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By R. A. Beall, S. L. Ausmus

The development of a completely water - free expendable graphite mold material , useful for reactive metal castings , has been detailed . Mixing and curing variables have been evaluated both by physical testing of the material itself and by castings of titanium , zirconium , and hafnium . The blend of powdered graphite , cornstarch , dextrin , cereal binder , linseed oil , and Carbowax -4000 is a successful mix when mulled in a carbon dioxide atmosphere , and properly cured and fired . The primary advantage of this material is its adaptability to standard foundry techniques ; i . e . , core blowing and hand ramming . Temperatures in the curing and firing cycles do not exceed 960 ° C , and no vacuum firing is required .

Jan 1, 1964

By J. B. Zadra, J. M. Gomes, Don H. Baker

Electrolytic deposition at 1,000 ° C in an electrolyte essentially consisting of 7 parts sodium pyrophosphate , 2 parts sodium chloride , and 1 part sodium tetraborate yielded tungsten of 99.9 percent purity . Scheelite concentrates containing 25 to 73 percent WO, and varying quantities of iron , lime , and silica were used as feed materials for the electrolysis . The metal contained less than 0.01 weight - percent each of iron , calcium , silicon , aluminum , carbon , and oxygen . Modification of the electrolyte permitted deposition of equal - quality metal from scheelite concentrates containing higher quantities of iron , calcium , and silica . The electrolytic separation of molybdenum and tungsten was accomplished by minor variations in the operating procedures .

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 K. A. Fowler, L. W. Higley

The effect of uranium on the transformation kinetics and the hardenability of a low- alloy steel was evaluated . Isothermal transformation curves were developed from metallographic studies , and hardenability was determined by standard Jominy end- quench tests . For the steels investigated , the addition of 0.15 weight- percent uranium was found to produce a significant shift in the isothermal transformation curve and caused a related increase in hardenability . These effects diminished rapidly when the uranium content was increased above 0.2 weight - percent .

Jan 1, 1964

By D. Bienstock, J. H. Field, M. J. Lempel

A computer program is presented to perform the detailed and numerous calculations required for determining the interface temperatures and steady - state heat flow through a furnace wall composed of several refractories in layers . A method is developed that will allow the designer to determine the various thicknesses for each refractory layer to minimize either the total wall thickness or the cost of the wall per unit of area . A sample problem is presented and analyzed to illustrate the techniques involved .

Jan 1, 1964

By Alla D. Mah

The energies of combustion of zirconium carbide and hafnium carbide were measured by combustion calorimetry and the heats of combustion and formation. of zirconium carbide and hafnium carbide were derived . The results are-- ZrC AH298.15 ( combustion) = -308.60 ± 0.55 kcal /mole , AH298.15 ( formation) -47.0 ± 0.6 kcal /mole , AH298.15 = HfC (combustion ) = -306.08 ± 0.20 kcal/mole , AH298.15 ( formation) -52.3 ± 0.4 kcal /mole . = INTRODUCTION This report contains the results of calorimetric measurements to obtain the heats of formation of zirconium carbide ( ZrC) and hafnium carbide ( HfC) . The work was conducted as part of a Bureau of Mines program for determining the heats of formation of oxides , carbides , and nitrides by combustion calorimetry . Combustion calorimetry is one of the most precise calorimetric techniques . The chief obstacle to obtaining accurate heat of formation values for carbides , and the chief reason for the variation in the results of different investigators , is the lack of purity of the carbide samples . Corrections for impurities always involve assumptions which lead to uncertainties . In general , a large impurity correction is accompanied by a large uncertainty in the final result .

Jan 1, 1964

By Richard F. Hewlett

An attempt has been made to fit assay data from an underground copper deposit to a three-dimensional polynomial surface as a means of expressing assay points in terms of their mine coordinates by a mathematical equation. The resulting equation was evaluated to predict the grade trend of the deposit. Although the fit obtained by this initial experiment is not considered accurate enough to provide good predictions about the deposit, the methodology is presented in this preliminary report to show the potential usefulness of the technique in mineral deposit evaluation. The technique also should be useful in determining the grade of blocks of ore for production scheduling and blending problems in open pit operations. Further experimentation is needed to increase the reliability of the computer program, to increase the precision of the method, and to make the solution more flexible for use on other mineral deposits.

Jan 1, 1964

By P. L. Woolf, N. Bernstein, M. M. Fine

Continuous experimentation utilizing a 3- by 36 - foot rotary kiln was conducted to demonstrate the feasibility of simultaneous induration and reduction of magnetic taconite concentrate . Lignite , or lignite - anthracite mixtures , and green magnetite pellets (64.2 percent Fe , dry basis ) were heated in a rotary kiln to about 2,100 ° F. After separation from excess reductant , the product pellets were found to be highly reduced and acceptably hard . A total of 140 tons of prereduced pellets with an average Fe content of 79.0 percent was produced at Minneapolis and smelted in the Bureau's experimental blast furnace at Bruceton , Pa . Two additional supplies of prereduced pellets were obtained from The Steel Company of Canada , Ltd. , Hamilton , Ontario , which contained 83.8 and 91.3 percent Fe , respectively . Smelting of prereduced pellets was compared with that of unreduced pellets obtained from The Hilton Mines , Shawville , Quebec , and from the Erie Mining Co. , Hoyt Lakes , Minn . Blast furnace tests established that a substantial decrease in coke rates and higher production result from the use of prereduced pellets .

Jan 1, 1964

By R. D. Berkenkotter

This report describes a weighted method for evaluating the mean and variance of assay data from samples of different length . The method , which produces unbiased estimates from which valid confidence limits can be computed , is appropriate for bedded deposits of variable bed thickness and for vein deposits of variable vein width . Assay data from the bedded Florida phosphate deposit is used to illustrate the procedure .

Jan 1, 1964

By R. V. Lundquist, H. Leitch

The solubility characteristics of three calcium aluminates , 12Ca0 · 7A120½ 3Ca0 A1203 , and 4Ca0 A12 03 Fe2O3 , were determined in water and in solutions of NaOH and Na₂ CO₂ to more clearly define their role in relation to the recovery of aluminum by the lime sinter and the lime - soda sinter processes . The calcium aluminates were prepared by sintering stoichiometric mixtures of CaCO3 , Al2O3 3H20, and Fe 0 at 1,375 ° C. The rates and extent of aluminum extractions were determined . The aluminum extractions from the aluminates were dependent on the presence of carbonate ions in the leach solutions , temperature , time , leach solution composition , and solid - liquid ratio of the slurry . The aluminum extracted from the calcium aluminates in water and in NaOH solutions varied from 4.6 to 22.9 percent . Virtually , complete extraction could generally be obtained for 12Ca0.7A120 and 4Ca0.A12 03 • Fe₂ 03 ; in one instance it was obtained for 3Ca0.A1203 , when an excess of carbonate ions was present over that required for the conversion of all of the calcium in the aluminates into CaCO3 . In some cases of poor aluminum recoveries , extractions could be improved by regrinding and releaching the solid residues .

Jan 1, 1964

By J. A. Ruppert, P. M. Sullivan

A study was made of filtration techniques for recovering the major part of the tin contained in iron - tin alloys known as hardhead . Special smallscale filtering apparatus and a three - stage cyclic process were developed . Eighty- seven percent of the tin contained in an alloy of 82 percent tin and 17 percent iron was recovered as pure metal by pressing at 975° C followed by a second pressing at 800 ° C and a final filtering at 250 ° C. Small amounts of Sb , Cu , and Fe impurities were removed by adding Al to the molten product and performing another filtration at 250 ° C.

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 Francis X. Cannaday

The purpose of this investigation was to find whether the moduli of elasticity obtained were the same for the following methods : ( 1 ) Deformation of a borehole in a prism subjected to uniaxial stress ; ( 2 ) deflection of a thin beam of uniform cross section uniformly loaded ; ( 3 ) sonic - pulse velocity measurements , and ( 4 ) strain measurements on a prism under uniaxial stress . The rock tested was chosen for its good elastic behavior and relatively good homogeneity and elastic isotropism . The same rock was used for all methods . Results indicate that for given environmental and stress conditions the moduli obtained by each of the four methods check one another within the limits of experimental error and that the differences introduced which are characteristic for each method are smaller than physical variations within the rock tested .

Jan 1, 1964

By Louis A. Panek, John A. Stock

A flat slot is created in rock to cause stress relief effects in a pair of hydraulic borehole pressure cells (previously installed in drill holes above and below the slot ) , which act as sensing devices . This relief is annulled by repressuring the slot by means of a flat hydraulic cell . The slot pressure at annulment is taken to be the existing ground stress at right angles to the plane of the slot . A number of trial installations in the rib of a mine drift showed that for a valid determination of ground stress the sensing devices that respond to relief and repressuring must be within a specified zone close to the pressure transmitter ; otherwise the indicated ground stress may be excessive . By using an additional pair of borehole pressure cells , installed a few feet away , the existing rock stress can be redetermined at intervals , irrespective of a change of stress intensity subsequent to the initial installation . Based on these findings , equipment and procedures have been developed that make possible the installation and operation of a permanent rock stress monitoring station for observing mining - induced stress changes . The station consists of a 12 - in - wide hydraulic pressure cell cemented in a flat slot and four 2- by 8 - in flat hydraulic pressure cells in nearby drill holes . All drilling for the installation can be done with an air leg drill and conventional bits . Once the installation is completed , all required information is obtained by Bourdon pressure gage readings . The apparatus is simple , relatively inexpensive , and reliable under operating conditions in a wet mine . Unlike most methods of rock stress determination , this scheme permits periodic remeasurement of absolute rock pressure over several years , without additional drilling or instrumentation . Similar to other flat slot procedures , stress measurements are obtained without making auxiliary tests to determine elastic

Jan 1, 1964

By M. R. Geer

Three coals from the Wilkes on - Carbonado district of Pierce County , Washington , were subjected to washability analyses to estimate the amount and quality of washed coal obtainable . Because the coals were unusually difficult to clean , the washability examinations were supplemented by table tests , tests in dense - medium cleaning units , and flotation tests . None of the coals could be reduced to the desired 10 percent ash by tabling and the response to flotation by two of them was poor . Dense -medium treatment provided coal of the desired quality , but with the most difficult coal the recovery efficiency was lower than usual .

Jan 1, 1964

By H. Kato, G. Asai, R. Blickensderfer, R. Siemens

Some relationships were established among crystallographic orientation , rollability , deformation texture , annealing behavior , slip planes , and ductile- brittle bend transition temperature of molybdenum single crystals . Six large molybdenum single crystals obtained from an ingot melted by electron beam were oriented by X - ray diffraction and rolled on crystallographic planes of low indices in a known direction . During room temperature rolling , cleavage occurred on 100 type planes . At 300 ° C the crystals were rolled to 95- percent reduction in thickness . The crystals ( 001 ) [ 110 ] and ( 011 ) [ 100 ] were most easily rolled . Pole figures were used to correlate the deformation textures of the rolled crystals with the initial crystallographic orientation . Several of the textures which developed could be explained as a rotation about a < 110 > axis of symmetry . The cube crystal ( 001 ) [ 100 ] retained much of its " cubic " orientation . The (001 ) [ 110 ] crystal developed the simplest texture , whereas the ( 211 ) [ 113 ] and ( 211 ) [ 120 ] crystals developed the most complex textures . The 1 - hour recrystallization temperature of the crystal ( 211 ) [ 113 ] was 700 ° C , which is about 300 ° C lower than that of commercial polycrystalline molybdenum . The poles of the slip planes ( as determined from gross slip lines at relatively low magnification ) tended to lie within 20 to 60 degrees of the pole of the rolling plane . The Knoop hardness was slightly dependent upon crystallographic orientation but more dependent upon rolling direction . The ductile- brittle bend transition temperature was dependent upon the rolling orientation and the dislocation density .

Jan 1, 1964

By T. F. Curry, L. B. Berger, H. A. Watson, S. J. Pearce

The conduct of work at elevated air pressures , such as in caissons and in tunnel - driving in subaqueous strata , poses safety problems not encountered in mining and tunneling operations at ordinary atmospheric pressure . This publication discusses some of the problems involved and presents information on the following subjects : ( 1 ) Physiological effects of gases at elevated pressure . ( 2 ) Use of respiratory protective equipment in rescue or recovery operations in event of fire or other emergency in pressurized tunnels . ( 3 ) Effect of elevated pressure on performance of some gasdetecting instruments ; interpretation of the results . Various types of respiratory protective devices are discussed in relation to their possible use at elevated pressures , especially the 2 - hour , selfcontained , recirculating - oxygen - breathing apparatus , which has had wide use in the United States during rescue and recovery work in the mining industry . A modified procedure that eliminates the hazard of oxygen poisoning enabling the safe use of this apparatus at elevated pressures , up to 45 pounds per square inch , gage , and tests to verify its practicability are described . procedure involves control of the partial pressure of oxygen in the breathing

Jan 1, 1964

By Harold M. Smith

The data in this report were prepared to show how Bureau of Mines routine crude oil analyses could be used to evaluate crude oils in terms of common commercial products . The use of Bureau of Mines routine analyses to determine hydrocarbon - type relationships for the gasoline and gas - oil fractions is demonstrated . For this purpose the correlation index , the aromatic profile and the naphthene profile are used to establish reasonably acceptable values for hydrocarbontype relationships . The derivation and meaning of these indications are discussed . These analytical interpretations are applied to a group of high - sulfur crude oils from the Near East , the Permian basin of West Texas , Venezuela , Colombia , California , and other locations , and the resultant data for gasoline , gas oils , lubricating oils , and asphalt are compared by appropriate tables and graphs . Because the Near East crude oils contain higher quantities of paraffins in the gasoline and gas oil ranges , they will yield good , lowsolvency solvents and good kerosine , jet fuel , and diesel fuels , but straightrun gasoline of inferior quality compared to similar products from either West Texas or Venezuelan high - sulfur oils . The Near East oils also should be good sources of lubricating stock . However , when used as stock for catalytic cracking or reforming , the Near East oils suffer by comparison because they are deficient in naphthenes .

Jan 1, 1964

By John Nagy, Henry G. Dorsett, Murray Jacobson

Laboratory studies show that ignition of a dispersed combustible dust in an open vessel may be prevented by adequate inerting . Factors affecting the inerting requirements are -- dust concentration , spark energy , ignition temperature , composition of the substances used for inerting , fineness of dust and type of combustible . The oxygen concentration of the atmosphere and in some instances the proportion of admixed inert powder and moisture required to prevent ignition are given for 367 dust samples . Variations in inerting requirements with strength of igniting source are discussed .

Jan 1, 1964

By R. W. Hiteshue, C. O. Hawk, H. H. Ginsberg, M. D. Schlesinger

The Bureau of Mines studied single - step catalytic vapor - phase hydrogenation of oils derived from coal and oil shale . Treatment of middle oil , from hydrogenation of bituminous coal , gave good yields of gasoline with a German - made molybdenum- zinc - chromium catalyst . The Bureau also achieved good results with duplicates of this catalyst made from domestic raw materials . In one set of experiments with the German catalyst , 38 to 52 wt pct of feed was converted to gasoline . The total liquid product was 91 to 98 wt pct of the feed . Not all this gasoline can be claimed as production , however , because about 20 pct of the feed was in the gasoline range , and part of it undoubtedly survived the hydrocracking treatment . Hydrogenation of crude shale oil in the presence of cobalt molybdate catalyst produced a total liquid product of 89 wt pct of feed . The hydrogenation converted 27 wt pct of feed to gasoline and 44 wt pct of feed to diesel fuel . The remaining liquid product , 18 wt pct of feed , was residue boiling above diesel fuel . The gasoline was of poor quality , with an octane number of 39.1 . The overall product seemed a suitable feed stock for a conventional refining operation . Coker distillate hydrogenation , using a cobalt molybdate catalyst , gave a total liquid product of 97 vol pct of feed ; of this product 60 vol pct was jet fuel and 40 vol pct was diesel fuel . High nitrogen and sulfur in all three of these raw materials severely poison the usual refining catalysts . Thus , the common objective in these

Jan 1, 1964