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By D. K. Deardorff, Laurance L. Oden, H. Kato, M. I. Copeland

The equilibrium relationship of hafnium and tantalum was studied to facilitate alloy and property investigations . The data obtained are presented graphically as the equilibrium diagram . Alloys were prepared from high - purity components by nonconsumabletungsten- electrode arc melting . Data for the equilibrium diagram were obtained by optical pyrometry , metallography , X- ray diffraction of heat treated specimens , X- ray diffraction using a high- temperature camera , and differential thermal analysis . During the investigations , a casting apparatus was constructed , and the existing melting - point apparatus was improved . The bcc allotrope of hafnium forms a continuous series of solid solutions , called beta , with tantalum which exhibit a minimum melting point at 20 wt pct tantalum and 2,110 ° C. At 24 wt pct tantalum and 1,050 ° C , hafnium- rich beta decomposes in a monotectoid reaction to yield alpha and tantalum- rich beta . The monotectoid isotherm extends from 5.5 to 60 wt pct tantalum . The twophase region , in which hafnium- rich and tantalum- rich beta solid solutions are immiscible , rises to a maximum temperature of 1,265 ° C at 38 wt pct tantalum . The solubility of hafnium in tantalum decreases from 40 wt pct at the monotectoid temperature to 20 wt pct at 750 ° C.

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 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 Gus Pantages, Bernard D. Blaustein, Charles Zahn, Irving Wender

Oils from coal hydrogenation have been examined at the Bureau of Mines to learn whether any centers of the optical activity reported in coal would survive catalytic hydrogenation at 450-525 ° C and about 8,000 psig pressure , and , if so , to obtain information about the nature of the active products . Oils from carbonization tars also were examined . Optical activity was found in the majority of the distillate fractions of the hydrogenation oils and in almost all distillates from the carbonization tars . No activity was observed in the tar - acid and tar - base fractions examined . Methods for isolating optically active concentrates included distillation through a packed column , liquid chromatography on silica gel , and adduction with urea . For the materials so processed , the optical activity segregated mainly in the paraffin - naphthenic and the hydroaromatic fractions . Although the specific compounds responsible for the optical activity were not isolated , experimental and spectrometric findings indicate that alkylsubstituted cycloalkane , cycloalkene , and hydroaromatic structures are most likely responsible for the optical activity of the concentrates . The optically active centers probably derived mainly from the steroids and terpenes in the biological materials that participated in the formation of coal .

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 H. O. Poppleton, F. E. Block

This investigation was made to develop a method of preparing high - purity thorium metal in quantities up to 20 kilograms per batch . Several methods for the preparation , purification , and reduction of thorium tetrachloride are discussed . Thorium tetrachloride was prepared by chlorination of decomposed thorium nitrate or oxalate with carbon tetrachloride or phosgene . tion of the crude tetrachloride was achieved by multiple distillations or by filtration of the molten chloride . It was found that high - purity thorium metal could be prepared by sodium reduction of thorium tetrachloride if chloride of sufficient purity were available . Byproduct salts and excess reductant were removed by vacuum distillation , and the resultant thorium metal sponge was consolidated by consumable - electrode or fixed - electrode arc melting . It was demonstrated that metal prepared by this method could be fabricated into bar , rod , or sheet , at room temperature .

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 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 C. J. Walker, Ray V. Huff

The feasibility of inert - gas cushions in underground gas storages was studied by the Bureau of Mines in accordance with a continuing program of cooperative research between the natural gas industry -- through the American Gas Association . As mixing of the inert - gas cushion with the stored natural gas is undesirable , the various mechanisms tending to bring about such mixing were the subjects of both theoretical and experimental studies . These studies indicated the practicability of such cushions is dependent upon both reservoir and operating conditions . Equations and tables of illustrative data relating the various reservoir and operating conditions to the expected time required for undesired mixing to occur in ideal reservoirs are presented . This information permits estimating the relationship of such factors in actual storage operations .

Jan 1, 1964

By M. H. Kersten, G. A. Brady, Jerry W. Ramsey

Anthracite samples were oxidized with nitric acid to prepare products representing intermediate stages of oxidation . Similar oxidizing conditions affected different anthracites to varying degrees as characterized by peptization behavior with 0.1 N NaOH . Techniques used in attempts to separate and characterize the products included esterification , absorption spectrophotometry , sublimation , chromatography , electrophoresis , metal salt formation , and solvent extraction . Mellitic acid , either free or in the form of metallic salts , was identified in the acid- soluble products from 10 tests in which the anthracite was treated with nitric acid for periods varying from 24 to 1,000 hours . pentacarboxylic acid was also found in some products . Other benzene carboxylic acids were not present in amounts detectable by the methods used in this study . The acid- insoluble residue from nitric acid treatment varied significantly in solubility behavior toward different classes of solvents . The most effective ones tried included polar oxygenated solvents and pyridine . Infrared spectra of the extracted material indicated that similar compounds were extracted by the different solvents . Aliphatic amines and aniline peptized the residue and o- toluidine reacted with it . Organic material separated from the residue by peptization with dimethylformamide contained 1 percent ash , consisting of more than 50 percent zirconium .

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 Donald O. Rausch, Robert H. Merrill, David W. Wisecarver, S. Jackson Hubbard

Results are reported for stress - relief borehole - deformation measurements made in three underground openings near open - pit mines in the Ruth mining district , Nevada . A total of 134 deformation measurements were made in 8 boreholes . These measurements determined the regional stresses in the horizons above , below, and at the elevation of nearby open - pit mine floors ; knowledge of these stress conditions is considered essential information relative to certain aspects in the designing of stable pit slopes . The determinations indicate that the stresses in the district are due to the gravitational load of the overburden in a confined stress field .

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 David W. Wisecarver

This report describes a tool to engage and/or place a Bureau of Mines type gage to measure borehole deformation in a horizontal , 1½ - inch - diameter , stress relief borehole . The tool was successfully used at a borehole depth of 105 feet . Practical usage up to borehole depths of 200 feet might be realized . The tool was designed to work inside EX- size ( 1½ - inch ID ) diamond - drill drive casing used as drill rod and through which the deformation gage is guided into an EX- size stress relief borehole . Through laboratory experiments it was found that by exercising a reasonable amount of care the deformation gage could be placed at a point within a ± .01 foot distance of a predetermined depth in a horizontal EX- size hole and that the deformation measuring piston or plunger of the gage could be oriented in the borehole within 0.5 ° of a preselected angle of orientation in a vertical plane .

Jan 1, 1964