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By John G. Whellock

Over the last decade new constraints have emerged in the metallurgical industry which challenge the very basis of design and construction of smelters and refineries. The hackneyed designs of the past will not now serve the revised objectives of: - minimal cost of ownership - improved productivity - reduced energy consumption - greater flexibility in feed or product - minimized recycle loops and by-products - more stringent environmental control The impact of these constraints has been channeled constructively into process intensification - exemplified at the large scale by the introduction of flash smelting technology and at the smaller scale by the application of rotary process vessels and converters for augmented heat and mass transfer. The design of successful process plants depends on the understanding of the unit operations and their interactions which is the discipline of systems engineering. With the advent of increased process intensification the importance of a systems approach to process design and implementation becomes paramount. This paper describes the systems approach with specific reference to medium scale projects in the primary and secondary metallurgical industry.

Jan 1, 1985

By D. S. Flett, D. W. West

The solvent extraction of chromium 111 has been studied for the system Cr 111, H,SO., H,O/RNH/RNH., xylene, where the primary amine used was Primene JMT. Rate studies have shown that extremely long equilibrium times are required, ranging from 1 hr at 80°C to 20 days at room temperature. Heating the solution prior to extraction increases the rate of extraction. The variation in the amount of Cr 111 extracted is an inverse function of the acidity of the aqueous phase. Thus, the slow rates of extraction appear to be connected with the hydrolysis of the Cr I11 species. Extraction isotherms for the extraction of Cr 111 have been obtained for two sets of experimental conditions, namely at 60°C and for a heat-treated solution cooled to room temperature. The separation of Fe 111 from Cr 111 and Cr 111 from Cu 11 in sulfate solution by extraction with Primene JMT has been studied and shown to be feasible. A survey of the literature relating to the solvent extraction of chromium showed that, although many systems exist for extraction of Cr VI, only a very few reagents have been found to extract Cr 111. The extraction of Cr III by di-(2-ethyl hexyl) phosphoric acid has been reported by Kimura.' A straight-line dependence of slope —2 was observed between log D,, and the log mineral acid concentration at constant extractant concentration. Since the slope of this plot reflects the charge on the ion extracted, it must be concluded that a hydrolyzed species of Cr III is being extracted. Carboxylic acids generally do not form extractable complexes with Cr III but di-isopropyl salicylic acie does extract Cr 111. Simple acid backwashing of the organic phase, however, failed to remove the chromium. Similar difficulty in backwashing was found by Hellwege and Schweitzer8 in the extraction of Cr I11 with acetyl-acetone in chloroform. The extraction of Cr 111 from chloride solutions by alkyl amines has been reported4-' but the maximum amount of extraction achieved in these studies did not exceed 10%: From sulfate solutions, however, Ishimori" has shown that appreciable amounts of Cr I11 were extracted by amines. The amines used were tri-iso-octyl amine, Amberlite LA-1 (a secondary amine, Rohm & Haas) and Primene JMT (primary amine, Rohm & Haas). The efficiency of extraction with regard to amine type was primary>secondary> tertiary. Appreciable extraction of Cr I11 was recorded for Primene JMT as the aqueous phase acidity tended to zero. The major difficulty with Cr I11 in solvent extraction systems stems from the nonlabile nature of the ion in complex formation. This accounts for the slow rate of extraction generally experienced and the difficulty encountered in backwashing the Cr I11 from the organic phase in the case of liquid cation exchangers. Consequently, the possibility of extraction of Cr I11 as a complex anion is attractive since the backwashing problems should be minimized in this way. From published data, it appeared that the extraction of chromium from sulfate solutions of low acidity by primary amines afforded the best chance of success for a useful solvent extraction system for Cr iii This paper presents the results of a study of the extraction of Cr I11 from sulfate solution by Primene JMT and examines the application of such an extraction procedure for the recovery of chromium from liquors containing iron and copper. Experimental Chromium solutions were prepared from chrome alum in sulfuric acid and sodium sulfate so as to maintain a constant concentration of sulfate ion of 1.5 molar. Solutions of Primene JMT were prepared in xylene and the amine equilibrated with sulfuric acid/sodium sul-fate solutions, of the same acidity as the chromium solution, until there was no change in acidity between the initial and final aqueous phases. The solutions of Primene JMT conditioned in this way were then used for the equilibration experiments. Equilibrations at 25°C were carried out in stoppered conical flasks shaken in a thermostat; equilibrations at all other temperatures were carried out in stirred flasks in a thermostat. After equilibration, the phases were separated and analyzed for chromium. In the tests on the rate of extraction, small samples of equal volume of both phases were withdrawn from time to time and the chromium distribution determined. The chromium analyses were carried out either coloi-imetrically using diphenyl carbazide, or volu-metrically using addition of excess standard ferrous ammonium sulfate and back titration of the excess iron with potassium dichromate. The oxidation of Cr 111 to Cr VI in the case of the raffinate solution was effected by boiling with potassium persulfate in the presence of silver nitrate and, for the backwash solution, by boiling with sodium hydroxide and hydrogen peroxide. Results Preliminary experiments indicated that extraction results were effected by the age of the chromium solution, higher distribution coefficients being obtained with solutions which had been allowed to stand for some time. Consequently a stock solution of chrome alum, 10 m moles per 1 Cr I11 in 1.4 M Na,SO,/O.l M &SO,,

Jan 1, 1971

By Armstrong

This is a world of change and has been from the beginning. There are constant efforts on the part of natural forces to wear down the high spots and fill in the low spots. Wind and water over eons of time tunnel through obstacles and build windways and waterways to make movement of air and water easier and more efficient. It is a natural, never ending, ever changing continuing effort. Man in his struggle to survive, and to progress, has had to adapt the terrain of the earth to fit his needs the best he could. First, he used natural caves to protect him from the elements; then he learned how to build earth and rock-moving tools from antlers, bone, rocks, and sticks and adapted his cave to increase his security and provide better protection from heat and cold and from his predatory enemies. As his numbers increased, so did the necessity of further adapting his environment to accommodate his needs. Water was usually not available when and where needed, especially in the desert areas where civilization developed, and long tunnels were drilled to intercept ground waters and lead them to underground caves carved out of soft limestone. Most of the tunnels of early man were to bring water from where it was to where man needed it. Then, as now, as man increased his chances for physical survival, he turned to the quality of life -- and this reflected in the concern for life after death. This lead to the elaborate shafts and tunnels for the protection and prservation of the more affluent noblemen and pharaohs of the early Egyptian civilization. Man used the underground for the stable temperature and for protection and safety.

Jan 1, 1974

By Stephen G. Mlot

Technical Study Work ?Technical study work enables informed decisions: -Obtain a higher price for a quality asset -Minimize expenditure on a project that won?t provide adequate returns -Optimize expenditure on a project to capitalize on the potential return

May 1, 2013

By J. M. Cummings

CONSIPERABLE information on the industrial or non-metallic mineral resources of British Columbia has been published. For a general resume of the subject, reference may be made to a paper presented by A. M. Richmond before the Annual General Meeting of the Institute in 1935 (1). To avoid duplication, the present paper is confined to a discussion of the existing industrial mineral industry of the Province and of the factors governing its present and future development. British Columbia's mineral production in 1936 had a value approximately 15 per cent of that for the whole of Canada. Preliminary estimates for 1937 indicate that this proportion has been maintained, although the totals have increased about 25 per cent. The following table presents comparative figures, for the year 1936, illustrating the relative importance of the major divisions of the mineral industry in British Columbia and in Canada as a whole.

Jan 1, 1938

By E Villaescusa, C Drover, I Onederra

Development face destress blasting is a construction technique in deep mining, which aims to prevent, reduce the frequency, or manipulate the timing of violent, stress-driven rock mass instability at the face. This paper presents a destress blasting design concept that was optimised for the specific rock mass conditions of a deep mine using the Hybrid Stress Blasting Model (HSBM) software. The design was then implemented in an area of the mine where stress-driven instability of the face regularly occurred during development. An adjacent tunnel was constructed in parallel without destressing, within the same rock mass conditions, as a control. The rock mass response to each excavation was quantitatively compared using high-resolution local seismic monitoring. Visual observations of the fractures created by destress blasting were also made. The analysis indicated that destressing reduced both seismicity and the rock mass stiffness ahead of the face. This was inferred from the spatial broadening of the development seismogenic zone and the typically significant reduction in the spatial density of seismic events. Seismic source mechanism analysis also indicated that destress blasting generated a much wider variety of failure modes than conventional blasting. Most seismic source mechanisms following destressing were associated with natural joint structures. A relatively small portion were consistent with newly created blast-induced fractures. The greater diversity of rock mass failure modes associated with destressing implied a lower potential for stain-energy accumulation within the rock mass at the face, and thus a lower risk of hazardous instability. Observations of visible rock fracturing indicated that the major principal stress influenced the damage intensity on natural geological structures within the destressed zone, and that numerical predictions of radial fracturing limits made by HSBM analysis were realistic representations of the real blasting performance.

Nov 29, 2022

By M. M. Fine

"INTRODUCTION One of the principal activities of the Bureau of Mines during the recent war was to help to increase the supply of strategic and critical minerals. Fluorite was one of the most critical of the nonmetallic minerals because of the increased demand for it as a flux in basic open-hearth and electric steel furnaces and as a raw material for the production of artificial cryolite used in the aluminum industry. Wartime developments in the technology of hydro-fluoric acid, such as the use of the anhydrous acid as a catalyst in high-octane-gasoline production and the use of organic fluorides as carriers for insecticides, also increased the demand for acid-grade fluorspar. 2/ In 1943 the consumption of acid-grade fluorspar was advancing at a more rapid rate than production and was only slightly less than production during the latter half of the year.The outlook for the postwar market for fluorspar is encouraging. Steel production is expected to remain high until the domestic demand for commodities not manufactured during the war is satisfied. The uses for hydrofluoric acid also are expected to increase under the impetus of war-initiated research. In consideration of these and other factors some authorities predict a new peacetime demand for fluorspar equal to 60 to 75 percent of the war production, 5/ 6/ and others believe that the fluorspar industry will be permanently expanded. 7/"

Dec 1, 1947

By Yong Pan, Purushotham Tukkaraja

Block caving is a preferred underground mining technique due to its high production rate and low operation cost. Before its final step into a mature caving system using gravity to break rock, drilling and blasting are required to form drawbells to connect the production level and undercut level and induce the initial caving propagation in undercut level. A large amount of toxic fume generated by blasting activities poses a big threat to people working in a confined environment and ventilation is assumed to be the most economical and efficient way to deal with this issue. Past research shows that it’s common to use traditional methods like using a formula or using numerical method (Computational Fluid Dynamic (CFD)) simulation to predict re-entry time after each blasting, but it fails to consider the percentage of toxic fume entrapped in muckpile, which could reach up to 70%. In this paper, CFD was used to investigate the blasting toxic fume characteristics under different entrapping percentages and under changing muck pile properties like broken rock size and porosity. It showed that CFD was a very useful method to study blasting fume in an underground mine and it took much longer time to dilute toxic fume into a safe level with higher entrapping percentage. The dilution time increased with a decrease of broken rock size and porosity.

Today's emphasis on the enterprise bargaining process must be seen as an opportunity for organisations to further develop occupational health and safety standards at work. In particular, this shift from a centralised industrial relations system to employer, employee bargaining, presents organisations with an excellent opportunity to develop OH & S at the `shop floor' level. This is despite real difficulties in presenting hard data on the cost benefits. Unfortunately, examination of enterprise agreements ratified by the Australian Industrial Relations Commission (AIRC), show that less than 32 per cent contain provision for occupational health and safety. Those addressing the issues of occupational health and safety have included segments such as: ò rehabilitation activities; ò a new emphasis for workplace occupational health and safety committees; ò formalising procedures related to hazard identification and control; ò the use of personal protective clothing; and ò occupational hygiene and health monitoring issues. For example, an enterprise agreement reached between CIG-Gases and their unions, included clauses which commit employees to attending ten safety meetings and two work place inspections each year, in order for them to receive any further pay rises.

Jan 1, 1995

By D. Hulse

Mineral resource classification is described in both the SME and CIM Standards for Mineral Resource Reporting. The CIM Standard states “… sampling … is sufficient to assume geological and grade or quality continuity between points of observation”, thus is a function of continuity and sample spacing. Continuity can be measured by use of a variogram model, but average sample spacing in three dimensions is more difficult to measure. The declustering algorithms provided with Geostatistics software, are commonly used to weight data for statistical analysis due to the sometimes-irregular spacing between drill holes during exploration. The weights are lower when data is closer, reflecting shared influence between samples, and higher for isolated samples reflecting independence. This paper will discuss the potential to use estimates of the declustering weight as an inverse relative measure for average sample spacing to gauge the confidence of the estimate independent of the single nearest sample. PROBLEM The classification of mineral resources and reserves has long been a combination of science, past experience of the estimator, judgment, and feeling. All of the definitions as presented in the standards of the various countries that participate in CRIRSCO are similar and deal with “sample points sufficiently closely spaced to support confidence in the continuity of …” This has been interpreted as the distance between the block estimated and the nearest sample (or samples). Geostatistics gave us the calculation of the estimation variance of the block, an implicit part of the calculation of weights in Kriging, to account for the confidence in the estimate. More recently, “Kriging Efficiency” has been used, however it is still dependent on the estimation error and responds in a similar fashion to the distance to the closest sample. It is also sensitive to the variogram nugget. Many of these methods result in very low distance/high confidence measures for blocks adjacent to a sample point with confidence decreasing (sometimes rapidly) as the distance to one nearest sample increases. This results in the “spotted dog” phenomenon where individual samples are surrounded by a higher classification near each sample decaying into pattern of decreasing confidence halos. In addition to the visual image of the spots, this raises the more practical problem of mine design when the classification changes between measured, indicated and inferred. This has led to ad hoc methods to classify material within the mining block so all of the stope receives that classification. These manual methods re both labor intensive and subjective. A popular technique is a multiple search method, where the estimator defines a minimum of number of samples from a minimum number of holes within a nested set of search distance that are used to classify estimates. These specified set of increasing distances are usually proportional to the variogram range. While this is generally a good technique and overcomes the spottiness of the closest sample or kriging error, it has certain issues including:

Jan 1, 2019

Using Dynamic Simulation Throughout a Process Plant's Life Cycle

Sep 13, 2010

By Keith Leonard Sutherland

This paper is a study of the differential flotation of the sulphide minerals in the presence of salts of silver, lead and zinc. In practice, accidental activation due to these salts is more important than their use as reagents to replace copper sulphate. The general method of investigation has been based upon contact tests, the temperature of 35°C being chosen in conformity with earlier work. Potassium ethyl xanthate and potassium amyl xanthate were selected as collectors and pure sulphide minerals were used. The experimental procedure has been outlined in earlier papers and all solutions were kept carbonate-free.14 Contact, or spreading of an air bubble, at a mineral surface indicates the presence of an adsorbed collector film. Purity of Reagents The xanthates were purified in the usual manner.' Neither the cyanide nor the sodium hydroxide solutions contained sufficient carbonate to give a precipitate with barium chloride solution. The silver sulphate was prepared from pure silver nitrate by evaporation with concentrated sulphuric acid until there was no evidence of brown fumes, This solution was diluted and the difficultly soluble sulphate washed with water so that unchanged nitrate was dissolved. The resultant crystalline powder was pure white. The lead and zinc salts were prepared by dissolving especially pure lead and zinc in C.P. nitric and sulphuric acid solution and the crystals drained. The standard solutions were checked by titration. It was felt desirable to use the sulphate radical wherever possible, but since lead sulphate was insufficiently soluble for the purpose of the experiments, it was necessary to use some other lead salt. A.R. copper sulphate was used without further purification. Results The results are presented in the accompanying figures; the areas of noncontact (nonflotation) are shaded in Figs. 8, 9, 10 and 11; in the remainder they lie to the right of the curve. Zinc Sulphate The curves in Fig. I are to be compared with those for Fig. 2, for which zinc sulphate is absent. This comparison shows that the influence of the zinc ion is usually small. Its influence is more marked, however, for chalcopyrite in the absence of cyanide. The influence of zinc sulphate is also marked for copper-activated sphalerite, for which tests were made only in the "absence of cyanide. The results are of importance in the separation of pyrite from copper-activated sphalerite when zinc sulphate is added in the lead flotation section (p. 204 of ref. I). Sphalerite does not adsorb the collector (i.e., become floatable) under the conditions chosen.

Jan 1, 1943

By Keith Leonard Sutherland

This paper is a study of the differential flotation of the sulphide minerals in the presence of salts of silver, lead and zinc. In practice, accidental activation due to these salts is more important than their use as reagents to replace copper sulphate. The general method of investigation has been based upon contact tests, the temperature of 35°C being chosen in conformity with earlier work. Potassium ethyl xanthate and potassium amyl xanthate were selected as collectors and pure sulphide minerals were used. The experimental procedure has been outlined in earlier papers and all solutions were kept carbonate-free.14 Contact, or spreading of an air bubble, at a mineral surface indicates the presence of an adsorbed collector film. Purity of Reagents The xanthates were purified in the usual manner.' Neither the cyanide nor the sodium hydroxide solutions contained sufficient carbonate to give a precipitate with barium chloride solution. The silver sulphate was prepared from pure silver nitrate by evaporation with concentrated sulphuric acid until there was no evidence of brown fumes, This solution was diluted and the difficultly soluble sulphate washed with water so that unchanged nitrate was dissolved. The resultant crystalline powder was pure white. The lead and zinc salts were prepared by dissolving especially pure lead and zinc in C.P. nitric and sulphuric acid solution and the crystals drained. The standard solutions were checked by titration. It was felt desirable to use the sulphate radical wherever possible, but since lead sulphate was insufficiently soluble for the purpose of the experiments, it was necessary to use some other lead salt. A.R. copper sulphate was used without further purification. Results The results are presented in the accompanying figures; the areas of noncontact (nonflotation) are shaded in Figs. 8, 9, 10 and 11; in the remainder they lie to the right of the curve. Zinc Sulphate The curves in Fig. I are to be compared with those for Fig. 2, for which zinc sulphate is absent. This comparison shows that the influence of the zinc ion is usually small. Its influence is more marked, however, for chalcopyrite in the absence of cyanide. The influence of zinc sulphate is also marked for copper-activated sphalerite, for which tests were made only in the "absence of cyanide. The results are of importance in the separation of pyrite from copper-activated sphalerite when zinc sulphate is added in the lead flotation section (p. 204 of ref. I). Sphalerite does not adsorb the collector (i.e., become floatable) under the conditions chosen.

Jan 1, 1943

By M. Tarvainen, J. Kallioinen

"Depressed metal prices coupled with increasing production costs have presented a great challenge for operators to control and reduce the costs of production to maintain profitability. Depleting ore reserves, added to the above has forced Outokumpu to take a hard look at its operations, to develop new methods to profitably extend the life of its mines. One of the areas investigated and approved for further development has been the use of larger and more energy efficient equipment. As a result, large flotation machines were developed and today 38 and 60m3 flotation machines are in use.Secondly, ore preconcentration has been developed to avoid processing the part of the ore that has little or no mineral values.Another quite recent development and the topic of this paper, has been the use of coarse flotation before conventional flotation. The main idea is that part of the valuable mineral is separated as early as practical by floating it with specially designed flotation equipment, installed in the grinding classification circuit. The new flotation cell is specially designed for this application and differs from the conventional cells in the tank design, feed arrangement and modified mechanisms in some cases."

Jan 1, 1984

By R. L. Sandefur

Any geostatistical study involves (implicit) hypotheses about 1. The distribution function 2. The drift of the data 3. The (underlying) variogram Once these are known, most other results follow from geostatistical theory. However, to date, there have been few theoretical studies on testing these implicit hypotheses. Most of the published studies in this area have dealt with the fluctuation of the variogram or the sampling distribution of the variogram (Journel and Huijbregts, 1978; Davis and Borgman, 1979). Questions regarding these hypotheses regarding a given deposit arise often. Coal geologists often infer channels and washouts on the basis of thicknesses data. Zoning is recognized in a variety of metal deposits. A test as to whether these inferences are valid on just chance occurrences would have widespread application. .It is standard geostatistical practice to "eyeball" fit variograms. In the early exploration phase when just a few pairs are available, the variogram often displays wide fluctuations and there may be considerable doubt about which variogram model to use.

Jan 1, 1982

The impact of smoothing on the definition of ore and waste boundaries using linear estimation and conditional simulation methods is discussed. The nature of transfer functions is examined including their ability to incorporate categorical data (e.g. a dominant lithology code). An Ore Block Optimization (OBO) transfer function is presented that provides a clear guide for the mining geologist. Advantages are seen in defining stockpile cut-off grades and meeting production targets such as maximizing head grade, maximizing ore tonnes or minimizing ore loss or dilution. Each of these scenarios impacts on mine profitability and grade control.

Jan 1, 1999

By Y. G. Seredkin, A. A. Vasiliev, A. Y. Senchenko, A. V. Aksenov

"The valuable materials resulting from the processing of gold-bearing ores are often refractory to direct gold recovery through cyanidation. There are multiple methods for chemical liberation of gold prior to cyanidation such as pressure and biological oxidation as well as atmospheric oxidation which is typically used in combination with physical activation of material by ultrafine grinding such as the Albion ProcessTM. This paper will examine the data from process testworks carried out to estimate the efficiency of the Albion Process™ for the oxidation of materials with a wide composition range prior to cyanidation. The data will be compared to that obtained by direct cyanidation of the feed (without oxidation) and from the testing of pressure oxidation on the feed prior to cyanidation. Albion Process™ tests were conducted in Institute TOMS with participation of Glencore Technology Pty Ltd (Australia). Refractory concentrates obtained from the ores of several Russian and CIS deposits were used as feed for the testing. These concentrates were also subjected to a material composition study and testing using conventional recovery methods. The resulted test data make it possible to perform an integrated assessment of process properties for materials with different compositions, compare performance of various process flowsheets for the materials under study, and conclude on efficiency of Albion Process™ application for gold recovery from refractory materials different in their composition.INTRODUCTION It is often the case that gold ore concentrates are refractory to gold recovery by direct cyanidation. This refractory nature is as a rule attributable to fine gold dissemination in minerals, most often in pyrite and other sulphides, as well as to the increased amount of components impeding cyanide leaching of gold due to cyanide consumption and reducing process conditions. The refractoriness of the concentrates results in low gold recovery values when conventional cyanidation technology is used. In this context, various additional processes are applied to breakdown such refractory sulphide concentrates, i.e. mechanical breakdown (fine and ultrafine grinding), chemical breakdown (atmospheric oxidation, e.g. Leachox, acid-oxygen oxidation, pressure oxidation – POX, bacterial oxidation – BIOX), and thermochemical breakdown (various roasting methods). Such breakdown processes allow for increase in recovery of finely disseminated gold during the downstream cyanidation, however, their application is cost-intensive and does not always ensure economic benefit."

Jan 1, 2018

By Denise Cristina de O. Nascimento

Natural lignocellulosic fibers are increasingly being used as polymeric matrix composite reinforcement owing to economical and environmental advantages as renewable and biodegradable materials. Among these, the piassava fiber extracted from a palm tree native of South America stands as one of the most rigid with a potential to be used as composite reinforcement. Therefore, the present work investigates the notch toughness behavior, by Izod impact tests, of epoxy composites reinforced with up to 40 % in volume of continuous and aligned piassava fibers. It was found that the incorporation of piassava fibers results in significant increase in the impact energy of the composite. Scanning electron microscopy analysis showed that the nature of the piassava fiber interface with the epoxy matrix is the major responsible for the superior toughness of the composite.

Jan 1, 2009

By Quanjun Liu, Rongping Lin, Rongdong Deng

Arsenic contamination significantly affects the quality of copper concentrates, presenting challenges during smelting processes. Considering that covellite and enargite have similar surface properties, they are difficult to separate by flotation, resulting in copper concentrates with excessive levels of arsenic. To address this issue, this study systematically investigated the flotation separation of covellite and enargite in microflotation and bench-scale flotation tests using calcium lignosulfonate as a depressant, with the results indicating that calcium lignosulfonate can be used to separate covellite and enargite because it enables the separation of arsenic-bearing copper minerals into high- and low-arsenic (As 0.57%) copper concentrates. According to contact angle and adsorption tests, scanning electron microscopy–energy dispersive spectroscopy, and X-ray photoelectron spectroscopy, the differential adsorption of calcium lignosulfonate onto covellite and enargite is the primary reason for their distinct flotation behaviors in the presence of calcium lignosulfonate. The selective depressive effect of calcium lignosulfonate provides a novel approach for improving the flotation separation of arsenic-bearing minerals from copper sulfide minerals.

Feb 28, 2024

By L. S. Darken, H. A. Wriedt

An investigation has been made of nitrogen absorption by the lattice defects in a low-carbon steel afte~ Plastic deformation. Specimens in which defects were distributed by various combinations of cold rolling and vacuum heat treatment were equilibrated with controlled ammonia + hydrogen mixtures at 300° to 450°C to study the relation between the solubility and the thermodynamic activity of nitrogen. The results are interpreted in terms of nitrogen being absorbed upon two different types of defect sites, called A sites and B sites. The concentrations of these sites are calculated for specimens with various histories of straining and annealing; and the thermodynamic relations descrihing the equilibrium distribution of nitrogen among the A, B, and ordinary interstitial sites in ferrite are evaluated as follows: THE generalization that the solute atoms in a solid solution interact with imperfections in the solvent lattice is now universally recognized and the subject of an extensive literature. All types of imperfections—point, line, or surface—exhibit these interactions, but the relative importance of each type depends upon its concentration, the strength of its interaction with the particular solute atom, and whether the interaction is attractive or repulsive. The strength and sign of the interaction vary with the vectorial displacement of the solute atom from the imperfection in the crystal. The concentration of lattice defects increases during plastic deformation and the effect of the imperfections upon the solute atoms is usually perceived only after cold work or irradiation. Two experimental methods have previously been used to observe the effects of interaction between nitrogen atoms and lattice imperfections in a iron. Internal friction, which was first used for this purpose by Dijkstra,1 has been applied more often than the electrical-resistivity method of Cottrell and Churchman.2 The method of the present investigation has not been used before.* Uniform specimens of steel with a metastable defect structure are produced by cold rolling and subsequent heat treatment below the recrystallization temperature. Variations in the defect structure are obtained by varying the amount of strain and the heat-treatment conditions. The specimens are then saturated with nitrogen at moderately elevated temperatures in ammonia + hydrogen mixtures having various thermodynamic activities of nitrogen below saturation with Fe4N. From the nitrogen contents of analyzed samples, the metastable equilibria of interactions between the defects and nitrogen can be established and the concentration of sites for nitrogen atoms in the lattice defects calculated. A steel was used in the present experiments instead of purified iron or iron alloys because the amount of nitrogen absorbed at defects is larger in the steel over a much wider range of experimental conditions and could therefore be measured more accurately. The effect of alloy composition is discussed in Part II of this paper; it is sufficient to say here that impurities and phase heterogeneity in ferritic alloys favor the generation and/or retention of larger defect concentrations during plastic deformation and annealing at 300° to 500°C. MATERIALS AND EXPERIMENTAL PROCEDURE The experimental specimens were prepared from stock of a low-carbon steel, which will be called "X steel" here, with the composition: C, 0.12 pct; Mn, 0.43 pct; P, 0.010 pct; S, 0.034 pct; Si, 0.007 pct; As, 0.086 pct; Cu, 0.022 pct; Ni, 0.009 pct; Cr, 0.003 pct. The stock was all from a single ingot made by the basic open-hearth process, which was hot-rolled to strip 0.080 in. thick.. This hot-rolled strip, given the code designation "XH", was the starting material for preparing a series of cold-rolled sheets. The latter are designated "XC27",

Jan 1, 1965