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By E. D. Gardner

FIFTY years ago the Utah Copper enterprise at Bingham was just getting under way. An epic in metal mining was in the making. Throughout the West the bonanza deposits were approaching exhaustion and most ore still went direct to smelter. But concentrators were shortly to be constructed for treating milling grade ores, and most important, the pilot plant for the Utah Copper enterprise was being built that year at the mouth of Bingham Canyon. The same decade was to see development at the Inspiration mine in Arizona of the most important new mining method for 50 years to come—undercut block caving. Although the average grade of ore being mined has been declining for 50 years, and wage rates and prices of supplies have been greatly increased, the mining industry has continued to grow and to prosper. Technology has advanced to a point where minerals can be mined under the most severe conditions. The hardest rock can be drilled and broken and the heaviest ground handled. Large or small, an ore-body can be mined successfully, at any desired rate of production. It is possible to pump great volumes of water and to ventilate the most extensive workings; air conditioning has made practicable the mining of ore where the rock temperatures are beyond those that can be borne by man. Mining today in the U. S. is a huge earth-moving operation. In 1953 nearly 2 billion tons of material were mined for direct use or for processing. Stripping at open-cut mines totaled about 1.7 billion cu yd. Table I gives relative tonnages of the branches of the mineral industry in 1953. In addition to the solid materials moved, 350 million tons of petroleum and 340,000 tons of gas were produced in 1953. Fifteen million tons of salt and 5 million tons of liquid sulphur were pumped from wells. An appreciable amount of copper was recovered by leaching old mine workings and dumps. Total value of minerals produced in 1953 was $14.4 billion: oil and gas $7.6 billion, coal $2.6 billion, nonmetallics $2.4 billion, and metals $1.8 billion. Formidable problems face some branches of the industry today, especially pertaining to increased output tons per manshift. The time has come when these problems should be reappraised. With current wage rates, the industry no longer can afford to pay men to do manual labor. It should be recognized, also, that the miner is a skilled worker; efforts to promote the dignity of his calling and his pride of accomplishment have yielded beneficial results. Mineral deposits occur under widely varying conditions. In most instances the degree of support needed by the roof and walls is the deciding factor in selection of an underground mining method. The degree of support needed, in turn, is governed by natural physical characteristics of the ore and its enclosing rocks. Mine operators, of course, learn to judge ground by observation, and an experienced mine boss generally can anticipate what will happen following any given mining operation. A more scientific approach, however, would be advantageous in most cases. More should be known about the strength of the ore and the enclosing rocks, more about stresses set up in the ground when ore is removed, and more about the mechanics of moving ground. Better understanding would work both ways: first, favorable rock conditions could be fully utilized for more efficient mining, and second, hazards of rock falls could be minimized, loss of ore in mining reduced, and expenses caused by ground pressures and subsidence lowered. In general, mining comprises breaking the ore or rock in place, supporting the mine workings, and transporting the ore to the surface. This latter is a materials handling problem. Ventilation, of course, must be provided, and the mines must be kept free of water. Development work at some places is the most important cost item in extracting ore. Drilling and blasting remain the usual practice for breaking ore or rock from place except, of course, at block-caving mines. The drilling and blasting practice at a mine must fit the mining method. In laying out mining procedures attention is being given to

Jan 1, 1956

By J. B. Clemmer, P. E. Churchward, C. Rampacek

A cyclic method for processing manganese ores using sodium sulphate as the basic reagent is described. Sodium sulphate is electrolyzed in a diaphragm cell to give an anolyte-containing agentisdescribed.Sodiumsulphuric acid and a catholyte-containing iselectrolyzedincaustic soda, a part of which is carbonated in a cyclic manner to form soda ash. The reduced ore is leached with the anolyte to dissolve the manganese and the impurities are precipitated by addition of catholyte. Manganese in the pregnant todissolvethemanganeseandtheimpuritiessolution is precipitated as synthetic rhodochrosite with a carbonated catholyte, and sodium sulphate is regenerated. Calcining the manganese carbonate gives a high grade product and the carbon dioxide is returned to the carbonation step. The results of laboratory tests using cells equipped with synthetic-fiber diaphragms and permselective membranes, which permit transfer of anions or cations during electrolysis, are described. A METHOD which has been considered for pro-cessing manganese ores under emergency conditions to recover a product suitable for smelting to ferromanganese involves reductive roasting of the ore for leaching with dilute sulphuric acid followed by precipitation of the manganese from the purified pregnant solution with sodium carbonate. Although the process is operable and involves no novel or untried steps, it is noncyclic in regard to reagents. Research seemed warranted to determine if a cyclic process could be developed by electrolyzing the sodium sulphate formed during precipitation of the manganese with soda ash to regenerate sulphuric acid and sodium hydroxide. Reduced ore would be leached with acid anolyte to dissolve the manganese. The iron, alumina, and other dissolved impurities would be precipitated with the caustic catholyte, and the manganese in the purified pregnant solution would be precipitated as artificial rhodochrosite with carbonated catholyte to regenerate simultaneously sodium sulphate for electrolysis. Waste boiler gas and CO, from calcining the manganese precipitate would be recycled for carbonation of the caustic catholyte. There is a surprising lack of data in the technical literature on diaphragm electrolysis of sodium sulphate. One of the more comprehensive papers, by Atwell and Fuwa, describes the problem involved in electrolyzing byproduct sodium sulphate from the viscose process with particular regard to the design and operation of asbestos diaphragm cells. Frisk' also investigated electrolysis of sodium sulphate from viscose-spinning baths to recover caustic soda and sulphuric acid. The objective in these investigations was to produce, by electrolysis and evaporation, a concentrated caustic-soda solution and a sulphuric-acid solution low in sodium sulphate. Because of these requirements, the process was not too attractive despite a favorable yield of caustic and acid with a reasonable power consumption. Because strong acid and base are not required for processing manganese ores and nonelectrolyzed sodium sulphate is not objectionable in either reagent, the present problem was somewhat simpler than that of these investigators. The purpose of this report is to summarize briefly the results of laboratory electrolysis of commercial sodium sulphate in diaphragm cells of different types and the application of the acid and caustic for processing manganese ores in a cyclic manner. Electrolysis in Permeable Diaphragm Cells The principal problem in electrolyzing sodium sulphate in a permeable diaphragm cell is to prevent mixing of the acid and base formed in the anode and cathode compartments. It is not enough to separate the anolyte and catholyte by a single diaphragm. A three-compartment cell in which the sodium-sulphate solution is fed to the center compartment and flows through the permeable diaphragms to the anode and cathode compartments is more efficient electrically. Diaphragms should be porous enough to allow flow of solution to outer compartments but tight enough to prevent gross mixing of the anolyte and catholyte. In addition to being resistant to acid and alkali, the diaphragms should offer minimum resistance to the flow of current. It is also important that the electrolyte contain a high concentration of sodium sulphate to furnish an abundance of sodium and sulphate ions and thereby decrease the current carried by hydrogen and hydroxyl ions. A practical limitation of sodium-sulphate concentration is imposed by the decreased solubility of sodium sulphate with decreasing temperature. At 20°C, a concentration of 200 g per liter sodium sulphate can be maintained. Little is gained in conductivity by using a concentration greater than 200 g per liter. The small-scale continuous electrolysis tests were made in a 12x12 in. open-top bakelite cell equipped

Jan 1, 1956

A hard lump char containing only 4 to 5 per cent ash, 0·25-0·30 per cent sulphur and a trace of phosphorus has been produced from Latrobe Valley brown coal by slow drying and carbonization of ordinary industrial briquettes at temperatures between 7000 C and 14000 C. The briquette char can be made with a variety of reactivities by varying the maximum temperature of carbonization; the higher the temperature, the lower the reactivity. The strength of the fuel compares favourably with metallurgical coke made from black coal, though it may not be quite so resistant to abrasion. Experiments in a small experimental cupola indicate that it will make a satisfactory fuel for use in iron foundries. It may also find extensive application as a smokeless fuel in other branches of industry and in household heating appliances.INTRODUCTIONVictoria, like South Australia and Western Australia, is apparently without 'significant deposits of black coal of coking quality but there are huge reserves of brown coal of high moisture content (60-66 per cent) in the Latrobe Valley (well over 20,000 million tons have been proved) and there are other important deposits in the south central portion of the State (Herman, 1952).For three decades Victorian industries, including a few metallurgical firms, have been using the briquettes made at the Yallourn factory of the State Electricity Commission of Victoria (S.E.C.). These briquettes, having a moisture content of about 15 per cent and a calorific value of approximately 9,500 B.T.U. per pound, are satisfactory for certain grate-type furnaces but they are not suitable for use in cupolas of other shaft furnaces because they disintegrate badly on rapid heating.

Jan 1, 1956

By J. A. Rowland

Magnesium alloys containing nickel, nickel and manganese, lithium, lithium and manganese, and lithium and aluminum were investigated. Melting, casting, and mechanical working techniques and the heat treatment of various compositions were studied. Amenability to cold and hot working was shown for many compositions. The magnesium-nickel and magnesium-nickel-manganese alloys failed to develop superior mechanical properties and were very low in resistance to corrosion. The magnesium-lithium series, although entirely plastic, had low strength properties. The addition of small amounts of aluminum to the Mg-Li base did not affect greatly either the ductility or the strength; further additions developed increased strength, but only at room temperature, and the alloys became brittle with age. Continued study, concentrating on the ductile lithium-rich beta phase as a base composition for ternary and quaternary systems, is recommended.

Jan 1, 1956

The construction of mine headframes of reinforced concrete is not a new departure as many structures have been built of this, material particularly in Canada and South Africa. This type of construction has been satisfactorily tested in service and is now accepted by the mining fraternity.The two headframes at New Broken Hill Consolidated Limited are the first structures of this type to be built in Australia, and provide an interesting application of reinforced concrete design and construction.Reasons for Adoption of ConcreteDuring 1947 the writer visited D.S.A. and Canada and inspected three headframes, of reinforced concrete construction.Leading details are as follows:(i) Hollinger Gold Mines. (Timmins, Ontario) : Height of sheaves 110 ft. Shaft has provision for 4 skips each of 12,000 lb. capacity. Structure incorporates surface crushing plant.(ii) International Nickel Corporation-Murray Shaft (Sudbury): Height to sheaves 153 ft. 6 in. Shaft provides for 2-12 ton skips and 2 cages. Surface crushing plant built integrally with frame.(iii) Asbestos-Johns Manviae (Quebec): Height of sheaves 116 ft. Shaft provides for 2 skips 200 cu. ft.

Jan 1, 1956

By Foster Fraas

The electrical conductivity of minerals increases with increase in temperature as a result of the thermal activation of the electrons. Some oxidizable minerals have a change in the stoichiometric proportions after heating in air, and the conductivity does not return to the original value after cooling. Similar changes occur in reducing atmospheres. Other minerals, such as carbonates and hydrates, are completely decomposed. Electrical resistivity measurements on single particles when compared to standard separation measurements show that minerals having resistivities above 1013 ohms respond as nonconductors. Those below 1011 respond as good conductors.

Jan 1, 1956

By M. E. Volin

To extend or delimit the known ore reserves of the Black Wonder manganese de-posit, the Bureau of Mines undertook an exploration project consisting of trenching, underground excavation, long-hole drilling, and sampling. The mineralization is spread over 6 square miles containing numerous small individual manganese deposits. There has been only small production from some of these deposits; however, simultaneous operations from many such small deposits could contribute considerably to the production from the district. A custom mill to treat oxide ore for battery use was built near Patterson in 1942 by the General Dry Batteries Co., Inc. It operated during World War II and was removed in 1944 when the manganese mines ceased operation. Except for some small experimental shipments, there has been no activity in the district since that time.

Jan 1, 1956

By T. L. Joseph, G. Bitsianes

The gaseous reduction of dense iron ore is a topochemical process in which reduction takes place at distinct interfaces between solid phases or layers. Under normal conditions, these interfaces remain parallel to the exterior surface of the ore body as they move inward. Certain conditions, such as cracking, high porosity, impurities, entrapped residual oxides, may cause departures from normal topochemical behavior. THE gaseous reduction of dense iron ore proceeds at interfaces between several solid phases or layers.',' Under normal conditions, these interfaces progress inward and remain parallel to the exterior surface of the ore body. This topochemical behavior is clearly illustrated in Fig. 1 which shows partially reduced specimens of natural and synthetic hematite. Using a coordinated sequence of macro, micro, and X-ray examinations, the authors1-'2 found that the number of interfaces and participating phases was in agreement with the Fe-0 system. Above 570°C, reduction of the ore involved a maximum of three common boundaries between four solid phases: iron, wiistite (Fe,O), magnetite (Fe,O,), and hematite (Fe,O,). Below 570°C, reduction proceeded through two interfaces between three phases: iron, magnetite (Fe,O,), and hematite (Fe,O,). The decrease in the number of phases below 570°C was due to the instability of wiistite below this temperature. The sequence of phases was also consistent with the equilibrium requirements. For example, the layers of iron oxides that were formed in topochemical fashion were always orientated in the order of increasing oxygen content. Thus, in Fig. 1 an outer layer of metallic iron is followed in turn by a thick intermediate band of black wiistite, by a thin layer of light magnetite, and finally by a relatively large core of hematite. This arrangement of the oxide layers was due to restrictions in reducing conditions which were imposed by the physical structure of the solid. The highly reducing gas on the outside of the particle gradually lost its reducing power as it penetrated into the specimen. On a macro scale, the layers of the various oxides appeared to be sharply defined and uniform in composition. Microexamination of the sections, however, revealed that the interfaces did possess measurable widths which varied with the porosity and chemical activity of the oxide phase undergoing reduction. For example, Fig. 2 shows three interfaces in a dense hematitic ore which was partially reduced at 850°C. At the iron-wiistite interface where the greatest porosity developed, the reaction proceeded over a zone 25 to 30 microns in width. Toward the interior, the interfaces became progressively narrower until at the magnetite-hematite boundary the reaction zone was about 1 micron wide. In this region the structure was exceedingly dense; the hematite possessing a porosity on the order of 3 pct. A careful micro study across polished layers of the various oxides revealed generally homogenous and single-phase structures. As reported in a previous paper,' the wiistite layer was characterized by an increase in oxygen content with depth of penetration. The topochemical behavior of reduction was studied in six types of ore of different origin, composition, and physical structure. In most cases, reduction proceeded at the boundaries of well defined layers or phases, and this behavior may be regarded as normal for most dense fine grained ores. Deviations from Ideal Topochemical Behavior A number of deviations from the normal topochemical behavior were noted. In these cases, the continuity of the reduction interfaces was disrupted in one of four ways: 1—Cracking of the specimen interrupted the geometric configuration, and the interfacial advance was no longer parallel to the exterior surface. 2—As a result of high porosity, the interfaces were spread over an appreciable distance and all but obliterated. 3—Impurities in the ore promoted a variety of deviations, including cracking. 4—A residual oxide phase was entrapped in the reaction product and left behind the advancing macro interface. Results from Cracking: A crack leading into the interior of an ore specimen presents a path of least resistance for the counter-flow of reducing gases and gaseous reduction products. Higher reducing conditions can be maintained along such cracks and reduction accordingly will propagate well ahead of the normally advancing reduction interfaces. Cracking was caused by a number of factors, one of which was the thermal spalling of impurities in the massive form. A more general type of cracking was due to reduction and was found in all dense varieties of natural and synthetic hematite, particularly in the temperature range of 500" to 700°C. The effect is shown clearly in Fig. 3. In this case, a dense sphere of pure hematite was partially reduced at 650°C for 100 min. The macrosection shows that one large reduction crack had penetrated the specimen and disrupted the normal topochemical advance of the interfaces. The outer layer of iron was only slightly affected but the thin dark layer of wiistite, adjacent to the ferrite, had widened perceptibly as it progressed along the crack. Farther inward, the magnetite layer was greatly disrupted and had penetrated irregularly to form islands of unaltered white hematite. A great deal of internal cracking is evident in the magnetite phase. From a practical point of view, the cracking of dense ores in the blast furnace could lead to desirable as well as undesirable effects. The general result

Jan 1, 1956

By R. O. Pynnonen

This circular is a study by the Bureau of Mines of 346 accidents in underground iron-ore mines of the Lake Superior district from June 1949 to August 1954. These accidents caused 354 lost-time injuries, including 28 fatalities and 2 permanent-total disabilities. The accident reports were analyzed by the Bureau to show the causes of injuries and the time charges and unsafe practices or conditions that caused the accidents. Also shown are the times of occurrence, ages of the injured by job classification, and experience of the injured in mines and on the job being performed when hurt. Detailed information is presented on approximately 14 percent of the total number of Lake Superior district underground mine accidents that resulted in lost-time injuries during the period covered. These facts are presented to aid accident-prevention measures in underground mines and as a record for measuring future safety accomplishments.

Jan 1, 1956

By Stephen Krickovic

AS it is commonly understood in the bituminous coal mining industry, pillaring means removal, as completely as is practical, of all pillars formed in the development of headings and rooms on first mining. The degree to which this can be accomplished, termed percent of recovery, is of course dependent generally upon the physical conditions of the bottom and the overburden, the system of min-

Jan 1, 1956

By K. B. Higbie

The quantitative separation of tantalum from columbium has been obtained through several liquid-liquid extraction processes. The valuable metals are separated by selective extraction from organic feed solution using a mineral acid or by selective extraction from aqueous feed solutions employing an organic solvent. The greatest degree of separation was obtained when organic ketones, particularly methyl isobutyl ketone, were used. Approximately 200 combinations of various organic solvents and mineral acids were tested as possible separation systems in which the tantalum or columbium content was extracted from organic solutions of the anhydrous pentachlorides.

Jan 1, 1956

By F. W. Wessel

This report summarizes Bureau of Mines laboratory tests of four tungsten¬-bearing materials of various grades, The test work has demonstrated that the dry reaction between sodium carbonate and scheelite is best conducted at 900° C. or a few degrees less. The sodium carbonate requirement, in addition to the stoichiometric equivalent of the scheelite, is in some inverse relationship to the grade of tungsten in the ore. Residence time and particle size exert a definite but minor control on the reaction. Pressure-digestion tests on an impure concentrate indicate the technical feasibility of extraction by this process. INTRDUCTION Over 100 years ago Oxland discovered that tungstic oxide could be removed from wolframite and converted to a soluble form by reacting the mineral with a soluble alkaline salt at elevated temperatures. He patented this discovery, and this patent 4/ since has been the basis for most tungsten extraction. Much literature exists on this process and its modifications, and the characteristics and possibilities of the reaction are quite well defined.

Jan 1, 1956

By Louis A. Panek

The practice of roof bolting or rock bolting to stabilize rock surrounding underground excavations has increased tremendously within a few years. This widespread application has led to many questions concerning the mechanics of bolting and has pointed up the need for a quantitative method of designing bolting systems. To answer these questions a research program was initiated to determine the principles of roof bolting. The first problem chosen for investigation was the use of bolts to reinforce bedded roof, since the great majority of bolts are used under these conditions. The attack employed is a combination of theoretical and experimental stress analysis. Centrifugal testing of models was chosen as the experimental method because it is particularly suited to the study of stratified roof. This report describes the models, the experimental method, and the model-prototype relations. By using dimensional analysis, a general expression for a roof-bolting design formula in terms of the structural variables has been obtained. Certain model-prototype similarity requirements have been relaxed, thereby minimizing the number of variables to be studied and extending the applicability of quantitative test data to a large class of full size structures.

Jan 1, 1956

By A. L. Engel

Production of chromite in California has been from many small, high-grade mines. The opening of the Purchase Depot at Grants Pass, Oreg., in 1951 has stimulated chromite mining in California, and a large number of properties are being reexamined as there is a possibility that some low-grade ores from many of these properties can be beneficiated to meet the purchasing schedule. The Bureau of Mines in its program of conservation is continuing ore-dressing tests on chromite ores to better evaluate their potential. This report is a compilation of preliminary concentration tests on samples from five different properties in California. The concentration tests were made on ores from the David mine, Butte County, the Seiad Creek mine, Siskiyou County, the High Plateau mine, Del Norte County, Bud's mine, Tuolumne County, and tailings from the Miller concentration plant in San Luis Obispo County, Calif., to determine the possibility of beneficiating these ores so that they will meet the specifications for the Government stockpile.

Jan 1, 1956

By W. L. Dare

This information circular is one of a series the Bureau of Mines plans to publish describing the methods and costs of mining uranium on the Colorado Plateau. The Big Buck mine is one of the larger underground uranium-vanadium ore mines on the plateau. The mine is about 39 miles southeast of Moab in the Big Indian mining district, San Juan County, Utah. The Big Buck claims were located late in 1947, when uranium mineralization was discovered in the Cutler formation at its outcrop along the escarpment that forms the west side of Big Indian Wash. Charles A. Steen made the first major discovery of uranium ore in the Chinle formation in the Big Indian mining district on July 6, 1952, when 14 feet of high-grade uranium ore was encountered in a diamond-drill hole drilled on his Mi Vida claim. The Big Buck ore body now being mined by Standard Uranium Corp. is a southeast extension of Steen's original discovery.

Jan 1, 1956

By C. E. Lesher

Two processes for agglomerating fine sized ores with low temperature coke are described. One process (Orcarb) agglomerates ores with limited amounts of carbon; the other (ore-carbon pellets) pelletizes fine sized ores, using low temperature cokes as the binder. Data are presented on the products obtained when taconite, magnetite, and hematite concentrates and several titanium oxide ores were used. REDUCTION of finely divided oxide ores has long been a major metallurgical problem. Various methods of agglomerating, notably briquetting, sintering, nodulizing, and pelletizing, have been developed and are in industrial use. Carbon is the usual reducing agent for oxide ores and attempts have been made to agglomerate fine ores with coking coal in order to get the metallurgical advantages of intimate contact and increased particle sizes suitable for subsequent smelting or reduction.1-3 For the past three years, research has been in progress on two processes for combining fine sized ores with reactive carbon in the form of low temperature coke. By one process, designated Orcarb, the ore is coated with coke carbon in amounts limited to that required for reduction and the result is an appreciable but limited increase in product particle size over that of the original ore. The second process, called ore-carbon pellets, produces pellets of fine ore bound by low temperature coke. The first objective was to develop a process for combining an oxide ore with only enough carbon for its reduction, the amount being that derived from the simple reduction equations. The carbon (that amount theoretically required for the reduction of the oxides in an agglomerate with ore), calculated to CO, ranges from 10 pct for zinc calcines Or phosphate Ores to 21 pct for rutile and 26 pct for silica. The carbon required for reducing iron oxides falls between the extremes—10 and 26 pet' When the carbon in the agglomerate is low temperature coke, reduction by hydrogen may be expected to take place, thus modifying the calculated carbon require- ment. On the other hand, in practice, an excess of reducing agent over that required in theory is normally used. Screen sizes of three iron ores on which the greater part of the experimental work was performed are given in Table I. Most of the testing was done with Freeport (Renton Mine) coal, but Pittsburgh and Elkhorn bed coals were also used. The first objective was to agglomerate the ore with sufficient low temperature coke to provide carbon for reduction, i.e., in the range from 10 to 25 pct. This was accomplished by preheating the ore, mixing with pulverized coking coal, and completing the coal carbonization in a plain steel rotating retort. The pilot retort, as it is now constituted, is shown by diagram in Fig. 1 and photograph, Fig. 2. Ore is fed into the upper kiln by a screw; it is heated to 900° to 1100°F by direct flame and it is then discharged into an insulating hopper from which it goes

Jan 1, 1956

By T. E. Evans, C. T. Baroch

ZrB2 was produced in batches of 4 to 6 Ib by interaction of ZrO2, B4C, B203, and carbon at around 2000°C in a simple graphite resistance furnace. Techniques of production are discussed and the final design of a suitable furnace is described in detail. Several other borides were made by the same technique and the process appears to have possibilities for commercial production. N seeking out new hard and refractory com- pounds, many researchers have turned to the investigation of the borides and excellent papers have been published on the properties of these compounds. Few papers, however, have appeared on the techniques and problems concerned with the production of these high temperature substances. This report describes progress made in developing a method for preparing zirconium diboride, ZrB2, on a pilot plant scale. The literature of the borides and other refractory hard metals recently has been reviewed, annotated, and classified so completely' that it is needless to attempt such an outline here. It is enough to say that three borides of zirconium have been reported: ZrB, ZrB2, and ZrB12.2 ZrB2 is the most stable of these and is especially stable in the presence of carbon up to and including its melting point of around 3000°C. Like most borides, it can be prepared in several ways. It can be prepared by synthesis of the elements, but these are expensive and difficult to produce in a high state of purity. Obviously, production directly from the oxides would have decided economic advantages. In electrolytic production such as that of calcium boride,:' the product is recovered as a sludge mixed with electrolyte; and separation of product from adhering electrolyte and regeneration of the electrolyte is an involved and difficult process. The work on borides was started on a small scale in 1948. Late in 1949, Naval Ordnance expressed a specific interest in ZrB2 and the project then centered on this compound. After the usual experimental work necessary in a new field, ZrB2 of good quality was produced by heating mixtures of B4C, ZrO2, B2O3, and carbon to a temperature of about 2000 °C in a resistance-type electric furnace. Over 100 lb was made for experimental use tests, and the method of production probably could be expanded into a commercial operation. A similar process has been described by Kieffer and coworkers.' The main chemical problems were the development of proper charges to insure complete reduction of the elements, determination of the proper temperature range at which these reductions took place, and adoption of techniques necessary to pre- vent inclusion of such impurities as carbon and nitrides. The mechanical problems consisted of developing a simple practical furnace that would attain the high temperatures required and permit use of a controlled atmosphere when necessary and determining of suitable refractories. Both problems were solved by designing a crucible resistance furnace. Crucible Resistance Electric Furnace Attempts were first made to produce ZrB2 in an electric arc furnace, but such a furnace would not provide the degree of carbon control required for producing clean graphite-free borides, so it was decided to try working in a crucible. Obviously, the furnace would have to be constructed of graphite, as the temperatures required are too high for other refractories or heating elements. Crucibles were made by hollowing out segments of graphite electrodes, which were fitted with a cover and clamped between two electrodes so that the current passing through the thin wall of the crucible would generate heat, using the principle of the Helberger crucible furnace."? Preliminary tests with this type of furnace were encouraging and led to the furnace design shown in Fig. 1. The essential components were a thin-walled graphite crucible resting on a graphite block, which formed the lower electrode assembly, and a top electrode assembly swung from a pipe column making contact with the top of the crucible. The space around the crucible was filled with graphite prepared from waste electrodes crushed to about ¼ in. This packing had excellent insulating properties, both electrically and thermally, and could be removed easily and quickly from around the crucible by means of an industrial vacuum cleaner. The largest resistor crucibles were machined from 8 in. electrode stock and were 26 in. long, with a side wall Yi in. thick and a 1 in. bottom. Temperatures were determined optically by sighting down a 1 in. hole drilled longitudinally through the top electrode and the crucible cover. Sealing this hole at the top was a water-cooled brass sight-glass assembly, shown in Fig. 2. An opening was provided for a light flow of helium to keep the sight opening clear of smoke, and a glass prism above the sight glass changed the line of sight to the horizontal for easier reading. More recently, the prism and optical pyrometer were replaced by a photoelectric recording pyrometer. At first the charges were placed directly in the resistor crucible but this meant that everything had to be withdrawn from the furnace every time the charge was emptied. Later, smaller crucibles were made up that could be placed inside the resistor

Jan 1, 1956

By R. H. Nielsen

A new, cheaper precipitation scheme has been developed to produce purified zirconium oxide, Technical-grade sulfuric acid is used to precipitate a basic zirconium sulfate from a hot dilute hydrochloric acid solution. With close control of temperature, pH, and zirconium - sulfate ratio, excellent purification and complete zirconium recovery can be attained. The process has been successfully applied for 3 months and has proved to be a more satisfactory procedure than the ammonium phthalate process used previously. INTRODUCTION The Northwest Electrodevelopment Laboratory of the Federal Bureau of Mines has developed and improved the Kroll process for the production of pure ductile zirconium and hafnium. metal. Since 1946 over 1 million pounds of zirconium sponge metal has been produced, mostly high-purity material for the Atomic Energy Commission

Jan 1, 1956

By E. L. Garton

Bureau of Mines routine crude-oil analyses of 88 samples from 60 fields are presented in this report. Similar analyses from other fields in California have been published in previous reports listed in the appendix, page 52. Yearly production of crude oil in California and the percentage of United States production represented by California production for 1948-54 are given in table 1. [ ] Analyses in this report are of samples from the fields listed in table 2, with production data for 1953, cumulative production through 1953, and year of discovery of each field. Information regarding the source and general characteristics of the samples is included in table 3 with a summary of analytical and computed data.

Jan 1, 1956

By M. E. Tyrrell

This Bureau of Mines investigation was made to determine the possibilities of using Florida beach-sand concentrator wastes in ceramic products. Sands used in the investigation originated in the Trail Ridge area of Florida, where continued operation of processing plants for recovering titanium minerals promises a dependable source of raw materials. Three general classes of ceramic products were studied, namely: (1) Structural, (2) refractory, and (3) electric-furnace slags.

Jan 1, 1956