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By D. Bienstock

In connection with air-pollution studies, the Bureau of Mines is cooperating with the U.S. Public Health Service in investigating the use of solids for removing sulfur dioxide in concentrations of less than 0.5 percent from combustion and waste gases. Removal of sulfur dioxide at flue-gas tempera¬tures would no longer result in the cooling of scrubbed gas, which is inherent to liquid scrubbing processes used exclusively in industry today. Results are reported of extensive investigation, using metallic oxides as absorbents, adsorbents, and oxidation catalysts at 130° and 330° C. (temperatures at which flue gas may be treated in powerplant practice). The most active absorbents tested were the oxides of manganese, cobalt, copper, and alkalized alumina; 23 to 33 grams of sulfur dioxidn were removed by 100 grams of absorbent at 130° C., while scrubbing more than 90 percent of the sulfur dioxide from a simulated flue gas, and 19 to 61 grams of sulfur dioxide were removed at 330° C. A more detailed study is reported on absorption and regeneration, using manganese oxides and alkalized alumina. Adsorption of sulfur dioxide on activated carbons and molecular sieves at elevated temperatures is considerably less efficient than removal by absorption--a maximum of 7 to 8 grams of sulfur dioxide could be removed with 100 grams of adsorbent at 130° C. A potash-promoted vanadium pentoxide is effective in converting sulfur dioxide to trioxide; complete conversion in a simulated flue gas containing 0.35 percent sulfur dioxide was obtained at 365° C. Pilot-plant and cost studies are being made by the Bureau to determine the economic feasibility of removing on an industrial scale the sulfur dioxide present in gases in low concentrations.

Jan 1, 1961

By David M. Gullikson

Since publication of the paper on the composition of California oilfield waters by Jensen (6)3/ in 1934 the only other information on the subject was published recently by Chave (4). To supply needed information on the composition of California waters in areas of current drilling activity, the Federal Bureau of Mines collected formation water samples for analysis. Thirty-eight samples from oil-and gas-producing formations in 12 fields located in Ventura, Kern, Glenn, and Colusa counties were analysed by the Bureau's San Francisco Petroleum Research Laboratory. The samples were selected particularly from fields where the water composition was not well known or where interpretation of electrical logs has been difficult and the interpretation may be affected by unusual composition of the water. These samples were obtained from rocks ranging in geologic age from Cretaceous to Upper Pliocene. Fifteen constituents of these waters were determined including sodium, potassium, calcium, magnesium, strontium, barium, lithium, chloride, iodide, bromide, carbonate, bicarbonate, sulfate, borate, and residual acidity. These analyses are the first to be published on California oilfield waters in which determinations for potassium, strontium, bromide, iodide, boron) and naphthenates were made on a significant number of samples. The electrical resistivities of tae samples were determined at 75° F. and 175° F.

Jan 1, 1961

By David M. Gullikson

As part of its program of petroleum production research the Federal Bureau of Mines has long been engaged in the study and development of systems of analysis of oilfield waters (8, 12, 20, 21, 22, 27, 30).21 However, many of the early chemical procedures developed by the Bureau and widely adopted by the petroleum industry are time consuming, and some are unreliable for determining certain constituents found in California oilfield waters. Because of the need for more rapid and more accurate methods having greater sensitivity with low concentrations of some constituents, a study has been made by the Bureau's Petroleum Research Laboratory at San Francisco, in developing new techniques and modifying previously published techniques for analyzing oilfield waters by flame spectrophotometric, potentiometric, and colorimetric methods. Test solutions were synthesized for testing the suitability and accuracy of the procedures, and the effect of interfering ions. These solutions contained known quantities of characteristic constituents of oilfield waters including sodium, magnesium, potassium, calcium, lithium, strontium, barium, sulfate, chloride, bromide, iodide, carbonate, bicarbonate and borates in a wide range of concentrations. The compositions of these synthetic brines are listed in table 22. Many California oilfield waters contain salts of petroleum-derived organic acids and several synthetic oilfield waters also were prepared to which large quantities of naphthenates or salts of petroleum acids were added.

Jan 1, 1961

By William J. Campbell

This study was a part of two programs: The first, to develop and evaluate high-temperature refractories; the second, to investigate reaction-rate kinetics and phase equilibria in the sinter step of the lime-soda process for the recovery of alumina. High-temperature X-ray diffractometer techniques are to be used extensively in both programs. This paper summarizes developments in the field of high-temperature X-ray diffractometers through 1959, evaluates various furnace designs, and describes briefly the X-ray diffraction facilities of the Federal Bureau of Mines. A more detailed description of the equipment and its calibration is planned in a future paper on thermal expansion and phase inversion of rare-earth oxides.

Jan 1, 1961

By William J. Campbell

The purpose of this investigation by the Federal Bureau of Mines was to design and construct a fluorescent X-ray spectrograph for dynamic rate studies of selective oxidation in molten metals and to establish basic principles for interpretation of data obtained by this method. An X-ray spectrograph was constructed in which the sample holder is a resistance wound furnace; it was operated up to 800° C. in oxidizing atmospheres. No difficulties were experienced with the cooling or heating systems nor with the protective layer of mica around the X-ray tube window, even though the oxidizing surface of the metal is only 0.5 inch from the X-ray tube window, Means are provided for heating under controlled atmospheres for selected time? temperature cycles.

Jan 1, 1961

By K. K. Kershner

Sulfide ore concentrates containing cobalt, nickel, copper, lead, and iron were salt roasted and leached on a laboratory scale. More than 95 percent of the cobalt, nickel, and copper was recovered. Heating patterns for salt roasting different concentrates were established. More cobalt, nickel, and copper were recovered from a bulk concentrate composed of a mixture of copper concentrate and iron concentrate. This mixture corresponded roughly with the mixture of these materials in stockpiles in southeastern Missouri. A temperature range of 375° to 400° C. was best for salt roasting. Metal chlorides were leached at a pH of 1 from chloridized charges of concentrates, Although the amounts of cobalt, nickel, and copper extracted were high, the amount of iron dissolved simultaneously interfered with subsequent separation and recovery of these metals. The amount of dissolved iron was reduced substantially by steam treating chloridized charges of bulk concentrate at 300° C. In this way, the ratios of cobalt, nickel, and copper to iron in leach liquors permitted satisfactory separation and recovery of these metals. INTRODUCTION The Federal Bureau of Mines is experimenting with chloridizing reactions.4 5 6 7/ Salt roasting of sulfide ores and concentrates, or their calcines, to form metal chlorides has certain advantages. Chlorides of

Jan 1, 1961

By E. R. Palowitch

A centrifugal float-and-sink test procedure has been developed by the Bureau of Mines to reduce the time for the gravimetric separation of coals finer than l4-mesh from as long as 24 hours to less than 1 hour. Comparative tests indicated that centrifuging a minus 14-mesh Pittsburgh-bed coal for 20 minutes at 1,500 revolutions per minute produced results that compared favorably with static float-and-sink test results. Standard deviations of the mean recovery and ash content of the float obtained centrifugally ranged from 1.31 and 0.04 percent, respectively, at 1.30 specific gravity to 0.21 and 0.05 percent, respectively, at 1.60 specific gravity. As in static separations, retreatment of the products separated at low specific gravities was required.

Jan 1, 1961

By F. H. Gibson

An investigation was made by the Federal Bureau of Mines of methods for determining phosphorus in coal, coal ash, and coke ash. Several of these methods are being considered for international standardization. As might be expected, methods and proposals from other countries for determining phosphorus differ considerably from those accepted an standard in the United States. Some of the methods differ fundamentally in principle from the American Society for Testing Materials (ASTM) standard used in the United States; others differ only in details of procedure. Because the Bureau considered that certain of the proposed methods might offer advantages in obtaining increased accuracy and precision or in decreasing the time required for making analyses, these methods were investigated, and the results compared with those obtained by the ASTM method. The methods investigated may be grouped into three types--volumetric, colorimetric, and gravimetric. All were about equally accurate and may be used alternatively. From a practical viewpoint, when only a limited number of analyses are made intermittently, the gravimetric procedure probably is the most suitable because no special apparatus or standard solutions are required. The volumetric methods are more rapid when more analyses are made. For mass production, the colorimetric methods, although requiring a suitable photometer or spectrophotometer, are more suitable because a large throughput should be feasible.

Jan 1, 1961

By J. B. Gayle

During the past several decades, there has been a steady increase in the number and size of experimental ovens used for carbonization research. Although many were originally intended principally for studies of coal expansion, current practice usually includes determinations of the properties of the experimental cokes. With respect to size and shatter characteristics, the cokes from the larger experimental ovens closely approximate those from duplicate charges carbonized in commercial ovens; however, they are consistently lighter and frequently less resistant to degradation by abrasive forces. To minimize these differences, some operators dry the experimental charges before carbonization. The resulting higher dry coal charge densities do, in fact, yield cokes with gravities closely approximating those produced commercially from the same coal or blend but without drying. The drying of the experimental charges may be criticized on the grounds that it represents a departure from commercial practice and may result in oxidation of the samples; for these reasons, the practice has not been universally adopted.

Jan 1, 1961

By J. J. Demeter

Experiments were conducted in 2- and 4-inch-diameter standpipes to evaluate the effectiveness of standpipes as pressure seals. During the experiments, these standpipes conveyed Alan-Wood magnetite (60 to 230 U.S. standard sieve mesh) by gravity flow from one vessel to another of relatively higher pressure. The information obtained has been helpful in a Federal Bureau of Mines investigation of how to make either synthesis gas or hydrogen by a modified steam-iron process employing a continuous recycling stream of granular iron-iron oxide at temperatures of 600° to 900° C. In this process the mixture of granular material flows by gravity from a reduction vessel at low pressures to an oxidation vessel at higher pressures. Data from the 2- and 4-inch-diameter standpipes indicate that it would be practical to use a standpipe as a pressure seal between the reductor and oxidizer. Investigators found that, by gravity flow, the standpipe could convey the Alan-Wood magnetite against pressure gradients up to 1.07 pounds per square inch per foot of column height.

Jan 1, 1961

By Robert H. Merrill

This report summerizes the various studies made to determine the size and support of roofs in the upper shale formation, White Pine Copper Mine, Michigan. These studies were a cooperative effort of the White Pine Copper Company and the Federal Bureau of Mines. Before this investigation, the upper shale formation had been found to contain about 30 to 40 percent of the total mineralization in the ore zones. Investigators estimated that this shale could be economically mined by room-and-pillar methods, provided that the roof would stand over spans of 25 to 32 feet. The problem remained to determine the number of bolts required to safely support these spans. Unbonded fractures in the roof structure of the deposit complicated the use of laboratory methods for determining bolted roof support. Therefore, a method was devised to determine the in-place support which would consider the unbonded fractures. In this method the roofs of 3 rooms with spans of 20, 28, and 36 feet were intentionally overbolted as the rooms were mined. Following stability tests that sometimes exceeded 6 months, the bolts were selectively removed and roof sag, roof strain, and changes in bolt loads were measured concurrently. The number of bolts required for support of these spans was computed from these data.

Jan 1, 1961

By S. L. May

Investigations by the Federal Bureau of Mines indicate that hafnium and zirconium compounds of acceptable purity can be extracted from Nigerian zircon concentrates. Chlorination and caustic soda fusion techniques were used to extract 85 to 95 percent of the valuable metals from the concentrate. The extracted hafnium and zirconium compounds were purified by recrystallization of the oxychlorides or by formation of complex salts during chlorination. The zirconium-hafnium product of the recrystallization method contained 15 parts per million of uranium, and the product of the salt-complex method contained less than 10 parts per million of uranium. The hafnium was separated from zirconium by solvent extraction methods. A zirconium product containing 0.3 percent hafnium and a hafnium product containing 4 percent zirconium were obtained. At the request of the Atomic Energy Commission (AEC), work was started to develop techniques for processing Nigerian zircon concentrates in commercial installations presently engaged in producing zirconium and hafnium metals from ores. The Nigerian zircon has a high hafnium content, but the presence of uranium and thorium is a problem not normally encountered in processing zircon concentrates.

Jan 1, 1961

By J. W. Town

This report summarizes the results of laboratory investigations conducted by the Federal Bureau of Mines to obtain hydrometallurgical information on the dissolution of mercury sulfides from ores, flotation concentrates, and pure mercuric sulfides. Statistical methods were used to design the experiments and evaluate the resulting data. Studies demonstrated that cinnabar is readily soluble in sodium sulfide, partly soluble in potassium sulfide, and essentially insoluble in ammonium sulfide. Additions of sodium hydroxide or potassium hydroxide to sodium sulfide solutions increased mercury extraction slightly; when either was added to potassium sulfide or ammonium sulfide solutions, mercury extraction was equal to that of sodium sulfide. Tests at the Albany Metallurgy Research Center showed that sodium sulfide would completely dissolve chemically pure mercuric sulfide, more than 95 percent of the cinnabar in 5-percent mercury flotation concentrates, and 60 to 90 percent of the cinnabar in low-grade ores. The double-leach tests showed that potassium sulfide would dissolve over 90 percent of the arsenic in mercury-arsenic products and 1 to 10 percent of the mercury; then sodium sulfide-hydroxide solutions would dissolve 80 to 90 percent of the remaining mercury and 5 to 10 percent of the arsenic.

Jan 1, 1961

By F. W. Wood

A program of research was conducted by the Bureau of Mines to investigate anomalies in electrical-discharge behavior during consumable-electrode arc melting of titanium and to study the effects of these irregularities on arc-furnace explosions. A major effort was devoted to an experimental survey of arc behavior and a qualitative definition of discharge phenomena.3/ An important conclusion was that the "glow" of industrial arc-melting terminology is not a glow discharge but a skittering arc in a displaced position. The conditions that permit displaced skittering were tentatively defined. The displaced skittering arcs tended to damage melting crucibles in two ways, and details of possible mechanisms leading to crucible rupture and explosive reactions have been proposed accordingly. However, no acceptable means of preventing crucible damage was discovered.

Jan 1, 1961

By J. S. Browning

Laboratory and pilot-plant tests of spodumene-beryl pegmatites of the Kings Mountain, N. C., area resulted in development of a new and improved method by the Bureau of Mines for separating and recovering spodumene, mica, and beryl. The process was successfully applied to other domestic pegmatites and a spodumene flotation-plant tailing containing about 0.5 percent beryl. The method comprised soap flotation of the spodumene, using combinations of sodium fluoride and lignin sulfonate as conditioning agents to recover 80 to 85 percent of the contained lithia in concentrates assaying over 6 percent Li20. About 80 percent or more of the beryl was retarded in the spodumene tailing. The beryl subsequently was activated, floated, and cleaned in a secondary circuit to yield beryl concentrates containing 6 to 7 percent BeO. The tests also demonstrated that a good recovery of high-grade mica could be produced.

Jan 1, 1961

By A. L. Engel

This report is a compilation of preliminary and, in some cases, more extensive concentration experiments by the Federal Bureau of Mines on low-and medium-grade fluorspar ores from three localities in Nevada and one in California. The work was done on samples obtained from Shoshone mine, Nye County, Valery mine, Pershing County, and the Broken Hills mine, Mineral County, all in Nevada, and Dirty Weather mine, Inyo County, Calif. These investigations were made to aid in the development of domestic fluorspar resources, in line with the Bureau's long-established program of conservation of mineral resources. The treatment methods employed in the experimental work described included simulated or "heavy-liquid" gravity concentration of coarse minerals and comparatively fine-grained minerals, and flotation concentration of finely-ground minerals. These methods were attempted in order to beneficiate the ores and produce concentrates which could be marketed readily, with as high a recovery rate as possible, while using simple treatment methods suitable for small-scale operation.

Jan 1, 1961

By Murray Jacobson

Data obtained by the Federal Bureau of Mines on the dust explosion hazard in air are presented for 220 samples of agricultural products. Information is given on ignition temperature of dust clouds and layers, minimum explosive concentration, minimum electrical energy for ignition, explosion pressure and rates of pressure rise, amount of inert dust required to prevent flame propagation, and, in a few instances, the permissible oxygen concentration in an atmosphere to prevent ignition by spark and by heated surface. The effects of particle size and source of sample on explosibility are shown. The relative ignition sensitivity, severity of explosion, and overall explosibility of the materials are characterized by empirical indexes. This report contains Ma obtained by the Bureau in laboratory studies on the explosion hazards of agricultural dusts. Recognition of the dangers will encourage adoption of adequate measures to prevent ignition and explosion during preparation, processing, and utilization of the materials. Agricultural products constitute one of the largest groups of materials used in America. More than 260 million tons of various grains, much of which now exists in dust form, was grown in 1958.6/ Over 600,000 tons of the annual production of 200

Jan 1, 1961

By W. A. Calhoun

The purpose of this investigation was to develop economical mineral dressing processes for removing objectionable quantities of impurities, such as quartz and pyrite, from refractory clay deposits in east central Missouri. The presence of excessive quartz in these clays causes crazing. Pyrite causes bloating and unsightly dark blobs on the surface of fired refractory brick. The iron concentration in the proper state of oxidation may also act as nucleation centers for carbon crystal growth which can result in bursting of the refractory. Numerous deposits, representing a very large tonnage, have been examined and prospected by various refractories companies and found to contain impurities in objectionable quantities. Upgrading these clays would greatly extend our reserves of high-quality refractory clays. Wet-tabling and wet-cyclone concentration were found to be effective for removal of impurities from clays. Of the two methods, wet-cyclone concentra¬tion would be cheaper and more effective. Although wet-tabling improved the refractory properties of each clay, beneficiation by wet-cyclone produced clays of superior quality. Clay recoveries by wet-cycloning ranged from 56.1 to 81.8 percent of the weight of the crude samples, and the beneficiated clays contained from 71.9 to 94.4 percent of the total alumina. The pyrometric cone equivalent (PCE) was increased from 1 to 3 cones by wet-cycloning. The beneficiated clays also met the reheat shrinkage requirements on refiring to 1,400° C. Missouri is one of the major domestic sources of fare clay. In addition to deposits of high-grade refractory clays, there arc many deposits that contain small percentages of impurities, which render the clays unfit for the production of high-heat-duty firebrick. Development of methods to beneficiate these submarginal clays to usable materials would greatly increase commercial fire clay resources.

Jan 1, 1961

By V. M. Benson

A simplified, routine method for determining lithium in lithium-bearing rock is presented. The sample is decomposed by repeated treatments with nitric, hydrofluoric, and perchloric acids. Since this procedure does not appreciably dissolve beryl, interference by beryllium (the principal interfering cation) is minimized for most samples. The salts are brought into solution with water and enough citric acid-ammonium citrate buffer is added to make the final volumetric dilution 0.20 M with respect to citrate. The addition of citrate greatly reduces anion interference in the hydrogen-oxygen flame, slightly increases the intensity of the lithium 671 millimicron emission line, and reduces the effect of most of the interfering cations to the extent that analytical separations are not necessary. The accuracy of results of single determinations of lithium in a pegmatite containing spodumene, lithium-bearing mica, and beryl are approximately equal to that obtained by other flame methods, INTRODUCTION This investigation was undertaken in Bureau of Mines laboratories to develop a reliable, rapid, routine analytical method for determining lithium in lithium-bearing minerals. The requirements of the procedure were that the method should be applicable to the analysis of a variety of lithium-bearing ores and test products, and the results would be reasonably accurate for materials containing 0.05 to 8 percent Li20.

Jan 1, 1961

By D. A. Wilson

Several promising systems for selectively oxidizing the iron in an iron-tin alloy commonly called "hardhead" were investigated in a research project conducted to devise a method for recovering tin from this troublesome alloy. A satisfactory oxidation method was developed and tested successfully on melts of 2,000 grams. Molten hardhead (near 1,080° C.) was blown with air to oxidize iron and leave tin in the reduced state. Recovery of available tin was 96 to 98 percent. Tin products contained 2 to 0.1 percent iron which was reduced to 0.06 percent by filtration at 250° C. Iron oxide formed during oxidation was absorbed by a fluid flux cover composed of 43 percent silica, 17 percent burned limestone, and 40 percent fused borax. Less successful but nevertheless promising results were obtained with mixtures of steam and hydrogen which were sufficiently selective at temperatures between 600° and 950° C. but did not result in complete oxidation of iron. Carbon dioxide-carbon monoxide mixtures also oxidized iron selectively but incompletely. Both stern and carbon dioxide systems produced sufficiently encouraging results to additional research on these systems.

Jan 1, 1961