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By Robert K. Koch, Henry E. Blake

Laboratory tests were made to determine if aluminum fluoride of commercial grade could be synthesized by reacting alumina hydrate with dilute ( 25 to 75 grams per liter of fluorine ) aqueous fluoride solutions . • Products containing up to 90 percent aluminum fluoride ( A1F ) were synthesized by reaction of alumina trihydrate ( A120 3H2O) with either dilute hydrofluoric acid ( HF ) or ammonium fluoride ( NHF) solutions , the ammonium fluoride solution resulting from ammonia ( NH ) desilication of a hydrofluoricfluosilicic acid ( HF - H₂ SiF ) solution . Fluorine recoveries of over 80 percent were obtained with either type of solution . The hydrated precipitates of AlF, and ( NH4 ) , A1F ( ammonium aluminum fluoride ) obtained by reacting hydrated alumina with these solutions were subsequently converted to anhydrous AlF, by controlled heating .

Jan 1, 1964

By Vernom F. Swanson, George E. Fish

A study was made during 1959-60 of reported nelsonite occurrences in Nelson and Amherst Counties, Va. The investigation was limited to core drill- ing on one deposit and beneficiation studies on three deposits. Three diamond-drill holes totaling 562 feet were drilled on the E. M. Hughes property to determine subsurface continuity. Although outcrops as much as 30 feet wide were present on this property, the only nelsonite intersected in the holes ranged from 4 to 18 inches thick. The ilmenite content of the core ranged from 50 to 75 percent. These nelsonite deposits are of secondary importance as a source of titanium, being small, rarely exceeding 1,500 feet in length and 30 feet in width, but they are high grade. Due to the proximity of some of the bodies it might be possible to mine several of them as one operation feeding one mill. Electromagnetic separation on composited samples recovered 83.0 percent of the Tio as an ilmenite concentrate in 68.5 percent of the weight. Two flotation procedures were developed. The first method, using oleic acid as a collector and fluo silicic acid as an apatite depressant on deslimed feed, produced an overall recovery of 59.3 percent in batch tests. The second procedure eliminated desliming. Laurylamine hydrochloride removed silicates in an acid pulp followed by an alkaline apatite flotation with oleic acid as the collector and dextrine as the ilmenite depressant. The ilmenite-rich tailing represented a 66.2-percent recovery of Tio in the batch tests.

Jan 1, 1964

By James S. Browning, W. H. Eddy

Laboratory batch and small - scale continuous flotation tests were conducted on a ferruginous barite - fluorspar ore from near Sweetwater , Tenn . , to determine the feasibility of producing commercial - grade fluorspar and barite concentrates . The lignin sulfonate - sodium fluoride - fatty acid method of floating fluorspar produced acid - grade concentrates . Flotation of the barite from the fluorspar tailing using petroleum sulfonate yielded concentrates suitable for use as a weighting agent in oil -well drilling muds . The continuous flotation tests , treating about 150 pounds of ore per hour , yielded fluorspar concentrates that assayed 98.3 percent CaF2 and barite concentrates that assayed 91.2 percent BaSO4 . The recovery of the two minerals was 91.2 and 85.2 percent , respectively .

Jan 1, 1964

By H. R. Babitzke, H. Kato, R. E. Siemens

An investigation was made to provide further information for evaluating columbium- hafnium alloys for use as high - temperature structural materials . The columbium- hafnium system was investigated between 700 ° and 2,400 ° C by melting point , thermal analysis , X - ray diffraction , electrical resistivity , and metallographic techniques . The equilibrium diagram is the beta isomorphous type , with columbium tending to stabilize the beta phase . Addition of 60 atomic percent columbium stabilizes the beta phase at 700 ° C. The allotropic transformation temperature of hafnium is 1,750 ° ± 20 ° C. A minimum melting point occurs near 75 atomic percent hafnium .

Jan 1, 1964

By G. W. Birge, D. E. Wolfson, J. H. Lynch

Fourteen coal samples representing the Flag , Fire Clay , Whitesburg , Amburgy , Upper Elkhorn No. 3 , Upper Elkhorn No. 2 , Upper Elkhorn No. 1 , and Lower Elkhorn beds in Letcher County , Ky . , were carbonized by the Bureau of Mines - American Gas Association ( BM- AGA ) method , and yields of products and physical properties of cokes were determined . The samples tested were high- volatile A bituminous in rank , with dry , mineral - matter- free fixed - carbon contents ranging from 55.3 to 62.2 percent . Five of the samples , as received , were chemically unsuitable for metallurgical use because of excessive ash and/ or sulfur content . Generally , strength indexes of the cokes were low and all of the coals would require blending with higher rank coal to obtain satisfactory blast furnace fuel .

Jan 1, 1964

By Joe L. Castagno, Kenneth H. Johnston

Several hundred membrane - filter tests were made as part of a program to develop equipment and procedures to evaluate the quality of waters and to determine the quality of water suitable to efficiently flood oil sands of known permeability . Results indicated that neither the color of the water nor that of the precipitate on a membrane filter is a criterion for determining the quality of injection water . Reasons for poor water quality include poor operation of filtering systems , dirty filtering aggregates , excessive amounts of oil in injection water , commingling of incompatible waters , and excessive use of chemicals . A good water is required to efficiently flood sands of low permeability , but fair results may be obtained in flooding more permeable sands with poorer quality water .

Jan 1, 1964

By Henry M. Harris, Hal J. Kelly

Electrical dewatering tests are described in which the laboratory cells were designed for continuous operation using an endless metal belt as the anode . The test slurries were dilute , containing from 2.5 to 14.4 percent solids (specific gravity of 1.02 to 1.10 ) that were all minus 8 microns in size . Recovery of the solids of low water content was the practical objective of the investigation . Process variables evaluated and reported are : The effect of feed rate , amount of electrolyte , samples from different sources , and the use of two cells in series . These variables are evaluated on the basis of yield of clay per kilowatt - hour , recovery , and the amount of solids in the deposited clay . Recovery , yield , and solid content of the belt anode product are interdependent , and changes that will improve one of these characteristics often are accomplished at the expense of the others . Tests in which recoveries range from 50 to 60 percent usually result in yields of 8 to 9 kilograms (kg ) of dry clay per kilowatt- hour (kwhr ) . Under these conditions , the solid content of the deposited clay approximates 50 percent . One test sample , composed of kaolinite , showed very high yield , 13 to 16 kg per kwhr ; high recovery , 53 to 58 percent ; and 52 to 54 percent solids in the cake .

Jan 1, 1964

By F. E. Joyce, Charles Prasky

This report describes the response to high- temperature sulfatization of a variety of manganese minerals and companion compounds which may occur either as a principal component or as a gangue material in low- grade manganese deposits . Fourteen manganese samples representing oxide , carbonate , and silicate minerals as well as seven compounds which might occur as gangue with manganese minerals were tested batchwise in a bench- scale apparatus under conditions which would be favorable for the sulfatization of manganese . The manganese minerals substantiated thermodynamic predictions and responded to sulfatization but to varying degrees . The gangue materials , MgO , MgCO,, CaO , and CaCO3 , were sulfatized readily in contrast to the iron oxides and the aluminacontaining material which were not .

Jan 1, 1964

By I. L. Nichols, K. C. Dean, P. H. Johnson

Hydrochloric acid , sulfuric acid , and chloridizing roast- water leaching methods for dissolution of cesium and rubidium from Maine , Canada , and Southern Rhodesia pollucite ores and their flotation products were investigated by small- scale tests . Optimum conditions were determined to be ( 1 ) for hydrochloric acid leaching , use 12.7 equivalents of 8.8 normal acid per equivalent of cesium in the sample and leach for 6 hours at 100 ° C ; ( 2 ) for sulfuric acid leaching , use 12.7 equivalents of 14.4 normal acid and leach for 2 hours at 120° C ; and (3 ) for chloridizing roast - water leaching , roast minus 200 - mesh ore, limestone , and calcium chloride in a ratio of 2 : 4 : 1 , respectively , for 1 hour at 900 ° C , and leach the calcine for 1 hour at 80 ° C with enough water to give 35 pct solids . Extractions of cesium from ores and flotation products containing over 20 pct cesium were in excess of 97 , 93 , and 96 pct for the hydrochloric acid , sulfuric acid , and chloridizing roast - water leach processes , respectively .

Jan 1, 1964

By A. F. Colombo, R. T. Sorensen, D. W. Frommer

The Bureau of Mines developed a flotation method for concentrating spiral tailing produced from pilot plant tests on the Champion mine ore fines . The feed material contained about 49 percent Fe and 15 percent SiO2 and was posed mostly of specular hematite , muscovite , and chlorite . Bench- scale , batch flotation research developed a reagent suite composed of tall oil - fatty acid , fuel oil , sulfuric acid , sodium fluoride , and sodium silicate for recovery of iron minerals in the froth product . Concentrate made with the reagent suite contained 87.3 percent of the iron and analyzed 65.6 percent Fe and 1.9 percent SiO2 . Continuous flotation tests were made with a nominal feed rate of 400 lb /hr , but without middling recirculation . Using nearly the same amount and complement of reagents as in the batch tests , three similar continuous tests gave concentrates averaging 63.9 percent Fe and 3.1 percent Sio while recovering about 86 percent of the iron .

Jan 1, 1964

By F. W. Hoertel

Tungsten from the hydrogen reduction of WF was vapor - deposited to coat MERM (Material Evaluation Rocket Motor ) graphite and rhenium- lined graphite nozzles . These nozzles have surface configurations that preclude the conventional fabrication of high- density- tungsten liners . Operation at 550 ° C produced selectively placed uniform coatings of specified thicknesses at near theoretical density . An acceptable coating could not be deposited on a beryllia nozzle because of an undesirable side reaction between the substrate and one or more of the products of the reduction reaction .

Jan 1, 1964

By Wilbur I. Duvall

This paper presents arguments which show that a velocity seismograph should be used to measure building and ground vibrations produced by blasting . However , portable velocity seismographs suitable for this type of measurement are not commercially available . The paper describes how a velocity seismograph can be assembled from commercially available velocity gages , amplifiers , and recorders . Also , specifications are given which could be used in the design and manufacture of a portable velocity seismograph suitable for measuring vibrations from blasting .

Jan 1, 1964

By H. A. Dierks, H. B. Link

The purpose of this investigation was to develop a practical feeder apparatus to introduce comparatively large pieces of coal and similar material into a pipeline under pressure in connection with the vertical hydraulic transportation of solids , termed " hydraulic hoisting . " This method of hoisting the precrushed run - of - mine product of an underground mine has been given unusually wide attention abroad and could be of considerable significance to the U.S. mining industry in its search for operating improvements and cost reduction . A lock-hopper assembly was developed after a series of sinking velocity tests were made by dropping anthracite in a column of water . The system functioned reliably as an automatically operated feeder apparatus .

Jan 1, 1964

By Robert H. Merrill, James V. Williamson, David M. Ropchan, George H. Kruse

In- situ rock stresses were determined by flatjack and borehole - deformation methods . Estimates of the stress distribution around a flatjack were obtained by a combination of flatjack and borehole - gage techniques . The investigations were part of a study , conducted jointly by the State of California and the Federal Bureau of Mines , to determine the stress in rock at the site of an underground powerplant for the Oroville Dam near Oroville , California . The stress distribution around each of three flatjacks was nonsymmetric ; however , stresses obtained from 9 flatjack and 157 borehole measurements are considered reasonably accurate for engineering purposes . The stress near the edge of the openings is between 800 and 1,600 psi ; the stress in the undisturbed rock is approximately 500 psi , nearly hydrostatic .

Jan 1, 1964

By F. E. Block, Stephen D. Hill

The necessity for measuring radiation dose is encountered in studying both the beneficial and damaging effects of ionizing radiation on materials . It is also necessary to know the radiation dose absorbed by the reactants in order to evaluate the efficiency of reactions or processes that are promoted by radiation . Thus , a significant effort was made at the Albany cobalt 60 facility to investigate techniques by which the exposure radiation dose can be determined . Methods including ferrous sulfate , ceric sulfate , and methyl methacrylate chemical dosimeters , ion chamber dosimetry , and an absolute radiation calorimeter were investigated . Isodose curves were constructed for several standard source configurations using the dosimetry techniques which were investigated .

Jan 1, 1964

By K. D. Plants, J. H. Holden, L. F. Willmott

Pulverized high- volatile A bituminous coal was gasified with oxygen and superheated steam in a pressure - gasification pilot plant equipped for steampickup feeding . The pilot plant operated satisfactorily at relatively high steam- to - coal ratios , but steam- to - coal ratios could not be reduced much below 0.5 lb / lb without condensation of steam or softening of the coal . Carbon gasified , gas composition , and coal and oxygen requirements were essentially the same as for a pilot plant equipped with a fluidized coal feeder . Average results from the pilot plant equipped for steam- pickup feeding were coal requirement , 37.3 lb/M ( 1,000 ) scf of CO + H₂ produced ; oxygen requirement , 358 scf /M scf CO + H₂ produced ; and carbon gasified , 87.7 percent .

Jan 1, 1964

By R. T. DeWoody, W. C. Miller, W. Chester

Studies were made to determine the effect of the shape of a pneumaticrock- drill exhaust muffler on its efficiency, and the origin and reduction of exit noise from the mufflers. Tests of mufflers of three different shapes proved that the shape is not critical and that a muffler could be incorporated into the shell of the drill. Petal diffusers are beneficial in reducing exit noise but add another projection to the machine. Increasing the number of exit openings while maintaining the same area of exit opening has a markedly beneficial effect on the exit noise and appears to be the most satisfactory treatment.

Jan 1, 1964

By T. A. Henrie, E. K. Kleespies

Electrolytic studies were conducted to determine the transfer rates of the alloying constituents from molten titanium anodes to solid titanium cathodes in molten salt systems . The metals , nickel , tin , copper , bismuth , and manganese , were selected on the basis of thermodynamic data and the melting point of the alloy system . The transfer of nickel , tin , and bismuth was very low . The content of these elements in the cathode was in the range of less than 0.01 to 0.001 percent . The copper transfer was 0.6 to 0.8 weight - percent in electrolytes containing titanium chlorides and 0.12 weight - percent in titanium fluoride salt systems . The manganese transferred at rates comparable to that of titanium . Highpurity titanium and titanium- manganese alloys of uniform composition were produced by electrorefining molten titanium alloys in chloride electrolytes . Comparisons are made between the calculated and the actual quantities of metal transfer .

Jan 1, 1964

By T. E. Green, E. F. Spano, W. J. Campbell

A combined ion exchange X- ray spectrographic method was evaluated for the determination of 11 metallic elements in high - purity tungsten : Aluminum , calcium , chromium , cobalt , copper , iron , magnesium , manganese , nickel , titanium , and zinc . Copper , nickel , and manganese in the 5- to 100 - microgram range ( 1 to 20 parts per million based on 5 - gram samples of tungsten ) , calcium in the 10- to 100 - microgram range , and cobalt in the 5- to 20 - microgram range can be determined within an accuracy of ± 10 percent of the amount present . Limits of detection of these elements are 0.05 to 0.14 microgram . The overall method was unsatisfactory for the determination of aluminum , chromium , iron , magnesium , titanium and zinc in tungsten .

Jan 1, 1964

By E. G. Davis, H. P. LeVan, L. S. Smith

Leaching of a Georgia umber ore when using both ferrous sulfate and pickle liquor was studied in the laboratory . The ferrous sulfate content of the leach solution was the major factor affecting the extraction of manganese from the ore . Time , temperature , and the sulfuric acid content of the leach solutions had relatively little effect on leaching of manganese from the ore ; however , these factors did affect the amount of iron extracted from the umber and/or precipitated from solution . Simulated countercurrent leaching of the ore with pickle liquor containing 130 gpl (grams per liter ) ferrous sulfate ( 48 gpl ferrous iron ) produced a pregnant solution having 16 gpl manganese and 41 gpl iron . Filtration tests of the leach slurries indicated that separating the leach solution and solids by vacuum filtration was impractical , whereas pressure filtration was feasible when the cake thickness was limited to about three- fourths of an inch . Fired pellets of the filter cake yielded a firm , hard product analyzing 56 percent iron and less than 0.1 percent sulfur .

Jan 1, 1964