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By S. Storchheim

MORE and more attention is being paid to the bonding of metals in their solid states. For a better understanding of this technique for joining metals and how it is affected by changes in temperature, pressure, and time at temperature and pressure, a detailed report concerning nickel to aluminum bonding has been published.' In order to broaden the knowledge accrued, some additional work concerning solid state joining of aluminum to copper and aluminum to zirconium was performed. The investigation of the Al-Cu system was considerably more extensive than the investigation of the Al-Zr system. For the A1-Cu system, not only were tensile sudies made but intermetallic penetration rate investigations also were carried out. The effect of temperature on intermetallic penetration rate for the A1-Cu system was determined at 11 tsi pressure, held 2 min. Procedure Apparatus: The hot pressing technique was the means of solid state reaction used and required the equipment depicted in Fig. 1. The following procedure was involved: The two metals to be reacted were placed in an aquadag-lubricated 18-4-1 tool steel die, 16 in. high by 1.440 in. ID, between punches of 1.366 in. diam made of the same material. A thermocouple well was located in the die body 3½ in. down from the top of the die, while another well was located centrally in the bottom punch 8½ in. from the bottom of the die. This die assembly was located in three cylindrical ceramic heating furnaces placed in tandem. Each furnace was controlled individually by a Variac power transformer. In turn, the die and furnaces were placed in a water-cooled stainless steel pot which could be evacuated. A cover, which contained a centrally located Wilson seal with an 18-4-1 1 in. diam ram running through it, was bolted on the pot. After sealing, the pot was evacuated by a roughing pump to 200 microns pressure, after which a diffusion pump was used to bring the pressure down to 5 to 15 u. At this pressure, the furnaces were turned on. As soon as they started to heat, out-gassing of the entire unit raised the pressure to 30 to 400 p. By the time the specimens were at temperature ready to be pressed, approximately 4/2 hr, the vacuum pumps had re-established the 5 to 15 u pressure. Once the desired temperature was reached, the required pressure was applied for a predetermined length of time to the 1 in. ram, through to the top punch, and to the specimen. When the time for keeping the specimen under pressure had elapsed, the pressure was released, the energizing coil current turned off, and the assembly allowed to cool. After cooling, the die was removed from the pot and the specimen was ejected. Specimen Preparation: Two different types of specimens were made for this investigation. One was for subsequent tensile testing, while the other was for determination of intermetallic alloy zone penetration into the parent metals. Tensile Bars—Commercially rolled copper pieces in. thick or zirconium sheet pieces 1/32 in. thick and 1.366 in. diam were placed between commercial 2-S aluminum rod 1 in. thick and 1.366 in. diam. This sandwich in turn was slipped into a 2-S aluminum sleeve 1.438 in. OD and 1.370 in. ID. This sleeve lined the couple up and prevented the aquadag lubricant from getting in between either the A1-Cu or Al-Zr interfaces. Immediately prior to the specimen assembly, the copper or zirconium was abraded on the flat surfaces with 320 grit silicon carbide paper, producing clean smooth surfaces. The aluminum was chemically cleaned just before assembly by: l—degrease in acetone, 2—distilled water rinse, 3—immersion for 3 min in 5 pct NaOH at 70" to 80°C, 4—distilled water rinse, 5—immersion for 2 min in 50 pct HNO3 solution at room temperature, 6—distilled water rinse, and 7—drying in a blast of gas. After the A1-Cu sandwiches were hot pressed and ejected, the specimens were machined such that the aluminum sleeve was removed, and the remaining aluminum was then threaded; the bar so produced was tested later for tensile strength. In all the instances where Al-Cu couples were tested, the specimens broke during the test at the Cu-A1 interface and never within the aluminum or copper. The ultimate tensile strength values at times showed considerable scatter for a set of given reaction conditions. Because of this, as many as three to five specimens were made for a particular set of conditions. The trend of the average tensile strengths obtained was not as conclusive as was the trend of the maximum tensile strengths, the latter values being obtained under optimum reaction conditions. Therefore, the values of ultimate tensile strength given herein are maximums.

Jan 1, 1956

By J. D. McLenegan

The purpose of this investigation was to prepare a market survey of the refractories industry in California and Nevada (referred to in subsequent paragraphs as the region), and to determine the degree of self-sufficiency and the potential capacity for anticipated growth. The report includes estimates of the total annual refractories consumption, the quantity of refractories imported into the region, the tonnage of raw materials required for their manufacture, and the resources of fire clay and high-alumina minerals in the region.

Jan 1, 1956

By J. M. Riley

A fluorometric method using morin in an alkaline-buffered chelating solution has been developed by the Bureau of Mines for determining beryllium in ores and mill products. Apparatus for measuring fluorescence intensities of the beryllium-morin reaction is described. Preparation of the sample for analysis consists essentially of digestion with sulfuric, nitric, and hydrofluoric acids, fusion of the residue with sodium carbonate and sodium borate, Solution of the melt with sulfuric acid, and proper dilution. Chemical separation of other ions is usually unnecessary. The method rave reliable beryllium determinations on samples in the 0.01- to 0.37-percent BeO range. The method is particularly applicable to low-grade beryllium ores; however, semiquantitative beryllium determinations have been made on beryl containing 12.0 percent BeO.

Jan 1, 1956

By A. J. Kauffman

The alluvial deposits of the Pacific Northwest have been investigated and worked with varying degrees of intensity since about the middle of the 19th century. Earlier efforts, of course, were centered about the placer-gold content of the deposits; later, the Oregon beach sands were exploited for their chrome content, and, still more recently, deposits in Idaho were worked for their content of monazite, a rare-earth mineral which also contains significant quantities of thorium. The composition of alluvial deposits seems to depend mainly upon the nature of the source rock from which the detrital material was derived and upon the resistance of the individual mineral grains to the agencies of weathering and transportation. The processes of crushing and concentration used in ore dressing are applied in a leisurely but nonetheless effective manner when exposed rock masses are eroded by natural forces. Weathering effects a continuous disintegration and chemical decomposition, wherein resistant minerals are set free as individual grains and new minerals are formed. Erosion carries these detrital products down the slopes into natural waterways, where a mechanical separation of heavy particles from light is accomplished by the running water. The accumulation of such resistant, heavy particles through the ages has resulted in formation of the black-sand deposits. In addition to the associated gangue minerals, heavy sand deposits in the Pacific Northwest may contain the following constituents of possible economic value: Gold, platinum, chromite, ilmenite, magnetite, garnet, zircon, monazite, columbite-tantalite, and radioactive blacks.

Jan 1, 1956

By A. M. Gaudin, Olav Mellgren, P. L. De Bruyn

In commonly used to prepare the surface of the mineral to be floated so that attachment to air takes place. The quantity of agent required to make the mineral hydrophobic is usually very small, of the order of 0.1 to 0.25 lb per ton of mineral. Details of the mechanism of pyrite collection are for the most part unsettled. Adsorption of collector has long been believed to involve an ion exchange mechanism as demonstrated for galena' and for chalcocite. In the work on chalcocite it was also demonstrated that a film of xanthate radicals unleachable in solvents that dissolve alkali xanthates, copper xanthate, or dixanthogen was formed at the surface of the mineral. The unleachable product increased with increasing addition of xanthate up to a maximum corresponding to an oriented monolayer of xanthate radicals. Pyrite is extremely floatable with xanthate if its surface is fresh,,' but the floatability decreases rapidly as oxide coatings increase in abundance. Pyrite shows zero contact angle when in contact with ethyl xanthate solution at pH higher than about 10.5; at neutrality. a contact angle of 60° is obtained at a reagent concentration of 25 mg per liter. Alkali sulfides and cyanides are pyrite depressants.

Jan 1, 1956

By F. A. Forward, V. N. Mackiw

The paper relates to the laboratory and pilot plant studies that have been carried out by Sherritt Gordon Mines Ltd., Metallurgical Research Div., in developing the ammonia pressure leach process for extracting copper, nickel, cobalt, and sulphur from high grade nickel concentrate produced from Lynn Lake ores, and describes in some detail the chemistry of the process. IT is well known'.' 2 that copper, nickel, cobalt, zinc, ferrous iron, and a number of other metals combine with ammonia in aqueous solution to form complex ions of the form [Me(NH,)x]"+. The stability and solubility of these ions depend on the concentration of the metal ion in solution, on the amount of NH, present, and on the amount and type of anions present, e.g., OH-, C0;-, NO,, C1-, SO;-. If ammonia is partially or completely removed from such solutions, for example by boiling, the soluble ammines tend to decompose and the metals precipitate as basic salts. These properties of metal ammines have found practical application in the commercial recovery of copper, nickel, and cobalt from a variety of ores. In an operation formerly conducted at Kennecott"" the mill tailing containing 0.80 pct Cu as copper carbonate was leached by percolation with an ammonia-ammonium carbonate solution to dissolve the copper as the ammine. At Calumet and Hecla0-" With a mill tailing containing about 0.4 pct Cu as metallic copper, it has been found necessary to aerate the ammonia-ammonium carbonate leach solutions between stages to oxidize the solubilized copper. At Nicarol"-" where nickel and cobalt occur as oxides and silicates which are not soluble in ammonia, the ore is heated to decompose silicates and to selectively reduce the nickel and cobalt to metal, leaving the iron as Fe,O,, and is then leached with ammonia-ammonium carbonate solution accompanied by aeration to dissolve nickel and cobalt as ammines. In each of these leaching operations, the anion present is CO, and the metals can be precipitated from the leach solution as oxide (copper) or hydroxide and carbonate (nickel and cobalt) by boil- ing off NH, and C02 both of which are recycled to treat a subsequent ore charge. The products-—oxide, hydroxide, or carbonate—can be treated by conventional smelting, calcining, or electrolytic methods to convert them to refined metals. Thus the procedures mentioned utilize the properties of the ammines to extract copper, nickel, and cobalt from nonsulphide ores and separate them from the leach solutions. These processes have the advantage that they can be carried out in closed vessels at atmospheric pressure, that the leaching solutions are specific for the desired metals, that the metals can be recovered as relatively pure compounds by the boiling operation, and that the NH, and CO, can be recycled. Also, as the leach solutions after boiling and filtration are substantially free of metals, NH,, and CO,, they can be discarded, thus facilitating the control of the water balance in the leaching circuit. When, as is the case with Sherritt Gordon concentrates, sulphides are treated with ammonia solution in the presence of oxygen, the leach solution contains SO,--, and an entirely different set of conditions is encountered. The ammine sulphates (of nickel, for example) are more soluble than the carbonates and can be only partially decomposed by boiling. The SO, and NH, in the solutions can not be recovered by boiling. Thus, despite the more favorable leaching conditions resulting from high solubility of the ammine sulphates, the recovery of metals, NH,, and SO, from the solutions must be effected by other means. Sherritt Gordon Nickel Concentrate Treatment The Ni-Cu-Co flotation concentrate produced at Lynn Lake'" contains 12 to 16 pct Ni, 1 to 2 pct Cu, 0.2 to 0.5 pct Co, 33 to 40 pct Fe, 28 to 34 pct S, 8 to 20 pct insoluble, and less than 0.02 oz per ton precious metals. The nickel is present chiefly as pentlandite, the copper as chalcopyrite, and the iron as pyrrhotite and pyrite. Most of the cobalt is thought to be present in pentlandite, although it is known that a small amount occurs as Co-Ni-pyrite.

Jan 1, 1956

By W. A. Stickney

The Bureau of Mines conducted beneficiation and smelting studies on siliceous offgrade manganese samples to indicate effective methods of manufacturing silicomanganese from materials that cannot be economically beneficiated to meet General Services Administration (GSA) specifications for stockpiling. Laboratory and pilot-plant flotation tests were conducted on 2 samples, 1 from the waste-tailings dump of the Domestic Manganese & Development Co , Butte, Mont., and the other from the Nettie mine in the Butte-Philipsburg area. Smelting tests were made on the combined concentrates from the pilot-plant flotation tests and on part of the tailings sample The flotation scheme found to be adequate in laboratory tests and later in the pilot-plant tests consisted of flotation by a fuel oil-tall oil emulsion in an acid circuit (pH )-1-.8 to 5.0). The oil-emulsion reagent flocculated the manganese minerals and selectively floated them from the siliceous gangue, In the pilot-plant flotation test on Butte-mill tailings 90.1 percent of the manganese was recovered in a concentrate that analyzed 32.6 percent Mn, 4.8 percent Fe and 28.1 percent Si02. In the test on Nettie mine ore 90.8 percent of the manganese was recovered in a concentrate that analyzed 36 6 percent Mn, 5.5 percent Fe, and 26-4 percent Si02.

Jan 1, 1956

By J. N. Ong, J. P. Ratledge, J. H. Boyce

SINCE German operators opened the Tsumeb mine in the early 1900's, continuous operation has been interrupted only by enforced shutdowns during two world wars and the depression of the 1930's. Original metallurgical practice was blast furnace smelting. This was applicable only to low zinc ore, leaving large tonnages of high zinc ore to be stockpiled on the surface. A gravity concentrator using tables, buddles, and jigs operated for several years, but differential flotation of the ore did not get beyond the experimental stage. When the property was put up for sale by the South African Custodian of Enemy Property there was an estimated 434,000 tons of ore on surface dumps. The dump material, assaying 4.48 pct Cu, 15.8 pct Pb, and 10.9 pct Zn, had become highly oxidized during a stay of many years on the surface. But these dump ores had to be used in evaluating possible metallurgy because the shaft became flooded after the 1940 shutdown and underground ore was unavailable. Many companies examined Tsumeb but quickly lost enthusiasm because of the formidable metallurgical problems presented by the dump ore. However, on the basis of extensive test work, the present company decided that differential flotation would be successful and purchased the property after competitive bidding. Geology and Mineral Association is Complex The Tsumeb mine lies near the northern boundary of South West Africa at an altitude of 4200 ft. The village of Tsumeb is 335 air miles northeast of Wal-vis Bay, territorial port of entry. The orebody is a hydrothermal replacement deposit associated with an irregular intrusion of aplite cutting folded pre-Cambrian dolomite beds. In plan the deposit is a lens of 250x600 ft maximum dimensions. In section the orebody dips 55" south from the surface to 2000 ft, below which there is a reversal in dip to 75" north. Mineralization is localized in the aplite and in the adjoining brecciated dolomite. In the upper levels the ore is largely confined to a single lens, but below the 1890 level massive sulphide ore forms north and south lenses that partially enclose a pipelike body of medium to low grade disseminated ore, part of which is of too poor a grade to mine. Drilling below the 24th, or bottom level, has disclosed that a high percentage of the mineralization from the 3000 to 3300-ft horizons is comprised of copper and lead oxides. The deep oxidation may be local, since it appears due to circulating waters in a major fault cutting the orebody. Tsumeb ranks as one of the highest grade base metal deposits in the world. It is geologically and mineralogically famous for 41 copper, lead, zinc, vanadium, and germanium ore minerals, but its complex mineral assemblage is not attractive to metallurgists. In addition, there is a gradual change in oxidation intensity from the upper levels to the lowest level now operating, which is the 24th. This is well illustrated by the copper minerals. In the upper levels malachite and azurite are predominant, in the intermediate levels chalcocite, and in the lower levels tennantite. Throughout the mine there are sufficient heavy metal soluble salts to activate zinc, and large amounts of depressants are required even for so-called clean sulphide ores. When the same sulphide ore is exposed to prolonged oxidation aboveground, as was the case with the dump ores, reagent requirements become fantastic. Plant Construction First staff members arrived at Tsumeb in March 1947, and by May essential services had been restored and mine unwatering began. In 2 1/2 months company employees built a temporary jig and sorting plant for treating existing dumps to provide a saleable product during high metal prices. Meanwhile, concentrator design and construction was contracted to a South African firm, with subcon-

Jan 1, 1956

By John M. Gordon

DURING and after 1949, various groups of British mining engineers came to the Dominion Coal Company, Limited, at Sydney, N .S., to see at first hand the Dosco MINER ( 1). These visits culminated in 1952 with the ordering of four Dosco Miners by the (British) National Coal Board on an experimental basis through their Experimental Expenditure Funds. Others are now on order. The first machine was delivered in February, 1953, and, after slight alterations to suit the different power supply, the machine was made ready to work. Due mainly to the size of the machine, new rules and regulations governing its operation had to be put into effect and it was not until April, 1954, that the machine was put underground. It started to produce in June of that year. The three others were delivered early in 1955. The authors were sent to England by the Dominion Coal Company to install and demonstrate these machines and to work with the Coal Board engineers to- further interest in the machines in the British coal fields .

Jan 1, 1956

By R. J. Hundhausen

The Takilma-Waldo copper district in Josephine County, Oreg., was studied by the Bureau of Mines from September 1950 to April 1.951 and from December 1953 to April 1954. Funds for the investigation were provided by the Bureau of Mines and the California-Oregon Power Co., Medford, Oreg., on a cooperative basis. The copper mines in the district are credited with a total production of ore worth $1,700,000. Since 1933 the mines have been unproductive and, except for minor exploration, largely inactive. The history of the district indicates that the copper deposits were mined principally during periods of high metal prices.

Jan 1, 1956

By J. J. Dowd

1. The Pittsburgh bed is the most important bed in Marshall County, and virtually the entire production of coal in the county comes from this bed. 2. Known measured and indicated reserves in all beds, based on a minimum thickness of 14 inches and 1,800 tons per acre-foot of coal in place, were estimated at 3,158 million short tons as of January I, 1954. Of this total, 3,071 million short tons is in beds 28 inches and more thick. Areas in each bed except the Pittsburgh were omitted from the estimate because available data relative to the bed characteristics are too meager to make an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, such reserves should be added to the total estimated reserves.

Jan 1, 1956

A spectrochemical procedure applicable to the determination of iron, manganese, and magnesium in titanium metal and to the determination of alloying constituents in three types of titanium alloys is presented. Acid solutions of samples and standards are excited with a spark-type discharge and porous-cup electrode arrangement. The method is particularly applicable for analyzing samples for which a self-electrode method cannot be used. Calibrations are accomplished with synthetic standard solutions, resulting in a primary method that makes calibrations based upon results of other analytical methods unnecessary. Replicate determinations are reproduced to within 5 percent, and the average percentage deviations from reliable chemical values are less than 6 percent. The method can be extended readily to determine additional elements that are similarly soluble and have similar spectral sensitivities. It also can be used as a starting point to establish standards for a direct sparking procedure for analyzing titanium alloys. In view of the absence of established reliable analytical methods in the titanium industry, the spectrochemical method described here should prove to be a timely contribution.

Jan 1, 1956

By David Schlain

The galvanic corrosion properties of titanium and zirconium were investigated by the Bureau of Mines. The dissimilar metals involved in these experiments included magnesium, magnesium alloy FS1, aluminum alloys, zinc, steel, tin, lead, copper, Monel, nickel, and several stainless steels. Couples were immersed in synthetic ocean water, tap water, 5-percent ammonium sulfate solution, 5-1/2-percent sodium chloride solution, sodium hydroxide solution, 0.1 N hydrochloric acid, and various concentrations of sulfuric acid.

Jan 1, 1956

By H. R. Hose

The total crude fluorspar reserves in Western Europe, including the USSR and the Soviet sphere, Thetotalare estimated to exceed 17 million metric tons. The total fluorspar production in 1951 in Western Europe, excluding the USSR and Soviet sphere, amounted to 371,109 metric tons. The chief fluorspar-producing countries in Europe, excluding Russia and the Soviet sphere, are France, Western Germany, Italy, Spain, and the United Kingdom. TOTAL crude fluorspar reserves in western Europe, containing more than 35 pct CaF2, are estimated at 12 million metric tons, while reserves in the USSR and Soviet sphere may exceed 5 million metric tons. The bulk of these reserves are concentrated in the USSR, Spain, United Kingdom, Western Germany, and Italy. Since published estimates of the tonnages of individual mines and explored deposits are not available for most countries in Europe, the estimates given in Table I for individual countries are necessarily approximate, as they have been compiled from various sources and modified and combined according to the author's judgment. The majority of fluorspar deposits in Europe belong to the late Paleozoic metallogenetic epochs and have been found within or along the borders of the Hercynian massifs. Deposits in the Central and Esterel massifs of France, those of Western and Eastern Germany, Sardinia, the Catalonian coastal range and the Sierra de los Santos in Spain, and those of Devonshire and Cornwall belong to the Hercynian metallogenetic epochs. The deposits in southern Norway and Sweden belong to the middle Paleozoic or later, those of northern England to the late Paleozoic or later, those of northern Spain and Greece to the late Mesozoic, and those of northern and probably central Italy and Switzerland to the early Tertiary. Fluorspar occurs typically in veins, lenses, and stringers, but also in bedded replacement deposits and pockets, and may be colorless to white, yellow, green, pink, brown, blue, or purple to almost black. Except for the colorless variety, the only kind which can be used for the optical industry, the color of the fluorspar does not affect its ultimate use. Crystalline cubic or octahedral fluorite of CaF2 composition, with 48.9 pct fluorine and 51.1 pct calcium, has a specific gravity of 3.18. The ore in place, however, usually averages 3.0 metric tons per cubic meter owing to the quantity of other minerals asso- ciated with the fluorspar in the veins and the physical state of the fluorspar, which may vary from sugary to massive crystalline or microscopic inter-growths with barite or quartz. Barite of 4.5 sp gr, quartz of 2.66 sp gr, and chert and calcite are commonly associated with fluorspar. Other minerals usually present in lesser amounts are celestite, wad, silver, lead, zinc, copper, iron, and uranium minerals. In some cavity fillings the rhythmic deposition of the fluorspar, barite, and quartz into successive crusts may make it possible to handpick the crude ore on belts or to separate the fluorspar from other minerals while the actual mining is carried on. Where metallurgical grade lump spar is required for foundries, separation of quartz and barite may be made also by jigs and heavy media, and in some mines the lead and zinc sulphides may be separated and recovered by vibrating tables. However, except in the case of unusually high grade deposits, acid grade fluorspar is obtained by flotation. By this process fluorspar deposits grading down to 35 pct CaF2 in the crude ore can be worked at a profit when fluorspar, lead, zinc, and silver prices are high, as the sulphides of these ores can be separated from the fluorspar by flotation and concentrated.

Jan 1, 1956

By R. A. Cunningham, A. S. Murray

If a dense fluid such as mud or water is used for circulation, the formation drilled is influenced by a hydrostatic pressure. This pressure depends on hole depth arid drilling fluid density. Laboratory tests indicute that drilling rates in many forri~ations are decreased with increased pressure,—in some cases as much as 90 per cent. A comparison between laboratory and field tests indicates that drilling fluid head affects drilling rates in the field approximately the, same as in the laboratory. Drillirrg rates of many formations are increased by reducing drilling fluid head. INTRODUCTION For many years it has been noted that field and laboratory drilling rate tests did not agree even when the formations tested were the same. For instance, tests of some shales by the Hughes Tool Co. laboratory indicated drilling rates approximately 20 to 30 ft/hour, whereas in the ground this shale would drill only 3 to 5 ft/hour. A possible reason for this discrepancy is the effect of the high pressure which the drilling fluid exerts against the formation at the bottom of the hole. Consider a small element of rock (Fig. II that is to be removed by a rock bit. If the hole is filled with mud or water. the upper surface of the rock element is subjected to a pressure which depends on hole depth and fluid density. The mass of earth around this rock element presses against the circumferential surface and the lower surface. Because of the probability of shearing stresses between the rock element and the surrounding rock, this element is not under true hydrostatic stress. However, as a first approximation for test purposes the rock element was assumed to he under hydrostatic stress. The effect of hydrostatic pressure on some physical properties of rock has been studied.1,2,3 These tests show that the "differential" compres-sive stress:': necessary to cause rup- ture in rock cylinders is greater when tested under high hydrostatic pressure than when tested under atmospheric conditions. These tests were made with pressures greater than 20,000 psi which is in excess of those normally encountered in oil well drilling. Similar tests were made by the Bureau of Reclamation' using pressures equivalent to those encountered in oil well drilling. Again the "differential" compressive stress necessary to produce failure increased with increasing hydrostatic pressure. These tests indicated that drilling rates would probably decrease. Correlation between these tests and drilling tests was not practical. The purpose of this work is to study the effect of mud column pressure on drilling rate, assuming that the material drilled is in a state of hydrostatic strcss. This problem was initially investigated in the laboratory using variable bit loads and confining pressure;. Confirmation of laboratory results was obtained in the field from a series of carefully controlled drilling tests. Because of the necessity of testing many different types of formations. only results from representative formations will be presented here.

Jan 1, 1956

By Russell R. Trengove

Core samples from an ore horizon 2,000 feet below the surface were successfully obtained by rotary drilling at the property of the Eureka Corp., Eureka, Nev. The ore was soft and friable; cores were not obtained previously with diamond drills. Whipstocking was used to get samples in a zone 200 feet from a vertical hole. A technique in shipstocking, by which the direction and deviation of the holes were controlled by means of nonfriction-type survey instruments, was successfully employed.

Jan 1, 1956

By A. B. Needham

This report describes the exploration work done in 1941 in connection with the search for strategic minerals as authorized by the Strategic Materials Act approved by the President on June 7, 1939. It deals with the various manganese deposits and showings in the Tombstone mining district of Cochise County, Ariz. The exploration project comprised a study of the geology, mapping of the areas, and exploration of various mines and deposits by sampling old drifts, crosscuts, and scopes, supplemented by diamond drilling from underground stations. The Federal Government's manganese-purchasing programs have revived interest in occurrences such as the scattered deposits near Tombstone. Because of this, the Bureau of Mines project report on the Tombstone district, prepared originally in 1941 but not published, has been revised and now is being made public.

Jan 1, 1956

By Robert E. Hershey

1. This investigation shows that the most important beds in Claiborne County, from the standpoint of present production and reserves, are the Coal Creek and Jellico. Together, they contain 69 percent of the known recoverable reserves in the county. Reserves in five other beds are tabulated in this report; in order of quantity of reserves, they are: Blue Gem, Lower Pioneer, Pewee, Big Mary, and Rex. 2. Known measured and indicated reserves in all beds, based on a minimum thickness of 14 inches and on 1,800 short tons per acre-foot of coal in place, are estimated to be 60 million tons, as of January 1, 1953. Of this total, 55 million tons is in beds 28 inches and more thick. Areas in each bed were omitted from the estimate because available data relative to the bed characteristics are too meager to permit making an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, such reserves should be added to the total estimated reserves.

Jan 1, 1956

By W. G. Pfann

A simple method of obtaining multistage batch separations by crystallization was described recently. Known as zone-refining, it comprises passing short molten zones through a long solid charge. This technique can now be used on a continuous basis by means of the zone-void method described in this paper. Feed enters, at an intermediate point, a column down which molten zones travel, and waste and product leave at the ends. Materials move in the column through the agency of voids, which are introduced at the ends and travel toward the feed inlet. The voids and molten zones are moved by external heaters in a simple manner, and the principle of reflux is utilized. ANEW method of obtaining multistage separations by crystallization was described recently.' Named zone-refinina.,-, the method comwrises slowly passing a series of molten zones through a long solid charge. Solute becomes concentrated at one or the other end of the charge, depending on whether it raises or lowers the freezing point of the solvent. The separation increases with the number, P, of zone-passes, approaching a limit as P approaches infinity. Zone-refining has been highly effective in purifying germanium and other substances.2,3 and new applications are steadily increasing. Zone-refining is a batch method and as such it has certain limitations inherent in batch operation. If it could be made continuous, its scope and utility would be greatly broadened. This end has been achieved by the zone-void method described in this paper. In the zone-void method feed is introduced continuously at an intermediate point in a column down which molten zones travel, while impure waste and purified product leave at the ends. Both the flows of feed, waste and product, and also the travels of the zones, are actuated by external moving heaters in a simple manner; and the system utilizes the principle of reflux. The method provides, in the field of crystallization, the counterpart of the continuous fractiona-tion column in the field of distillation. The following will be discussed: apparatus and mode of operation, fundamental nature of the separation, design theory, and practical considerations. The method will be described in terms of a binary solute-solvent system in which the solute is an impurity to be removed and the solvent is the desired product. The distribution coefficient, k, defined as the ratio of solute concentration in the solid freezing out of a molten zone to that in the liquid in the zone, is assumed to be constant and less than one. The process is equally effective for k's greater than one and for ternary or higher order systems. Method and Apparatus The essential features of a continuous zone-refining process are represented in highly generalized form in Fig. 1. A series of molten zones, produced by moving heaters, travels slowly down the column or charge (to the left in Fig. 1). If there were no flows of feed, waste, or product, the process would simply be batch zone-refining, the action of the molten zones being to sweep solute down the column, solvent up the column. For the process to be con- tinuous, with stripping and enriching sections in the column, feed must enter, and waste and product must leave, as indicated. The zone-void process accomplishes both objectives, namely, the indicated movements of zones and the indicated flows of material. Zones are moved by moving heaters, just as in batch zone-refining. Materials are made to flow by creating voids at the waste and product exits and causing these voids to move to the feed inlet. Since there must be a net flow of material from the feed inlet to each of the outlets, the indicated movements of voids are in the desired directions, because movement of a void in a given direction corresponds to flow of material in an opposite direction. In order to produce the desired movements of voids, the column is folded into two vertical sections having the feed inlet in common at their upper ends. Voids are displaced upward by the liquids in the molten zones and their travel is actuated by the motions of the zones. Voids travel with the zones in the enriching section and move continuously. Voids travel opposite to the zones in the stripping section and move intermittently. Creation and travel of voids will now be examined in detail. The enriching section of a column in operation, with its void generator, is shown in Fig. 2. The column section is a vertical tube around which a series of closely fitting, regularly spaced heaters travel slowly upward. Each heater produces a molten region, the temperatures of the heaters and the cooling between heaters being controlled so as to maintain the molten zones approximately constant in size. A void is normally present atop the molten zone in each heater. As the heater rises, it continuously melts solid above it, which drips through the void into the molten zone and continuously freezes out solid below it, of concentration k times that of the liquid in the zone. When a molten zone and void reach the feed inlet, which is kept molten, the void is displaced by an equal volume of feed liquid. Generation of voids of controlled size in the enriching section is shown in Fig. 3. The void generator is a tube of small cross-section, provided with lateral heat-conducting fins which sense the position of the heater. Liquid can escape only when the entire outlet tube is within the heater. If any part of the outlet tube is outside the heater, liquid cannot escape,

Jan 1, 1956

By William H. Tavenner

1. The 1952 Annual Report of the West Virginia Department of Mines lists nine beds that arc being mined in Logan County, of which the Cedar Grove and Chilton are the most important. The Cedar Grove group, No. 2 Gas, and Alma beds have the largest remaining reserves, in the order given. 2. Known measured and indicated reserves in all beds, based on a minimum thickness of 14 inches and 1,800 short tons per acre-foot of coal in place, are estimated at 5,411 million tons as of January 1, 1954. Of this total, 3,939 million tons is in beds 28 inches and more thick. Areas in each bed were omitted from the estimate because available data relative to the bed characteristics were too meager for making an estimate that conforms with the definitions of measured and indicated coal adopted for this study. Should future drilling or development prove reserves in these areas, such reserves should be added to the total estimate reserves.

Jan 1, 1956