Further study of grain boundary fracture in the breakage of single multiphase particles using X-ray microtomography procedures

The present work aims to verify the 3D quantitative analysis of grain boundary fracture in the breakage of single multiphase particles using X-ray microtomography. The breakage of single multiphase copper ore particles (6 mm cubic particles) by slow compression was examined. From XMT reconstructed images using the Marching Cube method, interfacial areas between copper mineral grains and host rock were determined for both parent particles and progeny particles. In this way, the specific interfacial area ratio was calculated as a metric for grain boundary fracture. Preferential grain boundary fracture only occurs at low energy dissipation rates and the current results confirm initial results for 3 mm cubes published previously by Garcia et al. (2009).     

Adsorptive removal of arsenic from river waters using pisolite

This work presents the experimental results for arsenic removal from aqueous solutions using pisolite as a natural inorganic sorbent, a waste mineral product from Brazilian manganese ore mines. A pisolite sample was submitted to physical and chemical characterization; particle size analysis by screening, X-ray diffractometry, X-ray fluorescence, surface area determination by the Brunauer–Emmett–Teller (BET) method and atomic absorption spectrophotometry (AA) for the determination of the species concentration in the pisolite and in the aqueous solution samples from the experiments.Column and batch tests to contact pisolite and aqueous feed solutions were carried out for evaluation of the pisolite’s performance as a natural sorbent for arsenic removal. Experiments using activated pisolite and aqueous feed solutions prepared with Velhas River water were also performed. In the column system, 1.0 g of pisolite removed 1.41 mg of As (4.05% As extraction) from 630 ml of the aqueous feed solution and 1.0 g of activated pisolite extracted 3.51 mg of As (11.6% As extraction). Results for the batch tests with 100 ml of aqueous feed solution and 1.0 g of pisolite removed 1.29 mg of As (24.7% As extraction) and 1.0 g of activated pisolite extracted 3.17 mg (58.2% As extraction).     

Evidence for surface cleaning of sulphide minerals by attritioning in stirred mills

Recent developments in large scale stirred milling technology using ceramic media have allowed its application to relatively coarse particle streams. Apart from benefits in grinding finer more efficiently, benefits may also be derived from the surface cleaning action of stirred mills. This paper discusses evidence for the cleaning action of a stirred mill on the surfaces of chalcocite and effects on its subsequent flotation. Single mineral samples of chalcocite were ground with either stainless or mild steel grinding media. The effects of surface contamination by iron hydroxide on chalcocite floatability were studied using ethylene diamine-tetra acetic acid (EDTA) extraction, X-ray photoelectron spectroscopy (XPS) surface analysis and contact angle measurements. Depression of both coarse (+75 μm) and fine (?10 μm) size fractions was attributed to the surface precipitation of iron hydroxide species. Transfer of iron hydroxides from coarse particles to fine particles was observed with XPS analysis. Recovery of coarse particles (+75 μm) was improved by attritioning, while additional collector was needed to fully restore chalcocite recovery in both fine and coarse size fractions.     

A t10-based method for evaluation of ore pre-weakening and energy reduction

Currently the effect of the pre-weakening of ore particles by high voltage pulses is evaluated by the percentage change of A 1 b values between pulse-treated and untreated ore particles. The values of A 1 b, widely used as an ore breakage competence indicator in the mineral industry, are determined from the parameters of the JKMRC breakage models. In this study a t₁₀-based method was developed to predict the degree of size reduction, t₁₀, of pulse-treated particles from that of untreated particles broken at the same size/energy level. This method incorporates one parameter, C_Ab, which is equivalent to the percentage change of A 1 b values.The t₁₀-based method was validated using nine sets of comparative JK Rotary Breakage Tester data on pulse-treated and untreated ore samples over a wide range of impact specific energies and particle sizes. The t₁₀-based method can be used to calculate the energy reduction due to the pre-weakening effect in the downstream comminution process. It indicates that the energy reduction by pre-weakening increases with an increase in the target product fineness and the degree of pre-weakening, and with the decrease in feed particle size.     

Sub-populations and patterns in blast induced fine fragmentation

The understanding of fundamental mechanisms of fragmentation is still being developed. As such the fine fragmentation produced in a blast has been the subject to study. By examining the fines in the context of surface area instead of mass, several patterns and sub-populations have been observed. This paper is a study of fine fragmentation generated in small scale blasts. Each size distribution was transformed from mass into surface area. Each explosive charge was simulated in context of the energy it applied to the sample during breakage. This paper represents a small part of a larger study.The samples blasted in this study produced several aspects of self-similarity in breakage. Samples of the same rock type produced a similar surface area size distribution that was observed at a wide range of applied explosive energies. Each rock type had a characteristic surface area size distribution. Shape characteristics of measured fragments in the √2 sieve series shared similarities across a wide range of size fractions.Also paradoxically, the products of fine fragmentation were found to be multi-component in nature. A change in surface area size distribution was observed at 1 mm, which was found to be statistically significant. The fractal dimension of particles larger than 1 mm were found to be statistically different to particles smaller than 1 mm. Another change in particle character was found at 10 mm fragment size.The generation of fine fragmentation characterisation paradoxically has two fragment size thresholds of note, 10 mm and 1 mm, and is self-similar in nature. It is postulated that fragmentation is not a true fractal but the individual fundamental mechanisms that generate it may well be.     

Characterisation of coarse composite sphalerite particles with respect to flotation

The flotation response of a typical zinc-lead (Zn/Pb) ore, with respect to coarse composite (sulphide/non-sulphide) particles is reported. The flotation tests were carried out on a selected feed particle size range (−600 + 75 μm, at P₈₀ of 390 μm) and the recovery of Zn composite particles analysed on a size by size basis. The best results were achieved with the use of 75 g/t sodium isopropyl xanthate (SIPX), obtaining a Zn recovery of 77%, with a significant improvement at the coarse end of the particle size distribution. Computerised scanning electron microscope (QEMSCAN) was used to characterise value mineral grain size and degree of liberation, as well as gangue and sphalerite association in particles reporting to both concentrate and tailings. A new characterisation function (Locking ratio, LR) was developed based on the data from the automated mineralogical analysis to characterise particles into two-phase composites with different degree of locking texture (simple and complex). The function, which is based on the mode of occurrence of sphalerite, grain size, proportion and composition of the constituent minerals in each particle, was used to study the flotation response of the particles with different degrees of locking. The results highlight the difference in recoverability of the sphalerite bearing particles with different degrees of locking, with simple locking texture giving higher recovery than complex locking texture, for the same overall liberation.     

Density based separations in the Reflux Classifier with an air–sand dense–medium and vibration

The Reflux Classifier is a device consisting of parallel inclined channels above a fluidized bed. Water-based versions of the system have been successfully employed in industry for gravity separation of ?2 + 0.25 mm coal and mineral matter. In this study an air-fluidized system was investigated using a single 2 m long inclined channel with 100 mm wide channels and 20 mm perpendicular spacing. Sand (?355 + 125 micron) was used as a dense–medium and vibration at two distinct levels was used to improve fluidization stability. Tracer particles of ?6.35 + 1.00 mm nominal diameter and 1300 to 2400 kg/m³ density were used to study the effects of the vibration energy and vibration direction on the separation efficiency. The device was able to separate coal particles from a maximum of 8 mm down to 1 mm on the basis of density; hence this method has potential for industrial application. Results were analysed using a simple 2-parameter dispersion–convection model. Dense particles had negative slip velocities, low-density particles had positive slip velocities and the slip velocities were proportional to particle diameter.     

Using a high pressure hydrocyclone for solids classification in the submicron range

A 10 mm hydrocyclone was operated using a barite suspension with a maximum particle size of d^max = 7 μm. The test rig was equipped with a piston diaphragm pump for pressures up to 60 bar. At 40 bar and 20 °C, cut sizes d₅₀ were obtained down to 0.7 μm; increasing the temperature to 50 °C resulted in d₅₀ values down to 0.5 μm for a throughput of 0.6 m³/h. Another experiment was conducted at 40 bar using a batch hydrocyclone technology. Only the overflow was recirculated to the feed box, whereas the underflow was discharged via a collection box. Increasing the number of recirculations increased the separation of fines in the submicron range. The results showed that after 20 min particles with d^max = 1 μm were obtained in the hydrocyclone overflow. After 120 min, the particles size distribution had a d^max = 0.5 μm and a mean size of d⁵⁰ = 0.2 μm. This procedure requires high energy consumption and is thus suitable only for fractionating small quantities of particles in the submicron range.     

Stirred milling kinetics of siliceous goethitic nickel laterite for selective comminution

The objective of this study is to determine how grinding conditions affect the breakage rate with respect to the sample mass, major elements, and minerals present in siliceous goethitic (SG) nickel laterite. This information is helpful in determining the optimal grinding conditions for selective comminution and nickel upgrade. The kinetics of batch wet grinding of nickel laterites with feed sizes of 2.38–1.68, 1.68–1.18, 1.18–0.85, 0.85–0.6, 0.6–0.42, 0.42–0.3, 0.3–0.21, and 0.21–0.15 mm were determined using a Netzsch LME4 stirred mill under the following conditions: 1000 rpm, 50% charge volume, 150.0 g of solid. The grinding behaviour of the majority of the feed samples was non-first-order due to the fast breakage rate of soft minerals and the low breakage rate of hard minerals in the feed. Therefore, an enrichment of the soft mineral was obtained in the underscreen product by selective grinding. The effect of selective grinding on Ni upgrade was evaluated by looking at grinding time, feed size, and product size. Optimum grinding time with respect to Ni upgrade was 0.25 min for SG nickel laterite samples. Generally, grinding larger particles and/or collecting finer product size yielded better Ni upgrade results. The effect of selective grinding was evaluated by the changes of the major soft and hard minerals for the selected samples. Selective grinding was also examined with respect to the major element weight ratio (e.g. Si/Ni for SG nickel laterite). With respect to Ni upgrade, the best result was achieved from the 1.18–0.85 mm feed on the −400 mesh product after grinding for 0.25 min. The Ni grade increased from 0.73% to 1.30% (upgrade 76.8%), with 14.4% Ni recovery; the Mg grade increased from 1.30% to 3.96% (upgrade 205.6%); the Si grade decreased from 28.7% to 16.2%.     

α → γ → β-phase transformation of spodumene with hybrid microwave and conventional furnaces

Spodumene is the most important lithium containing hard rock mineral. In order to extract lithium from spodumene concentrate by leaching, the crystal structure of spodumene must be converted from the natural monoclinic α-form to the tetragonal β-form. The technical possibilities to generate the heat to the conversion process of spodumene concentrate via microwaves were studied. The heat treatment experiments were carried out with a domestic microwave furnace (700 W) with silicon carbide susceptor and with the conventional resistance heated furnace as a reference. In the microwave furnace the phase transformation of spodumene began after 110 s of heating and samples were converted almost completely to β-spodumene after 170 s. Partial melting of gangue minerals was observed in samples after 170 s of heating. Heating in microwave furnace for 170 s corresponded with the heating of approximately 480–600 s at temperature of 1100 °C in the conventional furnace. In addition to α- and β-forms an intermediate phase, hexagonal γ-spodumene, was identified from samples heated with both furnaces. The conversion of spodumene samples was verified with X-ray diffraction (XRD) and with field emission scanning electron microscope (FESEM).     

Post-regrind selective depression of pyrite in pyritic copper–gold flotation using aeration and diethylenetriamine

The present study investigates the effect of aeration and diethylenetriamine (DETA) on the selective depression of pyrite in a porphyry copper–gold ore, after regrinding (at grind sizes, d₈₀ = 38 and 8 μm) with respect to Au recovery and grade using oxygen demand tests, flotation, QEMSCAN, X-ray spectroscopy (XPS) and EDTA extraction analysis. It was found that pyrite depression increases after aeration and with decreasing grind size. This was observed to be due to the markedly higher oxygen consumption rate of pyrite at the 8 μm (kla = 0.10 min⁻¹) than at the 38 μm grind size (kla = 0.02 min⁻¹). The addition of DETA improved pyrite depression (9% with aeration only versus 39% with aeration + DETA) at the 38 μm grind size. Gold and copper flotation recovery followed pyrite recovery for the two grind sizes using XD5002 in the presence of air and DETA.The surface analysis (XPS and EDTA extraction) revealed that the significant pyrite depression at the 8 μm grind size was due to increased amount of surface iron oxides, oxy-hydroxides (FeO/OH), sulphate species and increased liberation of mineral phases (QEMSCAN analysis), whilst the poorer pyrite depression at the 38 μm grind size was due to insufficient liberation of mineral phases and the persistence of activating Cu on the pyrite surface. The addition of DETA increased pyrite depression at the coarser grind size due to a significant reduction in Cu(I)S and increased Cu(II)O species, correlating with the flotation results of pyrite under this test condition. Two-stage copper and pyrite flotation, followed by Au cleaning after regrinding to 38 μm grind size, under high pH or aerated condition is proposed as the recommended route to optimise Au flotation.     

The effect of particle size on acid mine drainage generation: Kinetic column tests

The rate of acid mine drainage (AMD) generation is directly proportional to the surface area and so to the particle size distribution of acid-forming minerals exposed to oxidation. Materials in various particle sizes are subject to weathering processes at field condition; however, the particle size dependent oxidation rate has not been investigated for understanding entire geochemical behavior at a mining site. Therefore, a comprehensive research program was aimed to investigate the effect of particle size on pH variation and acid mine drainage generation using kinetic column tests, and then to find convenient methodologies for upscaling laboratory-based results to the field condition. For this purpose, ore samples collected from Murgul Damar open-pit mining were grinded in three different particle size distributions that are coarse (minus 22.5 mm), medium (minus 3.35 mm) and fine (minus 0.625 mm) sizes, 34 columns were designed in different dimensions for kinetic column tests. It was found that the cumulative concentration of the many constituents measured from medium particles (minus 3.35 mm) are higher than coarser samples due to decreasing specific surface area with increasing particle size. Similarly, because of decreasing of hydraulic conductivity with increasing the fine content, the cumulative concentration of constituents measured from medium particles (minus 3.35 mm) are also higher than finer particles (minus 0.625 mm). Based on statistical and analytical analyses of the results of kinetic column tests, the time required to initiate acid formation at field condition varied between 489 and 1002 days depending on particle size distribution. In addition, considering the effect of particle size and the results of related statistical analysis, main oxidation (SO₄²⁻) and neutralization (Ca²⁺, Mg²⁺, Mn²⁺ etc.) products were also successfully upscaled to the field condition.     

Gold extraction by chlorination using a pyrometallurgical process

The feasibility to recover the gold present in alluvial material, by means of a chlorination process, using chlorine as a reactive agent, has been studied. The influence of temperature and reaction time was studied through changes in the reactant solid. The techniques used to characterize the mineral samples and the reaction residues were stereomicroscopy, X-ray diffraction, X-ray fluorescence and scanning electronic microscopy. Results indicate that gold extraction is favored by increasing, both, the temperature and the reaction time. The best recovery values were of 98.23% at 873 K and 3600 s and of 98.73% at 873 K and 5400 s, with very low attack of the matrix containing the metal. The powder of pure gold was not chlorinated at this temperature level.     

Effect of mechano-chemical activation on bioleaching of Indian Ocean nodules by a fungus

The effect of mechano-chemical activation of Indian sea nodules, while recording the zeta potential, particle size distribution and surface area, on the bio-dissolution of metals by Aspergillus niger has been investigated. Activation is a term used to indicate what takes place when increasing grinding time does not result in significant change in particle size but rather results in the accumulation of energy that may lead to the development of lattice defects within the particles that can aid biological attack. It was observed that the mechano-chemical activation improved the bio-dissolution of metals such as copper, nickel and cobalt from the sea nodules at initial pH in the range 4.0–5.0. With 10 min milling of particles of ?75 μm size, 86% material was reduced to ?10 μm size with a change in zeta potential from ?18 to ?34 mV. Above 95% copper, nickel and cobalt each was leached out in 15 days time from the nodules activated for 10 min at 5% (w/v) PD and 35 °C temperature with initial pH of 4.5; the biorecovery being almost similar when the material was activated for 30 min. In the case of nodules without activation, ?89% metal bioleaching was achieved in 25 days time at an initial pH of 4.5 under this condition. The mechano-chemical activation of sea nodules has thus influenced the bio-dissolution process, while providing a wider pH range available for processing of nodules with the involvement of organic acids such as oxalic and citric generated from the fungus.     

Ionic liquid-based modified cold-induced aggregation microextraction (M-CIAME) as a novel solvent extraction method for determination of gold in saline solutions

Modified-cold-induced aggregation microextraction (M-CIAME) was used for determination of gold in saline solutions. It is robust against the much higher concentration of salt (up to 40%). In this method sodium hexafluorophosphate (NaPF₆) was added to the sample solution containing Au-TMK complex and a very small amount of 1-hexyl-3-methylimidazolium tetrafluoroborate [Hmim][BF₄]. Afterward the solution was cooled in an ice bath and a cloudy solution was formed. After centrifuging, the extractant phase was analyzed using a spectrophotometric detection method. Under the optimum conditions, the limit of detection (LOD) was 0.7 ng mL^?1 and the relative standard deviation (RSD) was 1.65% for 50 ng mL^?1 gold. The method was applied for the determination of trace amount of Au in mineral and seawater with satisfactory results.     

Fundamental aspects of hematite flotation using the bacterial strain Rhodococcus ruber as bioreagent

Previous research showed the effectiveness of bacterial strains as flotation reagents on Hematite beneficiation. The aim of this work is to study and evaluate Rhodococcus ruber as a biocollector. The sample was conditioned with the biomass suspension by stirring under specific conditions as particle size, biomass concentration, pH solution and conditioning time. The results showed a change in hematite zeta potential profile after interaction with R. ruber, and its adhesion onto the mineral surface was higher at pH 3 and at concentration of 0.60 g/L (10⁹ cells/mL). Flotation studies were carried out in a 0.23 L modified Partridge–Smith cell flotation, and the highest floatability (84%) was achieved at size fraction −53 μm +38 μm under the conditions mentioned before. Complementary floatability studies were performed using the conventional frother Flotanol D24 combined with the R. ruber biomass, finding interesting results for the bigger particle size range. Thus, this research aims to evaluate the efficiency of bioflotation of minerals, particularly hematite, and the potential use of R. ruber as biocollector, projecting its future application in mineral flotation industry.     

Ore impact breakage characterisation using mixed particles in wide size range

The Drop Weight Tester (DWT) for ore impact breakage characterisation uses particles in five narrow size fractions, and the JKMRC Rotary Breakage Tester (JKRBT) uses four size fractions, both with three impact energy levels for each size fraction. It is time consuming to prepare these narrowly sized particles and to carry out size analysis on the 15 DWT or 12 JKRBT products, so a Wide-size JKRBT characterisation method was developed. In this method, the mixed particles in 13.2–45 mm size range are tested as one size class in the JKRBT by single-particle breakage mode. The wide-size feed is then divided into several virtual narrow size fractions by simulation, based on which the impact product size distributions are calculated using a size-dependent breakage model. Four sets of measurement data, consisting of two feed samples in the 13.2–45 mm size range with different size distributions tested with two impact energy levels, are adequate to determine the three model parameters. In the case where a benchmark ore of known breakage characteristic parameters is available, one Wide-size JKRBT impact treatment can determine the ore competence change parameter using a t₁₀-based model.     

Sample requirements for HPGR testing procedure

Green field projects demand relatively large amounts of sample from drill-cores. Besides chemical analysis, samples are required for mineralogy and liberation characterization, physical characterization, concentration tests and a number of tests for crushing and grinding parameters. If the project’s process route includes a possible HPGR grinding stage, lab-scale tests for scale-up and variability analysis are required. HPGR grinding characterization can be carried out in a small diameter roll HPGR, such as the LABWAL. Some commercial labs recommend 20–30 kg samples for steady-state tests, but this is a rather large sample from the point of view of a green field project campaign. The question that is being assessed here is how much sample is really required? Surely, the more material that is available the more reliable will be the test results. However, when the sample mass size is reduced, what is the impact on the data that is produced? In this work, six phlogopitite samples weighing 20 kg were tested in the LABWAL HPGR using six initial hydraulic pressures, 10, 20, 30, 40, 50 and 60 BAR. The specific capacity and specific power factors were determined, as well as the critical angle of nip, and the critical gap. Size distributions were measured and size-mass balance parameters were determined for the Austin model under the range of grinding pressures that were produced. With the data, a hypothetical industrial HPGR for the phlogopitite was designed for a standard capacity of 100 t/h and operating at 2 N/mm² specific grinding force. The work was then repeated using 10 kg samples and 5 kg samples. Results show that, under the conditions that were chosen, samples weighing 5 kg are sufficient for characterization in the LABWAL HPGR.     

Kinetics of saprolitic laterite leaching by sulphuric acid at atmospheric pressure

Mineralogical analyses of the saprolitic laterite material have been characterized by X-ray fluorescence (XRF), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermal analysis, scanning electron microscope (SEM) and energy dispersive X-ray analysis (EDAX). Results showed that the saprolitic laterite material consists mainly of nickel-substituted lizardite showing the pebble-like morphology and traces of magnetite and phlogopite. Leaching results showed that as much as 84.8% nickel could be leached under the experimental conditions of 10% (v/v) H₂SO₄, 90 °C reaction temperature, leached within 5 min, particle size d₅₀ = 25 μm, stirring at 500 rpm and liquid to solid ratio 3:1. The kinetics of nickel and magnesium leaching from the saprolitic laterite material have been investigated in a mechanically stirred reactor and the activation energies were determined to be 53.9 kJ mol^?1 for nickel and 59.4 kJ mol^?1 for magnesium respectively, which are characteristic for a chemical reaction controlled process. The similarity of the activation energies of nickel and magnesium leaching from the saprolitic laterite material by sulphuric acid means that nickel in lizardite is loosely bound within the octahedral layer and almost all of the nickel could be leached simultaneously with magnesium but without complete decomposition of the silicate structure.     

Evaluating waste rock mineralogy and microtexture during kinetic testing for improved acid rock drainage prediction

This study integrates detailed mineralogical and microtextural analyses of waste rock with the results of standard kinetic test procedures to identify the mineralogical changes that influence leachate chemistry over time. The integration of mineralogy and texture provides the opportunity for improved mine waste management strategies and acid rock drainage (ARD) prediction.Waste rock material from an abandoned gold mine in northern Queensland, Australia, was subjected to column leach kinetic testing over a 30 week period. The column feed comprised of a range of waste rock lithologies (porphyritic rhyolite, massive arsenopyrite, massive pyrite ± galena, and semi-massive polysulphide). In total, 12 individual columns were established to represent six lithologies prepared to two different size fractions (−10 mm and −4 mm). The mineralogy and microtextural characteristics of the column feed material was defined using quantitative X-ray diffractometry (QXRD), scanning electron microscopy and laser ablation (LA-ICPMS) at the start of kinetic tests, and at 5 week intervals during the length of the tests. These data were directly correlated with leachate chemistry (i.e., pH, SO₄ and select elements).Results of this study indicated that sulphide oxidation was strongly influenced by the morphology of sulphide minerals, their trace element contents, the presence of mineral micro-inclusions and galvanic interactions with other sulphide minerals. Waste rock with abundant arsenopyrite was consistently the most acid forming, and oxidised to scorodite (enriched in Zn, Pb and Cu). Pyrite was commonly As-rich as indicated by LA-ICPMS mapping. QXRD results indicated that the abundance of rhomboclase, jarosite, alunite and hydrous ferric oxides increased over time. Galena weathered rapidly to porous anglesite, particularly when in direct physical contact with pyrite. Sphalerite contents decreased consistently over the 30 weeks implying its oxidation, however few reaction products were directly observed. By week 30, the −4 mm fraction material generated lower pH leachate, higher mass release of elements and sulphate for the majority of samples. This indicates that the particle size used in kinetic tests can exert a significant control on leachate chemistry, especially in the absence of abundant neutralising minerals. This contribution demonstrates the value of integrating mineralogy and microtextural analyses during kinetic testwork to improve the interpretation of sulphide oxidation for better prediction of ARD.