using existing data acquired over a period of several years by different methods would introduce problems and limitations for precise comparisons. However, it was expected that the study would provide some general conclusions and certainly a number of preliminary conclusions on the nature of the mineral characteristics and their effect on sampling procedures, the requirements for sampling deposits of this type, and the comparative results of churn-and diamond-drill sampling in the same area of the deposit. All of this information would be essential for future sampling-methods research for computing grade and tonnage of ore.

Jan 1, 1963

By S. J. Hussey

This Bureau of Mines report presents a discussion of the statistical approach to the design of experiments and indicates, by concrete examples, how and when statistical design is essential for obtaining meaningful data with a minimum number of experiments. Every research worker plans his work and designs his experiments in a manner which, based on his experience, seems most rational to him and which he believes will produce the information essential for resolving the problems. If the results obtained are open to multiple interpretations and are not of definitive reliability, the failure of the experiment design to produce the desired information may be due to several causes, These include faulty judgment in selecting the factors to be tested, ignoring the importance of interaction between factors, failure to adequately control test variables, and assuming that meaningful trends in the results can be identified without comparison to a predetermined experimental error. An experienced researcher probably will deduce from the nature of the data obtained that the design is faulty and may by trial and error ultimately arrive at the correct solution to the problem. Statistical methods of planning research minimize the chance of faulty experiment design, embody concrete procedures for testing the validity and reliability of the test data and for indicating mandatory changes in the design, and enable the researcher to obtain meaningful information with the least number of tests.

Jan 1, 1963

By Robert C. Johnson

Water-swelling fluormicas and fluormontmorillonoids were synthesized and described. They were found predominantly in the system Mg0 - MgF2 - Si02, with varying amounts of Li+ or Na+, Some water-swelling synthetic minerals were prepared with only strontium or lead in the twelvefold position, Water- swelling compounds containing either K+ or Ba+ were not found. The synthesized water-swelling products were shown by electron microscopy, X-ray diffraction, and chemical analysis to be typically two-silica-layer, platy compounds, Except for the complete substitution of fluoride for hydroxyl, the compounds were similar to the natural micas or montmorillonites. The stability and properties of the compounds were further established by electrodialysis, by differential thermal analysis, and by anion and cation exchange methods. Fluoride in the interlayer positions was nonexchangeable except through decomposition of the product. Exchanging the sodium or the lithium of the synthetic fluormicas or fluormontmorillonoids with potassium ion, particularly those derived from KOH provided a product from which a completely inorganic paper of extraordinary flexibility was fabricated. This paper had excellent mechanical and electrical properties except for water adsorption and a high power factor. Neither of these problems was solved during this investigation. However, papers with dielectric strength from 1,500 to 5,000 volts per mil were readily fabricated, particularly from the lithium containing fluormicas or fluormontmorill onoids.

Jan 1, 1963

By Robert S. Warfield

The Bureau of Mines investigated a geologically favorable area in the Beluga River coalfield in south-central Alaska to determine if there were sufficient minable coal reserves for onsite utilization to meet the projected thermal power needs of the Anchorage area. A program of diamond core drilling and sampling delimited a shallow saucerlike structure estimated to contain indicated reserves of more than 20 million tons of subbitminous coal in a seam over 50 feet thick that could be mined by opencut methods. A large sample of fresh coal was taken across the full width of the seam for washability studies. This sample, with 4 volume-percent of clay partings eliminated, contained 24.4 percent moisture and 16.8 percent ash and had a calorific value of 7,162 Btu per pound. The studies indicated that mechanical cleaning would be of doubtful value.

Jan 1, 1963

By G. W. Birge

Twenty-eight samples, representing the Pittsburgh, Lower Kittanning, Stockton-Lewiston, Coalburg, Winifrede, Cedar Grove, Peerless, No. 2 Gas, Powellton, and Eagle beds, were carbonized by the Bureau of Mines--American Gas Association (BM-AGA) method, and yields of products and physical properties of cokes were determined. Expanding characteristics of 22 of the samples were determined in the Bureau of Mines sole-heated oven. The Kanawha County coals tested were high-volatile A bituminous in rank, with dry, mineral-matter- free fixed- carbon contents ranging from 53.9 to 66.3 percent. With few exceptions, they were chemically satisfactory for metallurgical use, and most of the coke-strength indexes were within the industrially accepted range for high-volatile blending coals.

Jan 1, 1963

By Walter C. Lorenz

Samples of materials containing pyrite from various coal mines and coalbeds were studied to compare their compositions and oxidizing characteristics. Pyrite was the only form of iron sulfide identified, but X-ray diffraction, emission spectrography, and microscopic analyses revealed similar suites of minerals and trace elements. The pyrite occurred usually in spherical clusters of very small crystals. The oxidation of pyrite in solutions of PeSO4 and Fe2(SO4)3 and in the presence of an iron oxidizing bacterium Ferrobacillus ferrooxidans, was studied through a manometric technique. FeS04 or Fe2(SO4)3 solutions had no appreciable influence on pyrite oxidation under the test conditions, The bacterium acted as a catalyst, greatly increasing the oxidation rates; however, in three samples that also contained calcites, bacterial oxidation was greatly reduced. The oxidation rates also increased approximately as the percentage of pyrite in the samples increased. For the series of samples studied, there was no definite correlation of the results with the location of the various mines nor with the acidity of alkalinity of the mine drainage.

Jan 1, 1963

By G. T. Krempasky

This report covers the installation and evaluation of lb reinforced concrete sets, 6 in each of 3 mines in the Goeur d'Alene mining district, Shoshone County, Idaho, and is the second of a series to determine the feasibility of a more permanent type of mine support. Closure measurements, where applicable, were made periodically of the concrete-set installations and were compared to the initial cross section of the sets. A different method of blocking was used at each test site; at one test site the type of blocking was changed several times during the test. Results from each test site are reported separately. No attempt was made to compare the cost of the concrete installations with the cost of other types of support used in the district. Such an evaluation of permanent types of support would require a longer period of time. At this time, tests are not complete enough to determine the applicability of underground concrete supports. However, results to date tend to confirm the general opinion that precast concrete mine supports could be used to advantage in openings that require support and must have long life, especially where decay of timber is an important factor.

Jan 1, 1963

By W. T. Abel

Laboratory tests were conducted with a closed, recycling system to evaluate the effectiveness of solid-in-gas suspensions as heat transport mediums. Micronized graphite in helium or nitrogen was circulated by a centrifugal compressor to determine the feasibility of the method and heat transfer capabilities of the mediums. Suspensions were circulated without plugging or eroding the compressor or piping. At low flowrates and light (0.1 to 0.2 volume-percent) graphite loadings, slightly less power was required to transport a given amount of heat with suspensions than with helium alone. Graphite deposition on the heat exchange surfaces of the cooler decreased the heat transfer effectiveness at higher solids concentration. Efforts to eliminate deposition are described.

Jan 1, 1963

By L. H. Adami

This paper reports the results of solution calorimetry conducted to obtain the heats of formation of crystalline FeS04?6.952H20 and FeS04?1.008H20, from. which values were derived for the stoichiometric compounds FeS04?H20 and FeS04?H20. Also included are derived values of the free energies of formation and dehydration. This work was undertaken primarily to fill a need for data for pure, easily obtainable ferrous compounds that are suitable for use as calorimetric intermediates, The ferrous sulfate hydrates meet the essential requirements for this use.

Jan 1, 1963

By G. W. Birge

Carbonizing properties of the principal coalbeds of Elk, Clarion, Jefferson, Clearfield, and Centre Counties, Pa,, are described in this Bureau of Mines report, Twenty-six samples, representing the Upper Freeport, Lower Freeport, Upper Kittanning, Middle Kittanning, Lower Kittanning, and Brookville beds, were carbonized by the Bureau of Mines--American Gas Association (BM-AM) method, and yields of products and physical properties of cokes were determined. Expansion or contraction of the majority of the samples was measured in the Bureau of Mines sole-heated oven. Chemical analyses, agglutinating values, and free-swelling indexes are given for all samples. In this area the coals generally are characterized by high sulfur and moderately high ash content, and their suitability for metallurgical use would depend largely upon satisfactory cleaning. The samples from Elk, Clarion, and Jefferson Counties were high-volatile A bituminous In rank, whereas, most samples from Clearfield County and all those from Centre County were of medium-volatile rank. Coals from Clarion County had dry, mineral- matter-free fixed-carbon contents ranging from 56.5 to 60.3 percent and were weakly coking. With the exception of two samples which contained excessive ash, the medium-volatile coals of Clearfield and Centre Counties were strongly coking and, as indicated by sole-oven expansion results, would require blending with lower rank coal to avoid oven damage.

Jan 1, 1963

By David Schlain

A small alumina reduction cell with a graphite crucible and boron nitride liner was developed by the Bureau of Mines as the initial phase of a study of the reactions which occur in the reduction of alumina by the Hall-Heroult process. Operating conditions in the cell such as temperature, time, current density, electrolyte composition, and electrode materials may be varied easily. Aluminum was produced in the cell at a current efficiency of about 75 percent and a cell voltage of 2.7 volts. Although the data are not wholly conclusive, the operation of the cell did not appear to be greatly affected by large changes in temperature, electrode spacing, current density, and alumina concentration in the electrolyte.

Jan 1, 1963

By Thomas L. McVay

Laboratory batch and pilot plant flotation tests were made to determine the feasibility of recovering commercial grade kyanite from a quartzite- kyanite rock from the Graves Mountain, Ga., deposit. Best results in laboratory and continuous tests were obtained using sodium carbonate for pH control, citric acid for quartz depression, and oleic acid as the kyanite collector. Over 80 percent of the kyanite was recovered in a concentrate analyzing 56.8 percent Al203 and 3.8 percent hydrochloric acid soluble Fe203. Subsequent treatment of the flotation concentrate by magnetic separation reduced the acid soluble Fe2O3 to 0.6 percent and increased the alumina content to 59.2 percent. Acid leaching of the concentrate gave a product analyzing 59.7 percent Al203 and about 0.1 percent Fe203. As a result of the beneficiation research, a commercial kyanite flotation plant was completed in September 1962 by private industry.

Jan 1, 1963

By N. H. Coates

A small, special-purpose centrifugal compressor was developed to circulate 60 pounds per hour of helium at 1,000° F and 250 psig because standard, commercial units were not available. Performance characteristics of this compressor were determined at helium flows of 2,000 to 18,000 std cu ft per hour, pressures of 100 to 250 psig, and temperatures of 100° to 1,000° F. This range is 2 to 90 actual cu ft per minute. Several graphs show the adiabatic head developed by the compressor over this wide flow range at various combinations of temperature and pressure. A compressor performance map relates pressure ratio to mass flow, temperature, pressure, and speed. This map can be used to accurately predict compressor performance factors within the range of operating conditions covered by the experiments.

Jan 1, 1963

By Michael Sokaski

A dense-medium cyclone pilot plant was built to clean 112-inch to 0 size coal. This pilot plant does not require the removal of the extremely fine material (usually minus 1/2-mm) from the feed, which is necessary in conventional dense-medium cyclone plants. The essential difference between conventional cyclone plants and the pilot plant is in the medium-recovery system. The latter uses a combination of sieve bend screens, classifying cones, and magnetic separators for medium recovery. Eight tests were run in the pilot plant at a feed rate of 5 tons per hour with four different raw coals and one crushed jig middling product. Sharp separations were obtained as indicated by an average error area of 27 and probable error of 0.047 for the 112-inch to 200-mesh size range. Magnetite loss averaged about 2.5 pounds per ton of feed. The influence of several factors on cleaning performance of the cyclone was investigated. The diameters of both the overflow and underflow orifices were found to be important for optimum cleaning performance, but these diameters could vary over a wide range without serious effect; however, if this range was exceeded, cleaning performance deteriorated. Better cleaning performance was obtained when the cyclone inlet pressure was increased from 9 psig to 13 psig. The size of the magnetite particles in the medium was found to have a substantial effect, and the best cleaning results were obtained with grade B magnetite. Demagnetizing the magnetite in an effort to decrease the effective particle size did not improve cyclone performance.

Jan 1, 1963

By Paul W. Johnson, Ralph C. Kirby, Frank A. Peters

An evaluation is presented for a process designed , on the basis of published work , to extract alumina as potassium alum from clay using sulfuric acid and potassium sulfate . The silica residue is separated by filtration . Ferric iron is reduced to ferrous iron , and the alum is crystallized from the solution , leaving the ferrous iron in solution . The alum crystals are separated from the solution and redissolved for feed to autoclave decomposition . In an autoclave the alum is partly decomposed to a basic alum , recovering five - ninths of the sulfuric acid and two - thirds of the potassium sulfate without using an acid plant . The basic alum is decomposed by calcining , and the potassium sulfate is then removed by washing with water . Operating costs for a plant producing 1,000 tons of alumina a day are estimated at $ 96.15 per ton of alumina . The fixed capital cost is estimated at $ 155 million . This process is not competitive under current economic conditions with the production of alumina from bauxite by the Bayer process . Improvement in leaching , basic alum decomposition , and washing could reduce the costs and improve the product which contains some potassium .

Jan 1, 1963

By E. C. Perkins, R. S. Lang, D. M. Taylor, H. Dolezal

The amenability of titaniferous slags and domestic mineral concentrates to chlorination was determined in a 6 - inch diameter fluidized bed chlorinator . Ilmenites from Valley County , Idaho ; Aiken , S.C ,; Trail Ridge , Fla .; and MacIntyre , N.Y .; and a titaniferous magnetite from Iron Mountain , Wyo . , were used in preparing the slags . The domestic minerals tested were an ilmenite concentrate from Valley County , Idaho , and a rutile concentrate from Magnet Cove , Ark . A high - grade Australian rutile was used as a standard for comparison . The impurity content of the slags and minerals tested , which was the most critical factor affecting their performance , was dependent on the geographical source of the material . All of the materials tested were amenable to chlorination in a fluidized bed although some required special operating conditions . Titanium extractions and chlorine utilization were over 90 percent for most of the slags and the Australian rutile . The Valley County , Idaho , ilmenite performed well in the reactor despite its 34 percent iron content .

Jan 1, 1963