Search Documents

By Alex Stewart

Most iron bearing ores treated by the R=N Direct Reduction Process yield products lower in phosphorus than the initial ores. The sulfur is also removed and generally is in the range of 0.02 to 0.05 percent in the final R=N product, independent of the sulfur content of both the ore and carbon fuel used. The mechanism and thermodynamic justification of the principal reactions leading to the removal of both phosphorus and sulfur and the control of sulfur in the iron concentrate produced are discussed and supported by the results of laboratory experiments. In substantially all iron ores (containing up to 4% sulfur as sulfate) and solid carbon fuels (containing sulfur from 1 to 8%) tested, the rejection of sulfur has been in the order of 90-95%, with not more than 0.02 0.05% sulfur in the final metallic iron product. With respect to phosphorus-bearing iron ores ranging up to 0.70% P205, the rejection to tailings has been in the order of 70-95%, resulting in not more than 0.03 - 0.07% phosphorus in the final product.

Jan 1, 1958

By John Chipman, Helen Towers

DEVELOPMENT of a simple radioactive tracer technique for measurement of the diffusion coefficient of calcium ion in liquid slag has already been reported. The investigation was of a preliminary nature designed to explore the possibilities of using radioactive isotopes and to establish a method, and no great accuracy was claimed for the results. It was shown, however, that Ca15 could be used successfully, and the values obtained for the diffusion coefficient appeared to be of the right order of magnitude. However, it was considered that a better technique could be devised for carrying out the diffusion. The experiments were, therefore, continued to find a more accurate method, to check the calcium results, and to extend the investigation to include measurements of the diffusion coefficient of silicon in the same slag. There were two flaws in the original technique. Convection was the cause of too many failures, and the interface between the two slags in the diffusion cell was curved rather than plane, probably due to a surface tension effect caused by the addition of the tracer Ca45 in the form of chloride. Two methods of overcoming these defects were tried. Since it was planned to study diffusion of the short-lived isotope Si"' also, the development of methods was restricted to those which gave promise of being reasonably rapid. Method 1—The principle was identical to that previously used with respect to the diffusion conditions, but there were three differences in technique. Temperature control was more rigid, the tracer was added to the slag as Ca45O rather than the chloride and, finally, an effort was made to translate to high temperatures the elegant method developed by Cohen and BruinV or bringing together the two liquid layers and beginning the diffusion. A master slag was melted in graphite, ground to a fine powder, and analyzed (38.5 pct Ca0-20.9 pct Al2O3-40.5 pct SiO2). The tracer was received as Ca45C12 in an aqueous solution of CaC12 + HC1. From this, calcium oxalate was precipitated, ignited to calcium oxide, and added as such to the slag to give an activity of approximately 5 µc per g. The mixture was then melted into the form of a cylinder 3/16 in. diam and about 1 in. long. A solution identical to the tracer solution without Ca45 was given exactly the same treatment. The resulting Ca40O was mixed with that slag which was to form the tracer-free half of the diffusion cell, and this was likewise melted into a cylinder of the same size. Slag cylinders, two with and two without Ca15, were set in graphite blocks as shown in Fig. 1, and the crucible was lowered into position in the fur-

Jan 1, 1958

By L. C. Brichta

During a study of the Badger-Peacock area from October 1950 to June 1953, the Federal Geological Survey and the Federal Bureau of Mines completed nearly 98 miles of resistivity profiling and drilled 96 test holes aggregating 17,628 feet of bore, In addition, seismic profile measurements were made along 8 traverse lines for an aggregate length of about 16,600 feet. The geophysical surveys were conducted by the Geophysics Branch of the Geological Survey; the drilling was done by the Bureau of Mines. Electrical-resistivity measurements disclosed 21 low-resistivity anomalies and 1 high-resistivity anomaly. Correlation of the resistivity data with the geological information revealed by the drilling disclosed that the low-resistivity anomalies indicated either slumped shale deposits in limestone sinks or undisturbed deposits of shale lying in erosional depressions in the limestone. The high-resistivity anomaly indicated hard, undisturbed limestone at or near the surface.

Jan 1, 1958

By F. A. Forward, A. H. Ross, J. Halpern

IN treating carnotite ores by carbonate leaching it is often necessary to subject the ore to a prior roast. Among the advantages that may result from roasting are: 1) improvement in settling and filtering characteristics of the ore; 2) destruction of carbonaceous impurities that would otherwise contaminate the leach solution and consume carbonate reagent; and 3) substantial increase in extraction of vanadium, which is usually low when the un-roasted ore is leached. Recovery of vanadium may be an important factor in processing carnotite ores, and the fact that vanadium is usually recovered in good yield by acid leaching has often been an economic advantage over results obtained with carbonate leaching. It has been found that response of an ore to carbonate leaching, following roasting, depends primarily on its composition and on the conditions of the prior roast treatment, particularly with regard to the roasting temperature, the atmosphere maintained above the charge during roasting and cooling, and the presence of certain reagents. These factors, especially the last, virtually determine the extractions of uranium and vanadium attainable by carbonate leaching, as well as the reagent consumption on leaching, whereas adjustment of the leaching conditions has only a limited influence. These variables were examined systematically to elucidate roasting and carbonate leaching of carnotite ores and to establish a treatment yielding high recoveries of both uranium and vanadium. Tests were conducted on samples of four different Colorado Plateau ores, described in Table I. Roasting Procedure: The roasting tests were conducted in an electrically heated furnace in which the temperature was controlled to +15oC. The ore (usually a 500-g charge) was ground to —100 mesh, mixed with the desired reagent, and spread in a silica tray to a bed depth of about 1/2 in. During the roast the charge was rabbled at intervals of 15 min. To provide free access of air the furnace was usually ventilated; however, in a few experiments a controlled atmosphere such as carbon dioxide or hydrogen was maintained above the charge. Leaching Procedure: The pulp, generally comprising 500 g of ore and a 2000-cc solution containing 80 g per liter of Na2CO3 and 20 g per liter of NaHCO3, was agitated in an autoclave at 120°C, under 30 psi O2. Samples were withdrawn periodically, and the solution and ore residue were analyzed. Under the conditions employed, maximum attainable extractions were generally achieved in 4

Jan 1, 1958

By W. A. Lang

COAL of sub-bituminous rank underlies much of the plains area of Alberta. This coal is geo-logically young, and occurs in Belly River and Edmonton strata of Up-per Cretaceous age. Generally, the seams are flat-lying, but in some areas they may dip as much as 5 degrees. The overburden, composed mainly of glacial clays and sand-stones, may vary in depth from a few feet to several thousand feet. Recovery of the coal has 'been by drift, slope, and shaft underground mines, and by open-pit stripping operations. Production has been obtained from a large number of mines, most of which have been relatively small and with preparation equipment limited to a loading tipple with screening facilities, and a picking belt where high-ash materials can be removed from the larger sizes. The coal has been sold for domestic and industrial space-heating, for production of process steam, and for power generation. In re-cent years competition from natural gas, propane, and oil has seriously interfered with the production and marketing of sub-bituminous coal, especially with the disposal of the smaller sizes at a realistic price.

Jan 1, 1958

By R. W. Stahl

Coal mining has been revolutionized by the continuous miner. This machine has replaced, or has combined into 1, 3 former operations: Cutting, blasting, and loading. During the 25-year period before this machine was introduced, advances had been made in transportation, but the actual "coal getting" remained virtually the same. As frequently occurs, the multiple-purpose continuous miner introduced a new hazard--more rapid liberation of methane. The coal output formerly obtained from 10 to 20 working places might now be obtained from 1. It is true that circulation of air was generally increased; but the bulk of this machine virtually precludes continuous flow of air across the face, where gas may accumulate. Apprehension about this possible hazard led the Bureau of Mines to test face atmospheres during operation; and Report of Investigations 5288, Methane Buildup During Cutting and Continuous Mining Operations (published in 1956), presents proof that real danger may be present in many otherwise well ventilated mines.

Jan 1, 1958

By Clark B. Risler

Conveyors constitute a critical artery, essential to the successful operation of most ore processing plants. Technological progress is permitting the recovery of metal from low grade ores which previously could not be worked economically. Significant in this progress are improved material handling techniques highlighted by the frequent and successful application of conveyors. From the standpoint of the plant manager the successful conveyors are those he never hears about. They continue to economically transport the loads applied to them, requiring only routine maintenance attention. When such conveyors are subjected to closer scrutiny you will find that they have been carefully selected and engineered to perform the required function under the anticipated conditions. Among the primary elements in a conveyor drive are the electrical motor and the speed reducer. The selection of these elements can be aided by the systematic consideration of several factors. These factors which focus attention on the critical operating conditions, will be individually evaluated and their effect upon the selection of the electrical drive system and speed reducer analyzed.

Jan 1, 1958

By C. B. Kettering

In the early operations of the Inspiration Consolidated Copper Company, which extended from 1914 to 1926, the ore as mined contained principally sulphide copper minerals, manly chalcocite (Cu2S), This ore was milled in a 20,000-ton concentrator and the copper was recovered as a flotation concentrate which, was smelted at the nearby plant of the I ternational Smelting and Refining Company. In those days no attempt was made torecovercopper from any oxide minerals present. As mining operations progressed it soon became evident that the proportion of oxide minerals present would steadily increase, and. it was realized that some method of treatment would have to be developed whereby copper could' be recovered from both oxide and. sulphide minerals contained in the ore. A research program was instituted and after some years of experimental and, pilot plant work a new hydro-metallurgical process was developed whereby it became possible to extract copper from both the oxide and. sulphide minerals in a single leaching operation. The solvent adopted consisted of a mixture of sulphuric acid and ferric sulphate,' Following dissolution, the dissolved copper would be recovered by electrolysis. Also in the process of electrolyzing, spent solutions of sulphuric acid, H2SO4, and. ferric sulphate, Fe2(SOk)3, would be regeneratede and. somade available for continuous reuse. The process appeared to be a success and the decision was made to build a full-sized leaching plant for the future treatment of I spiration mixed ore. Construction was started and the leaching plant was completed in 1926, With the start of ferric-sulphate leaching the Inspiration Concentrator was shut down and, with the exception of a few short time runs has not operated since that time. The ferric sulphate leaching process served. Inspiration well for some 30 years and during that time won a name for itself as a classic example of hydro-metallurgical treatment of mixed sulphide oxide ores. Originally the plant was designed. to process some 7,500 tons per day of a mixed ore containing about 1,2% copper, of which 60% was present as oxide and. 40% as sulphide, Down through the years various improvements were made for the purpose of increasing plant capacity and as well to change the limiting 'factor of sulphide-oxide ratio, The final result was a leaching capacity of 9,600 tons per day when treating a 1% copper ore with a reversal of the sulphide-oxide ratio to 60% sulphide and 40% oxide.

Jan 1, 1958

By William C. Browning

An economic drilling programme is one which costs the !east in chemicals, equipment, and time. The basis for such a programme with rotary drilling techniques is a drilling fluid in which bentonites do not swell. This is recognized in the growing trend toward gyp and other inhibited mud systems. Therefore, even though the mechanism of thinner action is a subject of applied colloid ,chemistry, the understanding of this mechanism is of economic importance in controlling the flow properties of inhibited muds. In phosphate, or sodium tannate, conditioned muds that are relative-!y free of contaminating-electrolytes, the thinner, or dispersing agent, is adsor.bed, ?creating an electrical double layer about the clay particles. The mutual repulsion of these charged particles effects colloidal stabilization, or deflocculation of the suspended clays, as discussed by Norton and others. In inhibited muds, however, the electrolyte concentration in the filtrate is sufficient to collapse the double layer and flocculation of the mud solids occurs, as evidenced by increased viscosity and gel values. Chemicals to control the flow properties of inhibited muds, therefore, are vital to the successful use of these systems as it is not always economical to adjust flow properties by watering back. Flocculation of suspended particles, as indicated in the work of Vervey, Overbeek, and others, is due primarily to gravity-like, long-range Van der Waals forces. Prevention of flocculation may, therefore, be secured by the interposition of any barrier between the particles, the thickness of which approximates the extension of the Van der Waals at-traction. Organic polyelectrolytes, such as Kembreak, Rayf!o, and Q-Broxin, may act to increase the double layer charge when used in small amounts in fresh-water muds. More important, however, is the fact that in inhibited muds an increase in concentration of the polyelecholyte permits the formation of a condensed film adsorption layer of the polyelectrolyte about the clay particle. When this occurs, the extremely viscous condensed adsorption layer creates a mechanical. barrier that prevents flocculation of clays, even in the presence of inhibiting concentrations of elecholytes. Rheological evaluation of the degree of deflocculation, or colloidal stability, may be made by utilizing the known effects of particle inter-action and volume concentration on the flow properties of suspensions. Rheological evaluation should be supplemented by direct microscopic or ultra-microscopic observation.

Jan 1, 1958

By R. R. Wells

This report summarizes the results of laboratory investigations by the Alaska Mining Experiment Station, Juneau, to determine the practicability of treating cinnabar-stibnite ore by bulk flotation and controlled-atmosphere roasting of the concentrate. Ore from the Red Devil mine near Sleetmute, Alaska, was selected for testing; it is typical of ores widely distributed throughout the Kuskokwim River Basin. The material, consisting of stibnite and cinnabar in ankerite, dolomite, and quartz, assayed 1.55 percent Hg and 2.87 percent Sb. Continuous treatment of the ore in a laboratory flotation circuit recovered 95.7 percent of the mercury and 82.6 percent of the antimony in a concentrate that assayed 20.4 percent Hg and 34.6 percent Sb.

Jan 1, 1958

By Frank H. Madison

The percentage depletion deduction on Federal Income Tax Returns under the provisions of the 1939 Internal Revenue Code and of Sections 611 to Section 615, inclusive, of the revenue act of 1954, have created innumerable administrative difficulties, and a new interpretation of "gross income from the property" in that the Courts have expanded the ideas of what constitutes "gross income from the property" to a degree unheard of and unthought of prior to the enactment of these two codes. Originally, under the Revenue Acts of 1917, 1918, and 1920 depletion was allowable, based upon mine valuations as of March 1, 1913; if the mine was owned prior to March 1, 1913; upon cost, as of the date of acquisition if purchased subsequent to March 1, 1913; and upon a "discovery" basis if the mine was discovered after March 1, 1913, The "jab" for mine valuations as of March 1, 1913 and for discovery valuations and depletion was not as bad as it has been made out to be. Thousands of valuations and estimates of reserves were made and agreed upon between taxpayers and Internal Revenue Service engineers and as the years went on the answers have been found to be "reasonable." However, human nature being what it is each case was a battle of wits - of a sort - and many resulted in severe differences of opinion and litigation. As tax rates increased the situation was not bettered. I could talk for several hours on this phase of depletion but it is all past now andwould not give any real service or better understanding of the matter.

Jan 1, 1958

By Hu Harries

WE RECENTLY completed a study for a client, who is an applicant to export gas from the Province of Alberta, on the effects of gas export on Alberta's economy. This study was part of the client's application ?before the Conservation Board, and, no doubt, some of you are familiar with it. Submissions by other applicants in earlier hearings before the Board and before the Royal Commission on Energy, as well as claims made by parties opposing export, have also brought forward a number of other opmwns regarding possible economic effects. Ali of these studies have been on a piecemeal basis. They have dealt with particular aspects of particular applications, and only indirectly and by inference with the overall question of gas ex-port. We have prepared this paper to review the overall picture and ex-amine, as far as time permits, all sides of the question. While the paper is entitled Economic Effects of Gas Export on Alberta, we felt that the area considered should in-elude northeastern British Columbia, not only because Westcoast, the first major gas export project, is essentially a northeastern B. C. project, but because this area has historically been, from the point of view of economic, if not of political, geography, part of Alberta. In this paper, when we talk of export, we mean export from the Province or, in this case, from Alberta plus northeastern B. C. Sales to other parts of Canada have exactly the same effect on the economy of this area as l1ave sales to the United States, provided, of course, they are made on equal terms.

Jan 1, 1958

By M. Clair Smith

This report is one of a series describing exploration, development, mining methods, and costs at United States open-pit mines; the Bureau of Mines prepares and publishes them in cooperation with the mining companies. Their purpose is to promote development and conservation of our mineral resources by disseminating technologic information on mining methods and practices at various United States mines. The exploration, development, equipment, and mining of a large, oxidized-copper ore deposit by open-pit methods, the leaching of the ore with sulfuric acid solution, and the recovery of the copper as cement copper are described herein.

Jan 1, 1958

The polymerisation of silica is found to interfere with thickening of leach pulps at Risdon. Hydroxyl ion and fluoride ion are catalysts for this reaction. Stability may be obtained by the presence of aluminium or ferric iron.INTRODUCTIONAt Risdon it has been a matter for satisfaction that, although the concentration, of silica in leach solutions is appreciable, it has ,given relatively little cause for anxiety.However the margin of safety is small and some intermittent difficulty in thickening leach residues during the last few years has prompted a further investigation, certain parts of which are described here since they may be of general interest.Leaching and ClassificationThe method of leaching which is practised at Risdon has been described in, two previous articles, by W. C. Snow (1936) and S. W. Ross (1949) to whiCh the reader is referred for detail. Continuous leaching is practised, the circuit solution flowing through five air agitated pachucas in series, to tlie first of which calcine is added. The circuit solution, which also enters the first pachuca, consists of spent electrolyte from, the electrolytic cells and contains 90 -gm. of free sulphuric acid per litre. About 80 per cent of the solublezinc oxide is extracted from the calcine in the first pachuca, at a pH value of 1-1 (7 gm.H2S04/1 at 55 to 60°C. In the later pachucas the leaching rate decreases sharply. The leach pulp which leaves the 'last pachuca contains an average of 17 gm. of free acid per litre, corresponding to a pH of 1.7; but, owing to variations in extraction, the end point fluctuates between 2.5 and 0·3 gm. free acid per litre (pH:> 1·5 to 2.5). The average flow through the plant is 1,250,000 gallons per day, which corresponds to a production of 300...

Jan 1, 1958

By Walter E. Lewis

The Cuyuna iron range in Crow Wing County, Minn., is the principal producer of manganiferous iron ore in the United States. The ore is mined from a manganiferous iron formation in the bedrock of the Cuyuna district. This iron formation is divided into two general lithologic types-thin-bedded and thick-bedded. The unoxidized, thin-bedded iron formation is composed of iron silicate with associated fine-grained carbonates of iron and manganese. The thick-bedded iron formation carries iron and manganese oxides with intimately associated silica. Oxidation and leaching of the original iron formation have been the most influential factors in producing manganiferous iron-ore concentrations in quantities large enough to exploit on a commercial basis. The unoxidized and the partly oxidized and enriched iron-formation materials are suitable as a source of ferrograde manganese ore. These materials have been classified according to their amenability to mineral dressing and degree of oxidation and leaching.

Jan 1, 1958

By A. Brown

THIS P APER has been pre-pared as a progress report on Mines Branch investigations into problems of ground stress in certain co al mines of Western Canada. As such, it should be considered as a companion report to the one ( 1) presented to the Mining Society of Nova Scotia in 1956 and which dealt with similar investigations in the coal mines of Eastern Canada. For the past 50 years, dynamic incidents in the form of 'bumps' and 'outbursts' have been occurring in the coal mines of the Inner Foot-hills belt of tl1e Canadian Cordillera. As these phenomena generally become more frequent with in-creased thickness of overburden, a limiting depth of mining of 2,500 feet has been set (2) for estimating recoverable reserves of coal. If such a view were accepted, from a long-term viewpoint very large resources of coking-grade ?coal -in a part of the continent deficient in such coals -would not be available to the nation. The terrain in which these in-6dents take place may be described in geological terms as being dominated by pronounced structure in strata ?consisting of a large proportion of highly indurated rocks. The Geological Survey of Canada has co-operated by carrying out structural studies (3) at the mines, supplemented lithological by stratigraphic observations.

Jan 1, 1958

By W. R. Aufricht, E. H. Koepf

The theory, measurement, and application of capillary forces in reservoir rock have been treated ex-tensively in the various petroleum publications.1,2,3,4 These forces are of prime importance in oil production, and data on capillary properties are among the most important tools used in the study of reservoir mechanics. The principal application of measured capillary pressure data by the production and reservoir engineer is in the determination of the initial distribution and mobility of fluids in the reservoir. The distribution refers to the magnitude of the oil and interstitial water saturations under capillary equilibrium conditions and to their variation throughout the reservoir as a result of changes in rock properties and nearness to free water. The magnitude of the water (or oil) saturation, as well as the porosity, is required in volumetric calculations of oil in place. In low permeability reservoirs, where long transition zones are common, the magnitude of the oil content, even below the depth interval where commercial rates of flow of oil can be obtained, must be evaluated since this oil contains energy available to the production of the remainder of the reservoir. The mobility of the water phase is of particular importance in water-flood calculations since mobile water may condemn what would otherwise be a successful water flood. In reservoirs with predominantly small pores, high immobile water contents are possible. Conversely, reservoirs with predominantly large pores may contain mobile water even though the interstitial water contents are relatively low. This presentation reviews the distribution and mobility of interstitial water contents as determined from capillary pressure data and shows typical data for various types of carbonate reservoirs. A discussion of the variations found in different types of carbonate reservoirs is given. DISCUSSION Interpretation of Laboratory Data Fig. 1 is a typical laboratory capillary Pressure curve where water saturation as Per cent of Pore space is plotted vs capillary Pressure (psig) for an air-water system. This par- ticular curve was obtained by measurement on a sample of San Andres dolomite with intergranular-type porosity. The sample studied had a permeability of 10.0 md and a porosity of 18.8 per cent. The capillary pressure-saturation relationship illustrated is an inherent property of the rock (a function of the size and distribution of the pores) and represents the ability of this water-wet rock to retain water against the pressure differential exerted by a non-wetting fluid (oil or gas) to remove it. In the laboratory a known pressure differential is exerted from a pressure source; in the reservoir the pressure differential is controlled by the density difference between the hvdrocarbons and the water. The laboratory capillary pressure values may be converted into terms of equivalent height of water column using known values of reservoir oil and water density and measured or average values of interfacial tension

Jan 1, 1958

By Harold Bloom

Dimethylglyoxime reacts with nickel in a buffered ammonical-citrate solution containing the detergent ?Aquet? and hyroxylamine-hydrochloride. The resulting nickelous dimethylglyoxime is extracted with xylene. Visual comparison with standards permits the estimation of from 50 to 10,000 ppm of nickel. Soil, rock, or sediment may be decomposed by digestion with (1-3) nitric acid, allowing about 70 determinations per man-day to be carried out. With minor modifications to the above procedure, sediment and soil may be semi-quantitatively analyzed for nickel at the sample site. The chemical equipment is easily portable and the analysis extremely rapid because the buffer, dime thylglyoxime and xylene are added simultaneously to the sample and no heating is required. The sensitivity varies with the "availability" of the nickel ions; under favorable conditions, one may obtain a positive test for as little as 10 micrograms in soils and sediments. This procedure is similar to one, for the field determination of heavy metals described elsewhere by the author.

Jan 1, 1958

By J. A. Chamberlain

DURING a recent trip across Canada and parts of the northern United States, the. writer examined some forty mine models. Construction -details and the uses to which the models were being put were outlined in a report to Eldorado Mining and Refining, Limited, and a specific model was proposed on the basis of the Company's particular needs at their Beaverlodge operation. It was felt, however, that portions of the report would be of some value to anyone contemplating building a mine model. For this reason, a synopsis of some of the more important aspects of the problem is presented here, together with a suggested model type that appears to have wide application. Thanks are due not only to Eldorado for permission to publish the following material, but also to the many mine personnel across Canada who allowed the writer to examine their models and gave freely of their time in discussion.

Jan 1, 1958

By B. C. Raynes

IN the early part of 1952, under the auspices of the U. S. Atomic Energy Commission, Horizons Inc. undertook an investigation dealing with the preparation of high purity thorium metal in order to develop an economically competitive production process for this metal based on a recovery of the metal by a fused salt electrolysis, since a survey of the literature of thorium chemistry indicated that electrolytic methods had not received much attention, despite the consideration that electrochemical production methods often offer attractive commercial potentialities. Thorium metal has been prepared by methods which fall into four general categories: 1) reduction of halides or double halides; 2) reduction of the oxide; 3) thermal decomposition of halides; and 4) electrolytic methods. Some of the important results obtained by various investigators since about 1900 in recorded attempts to prepare pure thorium metal are summarized in Table I. A bibliography of pertinent literature is included in this paper. Thorium is strongly electropositive and possesses a great affinity for oxygen and nitrogen. As a result the prospects for the production of high purity thorium from aqueous media or oxygen bearing compounds are remote. The most promising and profitable area of investigation for production of thorium metal lies in fused salt electrolysis. Thorium has been produced previously by this technique from halide salts in fused alkali chloride eutectic mixtures. Until recently, however, the lack of known large uses for thorium has inhibited the investigation of these methods. The basic problem in an investigation into fused salt production methods for thorium is to develop a suitable fused salt system for the economic preparation of thorium. The first portion of the work in these laboratories was a small scale investigation of the electrolysis of potassium thorium fluoride, KThF5, under a variety of conditions. High purity thorium was prepared in this manner, but the process did not appear to offer the simplest and most attractive continuous commercial operation. The work reported here relates to an all-chloride system employing thorium chloride as the cell feed. ThCL4 was produced as an anhydrous material stabilized in molten sodium chloride. This product, further diluted in NaCl, was subjected to electrolysis. The electrolytic process has been studied in cells capable of holding up to 50 lb total salt charge. Ductile, pure thorium metal has been reproducibly obtained in this operation. Considerable experimentation was carried out in the preparation of ThCL as a cell feed free from moisture, oxides, and other impurities. Thorium was cathodically deposited as a coarsely crystalline powder interspersed with residual bath salts. Aqueous procedures for separating and recovering the metal were developed. The thorium metal powder obtained has been evaluated with respect to its hardness, chemical purity, and certain other physical properties. Preparation of ThC1,—Thorium chloride, and the chlorides of some other metals (aluminum, beryllium, tantalum, zirconium, etc.) cannot be obtained from aqueous solution by direct heating and evaporation. Evaporation and heating of a solution of thorium chloride yields a hydrated salt or partially hydrated salt, and finally Tho,. Anhydrous thorium chloride is obtained by forming a hydrated ammonium chloride complex salt in acidified water solution, dehydrating this compound, and finally decomposing the double salt and subliming the ammonium chloride component. Various methods for the preparation of anhydrous thorium chloride, in accordance with this concept, were investigated as indicated in Table I1 from hydrated thorium chloride (ThCl, . 3H2O), and from thorium oxycarbonate (ThOCO,). In the method found most satisfactory for this work, thorium oxycarbonate was dissolved in an excess of concentrated HC1 to give a clear yellow solution. At least 2 mol NH,Cl were added to the solution per mol of contained thorium. Ammonium thorium chloride hydrate was crystallized from solution by cooling and saturation with HC1. The resultant complex, (NH,Cl),ThCl;xH,O, was dehydrated by evaporation at 130° to 150°C and thoroughly dried at about 250°C. The dried ammanium thorium chloride was then mixed with sodium chloride in proportions to form NaThCL or to produce a ThCL4-NaCl mixture with a given thorium content. The ammonium chloride was sublimed off at temperatures above 500°C in an inert atmosphere furnace to give an anhydrous chloride source electrolyte, essentially free of Tho, and of NKC1.

Jan 1, 1958