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By Ira Joralemon

THE sampling of disseminated copper deposits has been described often but the method of combining assays, to give the true shape and value of the orebody as it will be mined has received less attention. As the ore mined during five or ten years at several of the great disseminated properties has averaged materially lower in grade than the published estimates, the question of the sampling and estimating of these orebodies seems timely. In this paper, attention is given particularly to factors that may cause errors in the final estimate. Sampling of diamond-drill holes, churn-drill holes, and underground workings is briefly described in the first part of the paper; then the method of combining assays to give the average grade and tonnage that will be mined is taken up in some detail. The necessity of study of the geology of the deposit and of probable costs is emphasized. Finally, the methods of calculating tonnages are outlined. DIAMOND-DRILL SAMPLING There are three main requisites for accurate diamond-drill sampling. First, the core should be removed and the hole cleaned out at the beginning of every sampling interval, usually 5 ft. (1.5 m.). After the rods are let down, water should be run through them until it becomes clear. The water must be clear before drilling starts. In this way the material knocked down from the sides of the hole by the descending rods is washed away, instead of being left to salt the sludge, sample.

Jan 2, 1922

By Robert F. Mehl

THE mechanical behavior of metals and alloys is presumably conditioned by two factors; namely, the crystalline symmetry and the interatomic forces. Considerable attention has been given to the first of these factors through the recent advances in X-ray technique. It is the purpose of the present paper to call attention to the importance of the second of these factors, to point out promising methods of investigation, and to present some pertinent data. Plastic deformation takes place by slip along atomic planes.1 This slip may be inhibited in a number of ways: by the interatomic forces of cohesion which bind the atoms rigidly in a lattice structure, which in pure metals is usually of high symmetry; by lattice distortion caused by solid solution formation or by mechanical strain; by the intercrystalline boundaries where slip is restrained, probably by the non-registration of the atom planes in adjacent crystallites;2 and by the presence of small hard particles which serve to "key" the slip along the atom planes.3 In pure metals, and perhaps also in solid solutions, the atom planes of easiest slip are those exhibiting the greatest density of atomic population and the greatest interplanar distance4 and apparently can now be predicted from the analysis of the lattices. Concerning the interatomic forces, which resist this slip by holding the atoms firmly together, little is known. Most textbooks on physical metallurgy, following the work of Bottone,5 correlate the hardness of the pure metals with the atomic volume,

Jan 1, 1928

By H. Kazemi

A pressure fall-off test on the injection well of a forward combustion project may permit us to calculate the distance to the burning front. In the mathematical description and analysis of test data, we have considered the effect of temperature on the thermodynamic properties of reservoir fluids. The temperature distribution predicted by Chu' for a combustion wave has been used in analyzing a field test. Numerical solutions were obtained by simultaneous solution of the flow equation, the continuity quation and the equation of state. Although this analysis conccntrated on isotropic systems, the results can be extended to systems having directional permeability. INTRODUCTION Conventional pressure fall-off tests have been used extensively to determine reservoir characteristics in gas- or water-injection projects.- such tests consist of injecting fluid into the formation at a constant rate until steady state is nearly achieved, then discontinuing injection and measuring the bottom-hole pressure as a function of time. A plot of pressure vs the logarithm of time (measured from the instant of shut-in) yields a smooth curve characterized by three distinct regions (Fig. 1): Region I reflects the permeability alterations in the vicinity of the wellbore; Region II reflects the reservoir characteristics further away from the wellbore; and Region 111, the characteristics in the displaced fluid bank. The curves in Regions II and III are straight lines! the slopes of which are proportional to the reciprocal of the flow capacity of the formation behind and ahead of the interface as shown by Eq. 1, respectively:

Jan 1, 1967

By Robert F. Mehi

The mechanical behavior of metals and alloys is presumably conditioned by two factors; namely, the crystallinc symmetry and the interatomic forces. Considerable attention has been given to the first of these factors through the recent advances in X-ray technique. It is the purpose of the present paper to call attention to the importance of the second of these factors, to point out promising methods of investigation, and to present some pertinent data. Plastic deformation takes place by slip along atomic planes.' This slip may be inhibited in a number of ways: by the interatomic forces of, cohesion which bind the atoms rigidly in a lattice structure, which in pure metals is usually of high symmetry; by latticc distortion caused by solid solution formation or by mechanical strain; by the intercrystalline boundaries whcrc slip is restrained, probably by the non-registration of the atom planes in adjacent crystal1ites;2 and by the presence of small hard particles which serve to "key" the slip along the atom planes.5 In pure metals, and perhaps also in solid solutions, the atom planes of easiest slip are those exhibhing the greatest density of atomic population and the greatest interplanar distance4 and apparently can now be pre-dict,ed from the analysis of the lattices. Concerning the interatomic forccs, which resist this slip by holding the atoms firmly together, little is known. Most textbooks on physical metallurgy, following the work of Bot-tone,5 correlate the hardness of the pure metals with the atomic volume,

By K. L. Myers, R. Espell, C. Deringer

Construction of the AA Pad reclamation was completed in the fall of 2000. Seeding of the ET cover began in the late fall of 2000 and continued through May of 2001. On Saturday afternoon, June 1, 2002, a large, very localized thunderstorm struck the reclaimed AA Pad site. Eyewitnesses present at the time described a dark storm cloud parked above the site for less than half an hour. Average rainfall intensity was measured to be 122 mm (4.8 inches) per hour and peak rainfall intensity was estimated to be 213 mm (8.4 inches) to 259 mm(10.2 inches) per hour. At the time of the storm, the construction was less than two (2) years old and the vegetation had only a single season of growth. The entire period from the end of construction until the date of the storm was a drought period with below normal precipitation. Other than a few small snowmelt events, there was no precipitation event large enough to produce any significant flow in the channel network. Therefore, the very first significant runoff event was the extreme event of June 1, 2002. The storm essentially represents a large-scale field test of the design concepts used at the AA Pad site. Shortly after the storm, data was collected and analyzed with the intent of learning as much as possible about the performance of the cover system design with the expectation that the newly acquired knowledge might be utilized in future designs to further improve the performance of similar cover systems during extreme events.

Jan 1, 2003

By S. B. King

IT is the purpose of this article to give those not familiar with the subject an idea of the extent to which coal is mined by machine in the United States; to describe some types of electrically operated coal cutters; and in particular, some of the latest improvements and developments in these machines. Generally speaking, the article deals with the mining of bituminous coal in room-and-pillar mines, as the use of undercutting machines in the anthracite region of Pennsylvania is in its infancy, and when machine mining is referred to bituminous coal is taken for granted. The number of mines in the United States that are operating on the long-wall principle is very limited, and the number of long-wall machines in use is a very small percentage of the total. The advantages of mining by machine may be summed up briefly as follows: A. Increased safety to property and life, due to the large decrease in the amount of powder required when the coal is properly undermined. B. Reduction in the cost of mining. C. Improvement in the quality of the product; and, consequently, increase in market value, due to the greater proportion of lump and screen sizes secured by machine mining. D. Increase in the capacity of the mine, and more rapid development of new mines. E. Ability to mine veins in which the height of the coal or the character of the roof has prevented mining by hand, on a commercial basis.

Jan 6, 1914

The organization of the American Institute of Mining Engineers, 75 years ago, parallels the beginning of present-day steel-producing methods in the United States. This early association with the industry is emphasized by the fact that the first open-hearth furnace constructed and operated in this country was then only three years old, and the first commercial bessemer converter was just seven years old. Total steel production in the year 1871, as recorded by the American Iron and Steel Institute, was 84,000 net tons, of which 2,000 tons was produced by the open-hearth process, 45,000 tons by the bessemer, and 37,000 tons by the crucible, puddled iron, and other processes. The bessemer process had thus become the major source of steel production. Its capacity expanded progressively during the following decade, and by 1880 was the source of approximately 86 pct of total steel production. Most of this tonnage was made in eastern Pennsylvania and used in rail manufacture. At about this time, however, important changes began to occur which gave impetus to the production of steel on a much larger scale. The development of Lake Superior ores from 1870 to 1890 and the exploitation of the Mesabi Range in 1892 provided the industry with great quantities of high-grade ores. The abundance of coking coals and limestone in the region adjoining western Pennsylvania and the development of cheap water transportation on the Great Lakes tended to shift the center of iron and steel manufacture to an area west of the Allegheny Mountains. Encouraging these new develop-

Jan 1, 1948

By C. M. Haight

The mine blacksmith and drill-steel sharpening shop at the Franklin mine of the New Jersey Zinc Co. is on the surface, adjoining the main shaft. It is a brick building, 51 by 30 ft. inside dimensions, with a corrugated iron roof and concrete floor. .About two-thirds of the steels used are brought up through the main shaft; the remainder through two auxiliary shafts and are carried to the shop by team or truck. At each shaft sufficiently large stocks of sharp drills of various typcs are kept to replace all the dull steels that may be sent up; while at the shop enough sharp drills are kept to replace the dull steels in the stocks kept at the auxiliary shafts. Though this entails keeping a larger number of drill steels in service than might be required by other methods, there is less hurry in the sharpening shop and the steels have a longer period of rest. If a rest from use enables steel to recover from fatigue strains, this method secures that rest. The forms shown in Fig. 1 are supplied to each shift boss in books of 100. These are used to requisition sharp drills from the shaft stocks and cnable the men at the tops of the shafts to sort out the required sizes and to hare them ready to be sent to the various shaft stations. At one of the auxiliary shafts, the dull drills are placed on a platform from which they are dumped into the body of the wagon that takes them to the shop.

Jan 1, 1927

By Debbie Nakamura, Daniel Tempelis, John E. Shamma

The Metropolitan Water District of Southern California established a Board of Consultants to assist them in administering the design and construction of the Inland Feeder Program tunnels. The Board acts as an expert review body for the owner, looking at key issues that can potentially impact the success of the program. The use of the Board evolved over the life of the project, and its composition was modified to better address the needs of the owner, and the Program requirements. The experience, function, and value of such a board is analyzed and discussed in this paper.

Jan 1, 2003

By Eliot J. White

The physical properties and clay mineral content of the major oil-producing formations in the Powder River Basin of Wyoming were determined by analyses of cores from 100 wells. Interrelationships were established among permeability, restored water saturation, clay content, and bulk swelling capacity of the crushed sample and used to estimate the susceptibility of the formations to water damage. The ratio of water permeability to gas permeability (kw/ki) offers a convenient scale for semiquantitatively estimating the water sensitivity of sands. The irreducible water saturation was also found to have a similar relationship to the clay mineral content and the water sensitivity of the sands. The average relation of water permeability to gas permeability is different for each sand, as shown by the curves, and the relative positions of the curves indicate the degree of water sensitivity of each sand from which the susceptibility to water damage may be estimated. How accurately these estimates show formation behavior under field operations will not be known until studies of field performance can be made. The water permeabilities of the Muddy, Minnelusa, and Tensleep sands average about the same as the gas permeabilities, and these sands are classified as insensitive. The water permeabilities of the Sussex and Shannon sands, at the other extreme, are much less than the gas permabilities [when average ki is 30 millidarcys (md), kw is 6.1 md], and these sands are classified as highly water sensitive. The sensitivities of the five other sands are between these extremes.

Jan 1, 1962

By Donald A. Dahlstrom

The selection and sizing of filters depends on the characteristics of the type of filter and the feed slurry. In addition, the rate functions of cake formation, cake washing and cake dewatering must be determined in order to design the filter station on the basis of desired performance. This chapter discusses the applied theory used to determine the rate functions and illustrates how to incorporate these into the filter cycle to obtain the required objectives. This also permits the sizing of the filter and auxiliaries as well as the selection of the proper type of filter.

Jan 1, 1978

By R. W. Thompkins

"PREFACEPart 1 of this paper, published in the September issue, covered the occurrence of uranium, radiation from uranium ores, the uranium series, radioactive theory, radioactive equilibrium and application to the radon series, the working level, the theory of emanation and diffusion, transport by thermal diffusion of radon emanating from porous rocks, and definitions.The October issue carried Part 2, which dealt with radiation theory applied to uranium ores, other radon migration factors, factors affecting the radon gas release rate, the measurement of radon gas emanation rates, the tunnel concept, variation of emanation rate with grade and estimating radioactivity from grade analysis.Part 3, in this issue, concludes the series by discussing the techniques for controlling radiation and providing some example calculations.17.0. Techniques for Controlling Radiation17.1. Altering the Factors In the Diffusion EquationIt has been noted that radon gas emanates from the surfaces of exposed ore to the mine atmosphere. The diffusion laws establish the rate of this flow. The fundamental relationship is that the rate of flow (J) is a function of the pore concentration and the distance from the surface. It is expressed as: []If any of these terms is varied, either naturally or artificially, the rate of gas emanation will be altered.Altering the Diffusion CoefficientThe literature describes many ways to lower the radon gas emanation rates which are dependent on changing the diffusion coefficient:1. A layer of ice on top of a tailings dam or on a soil.2. Humid clayey materials and swamped soils over a radon source."

Jan 1, 1982

By H. R. Maggard, C. M. Bollinger

Solving the problem of detecting underwater explosions from "dynamite fishing" can be done by using a system of sonobuoys programmed to detect the acoustic waves from underwater explosions. The system includes three anchored sonobuoys, which have radio communication to a central station. Each sonobuoy will detect the direction the blast occurred, and then send the magnitude of the acoustic waves and the blast direction to the central station where the blast distance will be calculated. The central station can the send the coordinates to the authorities who can find the location using GPS systems onboard their boats.

Jan 1, 2004

By R. F. Favreau, Patrice Favreau

In many quarries and construction sites visited by the authors over the last 50 years, the latter have observed muck piles from blasting with explosives, which included numerous large blocks, in some cases of dimensions larger than the input to the crusher. The names of these sites cannot be given in the article because the owners insist that data obtained on such visits be kept confidential. Often the blasters felt that the natural fissures in the rock would compensate for the use of a low powder factor, and they asked the authors to explain why such blocks were present. A detailed analysis of the situation often indicated that the cause of the blocks is that explained by figures such as 6 and 7 below in the article.

Jan 1, 2018

By A. Hemami

In order to automate the operation of mechanical loaders it is essential to have a knowledge of the forces that act on the bucket and of the trajectory that the bucket should follow. A trajectory for the cutting edge of a bucket is derived from studies of the forces acting during the scooping phase. The proposed trajectory has a minimum energy consumption and is simple to automate. It is determined initially by setting to zero certain components of the resistive forces to the bucket motion which would otherwise result in unnecessary work and consequent energy wastage. The method for finding the appropriate trajectory is discussed on the basis of the properties of the material to be loaded and the loader size.

Jan 4, 1993

By Michelle L. Ramos

INTRODUCTION The Ballard Siphon was built in 1935 and consists of two 91.4 cm (36-inch) diameter wood-stave pipes. These pipes convey sewer flowsunder the Ship Canal from northwest Seattle and the Ballard Regulator to the North Interceptor and the West Point Treatment plant. The siphons were constructed using open cut construction, are now buried in the sediment on the floor of the canal, and have severely limited ability to be dewatered, inspected, or cleaned. The existing siphon is 394.7 m (1,295 feet) long from the junction structure on the southern shoreline to the regulator structure on the north. The location of the Ballard Siphon is shown in Figures 1 and 2. The area around the Ballard Siphon has become more populated and developed since the siphon was built. Additionally, the Ballard Siphon is subject to high flows that are greater than the capacity of the pipelines. This has resulted in predict-able Combined Sewer Overflows(CSO?s) whenever a large, long duration rain event occurs. The aged pipeline of uncertain viability has become a critical piece of the sewer system infrastructure. Because of the age of the pipelines and their importance, a sonar survey was completed on both barrels of the Ballard Siphon in December of 2005. The sonar images appeared to indicate crown intrusion of the wood-stave pipes, which suggested that the pipes were in imminent danger of collapse. As a result, an Emergency Declaration was executed by King County and the Ballard Siphon Replacement Project was initiated. Staheli Trenchless Consultants was retained to perform feasibility studies to deter-mine the viability of using microtunneling and horizontal directional drilling (HDD) for replacement of the Ballard Siphon. For the evaluations, the preferred site location was determined to be at or near the site of the existing Ballard Siphon in order to minimize the ancillary sewer work which would accompany moving to a new site. To meet flow demands and hydraulic requirements, the replacement siphon needed a mini-mum equivalent diameter of 182.9 cm (72 inches). This could be accomplished with a number of different siphon diameters and configurations including, but not limited to, three 106.7 cm (42-inch) diameter pipelines, two 152.4 cm (60-inch) pipelines, or two 91.44 cm (36-inch) pipelines and a 121.9 cm (48-inch) pipeline.

By R. K. Rajamani

The theoretical model based on fluid mechanics, in conjunction with the laser-Doppler velocimetry (LDV) measurements, elucidate the size-classification mechanisms in an industrial hydrocyclone. The model has no adjustable parameters and involves solving the Navier-Stokes equations to predict the liquid-phase velocities. The spatial-concentration gradients were determined considering the particle phase in the Lagrangian frame and the classification curve was determined by balancing the forces acting on the particle. The force balance requires liquid velocities, which in turn depend on the local volumetric concentration of the particles. Hence, complete modeling work involves coupling both the concentration and liquid-phase velocity calculations until convergence is reached. Finally, the experimental and predicted classification curves were presented for 250-mm hydrocyclone operating at high-percent solids.

Jan 1, 1994

By R. Poulin, R. Pakalnis, D. Peterson

Introduction A comprehensive project has been completed at the University of British Columbia that focused on the development of a commercially competitive composite cable bolt. Laboratory evaluation consisted of pull tests, preliminary shear tests, grout column testing and scanning electron microscope evaluation of the composite cable bolt. Field implementation at five underground mines throughout Canada were completed for technical and overall performance evaluation of the new product. The project began in 1989 under the sponsorship of HDRK Ltd., a consortium of mining companies including Inco, Noranda and Falconbridge Ltd. The objective was to develop a cuttable cable bolt that would serve as support for a continuous miner within a hardrock environment (Mah, 1994). The bolt was required to be cuttable by a continuous roadheader without adverse effects to equipment, personnel and the milling process. From the beginning, the focus was to employ existing cable bolt installation technology (Goris et al., 1994) whereby the cable bolts are grouted within a 4.8-cm-diam (1.08-in.diam) or larger employing a portland cement grout having a water: cement ratio between 0.35:1 to 0.4:1. The prototype, developed from Phase I, was technically comparable to that of conventional steel cable bolts. However, high cost and limited accessibility hindered its commercial acceptance. The second phase of the project was sponsored by the British Columbia Science Council and Pacific Pultrusions Ltd. of British Columbia to locally develop a glass fiber cable bolt. This phase of the project has resulted in the DAPPAM cable bolt (Pakalnis et al., 1994). DAPPAM Cable bolts are the second most used support method in Canadian underground mines after mechanical rock bolts. It is projected that 870,000 m (2.9 million ft) of cable bolts are installed annually in Canada (Poulin et al, 1994). The objective of the research program was to develop a glass fiber cable bolt with similar pullout strengths to the conventional steel cable bolts (267 kN - 60,000 lbf). More than 200 laboratory pull tests were conducted employing standard cable bolt test procedures, as outlined by the US Bureau of Mines (Goris, 1994), to assess optimum rod and surface composition, geometry, number required, pullout and shear characteristics, among others. This resulted in the DAPPAM cable bolt (Fig. 1). It consists of 10 individual 0.6cm-diam (0.25-in.-diam) rods enveloping a 2.2-cm (0.8-in.) outside diameter, high-density polyvinyl grout tube. The composite used in the construction of the rods is comprised of about 65% glass fiber within a 35% polyester resin matrix (by volume). Through pultrusion (a continuous fabrication technique), the fibers and resin are combined into a composite material. The strength of the overall composite is largely governed by the material properties, the alignment [ ] of the fibers relative to the applied load and the density and interaction of the overall components within the composite. A further modification to the composite was the addition of a sand grit to the surface of the individual rod. This increased the overall bond strength between the rod and the cement-based grout, used to solidify the cable bolt to the rock mass. The grout tube has an inside diameter of 1.9 cm (0.75 in.) and is rated at a pressure of 1.72 MPa (250 psi). During installation, the grout is pumped through the annulus of the grout tube thereby filling the hole from toe to collar. Laboratory and field trials concluded that a minimum drill hole diameter of 4.8 cm (1.08 in.) be used to ensure optimum grout coverage. Table 1 compares the design strengths (as tested) for DAPPAM vs. the ultimate strengths for a conventional 1.6cm (0.6-in.) steel cable bolt. The characteristics for the steel cable have been derived directly or indirectly by Goris et al. (1994). A design tensile strength of 289 kN (65,000 lbf) was proposed for the composite developed. However, recent tests have indicated maximum breaking strengths of more than 400 kN (90,000 lbf) (Fig. 2). Figure 2 shows the load vs. displacement pull out curves for steel and DAPPAM cable bolts. The methods of testing were standardized so as to be able to compare the results directly. The shear strength of the fiberglass cable is largely a function of the surface area sheared. Shear strengths of 89 kN (20,045 lbf) were obtained for the configuration shown in Fig. 1 when sheared normal to the axis of the cable. The testing procedure was similar to the shear tests performed on steel by Goris (1993). It is important to reinforce the implication that critical bond strength has on the success of an overall support system.

Jan 1, 1995

By W. M. McKewan

Magnetite pellets were reduced in flowing hydrogen at pressures up to 40 atm over a temperature range of 350° to 500°C. The rate of weight loss of oxygen per unit area of the reaction surface was found to be constant with time at each temperature and pressure. The reaction rate was found to be directly proportional to hydrogen pressure up to 1 atm and to approach a maximum rate at high pressures. The results can be explained by considering the reaction surface to be sparsely occupied by adsorbed hydrogen at low pressures and saturated at high pressures. PREVIOUS investigation1,2 have shown that the reduction of iron oxides in hydrogen is controlled at the reaction interface. Under fixed conditions of temperature, hydrogen pressure, and gas composition, the reduction rate is constant with time, per unit surface area of residual oxide, and is directly proportional to the hydrogen pressure up to one atmosphere. The reduction rate of a sphere of iron oxide can be described3 by the following equation which takes into account the changing reaction surface area: where ro and do are the initial radius and density of the sphere; t is time; R is the fractional reduction; and R, is the reduction rate constant with units mass per area per time. The quantityis actually the fractional thickness of the reduced layer in terms of fractional reduction R. It was found in a previous investigation2 of the reduction of magnetite pellets in H2-H,O-N, mixtures, that the reaction rate was directly proportional to the hydrogen partial pressure up to 1 atm at a constant ratio of water vapor to hydrogen. Water vapor poisoned the oxide surface by an oxidizing reaction and markedly slowed the reduction. The enthalpy of activation was found to be + 13,600 cal per mole. It was also found that the magnetite reduced to meta-stable wüstite before proceeding to iron metal. The following equation was derived from absolute reaction-rate theory4,8 to expfain the experimental data: where Ro is the reduction rate in mg cm-2 min-'; KO contains the conversion units; Ph2 and PH2O are the hydrogen and water vapor partial pressures in atmospheres; Ke is the equilibrium constant for the Fe,O,/FeO equilibrium; Kp is the equilibrium constant for the poisoning reaction of water vapor; L is the total number of active sites; k and h are Boltzmann's and Planck's constants; and AF is the free energy of activation. Tenenbaum zind Joseph5 studied the reduction of iron ore by hydrogen at pressures over 1 atm. They showed that increasing the hydrogen pressure materially increased the rate of reduction. This is in accordance with the work of Diepschlag,6 who found that the rate of reduction of iron ores by either carbon monoxide or hydrogen was much greater at higher pressures. He used pressures as high as 7 atm. In order to further understand the mechanism of the reduction of iron oxide by hydrogen it was decided to study the effect of increasing the hydrogen pressure on rebduction rates of magnetite pellets. EXPERIMENTAL PROCEDURE The dense magnetite pellets used in these experiments were made in the following manner. Reagent-grade ferric oxide was moistened with water and hand-rolled into spherical pellets. The pellets were heated slowly to 550°C in an atmosphere of 10 pct H2-90 pct CO, and held for 1 hr. They were then heated slowly to 1370°C in an atmosphere of 2 pct H2-98 pct CO, then cooled slowly in the same atmosphere. The sintered pellets were crystalline magnetite with an apparent density of about 4.9 gm per cm3. They were about 0.9 cm in diam. The porosity of the pellets, which was discontinuous in nature, was akrout 6 pct. The pellets were suspended from a quartz spring balance in a vertical tube furnace. The equipment is shown in Fig. 1. Essentially the furnace consists of a 12-in. OD stainless steel outer shell and a 3-in. ID inconel inner shell. The kanthal wound 22 in. long, 1 1/2, in. ID alumina reaction tube is inside the inconel inner shell. Prepurified hydrogen sweeps the reaction tube to remove the water vapor formed during the reaction. The hydrogen is static in the rest of the furnace. The sample is placed at the bottom of the furnace in a nickel wire mesh basket suspended by nickel wire from the quartz spring. The furnace is then sealed, evacuated, and refilled with argon several times to remove all traces of oxygen. It is then evacuated, filled with

Jan 1, 1962

By E. Miller, J. M. Eldridge, K. L. Komarek

The thermodynamic properties of liquid Mg-Ge alloys have been determined between 1000°and 1500°K by an isopiestic method. Germanium specimens, heated in a temperature gradient and contained in covered graphite crucibles of special geometry, were equilibrated with magrtesium vapor in closed titanium tubes. The crucible design allowed free access of magnesium vapor to the samples during the equilibration to form alloys of magnesium and germanium, but prevented magnesium losses from the crucibles on quenching the titaniuin tubes to terminate the experimental runs, thus preserving the equilibrium alloy compositions. The activities and partial molar enthalpies of magnesium and the integral thermodynamic properties of the system were calculated from the experimental data. THE Mg-Ge phase diagram' shows one congruent melting compound, Mg2Ge, of essentially stoichio-metric composition, two eutectics, and very limited terminal solid solubilities. Very little information is available on the thermodynamic properties of the Mg-Ge system. The free energy of formation of Mg,Ge was recently deter-mined2 by a Knudsen cell technique in the temperature range 610° to 760°C. The standard enthalpy of formation of Mg,Ge was measured calorimetrically by Bever and coworkers.3 The present study was undertaken as part of a general investigation of the thermodynamic properties of the homologous series of Mg-Group IVB systems, i.e., Mg-Pb,4 Mg-Sn,5 Mg-Ge, and Mg-Si. An isopiestic technique was used which was developed by the authors5 for investigating the thermodynamic properties of liquid Mg-Sn alloys. Specimens of the nonvolatile component, contained in covered graphite crucibles, are heated in a temperature gradient in an evacuated and sealed titanium reaction tube, and equilibrated with magnesium vapor of known pressure. The method employs crucibles of special geometry which preserve the high-temperature equilibrium composition of liquid alloys having a highly volatile component such as magnesium on termination of the experimental runs by quenching the crucibles to room temperature. EXPERIMENTAL PROCEDURE First reduction germanium of 99.999+ pct purity (Eagle-Pitcher Co., Cincinnati, Ohio) and 99.99+ pct magnesium metal (Dominion Magnesium Ltd., Toronto, Canada) were used. The graphite crucibles were machined from high-density (1.92 g per cu cm) graphite rods (Basic Carbon Corp., Sanborn, N.Y.) which had a maximum ash content of less than 0.04 pct. The non-reactivity of graphite with germanium at the temperatures used in this study had been previously established by Scace and Sleck.6 The experimental procedure has been previously described in detail.5 The selection of a particular crucible geometry for a run was determined by a combination of imposed experimental conditions, the principle being that more tightly covered crucibles were required to preserve alloy compositions during quenching when higher magnesium pressures and higher specimen temperatures were used. Depending upon the composition range of the equilibrated alloys the source of the magnesium vapor was either pure magnesium or a two-phase mixture of Mg2Ge + Ge-rich liquid of known magnesium pressure. The experimental runs can be divided into the following three groups on the basis of crucible geometry and magnesium source material. Crucibles with Small Holes and Pure Magnesium Reservoirs. The crucible dimensions were identical to those of the Mg-Sn investigation5 except that the hole diameters were reduced to 0.010 in. because of the higher temperatures and higher magnesium pressures involved in the Mg-Ge system. During an equilibration run, magnesium vapor diffused from the reservoir to each specimen through the small holes, one drilled through the crucible lid and two others drilled through graphite baffles positioned vertically inside the crucible between the lid hole and the specimen. Since the magnesium pressure was high, i.e., in the range 117 to 277 Torr, during the equilibration time of approximately 24 hr, equilibration was not impeded by these holes. A specimen composition at equilibrium was fixed by the relative temperatures of the specimen and the reservoir, and by the thermodynamic properties of the system. Upon brine quenching the titanium reaction tube to end a run the vapor pressure of magnesium above the liquid alloys decreased exponentially with decreasing temperature, and the small cross-sectional areas of the holes (4.9 x 10"* sq cm) drastically reduced magnesium losses from the crucibles. Because of its low vapor pressure, germanium losses from crucibles during a run were at most 0.2 mg for pure germanium and correspondingly less for the alloys. This crucible geometry satisfactorily retained the equilibrium alloy compositions on quenching for magnesium-rich (from 3 to 33 at. pct Ge) alloys provided their temperatures were below the melting

Jan 1, 1967