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By R. S. Dean

"INTRODUCTION The idea of direct steel is by no means new. Although the work of Bessemer and Siemens provided simple and effective moans for converting pig iron into steel and established the ""blast-furnace route"" as the almost universal method of producing steel, metallurgists have not ceased to dream of direct steel. By direct steel is meant any process by which iron oxide in ore is reduced to Iron of the same or greater purity than the final steel or wrought iron. That is, carbon or alloying elements would be added as needed, not reduced in unwanted quantities into the iron and then removed more or completely by refining (Bessemer or open hearth) only to be readded in desired quantities.In general, direct-steel processes are ""sponge-iron"" processes, because reducing iron oxide without simultaneously alloying the iron with carbon, phcophorus, sulfur, and silicon present in ore and fuel succeeds only if the temperature is below the melting point of the iron. Such solid iron formed by reduction of iron oxide at relatively low temperature is sponge iron, which is butlery and porous. When the reduction proceeds at the higher temperature at which the particles of metal can weld together or finally even melt to yield pellets or balls that do not have the porosity and low-density characteristic of sponge iron, the product might preferably be called simply ""direct iron."""

Jan 1, 1945

By Patrick D. McMaster

"INTRODUCTION According to the Roane Iron Co. of Rockwood, Tenn., the Chamberlain. Barnardville iron deposit produced approximately three million tons of iron ore previous to 1928. The deposit is divided into two synclinal bodies termed the north and south synclines. Production has come from the northern extremities of both bodies.The need for developing additional iron-ore reserves during the war prompted the Bureau of Mines to initiate an exploratory program on the Chamberlain-Barnardville deposit in February 1944, which continued until December 1944.ACKNOWLEDGMENTSIn its program of exploration of mineral deposits, the Bureau of Mines has as its primary objective the more effective utilization of our mineral resources to the end that they make the greatest possible contribution to national security and economy. It is the policy of the Bureau to publish the facts developed by each exploratory project as soon as practicable after its conclusion. The Mining Branch, Lowell B. Moon, chief, conducts preliminary examinations, performs the actual exploratory work, and prepares the final report. The Metallurgical Branch, R. G. Knickerbocker, chief, analyzes samples and performs beneficiation tests. Both these branches are under the supervision of Dr. R. S. Dean, assistant director."

Oct 1, 1946

This paper describes a detailed geostatistical study of producing copper orebodies at Mount Isa Mines Limited in Queensland, Australia. As a result of this work, kriging has been adopted for grade estimation for final stope design at Isa Mine. Extensive variogram and back analysis studies indicate that one relative variogram model can be used to give optimal kriged grade estimates from production sampling throughout the 100 million tonne copper orebody complex. The kriging method replaces a computer technique used at [sa Mine based on inverse distance weighting using parameters chosen from experience.Comparative stope designs based on 10 million tonnes of ore indicate a 16% increase in minable ore tonnage at a grade well above the cut-off, as a result of the geostatistical work.Although this paper is written as a practical description with simple explanations of geostatistical concepts, the theory and use of relative variograms has been expanded. A possible link is suggested between relative variograms and first order kinetics of natural mineral concentration processes.

Jan 1, 1982

By Charles B. Carpenter

The New Hope field was selected for study by; Bureau of lanes engineers because many problems met by, the operators during development and operation were unique to petroleum-engineering experience. Solving these problems is believed to have doubled the ultimate recovery of oil from the field. Since the discovery well was 'completed, in April 1943, an oil-productive area of 4,950 acres- has been delineated by the drilling of 64 wells, four of which were dry holes. Four oil-bearing reservoirs - the Bacon oolitic limestone, and the Hill, Pittsburg) and Elledge sandstones, all, in the Trinity group of the Lower Cretaceous series-- have been penetrated at depths ranging from 7,300 to 8,100 feet. Three of these reservoirs were found to be closed-type or solution gas-drive reservoirs, and one - the Hill - was an open-type or water-drive reservoir. During the course of the study, the Tide Water Associated, Oil Co. and -Seaboard al Co. of Delaware made available to the writers all well records, electric logs; and coring, production,, and pressure data. The ,writers performed Certain field and laboratory- tests on cores of ,the reservoir racks and' samples -of the reservoir Oils. Analyses of cores from the four reservoirs showed average .porosities ranging from 10 to 18 percent, average permeabilities of 17 to 297 millidarcys, and -average 'connate water contents ranging from 25.4 to 30.6 percent. Subsurface and recombined samples of reservoir oils indicated that the oils in the Bacon Hill, and Pittsburg reservoirs contained ,206 to 422 cubic feet of gas in solution per barrel initially, and that the, reservoir oils were undersaturated with gas. No samples' of oil from the Elledge reservoir were analyzed, and because of meager data this reservoir was not studied in detail. 4 The presence of free 'gas' or a' gas cap, however, indicated that the oil in the Elledge reservoir was saturated with gas. The rapid decline in pressures in- the' four reservoirs during the 'first year of operation alarmed the operators and provoked them to investigate the reservoir conditions to determine the cause.

Jan 1, 1949

By W. Joseph Schlitt, William D. Southard, Bruce P. Ream, Lawrence J. Haug

The operation of Kennecott's Bingham Canyon copper precipitation plant, one of the world's largest, is described. This description includes a brief historical review of precipitation at Bingham and the general layout and operation of the present cone cementation facility. Current practices are based on results of studies undertaken to define improvements needed in each unit operation. These improvements were required to meet changing plant conditions and were implemented primarily within the constraints of the existing facilities. Specific unit operations included were the cone precipitators, the cone discharge thickener, the cone effluent settling basins, and the plate and frame filter presses. As a result of these improvements, loss of precipitated copper decreased and the degree of precipitation increased, raising copper recovery by 9 t/d. At the same time, iron consumption was reduced by 22.5 t/d. Problems in drying the cement copper were also overcome so that a product containing 12 - 15% moisture could be consistently delivered for smelting.

Jan 6, 1979

By William D. Southard, Joseph W. Schlitt, Bruce P. Ream, Lawrence J. Haug

The operation of Kennecott 's Bingham Canyon copper precipitation plant, one of the world's largest, is described. This description includes a brief historical review of precipitation at Bingham and the general layout and operation of the present cone cementation facility. Current practices are based on results of studies undertaken to define improvements needed in each unit operation. These improvements were required to meet changing plant conditions and were implemented primarily within the constraints of the existing facilities. Specific unit operations included were the cone precipitators, the cone discharge thickener, the cone effluent settling basins, and the plate and frame filter presses. As a result of these improvements, loss of precipitated copper decreased and the degree of precipitation increased, raising copper recovery by 9 t/d. At the same time, iron consumption was reduced by 22.5 t/d. Problems in drying the cement copper were also overcome so that a product containing 12-15% moisture could be consistently delivered for smelting.

Jan 1, 1980

By Richard A. Thomas, Liming Yuan, Lihong Zhou, James H. Rowland

Hydrogen (H2) gas released during battery charging can result in cross-interference for carbon monoxide (CO) sensors used for early fire detection and compromise the integrity of the mine atmospheric monitoring system (AMS). In this study, a series of laboratory-scale and full-scale experiments were conducted to evaluate the responses of different CO sensors to H2 gas. In the laboratory-scale experiments, constant H2 concentrations in the airflow, from 100 to 500 ppm, pass through sensors. While in the full-scale experiments, increasing H2 concentrations generated as a byproduct from charging the batteries at the battery charging station rise to the sensors under different ventilation scenarios. The H2 concentrations at the CO sensor location were measured using H2 sensors and were correlated with the CO sensor response. The effects of ventilation and sensor location on the CO sensors responses were also analyzed. The results of this study can help mining companies to select appropriate CO sensors and improve the deployment of these sensors to ensure the safeguard of underground miners.

By N. J. Ferguson

An upsurge in demand for Australian coal has seen a much needed programme for a new generation of coal ports. This paper discusses design concepts in planning a large modern terminal, with the 25 Nt/a Port Kembla and the 50 Mt/a Newcastle facilities as practical examples. The need is emphasised for a studied Master Plan, in-built materials handling flexibility and staged development. Trends in bulk ship design and loading methods are noted. Features of these Australian designs include methods of dealing with poor ground conditions, functional civil engineering for environmental protection and optimal marine structure designs.

Jan 1, 1982

By R Mann, R Prasad, S Vink, V Nanjappa

The level of salinity that various aquatic organisms can tolerate without incurring any adverse effects is dependent on several environmental and evolutionary factors. These factors include the relative concentrations of different types of dissolved salts in the water that makes up their habitat, the regimes to which organisms are exposed to waters of differing salinity levels (including naturally derived variations), the degree to which an organismÆs life history stages have adapted to salinity, an organismÆs ability or behaviour to avoid adverse levels of salinity and an organismÆs capacity for osmoregulation.Release of saline water into rivers of the Fitzroy catchment has created concern about the impact on aquatic organisms. Not only is salinity itself a stressor on organisms but different ionic compositions will moderate the effects. Ecotoxicology experiments were conducted using artificial saline water based on mine water chemistry using sensitive macroinvertebrates collected from the catchment, as well as a range of laboratory organisms in accordance with the ANZECC and ARMCANZ (2000) guidelines. The 95 per cent ecosystem protection value calculated from species sensitivity distribution derived from the commercial tests was estimated to be ~2.0 mS/cm. For the protection of 99 per cent of the species the salinity has to be reduced by more than 50 per cent to 0.91 mS/cm. The electrical conductivity (EC) values, derived by commercial testing and species sensitivity distribution in this study suggests that salinity contaminant trigger values previously developed using a referential approach for protection of aquatic ecosystems from saline mine water releases in the Fitzroy may be conservative.CITATION:Vink, S, Mann, R, Nanjappa, V and Prasad, R, 2013. Determining the impacts of salinity on freshwater organisms, in Proceedings Water in Mining 2013 , pp 149-154 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Nov 26, 2013

By John R. Bartels

This report discusses an improved method for rerailing underground railcars devised in a joint effort by the Bureau of Mines and Hoesch MFD. This improved method utilizes a lightweight hydraulic ram with hand-pump activation to move a bridge-mounted roller carriage in conjunction with steel-reinforced air-lift bags. This method provides a lightweight portable system in which only two workers are required to perform the mine car rerailing operation. Because of the very narrow confines in underground mines, use of overhead cranes and other surface rail techniques is not possible. This new system is designed for very low profile work, and provides the necessary lifting force from light- weight compressed-air bottles.

Jan 1, 1985

By Harold P. Rue

The problem of removing hydrogen sulphide from natural gas has become within the last few years one of major importance to the natural gas and petroleum industry. Several gas fields in the United States produce natural gas containing hydrogen sulphide, and a number of oil fields produce gas which contains hydrogen sulphide. 3 The percentage of hydrogen sulphide in natural gas produced in these fields varies from a fraction of 1 per cent to as high as 20.5 per cent by volume. Hydrogen sulphide is probably the most toxic gas associated with natural gas, and from the standpoint of health and safety it is important that the hydrogen sulphide be removed if the gas is to be used for domestic purposes. Hydrogen sulphide, besides being toxic and therefore a hazard to animal life, is under certain conditions an active corrosive agent and very destructive to equipment. The annual loss caused by the corrosive action of hydrogen sulphide on equipment amounts to hundreds of thousands, perhaps millions, of dollars. The largest percentage of natural gas produced in the United States comes from wells which also produce oil. This associated gas invariably carries with it light fractions of petroleum, which when separated from the gas, condense to the liquid form at ordinary temperatures and pressure. Commercial application is made of this natural condition, and "wet gas" is processed to obtain so-called natural gasoline by employing the principles of absorption, adsorption, or compression and subsequent expansion accompanied by cooling. In the manufacture of natural gasoline from wet gas which contains hydrogen sulphj.de, if this contaminating gas is not first removed, some of the hydrogen sulphide may oxidize to form free sulphur and water. The free sulphur will dissolve in the gasoline produced by any of the aforementioned methods and cause the product to be positive to the corrosion test and there-fore unsuitable for commercial use in that condition. The objectionable sulphur compounds can be removed by washing the gasoline with a solution of caustic soda or other chemicals, but this treatment is expensive. It is advantageous therefore to remove the hydrogen sulphide from the gas before it is processed in a natural-gasoline plant.

Jan 1, 1932

By Donald E. Redmon

This Bureau of Mines report reviews injury experience in the nonmetallic mineral industries (except stone and coal) for 1968-69. For each of the years, 23 tables summarize disabling work injuries by department, source of injury, extent of disability, part of body injured, and nature of injury. Correlative information on employment, worktime, and operating activity is also presented.

Jan 1, 1973

By J. H. Field

The sulfur dioxide emitted in low concentrations in flue gases from the combustion of sulfur-containing coals and fuel oils is a significant factor in contamination of the atmosphere with sulfur dioxide. A review of methods for treating gases containing high concentrations of sulfur dioxide shows that they are seldom satisfactory for purifying flue gases. Processes developed specifically for treating flue gases using liquid absorbents are costly and may cause localized pollution, because the cooled flue gases can settle in the vicinity of the stack. Bench-scale research is being conducted to investigate the use of dry absorbents for sulfur dioxide removal at temperature levels of about 250°- 300° F. and 600°-650° F. Alkalized alumina has been found effective for treating simulated flue gas and Is regenerable by hydrogen, carbon monoxide, or producer gas. Other metallic oxides have been tested as absorbents also. Chemically impregnated activated carbons removed sulfur dioxide from the gas at 265° F. Vanadium pentoxide is effective as a catalyst for oxidizing of sulfur dioxide in the simulated flue gas at temperatures lower than have been used commercially for gases with higher concentrations of sulfur dioxide. Conversions of sulfur dioxide to trioxide wore studied as a function of temp- erature over a range of about 570° to 750° F.

Jan 1, 1959

By Margaret E. Egan

Reliable fire detection is essential for both safe evacuation and containment or extinguishment. In order to increase reliability by reducing the number of nuisance fire alarms in underground mines that use diesel-powered equipment, the U.S. Bureau of Mines has developed a diesel-discriminating fire detector (DDD). It was designed to discriminate between smoke produced by a fire and the smoke-laden exhaust of a diesel engine. Experiments were conducted by the Bureau to compare the smoke detection capabilities of the DDD with those of conventional fire detectors in response to smoldering coal and conveyor belting. A comparison was made among the alarm times of a carbon monoxide (CO) detector with an alarm threshold of 5 ppm, a smoke detector with an optical density alarm threshold of 0.044 of', and the DDD with an alarm threshold of 0.025 V. The results show that the DDD will reliably detect developing coal and conveyor belt fires. The average time delay separating the DDD alarm from the first detector to alarm was 76 s for smoldering conveyor belt and 65 s for smoldering coal. The longest time delay between the response of the DDD and the first detector to alarm was approximately 120 s.

Jan 1, 1993

By Marcie A. Greenberg

The Fence Lake Project is located in the Salt Lake coal field, an extension of the San Juan Basin. Geologic formations exposed in the Project area range in age from late Cretaceous to Quaternary. Coal is encountered in the Moreno Hill Formation (upper Cretaceous). Salt River Project (SRP) followed the basic textbook approach for the exploration, regional appraisal, detailed reconnaissance, detailed surface appraisal and three dimensional sampling (physical exploration). SRP is exploring this property as a potential fuel source for the Coronado Generating Station. Therefore, for the physical exploration stage, the quality sampling program was designed from a utility company viewpoint to determine possible impacts to the Station. Exploration drilling was completed in spring, 1982; September, 1982, and summer, 1984. Engineering, environmental, and land acquisition studies were added in the Summer, 1984 Program to more closely evaluate the potential Fence Lake Project coal supply option for the Coronado Generating Station. Studies, including drilling, are ongoing-at this time.

Jan 1, 1984

By Aner W. Erickson

"Preliminary examination of tungsten deposits on the Mountain View property near Hyder, Alaska, was made by Neal M. Muir, an engineer of the Bureau of Mines daring the summer of 1942. Fifteen samples were cut, rough esti¬mates of ore reserves were made, and it was proposed to extend the drift on scheelite-bearing vein 300 feet in a northwesterly direction.From May 22 to October 24, 1944, an exploratory project was conducted on the property by the Bureau. In the course of this work, the camp buildings were rehabilitated; the dam, hydraulic line, and machinery were repaired; 226 feet of drift was driven; 80 groove samples aggregating 3.9 tons in weight were cut; a 6,000-foot surface and underground traverse was run; and the area was mapped in detail.In its program of exploration of mineral deposits, the Bureau of Mines has as its primary objective the more effective utilization of our mineral resources to the end that they make the greatest possible contribution to the national security and economy. It is the policy of the Bureau to publish the facts developed by each exploratory project as soon as practicable after its conclusion. The Mining Branch, Lowell B. Moon, chief, conducts preliminary examinations, performs the actual exploratory work, and prepares the final report. The Metallurgical Branch, R. G. Knickerbocker, chief, analyzes samples and performs beneficiation tests. Both these branches are under the supervision of Dr. R. S. Dean, assistant director.Special acknowledgment is doe Neal W. Muir, project engineer, and Robert S. Sanford, acting chief, Alaska Division, Mining Branch, for their supervision of the field work and revision of the report.Acknowledgment is also made to Silbak Premier, Ltd., for rendering valuable assistance in the repair of equipment and for extending various courtesies to Bureau of Mines personnel during the conduct of this project.The Mountain View property is located at latitude 55° 59' north, and longitude 130° 03' west in the Salmon River mining district of southeastern Alaska, about 5 miles in a northwesterly direction from the town of Hyder, which lies at the head of Portland Canal, as shown in figures 1 and 2. Vein outcrops and surface workings are at an elevation of 950 feet and occupy the west flank of a low ridge between Skookum and Fish Creeks, as shown in figure 3. The portal of the long adit exposing the vein at depth is on Skookum Creek about 550 feet north of the confluence of Skookum and Fish Creeks.Access to the property is over a 4-foot wide trail built and maintained by the United States Forest Service. This trail is suitable for pack animals and is adequate for transportation of supplies and material for exploratory work. During the periods of camp construction and past exploratory operations a 4,000-foot, single-cable, aerial tramway, now in disrepair, served for transportation of materials and all machinery from the Salmon River Highway to the property. The cost of such hauling was high, amounting to $12 a ton. Topography is suitable for construction of a ""cat road"" 2 miles in length, connecting the property with the Salmon River Highway. It is estimated that such a road could be built for $5,000 a mile, and supplies, machinery, and concentrates could be haled over it at a cost of less than $2.50 a ton."

Sep 1, 1946

By Kung-Lee Wang

This Bureau of Mines study illustrates the economic significance of the Florida phosphate industry to the State and to the Nation. Environmental considerations related to phosphate industry activity are discussed briefly. Based on forecasts of Florida phosphate production in 1975, and using 1972 dollars, regional and national output value, income, and employment created by the phosphate industry were estimated for 1975. State and Federal government tax revenues generated by the phosphate industry, are also measured. Further, the concentrated impact of the phosphate industry on certain Florida areas and on regional industries is examined. Finally, the phosphate industry's importance to the U.S. balance of payments, U.S. agricultural production, and the Frasch sulfur industry is considered, in addition to byproduct fluorine, and potential byproduct uranium from fertilizer manufacturing.

Jan 1, 1974

By I D. Gregson, A S. Garcia, K M. MacAndrew

The design work undertaken by Rock Mechanics Technology (now part of Golder Associates (Golder)) has played a major part in successfully establishing mechanised room and pillar working in Indian coalmines, both for the development of new districts and for the re-establishment of old districts prior to pillar extraction on panel retreat.Golder has used appropriate design of pillars, extraction sequences and final snook sizes to minimise ground control risks during pillar extraction. Where the strata will not cave reliably, partial extraction systems leaving either a crush pillar or a substantial yield pillar have been adopted.Remote monitoring of selected pillars during the extraction process using stress cells, extensometry and convergence measurements provides confirmation of pillar behaviour and verification of designs.A new telltale device, giving a visible warning of impending caving, is now installed at all Indian pillar extraction sites and is proving very successful.CITATION:MacAndrew, K M, Garcia, A S and Gregson, I D, 2014. Coalmine pillar design and performance during mechanised pillar extraction in India, in Proceedings AusRock 2014: Third Australasian Ground Control in Mining Conference , pp 347–358 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Nov 5, 2014

By Anja Pfennig, Axel Kranzmann, Phillip Zastrow

"Properties of pipe steels for CCS technology require resistance against the geothermal corrosive environment (heat, pressure, salinity of the aquifer, CO2-partial pressure). To predict the reliability of two different injection pipe steels with 13% chromium and 0.46% carbon (1.4034, X46Cr13) as well as 0.20% carbon (1.4021, X20Cr13) steel coupons were heat treated by comparable routines prior to long term corrosion experiment (60°C, 100 bar, artificial brine close to a CCS-site in the Northern German Basin, Germany). In general higher carbon content exhibits better corrosion resistance with respect to corrosion rate, amount of pits and maximum intrusion depth in the case of local corrosion. At 100 bar hardened steels with martensitic microstructure have the lowest corrosion rates with an average of 0.003 mm/a after 2000 h exposure time. At ambient pressure normalized steels show the lowest corrosion rates, indicating that the corrosion is driven by grain boundaries.IntroductionEngineering a geological on-shore saline aquifer CCS-site (CCS Carbon Capture and Storage [1-3]) corrosion of injection pipe steels may become an issue when emission gasses, e.g. from combustion processes of power plants, are compressed into deep geological layers [4-8]. Typically 42CrMo4 (1.7225, AISI 4140) is used for casing, and for injection pipe the steel X46Cr13 (1.4034, AISI 420 C) or X20Cr13 (1.4021, AISI 420 J) is used. Saline formations are the most favorable storage sites in Germany [9], because of their large potential storage volume and their common occurrence. Leakage of CO2 back into the atmosphere may be a problem in saline aquifer storage, especially around the water level within the borehole. Carbon dioxide corrosion may cause failure of pipelines and wells as known from the oil and gas industry [4,6,10,11, 12].From thermal energy production it is known, that the CO2-corrosion is sensitively dependent on alloy composition, contamination of alloy and media, environmental conditions like temperature, CO2 partial pressure, flow conditions and protective corrosion scales [6-8,13- 20]. Considering different environments, aquifer waters and pressures, the analyzed temperature regime between 40 °C to 60 °C is a critical temperature region well known for corrosion processes as shown by Pfennig et al. [21-23] and various other authors [10,24-28] (figure 1). Here a maximum around 4.7 mm/year was found for the pit intrusion depth of 13% Cr steel X46Cr13. Still this may be predicted by the rather conservative Norsok-Model used in the oil and gas industry to calculate surface corrosion rates of carbon steels [29]."

Jan 1, 2014

By N. A. Gokcen

THE data of Chaudron,1 Tonosaki,2 and Collins³ on the thermodynamic properties of MOO, disagree widely. These authors, by using essentially similar methods, studied the following reaction: 1/2MoO2(s) + H2(g) == i/2Mo(s) + Ph,o H2O(g),K = —----- [1] Ph2 Tonosaki used a vacuum system consisting of a furnace containing MOO, and a water saturator whose temperature was kept at 25 °C with a thermostat. After repeated evacuation, hydrogen was admitted slowly into the system. The experiments were based upon the fact that at a constant furnace temperature and constant partial pressure of water, the total pressure of gas mixture over MOO? + Mo is constant. Any attempt to vary the pressure by external forces would vary only the amounts of MoO2, and Mo, after which the pressure should return to the equilibrium value in accordance with the equilibrium constant of reaction 1. The actual value of K was determined from the total equilibrium pressure (sum of Ph2o + Ph2) at each temperature. The total pressure of gas was varied within the range of 80.2 to 125.4 mm Hg, within a temperature range of 645" to 823 °C. The results were summarized as log K = 0.9413 — 1444.6/T for reaction 1. The ratio of H2O/H2 was considered to be uniform in spite of the presence of a thermal gradient across the static gas phase. It was shown by Rosenqvist and Cox,' however, that in somewhat similar circumstances the error resulting from thermal diffusion may be large. Collins³ improved Tonosaki's method by attempting to avoid thermal diffusion errors. His equilibrium data were obtained at 700°, 800°, and 900° C, and the result for reaction 1 was expressed as log K = 1.258 — 1822/T. The purpose of this investigation was to study reaction 1, avoiding the thermal diffusion errors, and to obtain equilibrium data in a considerably wide temperature range for the reliable extrapolation of the resulting thermodynamic functions. Experimental Procedure The diagram of the apparatus is shown in Fig. 1. Tank hydrogen was passed through a tube containing platinized asbestos at 425 °C in order to convert a trace of oxygen into water vapor. The flow rate was carefully controlled with a capillary-type flow-meter B and a bubbling column D. The gas was then presaturated sufficiently at P and led into a condenser system immersed in a thermostat, controlled to within ±0.002C. The temperature of the thermostat was measured with a thermometer calibrated against a certified standard. The temperature of P was adjusted to avoid the condensation of unduly large amounts of water as judged from the rate of flow out of the capillary tube M. Argon was purified by passing it through magnesium chips kept at 630°C. After passing through the flowmeter B', it was mixed with moist hydrogen emerging from the thermostat. The resulting gas mixture was then led into the hot zone of the furnace through the heated glass tubing and the silica tube S, thus insuring the same ratio of PII2o/Ph2 from the condenser to the reaction chamber, thus avoiding thermal diffusion. The entire gas system was of all-glass construction, except at the magnesium train. The furnace comprised a glazed alumina tube over which a 15-in. platinum coil was wound. The lower end of the alumina tube was tightly closed with a brass bottom and a silicone rubber gasket, and the upper end with two glass disks, each with a hole of 1/16 in. in diameter, through which the gas mixture escaped into the atmosphere. A back-up coil of kanthal wire facilitated the temperature control of the furnace. A coil of annealed molybdenum strip of 99.99 pct purity, 0.005 in. thick and 0.050 in. wide, and weighing 17 g was hung in the furnace with a 0.010-in. platinum wire attached to one end of a sensitive analytical balance. The temperature of the furnace was measured with a Pt-Pt-10 pct Rh thermocouple checked against a standard. The experimental procedure consisted of heating the gas purification trains, adjusting the gas flow rates, attaining a constant thermostatic temperature, flushing the entire system for 2 hr while heating the furnace to well above the expected equilibrium temperature and then cooling it at a rate of 0.3°C per min during which time the change in the weight of molybdenum was observed on the balance. For a given thermostatic temperature, i.e., a constant Prr,o/Px,, molybdenum oxidized upon cooling slightly below the equilibrium temperature. The procedure was then repeated by heating the furnace and thus reaching a temperature slightly above the equilibrium value. The average of the two temperatures, differing by 2" to 3"C, was considered to be the true equilibrium temperature. In order to determine the stoichiometric composition of the oxide phase present in this investigation,

Jan 1, 1954