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By D. W. Bridges, Donald R. Peterson, Masami Hayashi

Techniques are described for recovering about 80 pct of the cobalt and nickel contained in superalloy scrap by anodic dissolution of the scrap and simultaneous electrodeposition of a pure cobalt - nickel alloy at the cathodes in an electrolytic cell partitioned by permeable diaphragms into separate anode and cathode compartments . Superalloy scrap was alternatively prepared for subsequent anodic dissolution either by melting and casting massive scrap into suitably sized anodes , by packing moderate - sized discard scrap in inert metal baskets that subsequently served as anodes , or after concentrating the superalloy portion of grinding debris , by magnetic separation to reject corundum or other abrasives , slagging any remaining abrasives from molten grindings , and finally casting the superalloy metal into anodes . In the processing , purified electrolyte -- 1 N in NiSO4 and in NiCl₂ , and 0.1 N in CoSO4 and in CoCl2 --was charged to the cathode compartments and discharged from the anode compartments at a rate sufficient to overcome the backward migration of ionic impurities from the anodes to the cathodes . Discharged electrolyte was purified by reacting it first with SO2 and next with limestone , and then recirculated to the cathode compartments , in which a 50 pct cobalt - 50 pct nickel alloy was deposited on either blanks of stainless steel or starting sheets of cobalt - nickel alloy . The process was made self - sustaining by either adding H2SO4 to the catholyte feed to throttle the rate of cobalt - nickel deposition , thereby compensating for the slower rate of cobalt - nickel dissolution from the anode and losses occurring in electrolyte purification , or alternatively , adding H₂SO4 to

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 H. R. Shell, John L. Miller, M. V. Denny

In the mica research program conducted by the Bureau of Mines at Norris , Tenn . , many micas other than silicon fluorphlogopite have been synthesized . It has been well established since the initiation of the program that synthetic micas are important materials useful for their superior or unique properties as well as substitutes for natural micas . The possibility of controlling the physical properties of synthetic mica by isomorphic substitution of other ions in the fluorphlogopite lattice further emphasizes the importance of these materials . Accurate measurement and reporting of their properties constitute an essential part of the research program . The study of germanium fluorphlogopite is in keeping with the requirements of a comprehensive study on isomorphic substitution , specifically to identify precisely the material -- chemically , structurally , and optically . The X- ray measurements , including indexed powder and single crystal data , with a description of the methods used to obtain these data , are provided . 5 Earlier work on germanium mica by R. A. Hatch et al . (5) gave an estimate of the cell parameters from X - ray powder data , but no attempt was made to index the diffraction pattern or to determine the space group symmetry . Later work by E. A. Schatz and J. C. Withers (9) listed X- ray and optical measurements , but no attempt was made to index the mica or determine its symmetry . Roth (7) found that germanium dioxide having the a - quartz structure , when heated with equimolar percentages of MgO , CaO , Sr0 , or Ba0 at 1,235 ° C , formed ABO3 -type compounds , e.g. MgGe03 isostructural with enstatite (MgSiO3 ) . Geo₂ also has a rutile - type polymorph with Ge ++ ions in octahedral coordination . Germanium was substituted for silicon in the serpentine structure by Roy and Roy (8 ) using hydrothermal techniques . These authors wrote as follows : "The substitution of Ge + for Si + yielded a magnesia - germania serpentine , formed easily in euhedral hexagonal plates which in some instances were visible in the light microscope . Electron micrographs and the sharp X - ray diffraction patterns confirm a plate - like rather than tubular habit . " It has been shown in this investigation that substitution of germanium for silicon in the mica structure is readily accomplished without radically changing the characteristics of the mica . Substitutions in the mica structure take place in three locations : Tetrahedral , octahedral , and interlayer positions . The tetrahedral positions are normally occupied by Sit or by a combination of Sit with Al +3 the most common combination being 2A1 +3 and 6Si +4 · , The octahedral position , which has six - fold coordination in phlogopite , contains a larger cation such as magnesium . In muscovite it contains only 2A1 ions ; therefore , this mica is considered a dioctahedral mica , whereas phlogopite is considered trioctahedral . +3 The interlayer position has twelve - fold coordination with six oxygen ions from each of two adjacent tetrahedral silica layers . This is the cleavage plane of the mica and commonly contains the largest cation in the mica structure (e.g. potassium) .

Jan 1, 1964

By Charles H. Atkinson, Robert T. Johansen

Tremendous volumes of petroleum ( crude oil and natural gas ) at present cannot be recovered economically . The feasibility of using nuclear explosions for production stimulation therefore has been investigated . Data from underground nuclear tests conducted by the Atomic Energy Commission were reviewed , and the physical effects were evaluated for stimulating petroleum production . Calculations of the effect on ultimate recovery of increasing reservoir temperature with nuclear explosives showed disappointingly small increases . Production increases caused by fracturing of massive low- permeability reservoirs appear technically and economically promising . Petroleum reservoirs that might be converted from submarginal to commercial production are being located and evaluated as to potential reserves and as a location for a field test .

Jan 1, 1964

By H. D. Hess, C. P. Mabie

This report describes in detail the results of petrographic research conducted on 21 phosphate ores representing important deposits in southwestern Montana , southeastern Idaho , and northeastern Utah . The ores are described and categorized by mineralogical and chemical composition , thermal behavior of organic carbon , and textural constitution . Descriptive and genetic classification schemes applicable to western phosphate ores are discussed ; results from related studies made of the collophane mineralogy are also presented . The latter studies were centered on determining unit - cell dimensions and CO₂ , P2O5 , and fluorine content of collophane concentrates of 11 high - grade phosphate- rock hand specimens selected solely for this purpose . On the basis of this investigation , operational methods have been developed for quantitatively describing textural and compositional features that are likely to be significant in determining the response of phosphate ores to conventional beneficiation treatments ; systems for classifying the ores in relation to these features have been proposed . Studies to date point out distinct textural and compositional variations in the western phosphates and illustrate their importance in determining optimum beneficiation procedure .

Jan 1, 1964

By Robert J. Brennan, Edward R. Navrocky, John W. Buch

In an effort to establish a highly productive mechanized mining system for anthracite beds pitching between 10 ° and 20 ° , for which conventional mobile equipment is not adaptable , the Bureau carried out an experiment in longwall mining using an Anderton- type drum cutter loader and friction - type yielding steel roof supports . The roof- support system proved to be inadequate for breaking the overhanging roof at the break line supports , with the result that the roof broke over the solid coal . The accompanying subsidence destroyed the continuity of the roof in the work area , and the project was discontinued .

Jan 1, 1964

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

Studies on continuous - circuit leach - aluminum precipitation and leachelectrodeposition of mercury were made by the Bureau of Mines to determine optimum conditions and cost estimates for recovering mercury from mercury sulfide flotation concentrates . With 150 grams of sodium sulfide and 50 grams of sodium hydroxide per liter , from 98 to 99.8 percent of the mercury was extracted from flotation concentrates , with about 0.5 pound of sodium hydroxide used per pound of mercury produced . Precipitation of mercury from the caustic - sulfide solution with minus 8 - mesh aluminum shot required about 0.2 pound of aluminum per pound of mercury produced at a cost of $ 0.05 per pound of mercury . Electrodeposition cost with 7 mill power , based on 50 percent current efficiency , was below 2 mills per pound of metal deposited . Feed solutions ranged from 10 to 130 grams of mercury per liter , and current densities , from 2 to 70 amperes per square foot . The cost of open- pit mining 250 tons per day was estimated at $ 1.75 per ton , and flotation - leachingelectrodeposition of the ore , at $ 3.54 , resulting in a cutoff grade of about 0.1 percent mercury . The cost of underground mining 50 tons per day was estimated at $ 20.00 per ton , and the cost of milling the ore was estimated at $ 13.33 , which resulted in a cutoff grade of 0.6 percent mercury .

Jan 1, 1964

By L. B. Pankratz, R. Barany, W. W. Weller

Experimental determinations were made of the heats of formation at 298.15 ° K of cuprous ferrite and cupric ferrite ; the heat capacity of cuprous ferrite was measured over the temperature range from 50 ° to 298 ° K and the entropy at 298.15 ° K was evaluated ; the heat contents of cuprous ferrite and cupric ferrite above 298.15 ° K were measured to 1,500 ° K and 1,100 ° K , respectively . These thermodynamic values were combined with other pertinent data to obtain heat and free energy of formation values at high temperatures . The stability of the two ferrites with respect to their constituent oxides is discussed . Thermodynamic values are included for the decomposition of cupric ferrite to form cuprous ferrite , magnetite , and oxygen .

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 M. E. Kundick, W. E. Dieter, L. Cohen

The major details of design and maintenance of a seamless stainless steel fume hood system , developed by the Bureau of Mines , are described and illustrated . Operating and housekeeping routines are outlined .

Jan 1, 1964

By D. J. Bauer, V. E. Shaw

Bastnasite concentrate was processed to recover total rare - earth content and obtain high - purity ceric nitrate . Reaction of the concentrate with 45 percent caustic soda for 1 hour at 180 ° C in stainless steel vessels resulted in 99 - percent conversion to rare - earth hydroxides . A drying step followed by solution in nitric acid produced a tetravalent cerium fraction amenable to extraction with TBP . Single- stage separatory funnel experiments resulted in 90 -percent recovery of ceric nitrate at a purity of 99.9 percent . Fractional extraction in pressure - bubbler columns resulted in 98.5 - percent recovery of 99.5 -percent - pure ceric nitrate .

Jan 1, 1964

By Albert W. Deurbrouck

This report describes the preparation characteristics of the Pittsburgh and Upper Freeport coalbeds in Hancock , Brooke , Ohio , and Marshall Counties , W. Va . Over 4.5 million tons of coal was produced in these four counties in 1962. Most of this production came from the Pittsburgh coalbed . Twelve coal samples were collected for this study , 11 from the Pittsburgh bed and 1 from the Lower Freeport bed . Two of these samples could be upgraded to produce metallurgical - grade coal . The sulfur content of the Pittsburgh- bed coals was generally excessive --as high as 4.9 percent in the raw coal and 3.19 percent in the float 1.30 specific gravity fraction . The rank of the coals in this area ranges from high-volatile A to high-volatile B bituminous .

Jan 1, 1964

By R. J. Leary, W. M. Mahan, F. X. Tartaron

A new type of apparatus for prerefining molten blast furnace iron and to reduce the cost of subsequent steelmaking consists of a funnel - shaped device lined with firebrick into which a horizontal stream of molten pig iron is directed tangentially at the top . The rotary motion thus induced causes the stream to flatten itself upon the wall and flow in a spiral path to the outlet ; thus , the device was termed " vortex cone .' Oxygen and other refining agents are impinged upon the flowing metal in the cone where reaction is facilitated by the large metal surface exposed and the turbulent flow pattern . Experiments with water in 1 - foot - diameter funnels provided an idealization of the flow patterns to be expected with molten iron . A brick - lined reactor 3 feet in diameter was built for desiliconizing molten pig iron in lots of 1 to 2 tons . At flow rates of 0.3 to 0.5 ton min - 1 (430 to 720 tons per day ) this apparatus was 64- to 90 - pct effective in desiliconization with oxygen efficiencies of 19 to 41 pct . Detailed experiments to develop basic engineering data are underway , and adaptation of this principle to other reactions and reactants is planned .

Jan 1, 1964

By Charles J. Stehlik

This report deals with the changing behavior of mine roof bolt and roof rock as a result of repetitious production blasting . Observations were made in the upper shale production headings at the White Pine Copper Co. room and pillar mine , White Pine , Mich . Roof bolt compression pads and a stratascope were used in the investigations , which were carried out in three separate test sites in which nearly identical procedure produced comparative , repetitive , and anomalous observations . Results indicate roof bolt tension change and roof quality deterioration anomalies were coincident with blasting . The hypothesized cause of the anomalies is a seismic shock generated by the blasts .

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 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 Harry R. Nicholls

As part of the pre- and post - shot mine examination at Project GNOME , acceleration data were recorded underground from a series of chemical explosive shots . The cube root of the charge weight was used to scale acceleration and distance because charge weight was not constant . Regression analysis of particle acceleration - distance data gave the following propagation equation : A W1 /3 = 5.10 x 105 ( R / W¹ / 3 ) −2 .43 The quantity A W1 /3 is scaled particle acceleration expressed in g's - lbs¹ / 3 , and R/W1 /3 is scaled distance expressed in ft / lbs¹ /3 Data obtained from the nuclear explosion were scaled and fall within one standard deviation of the calculated propagation law for the smaller shots . Cube root scaling laws were adequate to group acceleration data from explosive charges varying by a factor of more than 1 x 10 in charge weight and over shot - to - gage distances varying from 100 to 46,000 feet . Data obtained from a series of small tests provided sufficient data from which reliable predictions of acceleration could be made for the large nuclear explosion .

Jan 1, 1964

By R. D. Groves

Laboratory research has demonstrated that high - grade copper powders can be produced under controlled conditions from cement copper products . The technique should enable small producers to prepare a directly marketable product by means other than smelting and electrolytic purification . A continuous drum- type precipitator was the preferred unit for producing fine - sized particles of cement copper that were further processed by chemical digestion in a copper sulfate solution , by reduction and sintering in a hydrogen atmosphere , and by grinding to a powder . The effects of variables related to all stages of the process were investigated . Treatment of leach solutions from three different sources resulted in copper powders containing 99.2 to 99.8 pct Cu , apparent densities of 1.97 to 2.25 grams per cu cm , good powder flow rates , and a size distribution of 54.9 to 60.1 pct minus 325 - mesh material .

Jan 1, 1964

By W. D. Ludemann, E. A. Loria, E. A. Rowe

The isothermal recrystallization of electrorefined vanadium has been studied as a function of annealing time , temperature , and prior deformation . Specimens were cold- rolled from 30- to 75 - percent reduction in thickness , then annealed from 700 ° to 1,200 ° C at time periods ranging from 1 minute to 96 hours . The course of recrystallization was followed by means of hardness , metallographic , and X- ray techniques , and a recrystallization diagram was constructed . Interpretation of the data indicated that there was around 50- percent softening due to recovery ( first stage of softening) before recrystallization began . The defining of recrystallization limits with respect to the amount of deformation was precisely established for electrorefined vanadium . More than 30- percent reduction was necessary for recrystallization to occur at 850 ° C. With 60- percent reduction , it was initiated at 750 ° C and completed at 950° C. The activation energy for recrystallization , as derived from the data , was 95,300 cal per mole for 60 - percent reduction and annealing at 750 ° to 900 ° C. Recrystallization by the mechanism of nucleation and growth was the principal process during the second stage of softening . minor part of the second stage of softening took place as strain- induced boundary migration , which was observed in specimens reduced 30 percent , bent in L- shape , and annealed at 950 ° C. Grain size decreased significantly only with the largest reductions and annealing between 750 ° and 950 ° C. Grain growth was expressed by the empirical relation D = KKtt"" ,, the exponent being the same at 60- percent reduction and annealing from 750 ° to 900 ° C. Accordingly , the activation energy for grain growth was 75,000 cal per mole .

Jan 1, 1964

By Morgan B. D

Since the mid 1950s, limonite deposits of a new type have been found in the northwest of Western Australia. The deposits consist of extensive fossil valley fillings up to several hundred feet in depth, of medium to high grade limonite, frequently containing limonitized fossil wood, and of Mesozoic or Tertiary age. The distribution of the deposits is closely linked with hilly outcrops of Archaean and Proterozoic jaspilite in the headwaters of the old valleys, from which the iron has been derived by leaching, and presumably re-precipitated by a process not unlike that which operates in forming bog iron deposits. Due to the relative resistance of tlie limonite to erosion, the rejuvenation of streams in the area in recent times has left limonitic remnants as mesas up to· several hundred feet above the levels of the present creeks, the courses of which generally are adjacent to or within a few miles of those of the old limonite filled valleys.The Robe River limonite deposits are the largest of this type known and can be traced for approximately 130 miles along the old stream, over 30 sq. miles of limonite remnants remaining at the present time.The present quantity of limonite in this system alone is probably in excess of 5,000,000,000 tons, and the original quantity must have exceeded four times this tonnage when allowance is made for erosion.Some thousands of millions of tons of this material contain in excess of 54 per cent Fe, with approximately 10 per cent combined water. The chief impurities are SiO2 and Al2O3, and minor elements are not present in objectionable amounts. A portion of these deposits was extensively tested by The Broken Hill Proprietary Company Limited (the B.H.P. Co. Ltd.) during 1962-1964. Most of the data presented in this paper are based on the work done on these deposits which are typical of those discussed. The overall problem of the origin of the limonite is discussed. It is apparent that the limonite originates from the jaspilitesof Archaean and Proterozoic age which form the highlands at the upstream ends of the deposits. The iron oxide has been chemically and/or mechanically derived from these jaspilites and deposited by one or more of the following mechanisms.A.-Chemical-sedimentary mainly by biological agenciesB.-Replacement of fluviatile sediments by iron-charged watersC.-Clastic sedimentary processesD.-Lateritization of fluviatile sediments.These various mechanisms are discussed; the authors favour machanismA.Manuscript received' at The Institute, 14th July, 1964.

Jan 1, 1964