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By R. T. Johansen, R. J. Heemstra

In water flooding the gradual accumulation of insoluble materials on the sand face causes the injection pressures to increase while decreasing the amount of water injected . This plugging material often is composed primarily of insoluble precipitates of calcium , iron , and magnesium . Treatment with sodium tripolyphosphate ( STP ) either eliminates or reduces the formation of precipitates . Field tests are discussed showing the almost immediate effects of using STP in the injection water . Methods of treatment , solubility of STP in fresh water and brines , and precautions to observe when starting to treat a waterflood with this chemical are given . Laboratory data show that the preferential wettability of a crude oil for reservoir rock can be reversed by adding a small amount of STP to the flooding water . This reversal in wetting tendency should not only decrease the injection pressures but also increase oil recovery by improving the sweep efficiency of a water flood .

Jan 1, 1964

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

The purpose of this investigation was to develop a wide variety of columbium and tantalum alloys and to determine their suitability for use at elevated temperatures . Sixty - nine columbium and tantalum alloys were investigated . For this study , columbium was alloyed with two or more of the following : nium, tungsten , vanadium , titanium, and zirconium . Tantalum was alloyed with vanadium or hafnium, or hafnium and carbon . The fabricability was determined by an arbitrary procedure . Hardness measurements , elevated - temperature tensile properties , and oxidation- resistance studies were made . Of the alloys studied , Cb - 15 Hf - 5W, Cb - 15Hf - 5W- 10Ti , Cb - 15Hf - 10W- 10Ti , Cb - 10V - 5W, Ta - 30V , and Ta - 20 to 33Hf exhibited excellent high - temperature properties . These alloys were not only easy to fabricate , but they also had good oxidation resistance and excellent high- temperature strength .

Jan 1, 1964

By R. R. Allen

Gieseler plastometer tests were performed on eight western coking coals at retort - immersion depths ranging from 2 to 3-3 /4 inches (measured to the center of the coal charge ) . Increased maximum fluidities were associated with greater retort - immersion depths , the most pronounced increases being observed on highly swelling coals when tested at 3-3 /4 inches . The maximum fluidity of one of these coals when tested at 3-3 /4 inches was 146 percent greater than that observed at 24 inches . Retort - immersion depth had no significant effect on the temperatures of initial softening , fusion , maximum fluidity , end of fusion , and solidification .

Jan 1, 1964

By R. A. Beall, W. E. Anable

The purification of hafnium by electron- beam melting at moderate energy inputs and at low pressures was examined in detail . Most metallic impurities and hydrogen were removed in the first few minutes of operation ; oxygen , carbon , and nitrogen were removed at a slower rate . Samples treated by electron bombardment suffered a small loss of weight and a gradual lowering of hardness . The magnitude of each change varied with the energy input and the duration of the melt . Analysis of the data confirms the loss of oxygen as a hafnium monoxide . Approximate activity coefficients for other contaminants are given .

Jan 1, 1964

By John Nagy, Austin R. Cooper

Information is presented on the pressure and rate of pressure development during a dust explosion . The data were obtained in laboratory studies in a 75- cubic inch vessel with mineral , agricultural and chemical dusts . The factors investigated include dust concentration , oxygen concentration of the atmosphere , admixed inert powder , and admixed moisture . Information is given also on the effects of these factors on the composition of the atmosphere after the explosion .

Jan 1, 1964

By William R. Wayment, David E. Nicholson

A modified percolation - rate test is proposed for use in determining flow rates through hydraulic backfill ; in contrast to the conventional test , a percolation- rate versus void - ratio relationship is established . requirements and a detailed test procedure are described . Equipment Results of a conventional test are compared with those of the proposed modified test . The proposed modified test method yields more accurate , realistic , and usable percolation- rate ( permeability ) data . The significance of obtaining accurate percolation rates for use in analyzing waterflow through hydraulic backfill is discussed .

Jan 1, 1964

By R. W. Hiteshue, R. W. Fridy, W. Kawa

A study of the production of coronene , a high - melting ( 440 ° C ) , highboiling ( 525 ° C) , polynuclear hydrocarbon , was made by the Bureau of Mines to determine the maximum yield obtainable by the hydrogenation of coal and coalderived materials . Experiments were made with anthracite and bituminous coals and with asphaltenes and centrifuged residue obtained from heavy oil produced in a pilot plant by the hydrogenation of a bituminous coal at 2,000 psi and 480 ° C. With anthracite , yields of coronene of 0.5 to 0.7 wt pct of moistureand ash - free coal were obtained at 6,000 to 8,000 psi , 700 ° to 750 ° C , and a residence time of 30 minutes . With bituminous coal , yields averaging 0.4 wt pct of maf coal were obtained at 6,000 psi , 800 ° C , and 30 minutes ' residence time . With asphaltene and centrifuged residue , yields of less than 0.02 wt pct of maf coal were obtained at 6,000 psi , 700 ° C , and 60 minutes ' residence time .

Jan 1, 1964

By W. C. Wahl, M. M. Fine

Leonardite , a naturally occurring , partially oxidized form of lignite with a high content of humic acids , was investigated as a binder for iron ore pellets . Although insoluble in original condition , leonardite forms watersoluble salts with good binding properties when treated with certain alkalis such as sodium hydroxide . Soluble leonardite imparts excellent dry strength to pellets , but green strength is somewhat lower than that obtainable with bentonite . However , green strength can be improved by adding a small amount of calcium hydroxide to the leonardite - concentrate mixture . Leonardite binders were used successfully on three of the four different concentrates tested .

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 C. E. Armantrout, H. Kato, M. I. Copeland, M. Krug

The investigation of the nickel - gadolinium phase diagram was undertaken to determine the alloying behavior of these two metals . The data from meltingpoint determinations , thermal analyses , metallographic examinations , and X- ray diffraction analyses revealed a phase diagram with three eutectic points and seven intermetallic compounds . Very limited solubility of the phases in each other was observed . The five phases , Ni Gd , Ni , Gd , Ni Gd , Ni, Gd , and NiGd¸ , melted incongruently at about 1,300 ° , 1,270 ° , 1,180 ° , 1,070 ° , and 775 ° C , respectively . Ni Gd and NiGd melted congruently at approximately 1,550 ° and 980 ° C , respectively . Four of the compounds were determined to crystallize in the hexagonal system : Ni Gd , Ni Gd , Ni , Gd , and Ni Gd . Ni Gd was determined to be cubic and NiGd , orthorhombic . The crystal system of NiGd was not determined . The eutectic points occurred at 13 , 67 , and 85 wt pct gadolinium , and the isotherms at 1,290 ° , 890 ° , and 700 ° C , respectively .

Jan 1, 1964

By R. V. Lundquist, A. E. Morris, E. L. Singleton

This experimental research was performed to determine rate - of - reaction constants on the MnO - C and Mn , C₂ - 3MnO systems at 1,100 ° , 1,150 ° , and 1,185 ° C. Reactions were conducted at atmospheric pressure under controlled flow of purified helium through the furnace chamber . The weight - loss method defined reduction percentages , and reaction products were identified by X- ray methods . The system Mn0 - C followed a linear reaction rate , and experimental results produced an apparent activation energy of 55.8 kcal per mole of Mn0 . The system Mn, C - 3Mn0 followed a parabolic rate of reaction law and yielded an apparent activation energy of 114.4 kcal per mole for the reaction .

Jan 1, 1964

By M. J. Kovalik, D. E. Wolfson, F. Fischler

Plastometric tests were made to determine the maximum thickness of the plastic layer for different U.S. coals . The effect of test variables on the maximum thickness of the plastic layer was studied . The values for the maximum thickness of the plastic layer were found to be related to the Gieseler maximum fluidity , plastic temperature range , free swelling index , and other plastic properties of coals . Only a general relationship was observed between the plastometric parameters obtained in these tests and the coking properties of coal .

Jan 1, 1964

By W. A. Stickney, J. W. Town

Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .

Jan 1, 1964

By D. A. O'Keefe, M. M. Wong

To obtain beryllium metal of higher purity , flakes produced from electrorefining scrap metal were used as cell feed for a second cycle of electrore fining at 500 ° C in an electrolyte composed of 51.7 mole - percent LiCl , 36.9 molepercent KC1 , and 11.4 mole - percent BeC¹ · Metallic impurities in the flakes totaled more than 108 ppm , the metallic impurities in the metal obtained from the two - cycle electrorefining were , with the exception of 35 ppm of calcium , below the spectrographic determination limits .

Jan 1, 1964

By Thomas C. Miller, Rudolph Sporcic

A relatively simple and inexpensive encapsulated hydraulic device has been developed by the Bureau of Mines to facilitate study of coal bumps , and to measure pressure changes in a coalbed as it is subjected to roof loading during mining . Construction of the device and application techniques are described . Preliminary feasibility tests in the laboratory and field indicate that the device responds satisfactorily to pressure changes in coal created by roof loading .

Jan 1, 1964

By George H. Holmes

Beryllium deposits in the northern Virgin Mountains , Clark County , Nev . , and Mohave County , Ariz . , about 70 miles northeast of Las Vegas , were investigated by the Bureau of Mines . The investigation indicated a widespread occurrence of beryllium- bearing pegmatites within an extensive belt of mica - schist . Several deposits with significant beryllium mineral concentrations were encountered . Only a few of the samples analyzed contained more than 1 percent beryllium oxide ( BeO ) ; in many of the samples , no beryllium was reported . The average tenor of samples from the more important occurrences was 0.25 percent BeO . Chrysoberyl is the predominant beryllium mineral in the pegmatite sills ; beryl predominates in the more massive bodies . Minute quantities of cesium and lithium minerals also occur , but no columbium , tantalum , or other rare minerals were found . Ore dressing tests on a composite sample containing 0.28 percent BeO which was representative of the pegmatite sills , indicated an 85 percent recovery of the chrysoberyl ( 70 percent recovery of total BeO ) by gravity concentration in a concentrate containing 17.6 percent BeO .

Jan 1, 1964

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

A series of economic evaluations of processes for producing metallurgicalgrade alumina from low- grade aluminous materials is being conducted by the Bureau of Mines to determine the relative processing costs . The two processes considered in this evaluation are concerned with the recovery of alumina from clay through the formation of ammonium alum . In the first process , dehydrated clay is leached with ammonium bisulfate solution ; in the second process , clay is baked with ammonium sulfate and then leached with water containing a small quantity of sulfuric acid . After the alumina is dissolved by either of these methods , the iron is reduced to the ferrous state to avoid crystallization of ferric sulfate with the alum . The recovery of pure alum requires two crystallization steps . The alum crystals are then redissolved and precipitated with ammonia to produce alumina hydrate , which is calcined to a - alumina . These evaluations are based on published work , and the proposed plants are designed for a capacity of 1,000 tons of alumina per day . The estimated operating cost per ton of alumina for the bisulfate leaching process is $ 117.06 , and for the sulfate baking process , $ 109.26 . Using a Marshall and Stevens chemical equipment index basis of 240.0 , the estimated fixed capital costs , in the same order , are $ 158 million and $ 146 million . Under current economic conditions , these two processes are not competitive with the Bayer process for the production of alumina from bauxite . Since small improvements will not reduce costs sufficiently to approach competitive costs , future research work with these processes should be confined to areas likely to result in major cost reductions .

Jan 1, 1965

By Howard P. Hamlin, John W. Sweeney

Shales from 14 locations in Indiana were sampled , tested , and evaluated to determine feasibility of producing lightweight aggregates by rotary - kiln and sintering methods . Sampling procedures and the geology of the significant shale units are discussed . Preliminary testing was conducted in a muffle furnace , and continuous tests were made in a 16 - inch by 14 - foot rotary kiln . The aggregate weighed 37.0 to 47.2 pounds per cubic foot . Concrete cubes employing the aggregate were tested to determine the qualities of the concrete . Compressive strength of the concrete using seven bags of cement per cubic yard , after autoclave curing for 6 hours , ranged from 3,600 to 5,850 pounds per square inch . Four samples made suitable lightweight aggregate in the laboratory rotary kiln . Four samples tested by sintering methods made unsatisfactory aggregate .

Jan 1, 1965

By John K. Alley, Robert C. Johnson

The primary objective of the research was to grow aluminum borate whiskers or fibers and to determine their properties . Molten salt bath and vapor deposition methods were used for synthesis . Whiskers exceeding 25 mm in length were grown . The best results were obtained by vapor deposition and most of the data presented were determined on whiskers produced by this method of synthesis . Three different aluminum borate compositions ( 4.8A1203 B₂03 , 3.8A1203 B203 , and 2.5A120, B203 ) were identified by X- ray and chemical analyses . The aluminum borates 4.8A1203 B20, X- ray diffraction pattern was indexed . Optical data were obtained on the three aluminum borates . In addition the following whisker properties and growth factors were determined : ideal atmospheric dewpoint for vapor deposition method , near 65 ° F ; temperature range of whisker formation , 1,000 ° to 1,400 ° C for the molten bath method of synthesis , > 1,000 ° to < 1,400 ° C for the vapor deposition method ; whisker growth rates by the vapor deposition method , maximum 12 mm per hour ; raw material vaporization , 50 to 60 percent of the fluoride lost in 1 hour ; tensile strength , maximum obtained 174,162 psi ; melting points , ranged from 1,675 ° to 1,795 ° C.

Jan 1, 1965

By R. S. Lang, C. C. Merrill

The recovery of zinc from oxidized zinc minerals by the caustic soda leach and electrolytic or chemical precipitation was investigated . With the exception of willemite ( 2 ZnO • Si0₂ ) oxidized zinc minerals were readily soluble in 180 to 240 g / 1 NaOH solutions . A high- grade zinc flake was recovered electrolytically from solutions which had been treated with zinc powder to precipitate copper and lead . Solutions were recycled to the leach stage with a recovery of about 85 percent of the zinc from an ore containing 21.2 percent zinc . Electrolysis was conducted at a current density of 120 amp / ft2 with a power consumption of about 1.5 kwhr /lb zinc . Zinc was also recovered from leach solutions by dilution of the solutions , carbonation of the solution , or the addition of sulfur to boiling solutions . A dilution ratio of 5 : 1 precipitated 59 percent of the zinc in 9 days . Carbonation of the solutions precipitated the zinc as zinc oxide ( ZnO ) and solutions could be recausticized for recycling . Zinc precipitated as the sulfide with sulfur was easily filtered and washed . Approximately half of the sulfur added to solutions was lost in the form of sodium thiosulfate ( Na S₂03 ) .

Jan 1, 1965