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By Zeng Zheng, Liu Chen, Yu Xing-Fu, Tian Su-Gui, Zhang Chao

"Single crystal nickel-base superalloy is prepared by using the various withdrawing rates. By measuring creep properties and microstructure observation, the influence of the element segregation on creep properties of the superalloys is investigated. Results show that the dendrite spacing and the segregation extent of the elements decrease with the enhancing withdrawing rate. The superalloy with smaller dendrite spacing has lower segregation of the elements and better creep resistance. The dislocations climbing over the rafted y’ phase is thought to be the deformation mechanism of the alloy during steady state creep. In the later stage of creep, the fact that some dislocations shear into the rafted y’ phase may twist the rafted y’ phase. As the creep goes on, the initiation and propagation of the cracks occur up to occurring creep fracture, which is thought to be the fracture mechanism of the superalloy during creep.1. IntroductionSingle crystal nickel-based superalloys consist of high volume fraction of ?? strengthening phase and ? matrix, and possess the excellent high-temperature mechanical and creep properties, therefore, they have become the main material to make the blades of the advanced aeroengines[1-3]. Some literatures report that the temperature-bearing and creep-resistance properties of the single crystal nickel-based superalloys can be remarkably improved as the increases content of the refractory elements, such as W and Re[4-6]."

Jan 1, 2012

By Martin P. Corriveau

It is not news to anyone in the mining industry that federal action in the prevention and abatement of air pollution has seriously affected the industry both directly and indirectly. It is the purpose of this paper to review how the development of federal action is directly affecting the coal mining industry's number one customer, the fossil-fuel-fired steam generating power plants and, consequently, the industry itself indirectly. In essence, Public Law 84-159 of 1955 as amended by the Clean Air Act of 1963 and its revisions in 1967 and 1970 progressively tightened federal coordination and management of air pollution control programs throughout these United States. The Environ- mental Protection Agency (E.P.A.) set up to direct the programs was charged to establish National Air Quality Standards, Standards of Performance for New Stationary Sources, and National Emission Standards for Hazardous Air Pollutants.

Jan 1, 1973

By Luis Bergh, Juan Olivares, Juan Durán, Juan Yianatos

"In the last decades heuristic approaches based on logic rules have been one favored tool to control flotation units and plants on top of distributed control systems. Fundamental knowledge on flotation processes, expressed in reliable models, and programs to assure the quality of the information, contained in available measurements, are still insufficient to develop robust predictive control strategies. In this paper the idea of using simplified models, when a known disturbance is coming into the process, is explored. As a first approach, the set points of the froth depth and air flow rate controllers are estimated based on this model. Since these target predictions are only approximate, a conventional feedback expert system, based on logic rules, continues the task of calculating the set points of the distributed controllers, in order to decrease the gap between actual and desirable metallurgical targets. This combined actions permitted a fast response of the process to change the operation of the circuit when a measured disturbance is detected. This control system was implemented and experimentally evaluated in a pilot rougher flotation circuit, with three pneumatic cells, with froth depth and air flow rate controllers in each cell. Since the circuit is operated for the air-water system, a phenomenological model, with parameters estimated from industrial data, is fed on-line with real operating variables and virtual values, characterizing the feed (grades, solids%, particle size distribution), in order to predict the metallurgical targets (recovery and concentrate grade). Several cases are discussed showing the benefits of this control system and the possible improvements to work on. INTRODUCTIONToday, large size mechanical flotation cells of 100 to 300 m3 are used in rougher operation in different flotation industrial plants, in Chile and worldwide. However, in spite of the advances in fundamental research and the notable growing in equipment size, with more complete instrumentation systems, there are still a lack of reliable data for industrial flotation modeling and simulation to advance in better control systems design."

Jan 1, 2016

By I. H. Warren, F. A. Forward, A. Vizsolyi

"Observations are reported on the pressure leaching of material produced by subjecting chalcopyrite to two types of heat treatment. Calcination of the mineral at 825°C, in the absence of oxygen, induces some sulphur loss by volatization, producing a material from which copper can be leached more rapidly than from chalcopyrite. Treatment of the mineral with elemental sulphur at 475°C leads to sulphur uptake accompanied by a change in mineralogical structure of the chalcopyrite. Copper is prefer-entially and rapidly leached from the sulphur-treated material. A tentative explanation of the sulphur-chalcopyrite re-action is presented."

Jan 1, 1968

At present the feasibility of developing underground facilities for the storage of a number of products including toxic waste, oil, nuclear waste and low pressure gas is under investigation in e number of countries. A possible method of storage is in large excavations, Preliminary ventilation design work has identified that the climatic conditions encountered within these large excavations are a limiting ventilation pollutant within the ventilation system. This paper examines the design of a variety of sizes of excavation from a ventilation viewpoint. The main phases of an excavations lifetime can be divided into four main phases, these being construction, civil and mechanical fitting, storage, full and sealed. The paper details ventilation design options for the first two phases of e vaults lifetime, giving climatic simulations to assess the likely climatic conditions within the excavations for e number of facility depths. The options for climatic control are given and analyzed by means of climatic simulations techniques. l. INTRODUCTION The feasibility of developing underground facilities for the storage of a number of products is under investigation at present in a number of countries. This paper details a possible design for such a facility where the product is to be stored in large underground excavations. A facility layout has been designed with the aim of allowing concurrent construction and storage operations. Thus from a ventilation perspective the facility consists of two circuits , a construction ventilation circuit and a product ventilation circuit both of which are served by an intake and a return surface connection The construction and storage circuits are considered as independent of each other , any interaction in the form of leakage must be from the construction to the storage circuit. From the facility design a ventilation network was developed to assess the ventilation requirements of the facility. In analyzing the pollutant loads for the construction circuit two pollutants were recognised to be critical to the ventilation design , these being diesel exhaust fumes and heat end humidity. In this paper ventilation design options for the construction and civil and mechanical fitting phases of the excavations are analyzed by means of climatic simulation and options for climatic control within the vaults are outlined . 2. FACILITY DESIGN A schematic diagram of a facility design is illustrated in Figure 1. There would be two distinct ventilation circuits , one to service the construction operations and the second to serve the storage operations which occur concurrently with construction , the circuits are separated by ventilation bulkheads . Access to the facility for intake air is provided by two drifts, one to serve each circuit. Two shafts act as returns to surface. The facility consists of two distinct zones for the storage of two types of product. One type is to be stored in smell linear excavations. The second zone is for the storage of a second product in larger excavations. The maximum cross-sectional area and perimeter for the smell linear excavations are 456.25 m2 and 83.2 m, while for the larger excavations they are 440.1 m2 and 86.4 m. Excavation construction consists of three phases: 1. Initial pilot tunnel development between main intake and return to provide through flow ventilation. 2. Enlargement to produce the required finished cross-section. 3. Civil and mechanical engineering work to fit out the excavation ready for storage. It is proposed to excavate the excavations using drill and blest methods utilising diesel equipment. Spoil is to be transported to surface by a conveyor belt system. At any one time the maximum number of working places requiring ventilation will consist of ; 3 storage sites, 2 excavations under construction, 2 excavations undergoing civil and mechanical fitting. [ ]

Jan 1, 1993

By K. S. Narayanan, Marcia L. Bartges, K. S. Venkataraman

The starting powders' physicochemical properties and consistency are essential for technical ceramic products to meet their performance specifications. The need for finer and more consistent powders has opened new technologies for synthesizing powders from atoms and molecules. However, submicron and near-micron powders obtained from conventional comminution and classification techniques are still competitive. This paper shows several examples from electronic ceramic applications of how we can use powder characteristics for micromanaging by design the ceramic properties such as the green and fired densities, slurry rheology, shrinkage during sintering, and the microstructure of the sintered bodies. The cross-disciplinary nature of the technology requires that the researcher not only should have a firm grip on the fundamentals of one or more disciplines, but also should be generally aware of the intricacies of other disciplines as well.

Jan 1, 1992

By C. N. Eze, C. K. Ezeh, O. Nnabuife, N. M. Ugwoju, S. C. Enemuor, V. Okechukwu

In this study, the efficacy of Providencia vermicola KUBT-1 in the leaching and beneficiation of Agbaja iron ore was evaluated under varying conditions of temperature, ore particle size, and pH. Agbaja iron ore is a Nigerian low-grade ore containing about 43%–52% iron and a high amount of gangue materials, including phosphorus (1.4%–2.0%) and sulphur (0.12%). The study was organised in triplicate in shake flasks with 48 samples. One millilitre of washed cells of Providencia vermicola KUBT-1 suspended in normal saline at 0.5 McFarland standard (108 cells ml-1) was introduced into each flask containing 50 g of sterilised ore in 100 ml of bioleaching medium, and the samples incubated at room temperature for eight weeks. The levels of upgraded iron, mobilised sulphur, and phosphorus were determined by atomic absorption and ultraviolet spectrophotometric analyses, respectively. Results showed that a particle size of 0.8 mm was optimal for iron upgrading and sulphur mobilisation while 1.0 mm ore size was optimal for phosphorus mobilisation. Up to 89.60% of the iron was upgraded while phosphorus and sulphur were mobilised, leaving residual values of 0.223% and 0.02%, in the ore, respectively. The organism produced best beneficiation results at a pH of 2.5 and a temperature of 3ºC. Correlation analysis with the Pearson’s correlation model showed a positive correlation between iron upgrading and sulphur-phosphorus removal (r =1.000, and r =0.967), respectively. These results present Providencia vermicola KUBT-1 as a promising candidate for large scale leaching and beneficiation of Agbaja iron ore.

Dec 15, 2025

By R. D. Longyear

[Some Problems Involved in the Interpretation of Diamond-drill-hole Sampling and Surve ing (paper by J. J. Collins, Mining Tech., Jan. 1946). ............... I Geologic Interpretation of Magnetic Exploration on the Mesabi Range, Minnesota (paper by R. H. B. Jones, Mining Tech., July 1946) ................... 2] DISCUSSION R. D. LONGYEAR.*-Mr. Collins is to be commended very highly for the brief summary he has made of the currently used methods of taking diamond-drill sludge samples and the principles involved in evaluating the results. This paper should stimulate further discussion and research on this vitally important problem. It is particularly imperative that geologists and engineers know when assay results on sludge recovery can be accepted quantitatively and when they must be considered only qualitatively. In most cases where the sludge recovery is less than 95 per cent or more than 125 per cent, it is safest to consider the assays as of qualitative value only. Certain cases, however, are known where a relatively small proportion of the sludge sampling will give a reasonably accurate measure of the value of the total sample. One such case is ore in which the valuable mineral is of approximately the same specific gravity as the waste mineral, such as chalcopyrite in a massive pyrite body. The essential point is to determine the degree of accuracy of sludge sampling in any given drilling project and to weigh the results accordingly. It should be emphasized, however, that sludge sampling can be made reliable in many localities where careless practice produces unreliable results. In many instances, it is desirable to empty the core barrel in the core shack instead of at the drill, so that the engineer can examine the core as it first comes from the core barrel. It should be pointed out, however, that the drill * E. J. Longyear Co., Minneapolis, Minnesota. runner should be permitted to study the core to guide his future drilling. It is hoped that with the return of more normal conditions after the war geologists, engineers, contractors, and manufacturers will be able to carry on more research along the lines of improved core-barrel design and drilling technique with the objective of increasing core recovery so as to eliminate as far as possible the necessity of relying upon sludge samples. H. M. ROBERTS.*-Whoever in the future will have to do with the search for ore bodies and their exploration will have frequent occasion to refer to the clear and comprehensive summary on diamond-drilling methods by John Collins. His review of the experience of the last 40 years in this technique is invaluable. As Dr. L. D. Ricketts wrote in 1932, "The principles on which an art is founded are usually few and necessarily basic in nature, but he who wishes to achieve the power to select his aides and give success to important undertakings that may be intrusted to him in the future must ordinarily undergo years of drudgery in order to gain the experience that will enable him to distinguish such fundamentals through the haze of reinforcing detail that clothes and tends to disguise them."[t] Ricketts went on to say that since the beginning of the century there has been much

Jan 1, 1946

By H. R. Barnhurst

IT would be a difficult matter to trace from the beginning the very few improvements made in the burning of fuels prior to 1860. Doubtless the crossing of the sticks of wood in building a, wood fire early appealed to our savage ancestry as a means of expediting its effectiveness for their crude culinary purposes. Stones and andirons came later in assisting the admission of air to the under part of the fuel bed, while beacons and cressets utilized metal bars as supports for the same purpose. It is probable that Tubal Cain owed his success to the use of bellows making possible the use of mixed fuel and charge upon a hearth. With the development of working in east iron, grate bars cane in, and they are still with us doing duty in every household and almost every art where heat is a factor. Little was done beyond these crude methods prior to 1860. With the advancement of knowledge came the fuel-gas producer, a. natural child of the retorts employed in supplying illuminating gas. It is only within the last 15 years that the conclusion became general that complicated systems for saving heat would not remedy deficiencies in its primary development, and within that tine there has been great advancement in the means of producing initially fire of high efficiency, so that to clay we are moving rapidly toward loth high development and high absorption, with the resultant of high efficiencies. In studying the subject of the availability of pulverized coal as a fuel, it may occur to ask, why has this not come up earlier? This question would be naturally prompted by recalling the fact that Thomas Crompton's English patents upon his methods were issued to Min nearly 40 years ago. A conclusive answer to this, however, is that Crompton at that time had very crude facilities for raking what was at best a, very imperfect pulverization of the coal, and the expense of preparation was very great. He does not seem to have been aware of the advantage of a thorough drying of the coal in the

Jan 10, 1913

DURING a period extending over about the last two and a half years, the performances of various types of rock drills in use at the mining department of the Zinc Corporation have been recorded as closely as possible. The main objective was the collection of sufficient data regarding internal water-feed hammer drills, when used for the same class of work as the older type reciprocating drill, to enable a decision to be formed on the following points:(1) Whether internal water-feed, hammer drills could efficiently perform the work previously carried out by reciprocating drills without excessive repair cost to the former.(2) If so, was it good policy commercially to eliminate the reciprocating type completely, writing these off together with the accompanying spares, accessories, and solid drill steel, and replacing with internal water-feed hammer drills, with lighter fittings, and the requisite amount of hollow drill steel.(3) What were the best types and makes of hammer drill for different classes of mining work(4) What was the economic aspect of the introduction of the principle of internal water feed to every type of machine throughout the mine.Prior to the strike of workers in May, 1919, Ingersoll-Rand E47 31-in. reciprocating drills had been used for stoping and for the major portion of driving, cross-cutting, and similar work. The accompanying columns and fittings were all 4t in. The drill steel used was solid octagon. Up to 1916 these machines were also used for winzing, after which time jackhamers were more successfully employed. These latter were of the usual types, varying in weight from 40 to' 46 Ib. Ingersoll BCR 430, Holman No. 2 spool valve, Sullivan DP33,. Waugh Clipper 55. These machines were all dry head; the drill steel was hollow hexagon, shanked.

Jan 1, 1923

Today, more and more tunnel ventilation systems are based on NO2 (or NO) and visibility measurements. Due to the significant decrease of CO emissions in countries with EU emission standards, which were adopted by Australia in 2004, CO is no longer a key factor for tunnel air quality monitoring and is often only measured for plausibility reasons (eg according to the German guideline RABT2006). Nitrogen dioxide, which is a good indicator for the overall air pollution along roads, is now taking over the leading role not only for ventilation control but also for air quality monitoring and in future probably for checking the function of air filtration plants in tunnels. Due to the lack of equipment for reliable and long-term NO2 measurements in road tunnels in the past, there are only very few standards giving limit values for NO2 in road tunnels. Furthermore there are not many records of NO2 readings over longer periods in different types of tunnels. SICK MAIHAK, a major supplier of measurement devices for controlling tunnel ventilation, has introduced the first monitor in 2006, specifically designed for measuring NO2, NO and visibility simultaneously in road tunnels. There are now experiences and results from the first tunnels equipped with this kind of system. This paper will present and discuss the results and experiences from these tunnels and explain the different levels of NO2 in different tunnel types. Furthermore, the status of air quality standards for road tunnels regarding NO2 limit values and the current status of discussion in various countries about NO2 limits will be presented.

Jan 1, 2008

By Raffaella Granata

The paper deals with the remediation of two areas formerly utilized for the disposal of hazardous wastes in a petrochemical plant. The works, designed on the basis of the criteria of maximum safety and minimum environmental impact, consisted in the confinement of the contaminated soil and groundwater within surface caps and perimetrical cut-off walls embedded in the underlying clay layer. The cut-off wall is 0.8 m thick and has a maximum depth of 33 m: it was designed to guarantee, as a minimum, the level of safety for a landfill for hazardous wastes, in accordance with the applicable National Standards. It was constructed with self-hardening mud and with the installation of an HDPE geomembrane. The HDPE liner of the cut-off wall was then sealed to that of the capping to obtain the complete encapsulation of the contaminated soil. A system of piezometers allows the monitoring of the cut-off efficiency measuring the fluctuations of the groundwater table and testing the chemical contents. Some wells installed within the contaminated areas will contribute to guarantee the full efficiency of the system in case of state of emergency, controlling the water-table level inside the confined areas.

Jan 1, 2006

By Martin J. Gavin

"Before discussing oil shales it may be well to consider briefly the conditions surrounding the petroleum industry in the United States, because these largely explain why so much interest is being manifested in oil shales. The United States is not only the greatest producer of petroleum in the world, its output amounting to about 65 per cent of the world's total production; but is also the world's greatest consumer, using more petroleum than it produces within its own borders. For the past four or five years it has been necessary to import oil at a continually increasing rate to make up the deficit between domestic production and domestic consumption. Experts who have made a close study of the future supply and demand for, crude petroleum are satisfied that under present production practice and with the development of possible undeveloped productive areas, the gap between domestic consumption and production will steadily .increase.As possible solutions for the impending domestic shortage of oil, various expedients are receiving attention. These may be grouped under three heads, as follows:(1) Temporary measures, such as curtailment of consumption, development of more efficient methods of production, and more efficient utilization of supplies of petroleum still available. It is unlikely that there will be any great curtailment in consumption of petroleum in the United States; rather, consumption will continue to increase unless a real shortage of oil actually forces curtailment of consumption. The other two possibilities mentioned deserve, and are resolving, serious thought. Much experimental work along these lines, some of which has already yielded excellent results, is being done. Obviously, however, any of these remedies are temporary ones only, so far as regards domestic production of petroleum."

Oct 1, 1920

By Lucas Travi

Um dos tratamentos superficiais mais conhecidos é a nitretação a plasma, que consiste basicamente na introdução de nitrogênio na superfície da ferramenta, na forma de nitretos de elementos de liga, em solução sólida, a fim de criar uma camada protetora que aumenta a vida útil do material. A nitretação a plasma permite o controle da camada formada através do ajuste de parâmetros como temperatura, mistura gasosa e tempo de tratamento. Porém para ferramentas mais complexas é comumente utilizado um novo processo de nitretação, a nitretação a plasma com gaiola catódica que tem como principal diferencial o aquecimento homogêneo das peças, evitando assim a heterogeneidade da camada nitretada. Outra vantagem é que neste processo não é comum ocorrer o acumulo de plasma o que evita o efeito de borda. Neste trabalho, será analisada a importância da menor rugosidade superficial aliada a dureza superficial no comportamento tribológico do material no processo de nitretação a plasma com e sem gaiola catódica. O resultado dos ensaios tribológicos demonstraram que o incremento de dureza associado a uma menor rugosidade superficial obtido para a amostra nitretada com gaiola catódica promoveu uma redução no coeficiente de atrito ao longo do tempo. A rugosidade superficial média para as amostras nitretadas com gaiola catódica foi menor que as nitretadas via processo convencional, aproximando-se do valor obtido para às amostras que foram polidas.

Aug 17, 2017

By Mojtaba Ahmadiantehrani

A previous study showed that up to 80% gold extraction could be obtained with 160 lbs/ton hypochlorite consumption at ambient temperature from a low grade Carlin-type carbonaceous ore. Crushing the ore to a finer size and agglomerating with cement decreases hypochlorite consumption by 60%; while, agglomeration and curing the cement-ore mixture with hypochlorite solution has no significant effect on total gold extraction. The high hypochlorite consumption is due to oxygen depletion as the solution percolates through the column, i.e., oxidation of gangue materials. These side reactions are reduced at sub-ambient temperatures resulting in a substantial further decrease in hypochlorite consumption. The optimum temperature range and additional reduction of hypochlorite consumption by introducing the reagent into the column at different elevations will be discussed.

Jan 1, 1992

By E Lima, D Gregory, C Faria, A Lapworth

Open pit mine enterprises are complex systems that depend on multiple parameters such as mineral grade distribution, geotechnical characteristics, economic conditions and engineering requirements, all of which vary in time and space with a different degree of uncertainty. The unpredictable nature of these inputs imposes a risk to mine owners and shareholders which in the worst case can lead to highly undesirable financial outcomes.Desktop studies commonly examine a set of scenarios based on adjusting variables such as commodity prices, mining costs, processing costs, and metal recoveries to understand their relative impact on the economics of a project. It is less common to systematically explore and simulate hundreds of alternative physical designs to understand and compare the financial risk associated with one or more mining projects.This paper presents a risk assessment tool set and methodology that uses web based cloud computing to enable multiple simulations of mine designs to be rapidly and efficiently executed. The methodology includes generating random sets of prices and costs values within their respective probability distributions. Pit designs are then created to maximise the profit for each set of input variables. Various approaches to analysing the results are discussed. Use of the same high performance computing environment for understanding the financial risk associated with the variability of the underlying geological resource model is also discussed, with provided examples using case studies from two of the major mineral producers.CITATION:Lima, E, Gregory, D, Lapworth, A and Faria, C, 2014. Simulating extraction shapes to understand financial risk using high performance computing, in Proceedings Orebody Modelling and Strategic Mine Planning Symposium 2014 , pp 351–360 (The Australasian Institute of Mining and Metallurgy: Melbourne).

Nov 24, 2014

By Helen Francis

Over the last decade, lower ore grades and deeper mine environments have demanded that mining companies develop new technologies (tools and processes) to ensure a mine?s economic sustainability. At Inco Ltd., this demand has lead to the focus of technological development within the area of automation. Delineation (Drilling and Interpretation) is a key step in the determination of ore grade and location and therefore was chosen as a priority area for enhancement through automation. Focusing on the tools (the diamond drill) automation, significant benefits have been consistently achieved in terms of productivity, process efficiency, operational safety, cost reduction, component life cycles and machine reliability. It is suggested that optimum benefits have yet to be achieved, and will not be achieved until the human aspects of automation have been properly addressed. Since project inception, the human aspects of automation were recognized as critical to the success of the diamond drill automation project. However, it was only upon the installation of the Automated Diamond Drill in the field and its continued use on a daily basis that this issue received due attention. The human aspects of automation can be broadly addressed as economic, physical and psychological. This paper, with examples from the field, will discuss the human aspects of automation in each of these areas. The paper will draw from observations and experiences acquired throughout this project and recommend implementation strategies that should be utilized in future automation projects to enhance both the acceptance of automation and the success of the automated process itself.

May 1, 2002

By Zengjie Wang

Investigation on hydrochloric acid leaching of the ilmenite from Panzhihua, China was carried out to prepare synthetic rutile. The leaching parameters were optimized to obtain high content of TiO2 in the products. The experimental data suggest that an optimum leaching can be realized with 30% acid, a solid/liquid ratio of 1/4 at 95°C for 4h, and ore ground for -400 mesh size. After the acid leaching, an additional alkaline leaching process using hot NaOH solution was performed, and then the products was in grain form followed by heat treated at 900°C for 2h in order to extract Si and increase the particle size of synthetic rutile. The final product has a high content of TiO2 (about 95%), a low content of chlorine consuming elements (total CaO+MgO =0.07%) and a suitable particle size distribution for chlorination process.

Jan 1, 2008

By B. K. Baird

The application of cutoffs during and after pit optimization is examined for a lower-grade multi-metallic copper deposit. Pit optimization requires calculation of the net revenue associated with each mining block, incorporating parameters such as metal prices, grades and expected recoveries, mining and processing costs, smelting and refining charges, and penalty element and royalty charges. Sensitivity analysis during pit optimization reveals which of these parameters have a significant effect on the total contained resource tonnage and total contained non-discounted revenue in the optimized pit. The cumulative effect of changing several of the more significant parameters is investigated. Application of a copper cutoff grade to a block inside the optimized pit could result in the less than optimal extraction of the resource. A block with copper grade below the applied cutoff could be economic due to the presence of other metals. Conversely, a higher copper grade block may be sub-economic. The relative merits of applying a copper grade cutoff, "equivalent grade" cutoff and dollar value per ton cutoff to blocks inside the optimum pit are discussed.

Jan 1, 1999

By J. F. Martin, L. M. Melnick, R. Rapp, R. C. Takacs

Recent studies on the determination of hydrogen in steel have shown that the hot-extraction method for removing hydrogen from a solid sample is preferable to its removal from a molten sample by vacuum fusion or by fusion in vacuum with tin. A number of techniques are available, however, for determining the hydrogen so extracted. They include: thermal conductivity, gas chromatography, pressure measurement before and after catalytic oxidation of the hydrogen to water and removal of the water, and pressure measurement before and after diffusion of the hydrogen through a palladium membrane. These techniques have been evaluated on the basis of initial cost, maintenance, speed and accuracy of analysis, and applicable concentration range. The results of this study showed that the palladium-membrane technique is best suited for routine use. FOR some time investigators have been concerned with the origin, form, and effect of hydrogen in steel. In such stdies', the analysis for hydrogen constitutes one of the most important phases. It is quite apparent that the results for hydrogen concentrations in a given steel are dependent on the method of obtaining the sample, storage of the sample until analysis, preparation of the sample, and analysis of the sample, including all the facets inherent in the calibration and operation of an apparatus for gas analysis. There are a number of means available for determining hydrogen. This is a critical study of some of the more common techniques in use today. In most conventional melting and casting methods, hydrogen concentrations of 4 to 6 parts per million (ppm) in steel are quite common. Because of the undesirable effects of hydrogen on steel there has been increased use of techniques such as vacuum melting,' vacuum casting, and ladle-to-ladle stream degassing, which lower the hydrogen content to levels on the order of 1 to 2 ppm. Therefore, the method used for determining hydrogen in steel must be sensitive and precise. In any analytical procedure for gases in metals there are two distinct operations—the extraction of the gas from the metal and the analysis of the extracted gas. To extract the gas from the steel, three methods have been employed: 1) fusion of the sample with graphite at high temperature; 2) fusion with a flux, such as tin, at a lower temperature; and 3) extraction of the hydrogen from the solid sample at a temperature below the melting point of the steel. Fusion with graphite is the least-acceptable method. The blank in this method is higher and more variable than in either of the other two methods. The hydrogen fraction of the total gas composition usually is between 10 and 50 pct; thus, a larger analytical error is possible. The vacuum-tin fusion4 extraction of hydrogen is probably the most rapid method in use today; the extraction time is usually about 10 min. However, with this system a bake-out of the freshly charged tin for 2 hr is necessary and a change of crucible and a charge of fresh tin are required after each day of operation whether one or thirty samples have been analyzed. In addition, frequent checks of blank rates are required since CO and Na are continually being given up by the steel samples dissolved in the tin bath. The composition of the gas in this method lends itself readily to analysis; although the hydroge concentration may fall to as low as 50 pct, more often it is above 90 pct, thus allowing a more precise analysis (because of less interference from other gases). In 1940 ewell' published the hot-extraction method for extracting hydrogen from the solid sample, comparing analysis for hydrogen extracted at 600°C with similar analysis for the gas extracted at 1700°C by fusion with graphite. Good agreement for hydrogen was obtained between these two methods, provided sufficient time was allowed for extraction at the lower temperature. carsone obtained good results in his comparison of this hot-extraction method with vacuum-tin fusion. Subsequent work by Geller and sun7 and Hill and ohnson' has shown that steel samples should be heated to at least 800°C to effect the release not only of the diffusible hydrogen but also of the "residual" hydrogen that may be present as methane. Since the rate of evolution of hydrogene9l0 depends on such factors as sample size and composition, thermal history, and extent of cold work, a fixed extraction time is not possible. Extraction times of 30 min are normal, but 2 hr are not unusual. Induction or resistance heating may be used in the hot-extraction method. With resistance heating the

Jan 1, 1964