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By E. A. Gulbransen, K. F. Andrew

Thermodynamic information on the solubility of hydrogen in exothermic metals is limited. Thus, the overall solubility decreased as the temperature rose, which suggests the heat of solution of hydrogen in the metal is negative; yet the terminal solubility in the metal phase increased, which suggests an endothermic reaction. A thermodynamic analysis, therefore, was made of the several equilibria involved when hydrogen dissolved in the metal. Equations were derived expressing the solubility, terminal solubility, and decomposition pressures of hydrogen in terms of the heat, entropy, and free energy of solution of hydrogen in the given phase. The relations between the thermodynamic functions for the a-zirconium and 8-hydride phase were developed. The thermodynamic quantities were determined experimentally by the measurement of the decomposition pressures over a broad composition and temperature range. Two new methods of analyzing the experimental data were developed for determination of the terminal solubility. STUDIES', ' of the impact strength of zirconium at room temperature indicated that small quantities of hydrogen, of the order of 10 parts per million, embrittles the metal. Micrographic' and X-ray diffraction' studies showed this embrittlement to result from the precipitation of a second phase upon slow cooling. These studies suggested that the terminal solubility of hydrogen in the metal phase increased with increase of temperature. This behavior appeared to contradict the effect of temperature on exothermic hydrogen occluders such as zirconium. For these metals, the solubility of hydrogen should decrease with increase of temperature. Before these facts could be understood, a thorough analysis of the several equilibria was essential. It was the purpose of this paper to consider the several equilibria involved when hydrogen was reacted with zirconium from both the theoretical and experimental points of view. Since the overall solubility of hydrogen in the metal has been considered by a number of workers, it was proposed to study the composition range 0 to 6 atomic pct H in detail. Literature Schwartz and Mallett' determined the terminal solubilities of hydrogen in the metallic phase from diffusion studies. They extrapolated concentration-penetration curves to the boundary between the solid solution phase and the hydride phase at the surface. Their results showed values of 2.6 atomic pct at 400°C and 5.2 atomic pct at 500°C. Extrapolations of the data to room temperature suggested very low values for the terminal solubilities. This study confirmed the hydrogen embrittlement results and indicated that the terminal solubilities increased as the temperature was raised. The solution of hydrogen in zirconium over the complete concentration range was studied by Hall, Martin, and Rees3 and by others. The results showed that hydrogen was absorbed up to a maximum composition of 66 atomic pct or ZrH This composition represented the t-hydride phase. The maximum amount of hydrogen absorbed increased with pressure and decreased with temperature. Due to this temperature behavior, zirconium was classed as an exothermic occluder." In 1930 Hägg studied the crystal structures of the Zr-H alloys over a broad composition range. Four hydride phases were found. However, the range of homogeneity of the several phases was not studied. Gulbransen and Andrew" recently studied the phase diagram of this system by X-ray diffraction methods and by a thermodynamic method based on decomposition pressure measurements. The results showed that only two hydride phases existed for low temperatures, the 6 and the .-phases of Hagg.' Both phases had broad regions of homogeneity. The lower limit of the two-phase region of a and d-phases suggested a terminal solubility of 4 atomic pct at 500°C. This value was in agreement with the results of Schwartz and Mallett.' To avoid hydrogen embrittlement at low temperatures, it was necessary to heat the metal in high vacuum at elevated temperatures. To choose the conditions of temperature and high vacuum, it was

Jan 1, 1956

By A. J. Barry

A method was developed for testing the anchorages obtained with 3/4-inch, expansion-type, headed bolt and shell assemblies. The apparatus is a modification of that used in testing -inch-diameter, slotted-type bolts. Four makes of expansion-type shells were used in 64 tests made in sandstone and shale roof. The results show that for 3 makes of shells the anchorage effectiveness is independent of the installed land, and for the fourth make of shell a better anchorage is obtained when instilled at a load of 8,000 pounds. The results also show that deformation of the expansion plug influences the majority of the anchorages obtained with two makes of shells. This deformation causes a larger increase in displacement for a given added increment of load. The data from 48 of the 64 tests were combined to establish a relationship between average displacement and increase in bolt load (above the installed load). This relationship can be used to evaluate the anchorage effectiveness of any 3/4-inch-diameter, expansion-type, headed bolt and shell assembly tested in the field.

Jan 1, 1956

Theories of ore genesis. have both practical and philosophical application-practical in that they influence our search for new ore bodies; philosophical in that they provide a test for our theories of petrogenesis-and our ingenuity.For example, the theory of granitization requires an explanation of ore genesis compatible with the general concepts of granitization.Our understanding of some processes of ore formation, such as supergene enrichment, or the formation of residual lateritic iron ores, is so complete as to permit of nq controversy.For other ores, like the oolitic iron ores of England and France, and elsewhere, or the segregations of chromite or ilmenite in basic igneous rocks, the broad principles are generally agreed on; dispute is limited to details of process.But for a wide range of ore deposits there is no such agreement. Completely incompatible hypotheses are advanced to explain' identical facts, and we have difficulty in finding new facts or criteria that will distinguish unambiguously between them.In thinking about such ores, a co:n;venient starting point is provided by Schneiderhohn's (1953) fourfold division of ore deposits:1. The secondary hydrothermal ore deposits occurring in Mesozoic-Neozoic cover strata of Europe.2. The "regenerated" younger ore deposits in Alpine type mountain chains.3. Post-Cambrian primary hydrothermal ore deposits.4. Ore deposits of the PreCambrian shields.To these we may add a fifth group:5. Stratigraphically controlled sulphide deposits.

Jan 1, 1956

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 N. Brown

IT has been observed that a hexagonal-close-packed crystal will undergo the same macroscopic displacements as an isotropic material if the basal plane is perpendicular to the axis of twist.&apos; Other orientations may produce both bending and twisting, but this analysis will be confined to pure torsion of a right circular cylinder. The z axis, the axis of twist, and the specimen axis are coincident. The displacements are given by Uq = rz, Ur = Uz = 0 [1] where 4 is the angle of twist per unit length. This requires rotational slip, as discussed by Frank&apos; and Wilman, which may be observed readily. The relative rotation of adjoining slip planes is simply produced by a movement of a planar grid of screw dislocations."." The screw dislocations are of the same sign and they move radially inward. For hexagonal-close-packed metals, the grid is hexagonal and the screw dislocations lie in the < 2110 > directions. The displacement of a point is the resultant of two displacements produced by intersecting screws sweeping over the point. The dislocations must pass over the point (r, o) in such a manner that its resultant displacement corresponds to the observed macroscopic displacement. If 6&apos; is measured from the [1010] direction, then for 0 < ? < ~/3, only the [1210] and 121101 type screw dislocations are needed to produce the required displacement. If n1 screws of type [1210] and n2 of type [2110] pass over a point, then, in order that Ur = 0 n, sin ? - n2 sin (/3 — 6&apos;) = 0. [2] If the tangential displacement is to be independent of 0, then n1 cos ? + n2cos (/3 —?) = N [3] where N is independent of ? and thus depends only on r. Nb is the tangential displacement where b is the Burgers vector. Since U? is a linear function of r, then N must be a linear function of r. If a2 is the outer radius and a, is the inner radius to which the plastic deformation has extended, then N = Nm2 r-a1 [4] This function meets the conditions that at

Jan 1, 1956

By Murray F. Hawkins, W. J. Ainsworth

In all types of subsurface pressure gauges the extension which occurs in the pressure-sensitive element is a function of the difference between the external (well or calibration) pressure and the internal pressure within the gauge, rather than a function of the external pressure only. The internal pressure is near atmospheric and depends upon (a) the quantity of air sealed within the gauge at the time of calibration or measurement, (b) the quantity of moisture (liquid water), if any, sealed within the gauge, and (c) the temperature at which the calibration or well measurement is made. Part of this correction for the change of internal pressure with temperature is taken care of by the customary temperature coefficient of the gauge. However, part of it is not, and while this portion may be only a few psi, it is nevertheless predictable or preventable, and should be considered in precision measurements. ERROR NO. 1 If air is sealed in the gauge at the same temperature and pressure for both the calibration and the well measurements, the usual temperature correction will take care of any difference between calibration and well measurement temperatures. However, if air is sealed within the gauge at temperature T1 and pressure P1 at calibration but at temperature T2 and pressure P2 for a well measurement, because different amounts of air are sealed within the gauge in each case, the internal pressure at. or corrected to, calibration temperature Tr will he different by where all temperatures and pressures are absolute. The calibration temperature is used, and not the well measurement temperature, because the usual temperature correction reduces the well measurements to calibration temperature. The correction term as calculated by the above equation is separate from. and in addition to, the usual temperature correction. Example: T, = 540°R, sealing temperature at calibration P, = 14.7 psia, sealing pressure at calibration T2 = 460°R, sealing temperature at well P2 = 14.7 psia, sealing pressure at well Tr = 660°R, calibration temperature AP = 660 [14.7/460 — 14.7/540] = 3.1 psi While this error is small even under these somewhat maximal conditions, it nevertheless represents a practical situation which did occur, and which as a matter of fact gave rise to this note. Where AP is positive, as above, the correction is added to the measured pressure; where negative, subtracted from the measured pressure. This correction should also be considered in successive calibration runs where the gauge, for example, may be warm from a previous calibration at an elevated temperature. ERROR NO. 2 Where a small quantity of moisture (liquid water) is sealed within the gauge at atmospheric conditions, the increased vapor pressure of the water at higher well or calibration temperatures will cause an increase in internal pressure. This moisture will come presumably from condensation within the gauge following temperature changes, from moisture on the operator&apos;s hands, and from atmospheric moisture (rain, mist, fog, etc.). Calculation shows that approximately 0.2 cc of water (three to four drops) is sufficient to saturate the air within an Amerada RPG-3 Gauge at 160°F, at which temperature the vapor pressure of water is about 5 psia. As the vaporization occurs in a sealed volume, the increase in internal pressure will be in excess of this 5 psi. At higher temperatures the pressures will be higher; however more water will be required to saturate the air within the gauge. Some experimental work was carried out with an Amerada RPG-3 Gauge at 200°F fitted with a 1,000 psi element, both with a dry recording chamber and with a small amount of water added. The results directly proved the existence of the error due to the presence of moisture, and, it is felt, indirectly, due to the differences in sealing temperatures and pressures, as both effects may be ascribed simply to an increase in the moles of gas within the recording chamber. SUMMARY In precision measurements the error introduced by sealing the gauge during a well test at a different temperature and pressure from that of calibration may be corrected for by using the equation presented, or it may be prevented by taking care always to seal the gauge at near calibration conditions. The error introduced by sealing moisture in the gauge may be prevented by taking care to keep moisture out of the gauge, or by removing the moisture by either warming or evacuating the gauge. Both of these errors are independent of the range of pressure measurement and the type of gauge, and are in addition to the usual temperature correction. ACKNOWLEDGMENT Appreciation is expressed to W. B. Kendall, Geophysical Research Corp., Tulsa, Okla., who pointed out the error from differences in sealing temperatures during some winter work in Canada. ***

Jan 1, 1956

By R. L. Perrine

The rise of drain holes drilled from a well to improve productivity is becoming increasingly common. This paper presents data on the productivity increase that may he expected. The data were obtained by use of an electrolytic tank mode1 of a reservoir. Parameter varied in the study to show their effect on productivity include the length, number, and arrangement of drain holes, formation thickness, and damage near the well-hore. The most important results are that very large increases in productivity can be expected only ill damaged wells. The distance, to which drain holes penetrate is of primary importance. Additional length is more effective than increasing the number of drain holes. INTRODUCTI O N In planning the use of drain holes to improve productivity, it is important to he able to estimate the increase in production that can be obtained for a given expenditure. It is also important to know what combination of parameters related to the use of drain holes can he chosen to give the largest production increase. This paper presents data on the productivity increase that may be expected, as obtained by use of an electrolytic tank model of the reservoir. In this study, :! number of parameters were varied to show their effect on productivity. These included the length, number, and arrangement of the drain holes. The presence or absence of a damaged zone of low permeability around the well-bore and the thickness of the producing formation were also considered. The productivity increase that might be expected due to drain holes is presented as the ratio: productivity of a well after drain holes are drilled and completed to the productivity of the same well in an undamaged state without drain holes. The symbol Q/Qo is used to represent this productivity ratio. Thus, the comparison in each case is with a formation of uniform and undamaged permeability. Additional notation includes I;, for the radial extent of the damaged zone, which is assumed to be cylindrical and concentric with the wellbore. Thus the effect of an actual block is approximated by a discontinuous varia-tion in permeability. For purposes of this paper, the permeability within the damaged zone, denoted by kb, is assumed to be 1/25 that in the remainder of the formation, or k. A necessary assumption in making comparative tests using an electrolytic model is that reservoir flow behavior can be approximated by single-phase, steady-\tate flow according to Darey&apos;s Law. In addition, the formation must be assumed to be homogeneous with equal horizontal and vertical permeability. The well-hore diameter in this study is assumed to be 11¾ in. and the drainage radius of the well equal to 500 ft. The drain holes are considered to have been completed without damage. THE ELECTROLYTlC MODEL &apos;She producing formation was modeled by forming a sheet of phosphor-bronze into a cylinder 40% in, in diameter to represent the boundary of the drainage area. This was enclosed in a waterproofed plywood box, and the box filled to an appropriate level with a dilute sodium chloride solution. Solution concentration was adjusted to give a total resistance from

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

Alfred Noble Joint Prize Committee F B Foley, &apos;56 American Documentation Institute F B Foley, &apos;56 American Geological Institute J L Gillson, Nov &apos;56, H A Meyerhoff, Nov &apos;57 Committee on Government Relations J L Gillson, &apos;56 American Power Conference Paul R Nichols, &apos;56 American Standards Association Mining Standards Board E R Borcherdt, Jan &apos;58, Otto Herres, Jan &apos;58 Alternates E W Bullard, Dec &apos;56, and J K Richardson, Dec &apos;56

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 R. W. Barnes

This circular presents results of a survey conducted by the Bureau of Mines to ascertain the extent to which dust-control practices are employed in the coal-mining industry. This survey was initiated because of increasing realization of the possible harmful effects of the inhalation of dust upon the health of coal-mine workers and the advent, during recent years, of new types of mining machinery and new mining methods that may have a direct effect upon the extent of exposure to airborne dust experienced by persons mining coal. Anthracite Mines The survey covered 169 anthracite mines that were operating from November 1, 1953, to July 1, 1954. It showed that large mines employing more than 100 men were doing most to control dust produced during mining.

Jan 1, 1956

By Eugene N. Cameron

Pegmatites of these areas have become important sources of beryl and lepidolite and have yielded cassiterite, columbite-tantalite, and other minerals. Examination of about 60 of these pegmatites leads the author to question the opinion of earlier investigators that the concentrations of beryl, lepidolite, and columbite-tantalite found have mostly formed by hydrothermal or pneumatolytic replacement of previously formed quartz-feldspar pegmatites. The author concludes, on the contrary, that present knowledge of the occurrence of minerals in zoned pegmatites can be applied to prospecting and mining of pegmatite deposits in these two areas of South West Africa. PEGMATITES occur in abundance in certain areas of South West Africa and in adjacent parts of northern Cape Province in the Union of South Africa. Some of the pegmatite deposits were prospected before World War I, and intermittent mining was done during the period between the two World Wars. The deposits of the Jooste lithium mines became an important source of lepidolite, and beryl, columbite-tantalite, wolframite, and other minerals were produced. Since World War II prospecting and mining have been carried on vigorously, with the result that South West Africa produced nearly 3000 tons of beryl during 1949 through 1953, together with more than 40,000 tons of lithium minerals, chiefly lepidolite and petalite. Small amounts of tantalite, columbite, and other minerals have also been produced during the postwar period. Most of this mineral production has come from two pegmatite areas roughly outlined in Fig. 1. One is the Karibib-Omaruru area of north central South West Africa. The second is the northeastern part of the Orange River pegmatite area, which extends into adjacent parts of Namaqualand, in northern Cape Province of the Union of South Africa. The writer visited the two pegmatite areas in July 1951. The visit was brief. but it gave an opportunity to compare some of the&apos; pegmatites of these areas with those studied and described in detail by many investigators in the U. S., Brazil, and Canada during and since World War 11.&apos;-l&apos; The writer has attempted to determine, in a preliminary way, whether the concepts of internal structure and distribution of minerals in pegmatite bodies developed out of these studies are applicable to prospecting and exploration of pegmatites in South West Africa. Previous Work In an important series of papers (1929 to 1942) T. W. Gevers, H. I?. Frommurze, S. H. Haughton, G. K. Joubert, and other geologists of the Geological Survey of South Africa described and discussed the pegmatites of the two areas.*-" These works are the principal sources of information on the pegmatite mineral deposits of South West Africa. The investigations showed that in the two areas pegmatites are profusely distributed in pre-Cambrian rocks. These rocks are meta-igneous and metasedimentary units that have been folded and subsequently invaded by younger pre-Cambrian granites and by other igneous rocks. The pegmatites are considered to be genetically related to the pre-Cambrian granites. Pegmatites occur in the granite bodies themselves but are most abundant in the surrounding metamor-phic rocks, a pattern repeated in many pegmatite districts of the world. The origin of the pegmatites and the factors controlling the occurrence of mineral deposits in them were discussed at length by Gevers and Frommurze (1929)" and later by Gevers 14, 15 pp. 41-51, Ref.

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&apos; 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,,&apos; 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&apos;.&apos; 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&apos;" 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 Y. C. Liu, W. R. Hibbard

An aluminum single crystal cold-rolled from (110) [1121 essentially retains its initial orientation after 99.6 pct reduction in thickness. The orientation of the recrys-tallized grains of this material can be described in terms of crystallographic rotations about principal poles of deformation texture. DURING the study of the recrystallization of a copper single crystal cold-rolled from a (110) [112] initial orientation, the orientation of the re-crystallized grains could be derived by a 30" rotation of the orientation of the cold-rolled matrix about its <111> poles.&apos; The present investigation was undertaken to extend the work done on copper&apos; to an aluminum crystal also cold-rolled from a (110) [112] initial orientation. Experimental Procedure The procedure of this experiment was similar to that reported for copper.&apos; An aluminum (99.998 pct) single crystal rod* 1 % in. in diameter was grown in back-reflection technique.&apos; The specimen (1.20x 1.004x0.6787 in. thick) was then rolled along the [112] direction. The final thickness was 0.0028 in., giving a reduction in thickness of about 99.6 pet. Specimens were cut from the rolled strip with scissors, and approximately in. of disturbed metal was removed with Tucker&apos;s reagent. The rolling edge remained intact. The specimens were sandwiched between two graphite plates and annealed in a lead or lead alloy bath which was electrically heated. Pole figures were constructed using the techniques previously described.&apos; Specimens were electrolytically polished4 and etched with 47 pct HNO8, 50 pct HC1, and 3 pct of 48 pct HF. The electrolytic polishing method and etching reagent employed for aluminum specimens were not entirely satisfactory and the microstruc-tures could not be studied in any detail. Results and Discussion The octahedral pole figure of cold-rolled aluminum strip is plotted in Fig. 1. The <111> poles spread in the transverse direction approximately 8" for the highest intensity areas. The spread in the transverse direction can be related to a rotation about two <110> directions lying in a plane containing the rolling direction and rolling plane normal. The two <110> directions and a scale of rotation for the <111> poles are shown in Fig. 2. The amount of rotation is consistent for three of the four <111> poles, about 35" to 40". The discrepancy for the fourth pole is believed to be due to limitations of the film technique. Alternate inter-

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 Holly J

Mr. Champness: I wish to congratulate the authors on their paper, which covers a large variety of subjects. Not every mine is in the fortunate position to effect cost reductions by the sinking of a new shaft, but, as the authors have endeavoured to show in their paper, with improved techniques further reductions are possible. I would like to ask two questions. Can the authors give me an approximate idea...

Jan 1, 1956

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

SINCE German operators opened the Tsumeb mine in the early 1900&apos;s, continuous operation has been interrupted only by enforced shutdowns during two world wars and the depression of the 1930&apos;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

An examination is made of some of the consequences of a magmatic gas phase developed during a late stage of differentiation of an acidic magma. Elements possessing halides with high partial pressures (Sn, Mo, W) may be removed from the magma by distillation into gas bubbles in the manner suggested by Fenner (1933). The common chalcophile elements are not affected by this mechanism, but form sulphides which may become attached to rising gas bubbles by one of three distinct mechanisms. The gas bubbles may then carry the sulphides upwards and concentrate them in some favourable locus, giving rise to an ore-forming fluid. The process would operate selectively upon different sulphides and is capable of providing an explanation of the paragenetic succession observed in ore deposits as well as other important geological criteria of ore genesis.INTRODUCTIONThere is a widespread belief among contemporary geologists that a large and important class of ore deposits is genetically related in some way&#183;to acidic igneous rocks. This class includes the tin-tungsten-molybdenum-bismuth type of mineralization as well as a variety of sulphide deposits.A basic problem confronting explanation of the genesis of these deposits is the manner in which trace elements which were originally widely dispersed in granitic magmas were segregated therefrom and concentrated into economic mineral deposits.The principles underlying the formation of one group of minerals deposits (pegmatites) related to granitic magmas ate reasonably well understood, largely due to the labours of Goldschmidt and his school. However, many geologists have noted that there appears to be some sort of fundamental discontinuity between pegmatite formation and the origin of the more common hypogene ores, particularly sulphides.Accordingly it has been suggested that these ores...

Jan 1, 1956