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The Pilbara Block is a nucleus of Archaean rocks which lies in the North West Land Division of Western Australia, and it constitutes a mineral province that has been divided into two areas-the West Pilbara Goldfield and the Pilbara Goldfield.In the West Pilbara Goldfield two contemporaneous environments are represented by laterally equivalent volcanic and sedimentary successions which together comprise the Roebourne Group. The two successions are lithologically similar to the classical Warrawoona (volcanic) and Mosquito Creek (sedimentary) successions of the Pilbara Goldfield; but in the West Pilbara Goldfield there is no sign of the erosional break which separates the Warrawoona Succession from the Mosquito Creek succession. The Roebourne Group and the igneous rocks which have intruded it belong to the Archaean Pilbara System.Evidence of preconsolidation movement and igneous intrusion into unconsolidated sediment suggests that tectonism and igneous activity, localized along lines of fracture in an unidentified basement, beganbefore lithification was complete. Movement was primarily vertical, and persisted into the Lower Proterozoic.Vulcanicity and chemical sedimentation, accompanied by a diminution of detr:tal sedimentation, is thought to have caused a relative enrichment in the metal content of the middle part of the Roebourne Group; and the metal may have been remobilized during diagenesis and metamorphism, and localized in zones of dislocation formed both before and after consolidation of the sediments.INTRODUCTIONThe name "Pilbara" has been widely applied in the area under discussion, and to avoid confusion the various uses are summarized below.1. The town of Pilbara, now abandoned, was a centre of mining between 1888 and about 1914. It lies some 90 miles FJSK of Roebourne (Fig. 1).2. The original Pilbara Goldfield was modified several...

Jan 1, 1965

By G G. Suffel

T HESE remarks on the occurrence of strata-bound massive sulphide deposits are submitted be-cause the writer recently visited the principal Cyprus deposits (in January, 1965) and has also a back-ground of many years spent largely in detailed observation and map-ping of the Horne and Amulet ore-bodies, now largely inaccessible. They are particularly related to the Symposium papers (September Bulletin) by Hutchinson and by Roscoe. Some comments are offered on the cupriferous pyrite deposits of Cyprus. As the writer is currently reviewing the published literature on the related deposits in Turkey, a brief account of some characteristic Anatolian sulphide occurrences is given. The discussion is closed with some thoughts on the relationship between these Mediterranean sulphide deposits and those of northwestern Quebec and the Superior province in general. The geology of Cyprus, as it relates to the sulphide deposits, is well summarized by Hutchinson (1965). After visiting Mavrovouni, Skouriotissa and Limni and after much thought on the possible ge-nesis of these ores, it seems quite logical to me that he is right. They are indeed closely related to late-stage submarine volcanism.

Jan 1, 1965

By S. A. Mersol, C. T. Lynch, F. W. Vahldiek

The microhardness of single crystals of tungsten disilicide has been investigated by the Knoop method. The average random room-temperature hardness of the WSi, matrix was 1350 kg per sq mm. Hardness crnisotropy was noted with respect to plane and indenter orientation as determined by single-crq.stal X-rny studies. Annealing at 1600" and 1800°C decreased the average hardness to 1310 and 1230 kg per sq tnm, respectively, and produced a second phase identified by X-ray diffraction and electron-microprobe analysis to be wSio.7. Ball-impact experiwzents produced rosettes at 850°C. Optical and electron microscopy showed evidence of slip and cross slip and twinning produced by microhardness indentations. Prismatic (100), [001] slip was found and cor~elated with hardness data. THE present study was undertaken to investigate the hardness anisotropy of as-grown and annealed single crystals of tungsten disilicide. The existence of the silicide WSiz in the W-Si system has been well-established and its structure thoroughly investigated zachariasen2 found WSi, to have a tetragonal C type of structure, similar to that of MoSi, with lattice parameters a = 3.212A, Kieffer et al. studied the W-Si system and measured the density and microhardness (at a 100-g load) of both polycrystalline WSi, and WSi,.,. The values found were 9.25 g per cu cm and 1090 kg per sq mm for WSi,, and 12.21 per cu cm and 770 kg per sq mm for WSi0.7, respectively. According to Samsonov et a1.5 the microhardness of polycrystalline WSi2 is 1430 kg per sq mm (at a 120-g load). EXPERIMENTAL The WSi, single-crystal boules investigated in this paper were grown by a Verneuil-type process using an electric arc by the Linde Division of the Union Carbide Corp.6 The largest specimens were 8 mm in diameter by 16 mm long. The crystals had an average density of 9.01 g per cu cm with a tungsten • silicon content of 99.9 wt pct. The major impurities were: 87 ppm O, 41 ppm N. 54 pprn C, 500 ppm Zr, 50 ppm Na, and 50 ppm Mn. The crystals were silicon-poor, the average silicon content being 22.20 pct (stoichiometric value is 23.40 pct), and tungsten-rich, the average tungsten content being 77.70 pct (stoichiometric value is 76.60 pct). As-received single crystals were ground and analyzed by powder X-ray diffraction technique using Cu Ka radiation. Laue and layer line rotation patterns were obtained on cleaved sections of WSi, single crystals. Electron-microprobe traverses of representative crystals were done using a Phillips-AMR electron microanalyzer. Carbon replicas were used to prepare electron micrographs. This work was done with a JEM-6A electron microscope. Prior to the metallographic examination, the specimens were mounted in Lucite and then polished for short times on polishing wheels using 9-, 3-, and 1-p diamond-grade pastes. Finally they were fine-polished with Linde A powder for 24 hr on a Syntron vibratory polisher. The samples were etched with 4H 2 O:1HF:2HNO3, which is a medium fast-acting etchant. The combination 1HF:2HNO3:5 lactic acid is also a satisfactory etchant. Annealing runs for selected specimens were made at 1600" and 1800°C for 3 hr at 1.0 to 3.0 x 10-5 mm Hg. A Brew tantalum resistance furnace with WSi2 powder for setters was used. The WSi2 powder was the same as that used for the crystal growth. Temperatures were measured with a calibrated W, W-26 pct Re thermocouple and a microoptical pyrometer. Powder X-ray diffraction, emission spectrographic, and electron-microprobe analyses were done after the annealing runs. For microhardness measurements a Tukon Microhardness Tester Type FB with a Knoop indenter was used. Although measurements were taken at loads ranging from 25 to 1000 g, the 100-g load was chosen as the standard load. All measurements were taken at room temperature. Only indentations of cracking classes 1 and 2 were considered.' DISCUSSION OF RESULTS Powder X-ray diffraction analysis showed the as-received crystals to be single-phase WSi2. Laue and layer line rotation patterns obtained on cleaved sections of WSi2 single crystals proved them to be tetragonal WS 2 2 The results also indicated that the c axis of the crystal was oriented parallel to the boule or growth axis. Electron-microprobe traverses across the matrix of the as-grown crystals showed them to be homogeneous WSi,. Optical and electron microscopy of etched crystals, however, revealed that they contained minute amounts of the "golden" and the "blue" second phases as opposed to the "white" or WSi2 phase. These two second phases were concentrated in inclusion and etch-pit

Jan 1, 1965

Laboratory flotation tests on sized fractions of a certain number of selected minerals with homologous fatty acid derivatives (i.e. sodium salts and amine acetates) confirm that the higher homologues are more efficient collectors than the lower. Tests were carried out on sized material and finer size fractions floated at lower collector concentrations.It is suggested that selective flotation is best achieved with the reagent which most readily floats the most friable mineral in the ore, and that grade of product will be improved with the lowest usable homologue.INTRODUCTIONFlotation of non-sulphide minerals with fatty acids as collectors is usually less selective than the flotation of sulphide minerals with xanthate collectors. It is common to use the gradation in collecting power of homologous series of xanthates, as well as the more specific effects of activators and depressants, to achieve the separation of sulphides.The original aim of the work was to ascertain whether sodium salts of fatty acids (anionic) and fatty amine aceta:tes (cationic) could be selected from a homologous series to achieve better selectivity in separation of nonsulphide minerals by flotation. Subsequently the importance of friability of minerals in selective flotation was observed and the aim was expanded to develop a more practical approach to the testing of ore.MATERIALS USEDMineralsA series of massive mineral specimens, as pure as could be obtained, was procured. The specimens were cleaned by removing extraneous material, and then crushed and dry...

Jan 1, 1965

By Ralph H. Whaite

The Bureau of Mines program for microfilming maps of abandoned mines in the Pennsylvania anthracite region is described. A catalog of the maps that have been microfilmed in the Eastern Middle anthracite field--the first area to be covered in the program--is presented. Additional catalogs will be published as significant mining areas are completed.

Jan 1, 1965

By John W. Sweeney

Shales and clays from Illinois were sampled, tested, and evaluated to determine feasibility of producing lightweight aggregate by rotary-kiln methods. Sampling procedures and the 1 ,,,y of the Pennsylvanian shale units are discussed. Chemical, X-ray spectrographic and X-ray petrographic analyses were run on the samples to determine if a correlation existed between chemical mineralogic composition and expansion. Preliminary expansion testing was conducted in a muffle furnace. Rotary-kiln tests were conducted in a 16- inch by 14-foot rotary kiln. The weight of the aggregate ranged from 27 to 59 pounds per cubic foot. Concrete cubes employing the aggregate were tested to determine the qualities of the concrete. Compressive strength of the concrete using the 7-bag of cement cement per cubic yard mix, after autoclave curing for 6 hours, ranged from 2,950 to 6,750 psi. No correlation was found between the chemical, X-ray spectrographic, and X-ray and petrographic analyses and expansion, Sixteen samples made suitable lightweight aggregates in the laboratory rotary kiln. The expansion temperature range of eight of the samples was extremely narrow, and difficulties would probably be encountered in processing these materials commercially.

Jan 1, 1965

By James R. Boyle

The mining methods and practices used at the Young zinc mine, American Zinc Co. of Tennessee, have resulted in a low-cost, high-yield operation. Zinc ore (sphalerite) occurs in limestone-dolomite beds of the Kingsport Formation and is mined by modified room and pillar method. Utilizing trackless mining equipment which incorporates a high degree of flexibility, this operation has had a steady increase in productivity.

Jan 1, 1965

By George L. Gates

The Bureau of Mines developed a rapid instrumental method of analyzing oil well scales containing primarily barium sulfate. After removal of oil and water by carbon disulfide) the scale was dissolved in strong hydrochloric acid. The cations, barium, calcium, strontium, magnesium, and iron, were determined with the flame photometer using the method of additions. Sulfate was deter-mined colorimetrically after separation by selective adsorption on an alumina column. Phosphate was determined colorimetrically and carbonate titrimetrically. The method was reasonably accurate, although iron and magnesium were found to have mutual interference.

Jan 1, 1965

By Charles E. Whieldon

Data on the oil fields in Mahoning Columbiana, Carroll, Jefferson, and Harrison Counties, Ohio, were collected from scattered sources and com- piled to make the information readily available to operators who may be interested in conducting secondary-recovery operations in the area. General geology, oil production, oil-productive acreage, core data, reservoir calculations by townships, and miscellaneous data and reference material are presented.

Jan 1, 1965

By W. E. Howlett, R. L. Slobod

Jan 1, 1965

By Arne Landsberg

A study of the chlorination kinetics of germanium, silicon, iron, tungsten, molybdenum, columbium, and tantalum has been made to determine the effects of temperature, chlorine concentration, geometric surface area and gamma radiation. The reaction products were volatile at the temperatures used this making it possible to follow the reaction rates by weight loss of the solid. Chlorination rates of germanium, silicon, and iron were found to be directly proportional to chlorine concentration while the rates for tungsten, molybdenum, columbium, and tantalum were proportional to the 0.5 to 0.6 power of chlorine concentration. A good correlation of reaction rate and geometric surface areas was not obtained because the true surface area of the samples could not be measured. Intense gamma radiation had no effect on reaction rates. The Arrhenius activation energies determined over the temperatures used are as follows: Germanium, 27 kcal/mole (233°-241° C); silicon 33 kcaL/mole (375°-517° C); iron, cold rolled, 20 kcal/mGle (259°-325° C) annealed, 21 kcal/mole (293°-337° C); tungsten, 43 kcal/mole (617-776° C); molybdenum, 37 kcal/mole (445°-4910 C); columbium) 34 kcal/mole (229°?255° C); and tantalum, 29 kcal/mole (370°-449° C).

Jan 1, 1965

By H. G. Sell, G. W. King

An investigation was made of the lensile proper-ties of recrystallized high-purity tungsten and a W-1 pel ThO2 dispersed-phase alloy over the temperature region of 800° to 2400°C. The thoria addition resulted in a modest strengthening effect over the entire temperature region. A decrease in ductility of both materials occurred above 0.5 Tm which was caused by void formation. Current theories of IT has long been recognized that a second phase of hard particles has a strengthening effect on a pure metal. At low or intermediate temperatures (<0.5 Tm), the strengthening effect is thought to arise mainly from the interaction of dislocations with dispersed particles. Above 0.5 Tm, dynamic recovery processes greatly alter the deformation mechanisms from those simply involving glide, and grain bound- strengthening by a dispersed second phase do not adequately explain the tensile results. Melallographic examination suggests that the improved strength of tire alloy results from the effect of thoria on the mierostructure. Stress-dependent thermally activated processes were found to occur high temperatures. aries may act as sources of weakness rather than strength because of grain boundary sliding. Grain boundary sliding at high temperatures has been postulated to be the primary factor giving rise to the formation of voids or cavities at grain boundaries1-3 which in turn cause premature failure and poor ductility.4 Voids, once formed, can grow by the condensation of vacancies from the equilibrium concentration&apos; or from the excess vacancies produced by the deformation.4,5 The high-temperature tensile properties of unalloyed tungsten have previously been investigated by Sikora and Ha116 and also by Taylor and Boone.7 The purpose of the present work was to investigate

Jan 1, 1965

By C. J. Beevers

Tlze influence of zirconium hydride precipitate mprphology on the fructure of Zr-H alloys tested at strain rates of 10- sec at 20° and - 196°C and at strain rates of -500 sec.-1 at 20°C has been inves-tigated. The critical stage in the embrittlement of these alloys was the fracture of the zirconium hyhide precipitates to form large interval cracks at a stress of 25,000 10 137,000 psi. In specimens con-temping up to 100 ppm H the preciptates existed as isolafed platelets in the zirconium matrix and their fracture as enhanced by low temperature (—196°C) and high strain rate (-500 set-f) loading. These resl~lts lead to the conclusion that the rate of strain hardening of the zirconium metal controls the frac-tzrm of the hydride platelets. Increased hydrogen contents of 500 to 2000 ppm resulted in an increase in the 1)volume fraction and size of precipitates and crlso led to crack propogation in the hydride at both 20 and —196C at the low strain rates (10&apos;* sec-&apos;). Quenching led to refinerment of hydride precipitate size and reduced the degree of embrittlement at — 196°C; this effect is attributed to the absence of fracture of the fine precipitates. The formation of zirconium hydride precipitates has been shown to be the cause of hydrogen embrittlement of zirconium.&apos; Several investigators&apos;-" have studied the problem in broad outline, demonstrating that impact-loading conditions, testing temperatures below room temperature, and increasing hydrogen content produce increased brittleness. For example, Muehlenkamp and schwope2 showed that the transition temperature for notched impact tests was raised from 150" to 350°C on increasing the hydrogen content from 45 to 490 ppm. The degree of embrittlement is also controlled by the morphology of the zirconium hydride precipitates. The solubility of hydrogen in zirconium decreases from 600 ppm at 550°C to 10 ppm at 20"C,~ so that the form of the zirconium hydride precipitates (ZrH2) can be modified by varying the cooling rate through the Zr-aZr + ZrH2 phase boundary.= Forscher showed that quenching a specimen containing 35 ppm H from above 315°C resulted in a reduction in area of 70 pct at -196"C, whereas slowly cooling from above 315°C resulted in a ductility of half this value. The role of the hydride precipitate in the fracture process has been examined by Young and schwartz6 and more recently by westlake.&apos; From metallo-graphic observations on slowly cooled Zr-H alloys they have suggested that cracks are nucleated in the hydride precipitates by the interactions of twins in the zirconium metal with the hydride. The experiments reported in this paper show that crack propagation in the zirconium hydride precipitates is the critical stage in the embrittlement of Zr-H alloys. The factors influencing fracture of the hydride precipitates and crack propagation in the zirconium metal will be related to the problem of embrittlement. EXPERIMENTAL TECHNIQUES The zirconium used in these experiments was produced from an ingot of vacuum arc-melted iodide zirconium forged down to 1 in. diameter at 800&apos; to 850°C. The 1-in.-diameter bar was surface-machined and cold-swaged to 0.375 in. diameter. After a vacuum anneal at 800°C for 1 hr the hardness was 60 to 70 Vdh. The total impurity content was approxi-

Jan 1, 1965

By Jerry W. Ramsey

The Bureau of Mines examined a low-, a medium-, and a high-volatile Pennsylvania anthracite by densimetric methods using four mesh si.s of each anthracite. Using high-pressure mercury the macropore volumes and distributions of these pore volumes determined, densities in mercury were calculated, and specific pore vo1.r. ware obtained from these mercury densities in conjunction with helium densities. The helium densities were also used with the ultimate analyses of these anthracites in calculating structural parameters by statistical densimetric methods. The effect of 106 or 108 rads of gamma irradiation in the presence of air and in vacuum upon the properties studied with two mesh sizes of each anthracite. Results of the statistical densimetric method seem to show some breakdown of condensed ring structural units at the lower irradiation level, with subsequent polymerization at the longer period of gamma irradiation. The structural parameters obtained also indicated that in going from high- to low-volatile anthracite, either the number of condensed rings per structural unit increased, or the degree of polymerization increased.

Jan 1, 1965

By Robert E. Barieau

In the design of plants to separate helium from natural gas, it is necessary to estimate the enthalpies of the various streams at various positions in the process. This Bureau of Mines report surveys the various methods that have been used to determine enthalpies and gives information on the organizations with such capabilities. The minimum information required for developing an enthalpy diagram is presented, and the relative merits of the various methods are discussed. It is concluded that methods that require no mass flow rate or energy measurements are to be preferred.

Jan 1, 1965

By R. B. Anderson

SULFUR poisoning of iron catalysts in the Fischer-Tropsch synthesis was investigated at the Bureau of Mines, because synthesis gas produced from coal contains sulfur compounds. Tests of two typical iron catalysts with synthesis gas containing known concentrations of H2S were made to determine catalyst life as a function of sulfur concentration to ascertain the type of gas purification required. Fixed beds of activated steel turnings and a fused iron oxide catalyst were investigated in sulfur poisoning tests at 21.4 atmospheres with IH2+100 gas containing 6.9, 23, or 69 mg S as H2S per cubic meter (0.3, 1.0, and 3.0 gr per 100 cu. ft.). In tests of reduced catalysts at constant temperatures, more than 80 percent of the activity was lost when 0.5 mg S/g Fe was introduced. Poisoning of nitrided or carbided fused iron oxide catalysts to a given extent required more than twice as much sulfur than for the corresponding reduced catalyst. When the synthesis temperature was increased to compensate for loss in activity, tests of the fused iron oxide catalysts at constant productivity could be continued for 19 to 98 days. The tests were terminated by clogging of the reactor, presumably caused by carbon deposition. One objective of the present work was to determine if synthesis gas, purified by the Bureau of Mines&apos; hot-potassium carbonate process for removing H2S, OOS, and CO2, is suitable for synthesis on iron catalysts. The sulfur content of the gas purified by tills process is in the range of concentrations used in the present work. In constant-productivity tests of nitrided fused iron oxide catalysts with synthesis gas containing 6.9 mg S/m3, catalyst lives are nearly long enough for serious consideration of tills mode of operation. However, factors relating to selectivity and stability of the catalyst indicate that this type of operation is impractical for a commercial process. On this basis additional gas purification, such as iron oxide boxes following a hot potassium carbonate scrubber, is desirable.

Jan 1, 1965

By A. J. Kauffman

This study compiles data on the zircon resources of the Pacific Northwest States, Alaska, and California, to determine the productive capability of industrial concerns to make ductile zirconium and hafnium, and to investigate markets for the nonmetallic products of zircon. West coast zircon resources are large but mostly marginal to submarginal. Development of a stable and profitable zircon mining industry on the west coast will depend upon recovery and utilization of the other associated heavy minerals needed by regional and national markets. The west coast has the only completely integrated facility for processing zircon sand to reactor-grade zirconium and hafnium and for making fabricated products from these metals. The future of the zirconium metal industry appears to be good because of increased use of the metal for nuclear propulsion and power-generating plants.

Jan 1, 1965

To enable ammonium nitrate-fuel oil (AN-FO) to be used on an equal weight basis with nitroglycerine explosives, smaller diameter bore holes became necessary with consequent modifications to drill steel and burden on holes. Detonation of AN-FO in small diameter holes proved successful both with and without primer charges but some alterations were required to adapt anoloders to the smaller holes.Important factors in training all operators in the new charging method were the retention of improved fragmentation, avoidance of excessive overbreak and keeping wall rock dilution to an absolute minimum. The successful storage of ammonium nitrate in climatic conditions with daily temperature fluctuations above and below the critical 90&#176;F has been achieved.INTRODUCTIONTechnical aspects of ammonium nitrate-fuel oil (AN-Fa) blasting agent are well covered in recent literature. This paper deals primarily with the manner of its introduction as the principal explosive underground at Great Boulder Gold Mines Ltd. and with the many problems encountered in the process. Following reasonably successful experimental firings in June 1962&apos;, using granular ammonium nitrate and an anoloder, permission was granted by theWestern Australian Mines Department to carry out test work in selected areas of the mine. The permit allowed for fuse firing only, and for a mixture of AN-Fa containing between 5t and 6 per cent fuel oil, with an adequate primer.The use of AN-Fa on an equal weight basis with nitroglycerine explosives, involved smaller diameter holes with alteration to ground burden and modification to drill steel.Initial tests indicated that it was apparent that AN-Fa could not replace gelignite on an equal weight basis if the...

Jan 1, 1965

By Larry A. Haas

The Bureau of Mines constructed a torsion effusion apparatus to measure the equilibrium vapor pressure of pure metals, alloys, and compounds at temperatures up to 1,500° K. The reliability of the apparatus was established by determining the vapor pressure of silver. The data obtained on solid and liquid silver in the temperature range 1,200° to 1,500° K can be expressed by the following equations:

Jan 1, 1965

By C. H. Schack

Extractive metallurgy techniques currently employed to recover silver from primary ores and secondary scrap were reviewed and evaluated to identify and delineate metallurgical problems whose resolution would increase the supply of silver from domestic materials. The survey revealed that practically all primary silver is recovered by froth flotation concentration of various types of ores, followed by smelting and refining of the separate lead, copper, and zinc concentrates. Silver losses during the complex processing are, with rare exception, inconsequential. Furthermore, any silver production gain from base metal ores, which contribute about two-thirds of the total primary silver, is directly dependent in improvement in the market for the base metals. Statistical data on new and old silver scrap are wholly inadequate to make reliable conclusions about scrap processing problems and the possibility of increasing the recovery of silver from the many forms of secondary silver- bearing materials. The available information indicates (1) that efficient silver reclamation practices are employed by the larger users of silver, and (2) that recovery of additional secondary silver involves solution of problems of collection rather than of processing. Several possibilities exist for limited increases in silver production from primary ores by improvement in metallurgical practices. Specifically, research is needed to (1) solve the problem of recovering silver from the copper ores of the Copper Range district, Michigan; and (2) devise economically feasible methods for recovery of silver from presently marginal or submarginal ores that because of grade, location, and frequently complex nature cannot presently be exploited by conventional techniques.

Jan 1, 1965