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By H. P. LeVan

The aced for reliable reserves of the essential element, manganese, has been a continuing concern of the Federal Government for more than three decades. Because of the increasing vulnerability of outside sources of supply efforts have been intensified to find a means for beneficiating United States domestic deposits. The deposits of most interest would of necessity be near, or have access to, suitable transportation to processing plants. The Georgia manganiferous iron deposits represent some 10 million tons4 of ore readily available to southern iron and steel industries, if a manganese recovery process capable of functioning in the presence of large quantities of iron can be developed. In addition, a successful method for beneficiating the Georgia ore could produce a significant quantity of high-grade iron concentrate. The Differential sulfatization process developed 47 the Bureau of Mines5 seemed to be well suited for this application, particularly because it results in low concentrations of iron in the leach liquors with relatively complete extractions of manganese. In this process, manganese in the presence of iron is preferentially reacted with sulfur dioxide at elevated temperatures and subsequently extracted with water.

Jan 1, 1962

By L. H. Banning

This investigation was undertaken to obtain basic information necessary for the design and operation of a plant for recovering metallic values from nickeliferous laterite and serpentine of the Philippine Islands. It was divided into three parts: (1) Mineralogical studies and preliminary mineral dressing tests; (2) electric smelting of the ores, upgrading of ferronickel by blowing with oxygen, smelting laterite slag to produce crude iron, and the production of mild steel; and (3) nickel and cobalt recovery from upgraded ferronickel. Results of the investigation indicate that it should be feasible to recover nickel, iron, and possibly cobalt products from the laterite and ferro-nickel from the serpentine. Mineralogical studies were made on representative fractions of the laterite and serpentine tonnage samples and on five selected samples; mineral dressing tests were made only on laterite. The nickel occurs principally associated with hydrous iron oxides and chemically combined with serpentine; garnierite was the only discrete nickel mineral identified, and it was found in a highly decomposed serpentine. The bulk of the cobalt was found in wadlike manganese oxide material. Approximately twice as much chromite was found in the laterite as in the serpentine, By mineral dressing techniques, laterite was separated into two fractions: one fraction contained over 90 percent of the nickel and cobalt, and 83 percent of the iron; the other fraction contained 74 percent of the chromium. A cobalt concentrate (1.1 percent Co) was produced by a scrubbing and sizing procedure.

Jan 1, 1962

By H. R. Shell

Fluorphlogopite mica was synthesized from inexpensive and abundant olivine, clay, feldspar, and sand (plus K2SiF6). The raw materials were melted in crucibles and in an internal resistance electric furnace. The melts yielded >95 percent mica. The major difficulty encountered was incomplete settling of the highly dispersed ferroalloy. This problem was not completely solved. Reducing agents tried in melts of 300 to 400 pounds were carbon, silicon, and silicon carbide. Carbon slowly reduced the iron of the raw materials, with much fuming. Silicon apparently was oxidized ahead of the melting and was ineffective under the conditions obtained. By far the best reducing agent was silicon carbide. With silicon carbide, fuming did not occur and ionic iron content of the mica flake approached 0 percent. However, even with SiC, the highly dispersed globular iron did not completely separate from the mica portion. The fluorphlogopite made during this investigation should be suitable for metallurgical use. A byproduct ferroalloy containing about 5 percent nickel, 3 to 5 percent chromium, and some cobalt was obtained. Because of the highly dispersed metallic ferroalloy, the mica was not deemed suitable for electrical or electronic uses.

Jan 1, 1962

By Frank Parrish

History and performance data of 17 water-injection projects in Cooke and Grayson Counties in north Texas are presented for the purpose of studying and comparing operating practices and oil-recovery techniques. Water is injected into Strawn and Canyon sands of Pennsylvanian age. The principal formation flooded is the Strawn, which ranges in depth from 725 to 6,900 ft in the projects covered. Estimated ultimate recoveries range as follows: Primary, 22 to 494 bbl per acre ft; and secondary; 63 to 296 bbl per acre ft. These figures represent the following percentages of original oil in place: Primary, 10 to 46 pct; and secondary, 8 to 23 pct. Shallower projects; 725 to 1,500 ft in depth, had higher average primary and secondary recoveries than did deeper projects. Crude-oil gravity, which ranges from 20° to 45° API, was not relatable to yield of secondary recovery oil. Analysis of the data indicates that five-spot injection patterns will yield the highest percentage of oil remaining at start of flooding; that is, 28.8 pct for five-spot injection patterns, compared with 20.8 pct for line-drive patterns and 11.6 pct for random patterns. Waterflooding in this area appears to be very successful. Secondary recoveries of most projects are expected to nearly equal primary recoveries.

Jan 1, 1963

By Hal J. Kelly

A number of problems that developed in processing the halloysitic clays of eastern Washington and northern Idaho were investigated by the Bureau of Mines. The deflocculating effect of tetra sodium pyrophosphate is compared with several other compounds, and on the basis of current theory, the advantage of sodium pyrophosphate as a deflocculating agent is explained. The adsorption of the sodium ion by clay in a clay"-water system was established by a radioactive tracer technique, and the deflocculating action of sodium pyro- phosphate was postulated. The effective dispersion of the halloysitic clays was limited by the occurrence of tightly bound aggregates of small, individual crystals. Disaggregation of the agglomerates was investigated by liquid extrusion and ball milling of dilute slurries and by extrusion of the clay in a plastic state. The greatest increase in the production of small particles was by high? pressure liquid extrusion.

Jan 1, 1963

By Allan F. Smith

The influence of hydraulic fluids on spontaneous heating in bituminous coals is determined by measurement of the temperature increases produced in coal-fluid mixtures heated to a temperature sufficient for the initiation of self-heating. Similar tests on as-received coal samples and water-coal mixtures are compared with the results obtained for the various hydraulic fluids. Three of the four coals were sampled from coalbeds known to have a history of spontaneous heating. The data provide a basis for predicting the possible effects in gob or carbonaceous refuse of coal mines.

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 R. D. Berkenkotter

Titanium and iron assays obtained from cores of three diamond-drill holes from the Cebolla Creek titaniferous iron deposit were evaluated by statistical techniques to obtain information concerning the mineral characteristics of the deposit and to make a preliminary determination of sampling requirements for the deposit. A range of sample volumes representing sizes from one-sixth NX core 2 feet in length through full NX core 10 feet in length were prepared by split-ting the NX core with a diamond saw and combining pulverized splits. Results indicate the existence of at least two statistical populations having different average grades of iron and titanium. Each has an assay frequency distribution that is not normal but is highly peaked (leptokurtic). Frequency distributions of assays from specific altered zones of the drill holes appear to be normally distributed. Increasing the cross-sectional area of the sample unit to change assay volume did not result in significant changes either in assay values or the resulting frequency distributions of assays. However, when assay volume is increased by increasing sample interval, the shape of the assay frequency distribution changes, and a normal distribution of assays is approached. Positive correlation exists between titanium and iron assays. The degree of correlation, although very significant, is too low to use for prediction purposes. Although the amount of data from three widely separated drill holes is not sufficient to establish an average grade for this large deposit, it indicates a range of expected assay values and provides some information for determining requirements of future sampling for evaluation purposes.

Jan 1, 1963

By Robert M. Becker

This report (the second in a series of five) presents the mathematical development in extending the theory of sample reliability from a sample consisting of a fixed number of items to a sample consisting of a fixed amount of items. Examples of a fixed amount of items per sample are samples consisting of a fixed weight or a fixed volume of unequal size particles. The probability distribution functions (those here called the compound binomial and compound multinomial functions) are developed from fundamentals. Their distributions are generalized to include some measured characteristic of the items. Infinite population moments are derived from moment-generating functions, while finite population moments are developed from corresponding infinite population moments using the finite probability operator defined in part 1 of this series.

Jan 1, 1964

By Jr. Gabler

Methods for the direct spectrochemical determination of impurities at the parts-per-million level in tungsten metal and oxide are presented. Several published procedures were investigated and numerous modifications were made in establishing procedures with improved precision and extended lower levels of determinability. Details of standards preparation are presented, experimental work is described, and three preferred methods are described in detail. A germanium carrier-distillation procedure is applicable to the determination of 13 elements in tungsten powder; a silver chloride carrier-distillation procedure provides for the determination of 24 elements in tungstic oxide, and a sustaining ac arc method is applicable to 26 elements in tungstic oxide. The choice of methods to be used depends upon sample form, elements and concentrations to be determined, and the precision and accuracy required. The investigations reported here were undertaken to develop direct spec-trochemical methods with increased accuracy and precision to determine impurities in high-purity tungsten and tungstic oxide, to define the lower concentration levels of detectability and measurement for the common impurities in tungsten by direct spectrographic means, and to present the details of the developed or modified methods that have proved applicable.

Jan 1, 1965

By Norman G. Foster

The mass spectra of four tertiary butyl substituted thiophenes are reported. A comparison and contrast with earlier structure correlations made by API-RP48 mass spectroscopists is presented. The fragmentation routes of these types of molecules are discussed and explained in terms of existing theories in mass spectrometry. Low ionization voltage data are presented to support the mechanistic picture developed. Structures are inferred about some of the ions, and these are correlated with existing theories. Metastable peaks in the spectra are used to support the fragmentation paths. The presence of doubly charged ions in the spectra is noted and the possible implications toward mechanisms discussed. The general picture of simple, small fragments leaving the ion moiety upon further fragmentation is developed in detail. Some suggestions are presented for further work utilizing isotopically labeled molecules to establish firmly the general picture of fragmentations of the alkylthiophenes.

Jan 1, 1966

By E. G. King

The Bureau of Mines made experimental determinations of the heats of formation of forsterite and chrysotile at 298.15° K. The heat capacities of two polymorphs of serpentine, chrysotile and antigorite, were measured over the temperature range from 50° to 298° K and the entropies at 298.15° K were evaluated. The heat content of antigorite above 298.15° K was measured to 850° K. These thermochemical data were combined with other pertinent data to give heat and free energy of formation values at high temperatures. Free energy values are given for the reaction, forsterite + water = brucite + serpentine at different temperatures and pressures.

Jan 1, 1967

By Elton L. Litchfield, Milton L. Weiss

Studies were made on the projectile impact sensitivity of explosives by subjecting explosive samples to the impact of metal projectiles fired from a 0.50- caliber gun . The projectiles , in the form of right cylinders , made plane surface to plane surface contact with the explosives . Pressures in the explosive were investigated with an expendable pressure transducer in some instances . The physical model of the projectile - explosive interaction describes , in principle , the duration of the peak shock pressure in terms of the projectile and explosive geometry and the steady- state penetration of the explosive . Of the explosives studied , liquid hydrogen- solid oxygen and liquid oxygen - solid or liquid hydrocarbon fuel were the most shock sensitive ( requiring an initiating shock of about 1.0 kb or 987 atmospheres pressure ) ; cast TNT was the least sensitive ( requiring an initiating shock of more than 110 kb pressure ) . Measurements of pressure in the explosive showed some moderate space resolution by the transducer and gave pressure distributions in agreement with expectations from the model of the shock processes . The appearance of the recovered projectiles and the calculated initiation shock pressures suggest that the solid explosives were initiated directly to high- order detonation , whereas the liquid explosives were probably initiated to low- order detonation-- with a subsequent , later transition to high- order detonation .

Jan 1, 1965

By William R. Hardwick

Present information indicates that a copper deposit can be safely fractured with a nuclear explosive and the copper successfully recovered by the in-situ leaching method. The process is not yet at the stage where it can be presented t ) the mining industry as a technique proven in all its aspects, but it is a method with high success potential. Unknown factors must be evaluated by a full-scale test before the economics or the extent of the use of the method by the mining industry can be predicted. Preliminary calculations indicate that the cost of fracturing a copper deposit nuclear explosives may range from l.8 to 55.2 cents per ton or in some case: less than a cent per pound of recoverable copper. Copper may be recovered at less cost than by conventional methods. Deposits with 4 pounds of recoverable copper may be economic and production from a deposit may begin in less than half the time required for conventional methods.

Jan 1, 1967

By R. V. Higgins

The Bureau of Mines investigated the use of electronic computers for obtaining more information about relative permeabilities of reservoir rock to oil and water. It was found that there are many possible combinations of relative permeability curves that will result in virtually the same recovery versus injection) but they require different times and rates to recover the oil even with different mobility ratios. Permeability curves obtained by the use of non-viscous oil and employed for calculating the waterfloods of viscous oils can lead to serious inaccuracies. For viscous oils) the wettability characteristics in the middle portion of the permeability curve affect recovery nearly as much as other portions of the curve; this) however) is not true for non-viscous oils in water-wet reservoir rock.

Jan 1, 1967

By William R. Barton

Sampling to determine development potential of beryllium deposits was conducted at 31 New England localities. A total of 54 additional areas where the geochemical environment appeared favorable were sampled to determine if economically interesting percentages of beryllia (BeO) might occur. Newry Hill-Plumbago Mountain, Maine, Iron Mountain, N.H., and Long Island, Maine, were investigated in some detail to determine the size and grade of deposits. The mineralized pegmatites at Newry Hill-Phunbago Mountain are extensive but very low grade; at Iron Mountain the ore bodies are very rich but of small volume; at Long Island beryl occurs with molybdenite, wolframite, and scheelite, but the tonnage of ore was not determined.

Jan 1, 1968

By T. N. Rushton

Rate minima are encountered in the reduction of magnetite with hydrogen. In a certain temperature zone, the reaction rate decreases with rise in temperature. This is inexplicable by classical kinetic theories; neither is a transition in reduction mechanism suitable for interpreting the observed behavior, This anomaly can be fully explained by hypothesizing two species of chemisorbed hydrogen with different adsorption coefficients and activation energies for adsorption. Competition between two energetic states of adsorption occurs with temperature rise, with the low energy state predominating below the anomalous temperature zone and the high energy state above it. The presence of two possible adsorption sites appears to be characteristic for oxidic adsorbents.

Jan 1, 1968

By Wilbert T. Malenka

A modified factorial experiment was used to determine the effect of operating factors in hydraulic mining of anthracite. Seven basic factors at various levels were considered. The significant factors were found to be pressure-volume, pattern, and jet traverse speed. Mining data were programed for computer, and a prediction equation was determined from printout information based on the hydraulic "jumbo" operating parameters and characteristics of anthracite, The source of error is discussed. The prediction equation is general in nature and might be useful in delineating performance characteristics in the design of equipment and/or more effective utilization in a medium with characteristics similar to those of anthracite.

Jan 1, 1968

By Ronald P. Hollenbeck

Shales in the Appalachian Region of Kentucky and Tennessee were sampled and tested to determine their use as raw materials for the manufacture of lightweight aggregate by the rotary-kiln method. Nine samples were obtained from eastern Kentucky and 143 samples were obtained from eastern Tennessee. As a result of preliminary testing of these samples, two sources in eastern Kentucky and 11 sources in eastern Tennessee were resampled for rotary-kiln tests. The rotary-kiln tests showed the two sources in Kentucky and seven sources in Tennessee contained shale that would produce satisfactory aggregate. Lightweight aggregate processed from these nine sources was tested in concrete shapes and was found to be suitable for use in structural concrete.

Jan 1, 1968

By Eldon C. Pattee

Reconnaisance samples of reported beryllium occurrences in Idaho, Washington, Montana, and Oregon were chemically and spectroscopically tested in a mobile laboratory. The two predominant types of occurrences were green beryl associated with Cretaceous intrusions and disseminated aquamarine associated with Tertiary intrusions. Although the beryllium content of known deposits in the Northwest is too low for economic development at present, total submarginal-grade beryllium resources in pegmatites are estimated to be 570,000 to 1,870,000 tons containing 0.024 to 0.167 BeO. A potential source of 500,000 to 700,000 tons of beryllium-bearing tactite in Idaho and Montana averages 0.033 to 0.080 percent BeO.

Jan 1, 1968