Analysis of Phosphate Ore Samples by Wavelength Dispersive X-Ray Fluorescence Spectrometry (WDXRFS): Implications for Grade Control during Mining and Process Optimization

Rapid quantitative determination of major and trace elements in silicate rocks and soils employing fused glass discs using wavelength dispersive X-ray fluorescence spectrometry

A non-oxidative alkaline sample digestion procedure using tetramethylammonium hydroxide and a high pressure, microwave assisted autoclave digestion system was developed. The silicon concentrations of the digested samples were measured by inductively coupled axial plasma optical emission spectrometry (ICP-OES). Details of the digestion conditions as well as the optimised instrumental parameters for ICP-OES are described. The method was developed and tested using silicon-spiked ascorbic acid and applied to samples of animal tissue and organs. The total silicon content of two different reference materials, NIST 1577b Bovine liver and BCR 184 Bovine Muscle having neither certified nor informational values for Si was determined. The results obtained are compared with the results of independent methods such as wavelength dispersive x-ray fluorescence spectrometry (WDXRF) and solid sampling electrothermal atomic absorption spectrometry (ETAAS). The method described achieves a limit of detection of 2 mg kg(-1) using 100 mg of solid biological or organic material and covers a concentration range of up to 500 mg kg(-1).

An accurate determination of cryolite ratio in industrial aluminum baths by wavelength-dispersive X-ray fluorescence spectrometry

This work aimed to upgrade a low-grade sedimentary phosphate ore through attrition scrubbing/desliming and an anionic/cationic reverse flotation technique. The mineralogical and chemical examination showed that the sample contained low-grade apatite minerals (P2O5 ~ 22.5%), and the main associated gangue minerals were gypsum and quartz. The effects of both collector and depressant dosage were investigated and optimized in each individual flotation process. The results of attrition scrubbing accompanied by desliming showed that a high content of P2O5 (27.97%) with a recovery of 72.1% was obtained in the coarse size fraction (+53 µm), and the majority of quartz and gypsum separated in the fine size fraction (−53 µm). The effect of using a new tall oil collector mixture was investigated during the anionic reverse flotation. Sodium tripolyphosphate (STPP) was used as a phosphate depressant during anionic and cationic reverse flotation. The flotation results of the deslimed sample demonstrated that cationic reverse flotation was much more desirable in terms of achieving a high grade and recovery of P2O5 compared to anionic reverse flotation. Considering the statistical design, a maximum grade of 31.23% P2O5 with a recovery of 95.22% was obtained in the non-floated fraction using 950.88 g/t of the collector (amine) and 500 g/t of the STPP.

A continuous-flow dialysis (CFD) method with on-line inductively coupled plasma optical emission spectrometric (ICP-OES) simultaneous multielement measurement for the study of in vitro mineral bioavailability was developed. The method was based on a simulated gastric digestion in a batch system followed by a continuous-flow intestinal digestion. The simulated intestinal digestion was performed in a dialysis bag placed inside a channel in a flowing stream of dialyzing solution (NaHCO3). The mineral concentrations in the dialysate were determined by ICP-OES using Y and Sc as internal standards. The pH of the dialysate was also monitored on-line to ensure pH changes similar to the situation in the gastrointestinal tract.The developed system was applied to determining the dialysability of five essential elements (Ca, Mg, P, Fe, Zn) for various kinds of foods, i.e., milk-based infant formula reference material (NIST SRM 1846), milk powder, kale, mungbean, chicken meat, jasmine rice, and Acacia pennata. The dialysis profiles of elements and pH change profiles can be useful in understanding the dialysis change and factors affecting dialysability. All studied elements were rapidly dialysed in the first 30 min of simulated intestinal digestion. It is expected that this system will be useful for estimation of dialysability and for studying the mutual effects of components in food.

The performance and response of two commonly used certified reference materials (CRMs) for mafic rocks MRG-1 (CANMET, Canada) and JGb-1 (Geological Survey of Japan), both gabbroic in composition, are evaluated for a set of mafic plutonic rocks (gabbros) from Boggulakonda (BK) occurring to the east of Proterozoic Cuddapah Basin, South India. In this study, quadrupole-inductively coupled plasma mass spectrometry was used to generate trace and rare earth element (REE) data using MRG-1 and JGb-1 as calibration standards separately for a comparative study. It is found that the two CRMs show highly variable major, minor and trace element compositions except RREE. When used for BK gabbros, JGb-1 has yielded better results than MRG-1 with respect to trace elements (HFS elements Nb and Ta in specific), whereas a good agreement was observed between both CRMs for REE concentrations when compared with certified data. The Nb- Ta element distribution patterns for BK gabbros in the spidergrams plotted using JGb-1 as CRM show relatively prominent and pronounced negatively spiking anomalies with reference to Th, whereas using MRG-1 as calibration CRM yielded unresolved and unclear Nb-Ta anomalies in the present study. The geochemistry (major, minor and trace) of MRG-1 is different when compared to that of JGb-1. Probably this is reason for the disparity in the results obtained by inductively coupled plasma mass spectrometry on mafic plutonic rocks. The study conducted on the BK gabbros, reveals better and reliable results using JGb-1 as CRM. This study also reveals the importance of using proper CRM for calibration having closely matching trace and REE concentrations in addition to major and minor elements, for obtaining reliable data in geological samples.

Determination of trace metals by ICP-OES in petroleum cokes using a novel microwave assisted digestion method

This work demonstrates the feasibility of wavelength dispersive X-ray fluorescence for the assessment of lead in animal bone powder. When applied to real bone samples, this analytical procedure produced results compatible with current knowledge of lead metabolism, emerging as an important tool in the investigation of relevant issues in Public Health.

Analytical aspects of the CEEM soil project

Gold production in South Africa is projected to continue its decline in future, and prospects for discovery of new high-grade deposits are limited. Many of the mining companies have resorted to mining and processing low-grade and complex gold ores. Such ores are technically challenging to process, which results in low recovery rates, excessive reagent consumption and high operating costs when compared to free-milling gold ores. In the Witwatersrand mines, options of blending low-grade gold ores with high-grade ores exist. Although it is well known that most of the Witwatersrand gold ores are highly amenable to gold cyanidation, not much is known on the leachability of blended ores, especially the effects of mineralogical and metallurgical variability between different gold ores. In this study, we apply a geometallurgical approach to investigate mineralogical and metallurgical factors that influence the leaching of blended ores in a set of bottle shaker and reactor column tests. Three gold-bearing conglomerate units, so-called reefs, i.e., Carbon Leader Reef, Ventersdorp Contact Reef and the Black Reef, all in the Carletonville goldfield, were sampled. The ores were prepared using a terminator jaw crusher followed by vertical spindle pulverizer (20 kg aliquot) and high-pressure grinding rolls (80 kg aliquot). Mineralogical analysis was conducted using a range of complementary tools such as optical microscopy, QEMSCAN and micro–XCT. The results show that Witwatersrand gold ores are amenable to the process of ore blending. Some of the ores, however, contain impervious inert gangue and reactive ore minerals. Leach solution can only access gold locked in impervious gangue minerals through HPGR-induced pores and/or cracks. The optimum ore blending ratio of the bottle shaker experiments (p80 = − 75 μm) comprises 60% Carbon Leader Reef, 20% Ventersdorp Contact Reef and 20% Black Reef and yields 92% recovered Au over a leach period of 40 h. Blended ores with high carbonaceous material (> 1 wt% carbonaceous material, (Black Reef = 36–60%) yield lower recoveries of 60–69% Au). Ore leaching at the mixed-bed reactor column (− 75 μm and − 5.6/+ 4 mm) yields about 70% over a leach period of two weeks. We therefore suggest that the feasibility of ore blending is strongly controlled by the mineralogy of the constituent ores and that a mixed-bed reactor may be a viable alternative method for leaching of the low-grade Witwatersrand gold ores. Material from certain reefs, such as the Black Reef, has synergistic/antagonistic (nonadditive) blending effects. The overall implication of this study is that ore blending ratios, effects of comminution on mineral liberation, an association of gold with other minerals, and gold adsorption behavior will greatly inform future technology choices in the area of geometallurgy.

A serious problem faced by the metal mineral mining industry is the challenge to the sustainable development of resource mining due to the continuous decline of ore geological grade. In the case of producing concentrates of the same quality, compared with using only high-grade raw ore, ore blending is a way to slow down the decline of ore geological grade by combining high- and low-grade raw ore. There are many ore blending models considering cost minimization or profit maximization as the target value, ignoring the fact that ore blending is intended to obtain a homogenized product. Moreover, the ore blending model cannot be solved by traditional operational research methods when blended grade stability of multiple elements is considered in the ore blending program. In this paper, a multi-objective ore blending optimization model is constructed for the comprehensive utilization of associated resources in ores. It minimizes the deviation of the grade of each metallic element in the blended associated ore from the beneficiation grade and the percentage of different types of rocks at the unloading point. To solve this multi-objective optimization model, an intelligent optimization method is proposed that is an improved multi-objective optimization algorithm based on the Non-dominated Sorting Genetic Algorithm III (NSGA-III). The case study shows that the proposed model and algorithm can effectively solve the mixing problem of polymetallic ores and obtain a satisfactory ore blending solution.

Acidification and trace elements lack in the soil deteriorates the healthy planting of crops in China. One effective approach to relieving soil acidification and infertility is to use alkaline-fused calcium magnesium phosphate fertilizer (FMP). As a carrier of many micronutrients, low-grade phosphate ore was used as the raw materials to prepare the alkaline FMP in this work. An efficient burdening for preparation of FMP based on the glass structure factors (Ob/Yb) was briefly introduced, and then the fusion characteristic of the low-grade phosphate ore with various Ob/Yb values was characterized. Melting experiments show that the increase of melting temperature and time can dramatically enhance the effective conversion of nutrient elements in phosphate ore. After melting at 1450 ℃ for 10 min with Ob/Yb of 3.06, 94.87% P2O5, 91.68% CaO, 93.69% MgO, and 92.46% SiO2 are activated in the alkaline FMP, which can be readily absorbed by the crop root system.KeywordsFused calcium magnesium phosphate fertilizerMelting temperatureMelting timeEffective conversion

ABSTRACTThe extraction of phosphoric acid by tributyl phosphate (TBP) in kerosene from hydrochloric acid leach liquor of El-Sebaeya low-grade phosphate ore was carried out. The influence of various factors affecting the leaching process such as particle size, reaction time, acid concentration, liquid/solid mass ratio, reaction temperature and stirring speed were thoroughly studied to estimate the favor phosphate ore dissolution in relation to impurity. Thereafter, the effects controlling the extraction step, including shaking time, solvent concentration, aqueous/organic phase ratio, and reaction temperature, have been studied in terms of the maximum P2O5 extraction efficiency and the minimum impurities extraction efficiency. The obtained loaded organic solvent was subjected to the stripping stage using double-distilled water. The outlet stripping liquor was concentrated by evaporation up to 62% P2O5.

In order to evaluate the slurry nebulisation method as an alternative method for analysis of sewage sludge, the metal content of sludge samples of different origins was determined. The concentrations of six elements: Cd, Cr, Cu, Ni, Pb, and Zn were determined by introducing the sludge as a slurry into an inductively coupled plasma optical emission spectrometer (ICP-OES). Calibration was performed by using aqueous standard solutions. For comparison, the sewage sludge was also digested by microwave digestion and introduced into the plasma as an aqueous solution. The accuracy of the method was checked by analysing a sewage sludge certified reference material (CRM 007-040 Sewage Sludge). The Student's t-test showed that values obtained using slurry nebulisation were close to the certified values at a 95% confidence level. The values of elements Cd 11.1 ± 0.8; Cr 37.7 ± 3.3; Cu 563.3 ± 38.4; Pb 119.2 ± 10.1; Zn 729 ± 68.2 mg kg−1 obtained using this method were comparable with those obtained using the conventional method. The slurry method can, therefore, be successfully applied to the determination of content of each element in sewage sludge with RSD less than 3%, without the need to predissolve them. This could avoid the use of hazardous chemicals, incomplete dissolution and loss of volatile analytes.

A review of the beneficiation of calcareous phosphate ores using organic acid leaching