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Jan 1, 1947

Dr Hanekom I would like to thank Dr Hanekom for a very valuable -contribution; it summarizes careful statistical test work which was an omission from the original paper. Minor manipulative details, the application of a finer measuring graticule and the reproducibility of the procedure are described and the author accepts with gratitude this ready-made answer to the first and second points of Dr Finkelstein's comments. Mr Williamson The author is indebted to Mr Williamson for historical background to early experiments with captive bubbles and it is conceded that the original paper described another avenue to an old flotation goal. The field of application is restricted and we would not work with all the material illustrated by Klassen and Mokrousov.1 The particles in Figure 74(a) are far too large and irregular; material in Figures (b) through (d) could be employed for semi-quantitative work in spite of obvious disadvantages; Figure 74(f) represents ideal conditions. We have studied this mineral-collector association in the size range given and results were satisfactory. For larger pick-up values than that illustrated an induction period of more than 0.01 second was required (actually 90 seconds for a maximum bubble load at pH 7.2 with 25 g/t oleic acid!). REFERENCE 1. KLASSEN,V. I. ANDMOKROUSOV,V. A., 'An Introduction to the Theory of Flotation,' Butterworths, London, 128, Figure 74, (1963). Mr Slander and Mr Kooij Researchworkers in a practical mineral development laboratory may well ask what contribution yet another micro-technique can make to the problems of large scale ore flotation. The obvious answer is that there can be little or no direct translation of results obtained with a static system comprising air bubble and pure mineral concentrate to a dynamic multicomponent operation. However, for the rapid study of one mineral or variable some small scale apparatus must be employed. In the Anglo American Research Laboratory, the described semi-quantitative pick-up technique has filled a niche and requirement. For ourselves, the system represents a definite advance over the contact angle approach in that samples of minerals conventionally prepared in laboratory or plant may be used, which is a desired step nearer flotation. We bracket this pick-up apparatus with the Hallimond tube1,2 and evidence is now to hand that pick-up curves may often be related to flotation recoveries obtained from this tube with pure mineral samples and from the Fuerstenau glass cell3 with the total ore at low pulp densities. We would not wish to push the comparison of pick-up results past this stage for there is much published development work relating the Hallimond and Fuerstenau equipment to flotation on a larger scale. At the Anglo American Research Laboratory for example, a test in a Fuerstenau cell is often the final integrated step in laboratory investigations into the TORCO process. As these contributors rightly point out, pick-up tests can offer nothing towards the determination of optimum reagent dosage for large scale flotation. This is the function of bench-type flotation cells with up to 2 kg batches of ore. At this level, collector performance and consumption and physical properties of the froth are more comparable with large scale operation. The pick-up cell, Hallimond tube and Fuerstenau cell are essentially equipment from which the effect of control parameters can be derived. For the assessment of collector behaviour, the pick-up approach is rapid and economic and we offer here a pick-up contribution towards the flotation of Witwatersrand uraninite with anionic sulphonate collectors (Fig. 1). A large crystal of the local mineral was not available for contact angle measurements and owing to its low concentration in Witwatersrand gold-bearing reef, a small sample was laboriously obtained by tabling, superpanning and heavy medium separation. The pick-up values of a sized portion were determined by the described procedure in the presence of nine petroleum sulphonate collectors. Responses fell into two categories; "normal" curves (dotted lines) and a group of collectors which were very active at low concentration but showed depression of pick-up at the higher levels. The similarity in form of curves for collectors 1 and 3 was apparent and reagent 3 was found to be simply a diluent of 1. Otherwise, collector performance could not be related to either sulphonate content or molecular weight of the active constituent. However, reagent 2 gave the best performance in a bench flotation cell with regard to overall uranium distribution but, as predicted, reagent 1 yielded the best grades. Later pick-up tests with a similar class of collector have suggested that depression at high reagent concentrations may be due to "bubble armouring" whereby an hydrophilic air-liquid interface is produced which rejects mineral attachment. Prolonged investigations with the same mineral sample have not been required except for the study of uraninite which lasted for more than a year. Variation in pick-up response could not be detected over this period during which the mineral was stored under distilled water. The only visible change was a small efflorescence of lead sulphate, readily removed and decanted off after stirring with a glass rod in the sample tube. In its main role as a "trouble-shooter", the pick-up method is applied to fresh mineral samples taken from a flotation plant and soon discarded or from a current run in the ore-dressing laboratory. After production of a concentrate, a solvent cycle, as described in the original paper, may be required to remove heavy organics or other contaminants as when a sample has been taken from circuits containing detergents, grease or return flotation solutions. This solvent cycle will not remove chemisorbed collectors and we prefer not to work with minerals from flotation tailings or with pick-up cell discards. It has been thought preferable to answer the contributors' other apprehensions with regard to sample preparation, activators, depressants and the physical properties of reagents in another paper on offer to this Journal. It covers pick-up investigations relating to the flotation of nickeliferous pyrrhotite at two Anglo American Corporation Mines, which approach seemed the correct orientation for a reply to another contributor to this paper.

By D. G. Krige

D. G. Krige: The stimulating contributions from Messrs Cooke, Curtis, Martus, Johnston, Van Wyk, Van Rensburg and Wroth are appreciated by the author and provide clear evidence of the importance not only of the principle of assistance to gold mines, but also of its scope and form. In general all the arguments, raised by Messrs Cooke, Martus and Johnston in favour of extending the scope of the new assistance scheme can be accepted as sound.

Solvent loading: It is agreed that it is advantageous, as far as reagent cost is concerned, to operate at maximum solvent loading. However, owing to the fact that no reliable automatic solvent flow controller is yet available, control tends to be erratic with the result that there is risk of losing uranium. As can be seen from Mr Tunley's plot, the graph representing total ammonia cost is fairly flat between loadings of 3.5 and 4.0 gpl, while the graph representing uranium loss in the raffinate is steep. It is, therefore, safer to operate slightly below optimum loading in the absence of absolute control. Should the purity of the final product gain importance, operation at optimum loading or even slightly above, may be advantageous. Solvent losses and clarification of pregnant solution: The cost of replacing solvent, as indicated by Mr Carman, represents a high percentage of the overall Purlex costs. It is, therefore, agreed that, amongst other factors, efficient clarification of the pregnant solution and mixer-settler design have an important bearing on the cost. However, as at Blyvooruitzicht, the Buffelsfontein plant can tolerate a suspended solids content of 50 ppm without serious deterioration in efficiency. An increase in the suspended solids content from 15 to 50 ppm normally accounts for an increase of approximately 1 ppm in amine loss. Clarification of acidic pregnant solutions is much more difficult than that of alkaline solutions. Sand clarifiers are being used at Buffelsfontein with moderate success. Clarified solutions containing less than 20 ppm of solids in suspension can be produced, depending on the quantity and type of flocculant used in the filtration process, the thickness and the grading analysis of the sand beds and the quality of supervision. An on-stream duty of approximately 0.15 gallon per sq ft of surface area is obtained. Hydraulic handling of clarifier sand, while cleaning, may effect the efficiency of a clarifier, as size segregation of sand particles may lead to inefficient "pockets" in a sand bed. Control of the solution level in the sand clarifier also affects the quality of the effluent. Exposure of the sand bed invariably causes a cloudy effluent. Recycling of the final and initial solution discharged before and after skimming the clarifier sand improves the clarification efficiency significantly. Post-precipitation of silica and possibly sulphate salts, after clarification, may give a false impression of inefficient clarification. This phenomenon is more pronounced when treating hot supersaturated solutions. Ageing and cooling of the solution before clarification assist in stabilising the solution and reduce precipitation after clarification. The maintenance cost of sand clarifiers at Buffelsfontein is in the order of 0.35 cent per metric ton of solution treated. A redundant ion-exchange column has been tested successfully, either as a primary or a secondary clarifier, depending on the quality of the filtrate treated. The conventional pebble and sand beds in the column have been retained. Operation was enhanced by the addition of a two-foot deep resin bed as a filtering medium. The suspended solids content was reduced to less than 5 ppm. Mixer-settlers: Mixer-settler design is a controversial subject but, in view of the high costs of solvent compared to relatively low pumping costs, it is believed that mixing and pumping functions should be separated. Separate facilities for pumping and mixing not only give greater operational flexibility but also permit eventual changes in the flow circuit as technology develops. Scrub technique: Unlike the pilot plant, where the crud was carried away in the aqueous phase, crud is carried over with the organic phase in the full-scale plant. This carry-over of crud into the strip bank aggravates crud formation in the first strip stage. This phenomenon may result from a slight difference in settler design and/or a variation in the relative phase depths in the two plants. Bypassing of the scrub aqueous solution from the fourth to the second stage was introduced in order to avoid dilution and partial neutralisation of the acid added to the third stage, as it is known that a low pH value enhances the transfer of iron into the aqueous phase. The low aqueous flowrate in the third scrubbing stage was overcome by introducing an aqueous phase recycle. Gleaning: Mr MacDonald's contribution on "gleaning" was most informative. This process for recovering solvent from raffinate seems to show at least as much promise as coalescers and other methods employed to date. Similar tests conducted at Buffelsfontein pilot plant gave 60 per cent amine recovery from raffinate containing 10 ppm amine. However, the circuit was not operated at equilibrium and recovery may be expected to drop as the amine concentration of the "Gleaner" circuit increases.

His face wreathed in smiles, J. Richard Lucas, Chairman of the Keynote Session, conceded that "the papers appeared to have been of some interest." This was a modest description of the opening day of technical sessions at the SME Fall Meeting and Exhibition, October 13 to 15, in Tampa, Fla. The auditorium had capacity for 800 spectators and there was hardly a vacant seat visible. The topic, Resource Development of the Fertilizer Minerals, was covered in four authoritative papers. H. S. Ten Eyck set the stage. Resources are always viewed in relation to future requirements, and these depend largely on population. If the population trend continues, the world's 3.3 billion people will increase to 6.7 billion people by the year 2000. About 70% of this increased population will be in developing areas which are not capable of supplying sufficient food and fiber for their needs. Fertilizer is a means of bridging the crop shortage. Projections of fertilizer requirements by 1970 are from 53 million to 67.5 million long tons of plant nutrient which compares with 1964 consumption of 37.7 million tons. Looking ahead to 1980, the growth continues with an estimated demand of 80 million to 113 million tons combined of N P and K.

Jan 12, 1966

Discussion of the paper of R. J. COLONY, presented at the New York Meeting, February, 1921, and issued With MINING AND METALLURGY No. 169, January, 1921. R. J. COLONY (author's reply to discussion).-The work of Sosman and Merwin on the system lime-ferric oxide, mentioned by Mr. Rankin, was not overlooked. When studying portland cements and portland-cement clinkers petrographically, however, the lime-iron compound was difficult to correlate with the very definite dicalcium ferrite described by those investigators, which possesses such well-defined optical properties. In portland cements, the calcium ferrite (or ferrate?) is an indefinite, fuzzy, and generally amorphous, or apparently amorphous substance that is distributed interstitially with respect to the other grains, from which it was very difficult to derive any satisfactory results. For this reason, the writer, tentatively, chose to regard it as related to the aluminate, and assigned to it the composition 3CaO.Fe203, which may be incorrect, however, as Mr. Rankin suggests.

Jan 8, 1921

Jan 1, 1947

Jan 1, 1947

Jan 1, 1947

By Simon C. Dominy

"There are two main issues stemming from Vallée’s (2002) comments on Dominy et al. (2001b). First, he raises the importance of quality assurance/quality control (QA/QC) during resource estimation programs, and second, he indicates that the resolution and understanding of continuity (grade and geological) issues are paramount in the classification of resources. In particular, continuity is critical at the boundary between the Inferred and Indicated Mineral Resource categories. The original contribution agrees with the importance of these points, and the principal author offers the following discussion and clarification. Further comment is also provided on the reporting of grade uncertainty through grade ranges.It is worth remembering that vein-gold deposits (e.g., shear-zone, lode-gold, mesothermal types etc.), particularly those containing coarse gold particles (e.g., >100 µm), generally show large variations in grade and an erratic grade distribution. In most cases, diamond drilling is a good measure of geological continuity (depending on drill spacing), but a poor measure of grade and its distribution. High-nugget effect deposits rank among the most difficult deposit types in terms of producing an accurate and precise resource estimate, and clearly represent a distinct deposit type."

Jan 1, 2002

By H. Arima, Y. Kudo

In general, the iron content of zinc leach residue produced by sulphuric acid leaching from calcine is disposed as jarosite or goethite into a tailing dam. More recently, these iron residues have been treated pyrometallurgically to avoid waste disposal. The Iijima refinery selected a different zinc leach residue treatment process for iron control when it was established in 1971. The Iijima refinery is the only plant in the world that has processed a zinc leach residue by the combination of SO2 pressure leaching and O2 pressure hematite precipitation. The process enhances zinc recovery and recovers gold, silver, copper, lead and rare metals in saleable by-products. This paper focuses on the two stages of autoclave application in the zinc leach residue treatment process. The detailed flowsheet and recent advancements to improve the quality of by-products are discussed.

Jan 1, 2004

A comprehensive understanding of the effects of autoclave configuration (batch, semi-batch, continuous) on the residence time necessary to achieve a target conversion is a prerequisite for design of commercial scale autoclaves. Particle size distribution, mineral and reagent concentrations, temperature and mixing also influence the conversion. This paper outlines the bases of using test data to predict performance of commercial scale autoclaves. Recommendations for coordinating test program design with selection of scale-up method are provided. Examples are given to illustrate the different levels of engineering effort needed to meet corresponding levels of design optimization and accuracy.

Jan 1, 1998

By I. Farr, M. R. Mock, J. C. Robison

"HPAL and POX autoclave vapor-space gasses are vented through an autoclave PCV (Pressure Control Valve). The downstream steam-born mist of liquid droplets and solid particles travels in excess of 1000 m/s with megawatts of kinetic power at temperatures up to 160 C. The characteristics of downstream states often result in problems with corrosion, erosion, noise and vibration. Comprehension of those and related characteristics aids in improved pressure control, overpressure control and autoclave level control. We introduce compressible multiphase flow concepts and constructs germane to such flow including choked flow, continuous phase change, shock waves and supersonic flow plumes. Flow modeling based on first principles quantitatively predicts such flows providing a tool for component sizing and a method to estimate effects of water injection on flow. Insight deduced from modeling aids in mitigation of afore mentioned problems of which we share some from-site examples.INTRODUCTION First principles related to fluid thermodynamics and compressible flow have been employed akin to their application in the rocket industry. We will present the results of the application of those principles conceptually and authentically without mathematical rigour while using language of the pertinent disciplines. The autoclave (AC) vapor space over the slurry of a POX (Pressure Oxidation) or HPAL (High-Pressure Acid Leach) system (depicted in Figure 1) is vented via a PCV (pressure control valve) followed by certain ducting, and perhaps a nozzle, before exiting at atmospheric (typically) pressure. As indicated by its name the PCV controls the AC pressure as the flow control component of a pressure control loop."

Jan 1, 2017

By Claudio Acuña, Sergio Romo, Gerardo Fuentes

The leaching kinetics of a zinc concentrate in autoclave reactors were studied. A sample of concentrate from Bolivia, with typical mineralogical characteristics of the Andes region, was used. A concentrate containing 49% zinc and 145 ppm of silver from Minera Viacha was characterized chemically and mineralogically (atomic absorption, X-ray diffraction, and SEM microscopy) and tested in bench scale reactors. Two types of autoclave batch reactors were used at 40 bars of oxygen pressure and three levels of temperature (150°C, 200°C and 250°C). The solid to solution leaching ratio was 1:10 (10% sulphuric acid concentration). The effect of the particle size of the concentrate on the leaching kinetics was studied (P80: 145 and 45 µm). Iron from the leaching solution was removed by precipitation by increasing the pH in order to generate a clean solution for zinc electrowinning. The zinc solution was used to evaluate the feasibility of cathode production at the laboratory scale. Zinc extractions with higher liberation (P80 = 45 µm) reached up to 98%. Ground concentrate with finer sizes resulted in agglomeration and the use of dispersing agents did not improve slurry mixing. The leaching solution contained 55 g/L zinc and 7 g/L iron; it was purified by precipitating iron. The precipitation was evaluated using sodium hydroxide and ammonium hydroxide. In the first case, a colloidal suspension of ferric salts was formed while in the second case, different iron compounds were precipitated. The precipitate obtained with ammonium hydroxide had better filtering properties. Electrowinning was carried out using two types of cathodes (stainless steel and aluminium) and solutions purified with ammonium hydroxide. Zinc cathodes formed on stainless steel presented a better physical quality than those formed on aluminium.

Jan 1, 2015

By M. S. Hunter, Al Bishop

In 1994, Lone Tree Mine invited Hunter Hawk to participate in a problem-solving arena at their mine located in Valmy, Nevada. Lone Tree was experiencing consistency problems with autoclave valve component quality and delivery. Based upon a prior working relationship at Homestake Mining Company's McLauglin Mine, located in Lake County, California, both customer and vendor enjoyed a measure of rap­po1i and trust - the keys to problem solving communication. This paper is an overview of the problem solving process that has contributed to Lone Tree's excellent record of 95 per cent autoclave availability since 1995.

Jan 1, 1998

By T. Krumins, L. Zunti, R. Frischmuth

"Titanium and titanium alloys are commonly selected for pressure oxidation autoclave vent piping and pressure control valve components, as well as autoclave internals and other process piping. In the autoclave vent application, titanium ignition risk is controlled by limiting oxygen concentration, and preventing high gas velocity gas impingement on surfaces. Oxygen concentration is dependent on the autoclave pressure and temperature operating conditions and therefore oxygen concentration and the associated titanium ignition risk is dependent on standard operating procedures, process control interlocks and permissive conditions. It is not uncommon for these standard controls to be deficient during atypical operating conditions, or for operations to deviate from the operating procedures, increasing the potential for a titanium ignition incident. Titanium ignition risk caused by elevated oxygen concentration in autoclave vent systems can be reduced with the introduction of an online autoclave overpressure calculation and the configuration of associated interlocks and permissive conditions. INTRODUCTION High temperature pressure oxidation (>190°C) is a well recognized and versatile metallurgical oxidative pre-treatment process commonly used to liberate gold from refractory sulphide ores and concentrates before conventional leaching with cyanide. Titanium and titanium alloys are highly corrosion resistant in pressure oxidation process conditions and are therefore commonly selected as materials of construction for many components including: autoclave internals, agitators, process piping, and components in autoclave vent systems. Operations that anticipate or have experienced aggressive corrosion in the vent system often have little choice in material selection other than the use of titanium (Krag & Henson, 1992). Titanium is not suitable for use with elevated oxygen concentrations and is considered a restricted material because of its high pyrophoricity and combustion propagation properties (Beeson, Smith, Stewart, 2007). Several serious incidents have occurred in which titanium materials have ignited in autoclave applications (Zawierucha, McIllroy, Million, 1995). In autoclave vent applications, titanium ignition risk is reduced by preventing elevated oxygen concentrations, maintaining low gas velocities, and minimizing the potential for gas impingement on surfaces. Oxygen concentration in the autoclave vapour phase and vent system is dependent on the autoclave operating pressure and temperature conditions and therefore titanium ignition prevention controls typically include process interlocks and operating procedures based on the selected nominal design operating conditions. However, it is not uncommon for these controls to be deficient or for operations to deviate from the nominal operating conditions over time, increasing the risk of titanium ignition. The introduction of an online calculation of autoclave overpressure and a maximum target autoclave pressure as well as associated process control interlocks and permissive conditions can alert the autoclave control room operator and prevent an elevated oxygen concentration from developing, and therefore reduce titanium ignition risk in autoclave vent systems."

Jan 1, 2016

By Tracy T. Morris, Luis G. Navaro

"Anodic copper slimes produced during the electrolytic refining of copper are routinely batch leached to remove copper. At the Amarillo Copper Refinery, an atmospheric leaching process was converted to an autoclave pressure leaching system to improve the removal of copper, reduce the consumption of oxygen, improve leaching times and enhance tellurium recovery. The benefits of pressurized versus atmospheric leaching of slimes were soon realized by obtaining the desired level of decopperization in a shorter time and with lesser quantities of reagents. The autoclave was designed and constructed with a unique oxygen injection system that enables good control of the leaching process and with no plug-ups. Other features include a mass measuring system that balances the quantity of slimes to be leached to the desired final solution concentration based on initial feed concentrations. The end result was a more efficient and controllable leaching process for removing copper from anode slimes.IntroductionThe electrolytic refining of copper consists of an electrolytic cell filled with a sulfiiric acid based electrolyte and pairs of copper anodes and cathodes. When a current is applied, copper in the anode dissolves and is plated onto the cathode. Impurities within the anode that are more noble than copper do not dissolve and end up at the bottom of the cell and are referred to as slimes. Gold and silver are the main slimes constituents of interest because of their monetary value, but there typically are significant quantities of selenium, tellurium, lead, antimony, arsenic, bismuth, nickel, silica and tin. Copper is also present, usually as a metallic or as a reactant with tellurium, selenium, oxygen or sulfur and can range from 10 to 30% of the slimes fall."

Jan 1, 2012

By E. M. Timoshenko

Autoclave technology can be effectively used for liberation of complex mineral raw materials to transfer valuable constituents into solution for their subsequent recovery or to refine feed material in order to remove deleterious impurities, e.g. arsenic. The high efficiency of autoclave processes is attributed to the fact that they are suitable for processing of refractory raw materials, have low capital costs, high productivity, ensure integrated utilization of the feed materials, produce innovative saleable products, completely eliminate any air emissions, provide low-waste or waste-less technology, mechanization and automation of production processes. In the immediate future, it might be expected that autoclave processes will find use on commercial scale for production of heavy non-ferrous metals in combination with other processes (hydrometallurgical, upgrading, sorption and solvent extraction, electrolytic, etc.) to ensure: - Integrated processing of refractory ores and concentrates (pyrrhotite, zinc, copper-zinc, lead-zinc, nickel-cobalt, copper, pyrite); - Production of metallic powders of base metals as commercial products (copper, cobalt, nickel, etc.), composites on their bases, final products and saleable salts. Processing technologies incorporating autoclave processes, especially at the stage of liberation (chemical upgrading) of raw materials are characterized generally by high overall recoveries of valuable constituents significantly exceeding recoveries common for conventional pyrometallurgical processes (for some elements by several tens of percent).

Jan 1, 2006

By A. V. Tarasov

The high efficiency of autoclave processes is attributed to the fact that they are suitable for processing of refractory raw materials, have low capital costs and high productivity, ensure integrated utilization of the feed materials, produce innovative saleable products, completely eliminate any air emissions, provide low-waste or waste-less technology, as well as mechanization and automation of production processes. In the immediate future, it might be expected that autoclave processes will find use on commercial scale for production of heavy non-ferrous metals in combination with other processes (hydrometallurgical, upgrading, sorption and solvent extraction, electrolytic, etc.) to ensure: -Integrated processing of refractory ores and concentrates (pyrrhotite, zinc, copper-zinc, lead-zinc, nickel-cobalt, copper, pyrite); -Production of metallic powders of base metals as commercial products (copper, cobalt, nickel, etc.), composites on their bases, final products and saleable salts. Processing technologies incorporating autoclave processes, especially, at the stage of liberation (chemical upgrading) of minerals, are characterized generally by high overall recoveries of valuable constituents significantly exceeding recoveries common for conventional pyrometallurgical processes (for some elements by several tens of percent). An example is processing of low-grade refractory pyrrhotite concentrates using autoclave liberation of feed material under pressure of a new reagent, i.e., sulfur dioxide. The use of sulfur dioxide ensures a significant improvement in the recoveries of non-ferrous metals and platinoids to sulfide concentrate and smelting of the latter increases the capacity of the smelting units employed and minimizes the yield of discard slag and loss of metals in slag; in addition, it resolves the problem of sulfur dioxide utilization.

Jan 1, 2003

By D. Tahija

The Getchell Mine produces gold from a geologically complex ore bearing high concentrations of arsenic and carbonate minerals. The mill treats the ore using high temperature aqueous oxidation in autoclaves, followed by conventional carbon-in-leach gold recovery. We laboratory tested a variety of Getchell ores to determine the effects on gold recovery of conventional factors such as grind size and retention time, as well as the influence of factors such as ore variability and preliminary carbonate destruction. Because the mill is currently operating, we were able to directly compare certain laboratory predictions with operational results.

Jan 1, 1999