The stability of the certified reference ores MP-1 KC-1 and SU-1 towards air oxidation

The stability of three certified reference sulphide ores, MP-1, KC-1 and SU-1, towards air oxidation has been measured at 50 degrees and 40, 62 and 82% relative humidity, and at 62% relative humidity and 34 degrees and 67 degrees . Both the relative humidity and temperature affect the rate of oxidation but their relative importance depends on the mineralogical composition of the ore. Changes in the water-extractable metals and elemental sulphur content on oxidation have been determined. It is concluded that these ores may be stored safely in sealed bottles under normal laboratory conditions.     

Oxidation of sulphide minerals--II: determination of metal in the oxidation products of galena, sphalerite and chalcocite

A 15% ammonium acetate and 3% acetic acid solution has been shown to be useful in the determination of the principal metal in small amounts of the oxidation products of galena, sphalerite and chalcocite. Its use in the determination of the extent of oxidation in concentrates or complex ores of these minerals is implied.     

XRF 熔融制样法测定铜精矿中的Cu、Fe、S、Pb、Zn、As、Bi、Mo

提出了以熔融制样法,用ＰＷ１４０４Ｘ射线荧光光谱仪测定铜精矿中Ｃｕ、Ｆｅ、Ｓ、Ｐｂ、Ｚｎ、Ａｓ、Ｂｉ、Ｍｏ,探讨了铜精矿的预氧化条件,熔融条件和玻璃化试剂地制样的影响。     

Extraction of contaminant metals from dumped metacolloid ores in order to reduce their hazardousness

Problems of human and environmental protection from discharges formed in out-of-balance ores dumped from nonferrous metallurgy were considered. To the most hazardous dumps belong those of metacolloid ores, discharges from which are contaminated with copper, zinc, iron, and also indium and cadmium. It was found that the most effective way to preclude the contamination is by using heap leaching of contaminant metals from ores in the chemical reclamation of the dumps. Mathematical dependences of the leaching rate of easily soluble compounds of metals (copper, zinc, indium, and cadmium) from metacolloid ores on the main technological factors of the process: sulfuric acid concentration, ore spraying density, and oxidation interval between sprayings were determined, the optimal process modes were found, and the cost-efficient production of metals in reclamation of dumps of this kind to a state in which they hardly contaminate the environment was calculated.     

稀土矿石成分分析标准物质的研制

介绍两种稀土矿石成分分析标准物质的研制过程。采用X射线荧光光谱法检验标准物质的均匀性和稳定性，标准物质的均匀性和稳定性良好。由8家具有权威性的测试单位协同定值及对数据进行数理统计，确定了该标准物质的标准值及标准偏差。     

Spectrophotometric determination of osmium with the use of 3-methyl-2,6-dimercapto-1,4-thiopyrone in concentrates and alloys

Taking into account the specific features of the complexation of osmium(VI) and osmium(IV) with 3-methyl-2,6-dimercapto-1,4-thiopyrone without a change in the oxidation number of the given element and properties of complexes formed in aqueous and organic solutions, schemes were proposed for the instrumental (including spectrophotometric) determination of osmium with the preconcentration and separation from concomitant components without distillation of its tetroxide from technological solutions or solutions of an alkalioxidizing sample decomposition. A procedure was proposed for the direct spectrophotometric determination of osmium(VI) in solutions; the accuracy of the procedure was verified with a standard reference sample of a platinum concentrate. The developed procedure was used for the determination of osmium in the flotation slime of ores from Dzhezkazgan deposits and in alloys.     

Multielemental photon activation analysis of copper-molybdenum ores and products of processing using a microtron bremsstrahlung

A method of Multielemental Instrumental Photon Activation Analysis (IPAA) of copper-molybdenum ores and its products processing using microtron bremsstrahlung is described. The activities of the irradiated samples were measured by means of Ge(Li) and HP-Ge-detectors. Quantitative determinations of elements were performed on standard reference materials. This method allows the determination of 10–24 elements in the samples. The results of these IPAA measurements are compared with the data of the Mongolian reference materials of copper-molybdenum ores and the products of processing.     

Spectrophotometric method for assessing oxidation of chalcopyrite-bearing ores and concentrates

The short-term oxidation of chalcopyrite ores and concentrates, during storage, can be monitored by measuring the absorbance of the purple Cu(I)-biquinoline complex that is formed when powdered samples are agitated directly with a water-acetone solution of 2,2'-biquinoline.     

电感耦合等离子体发射质谱法测定钨矿石中的钨华

建立电感耦合等离子体发射质谱法测定钨矿石中钨华的含量。用氨水溶液对矿石样品进行浸取分离,将浸取液稀释10倍体积后测定,以3%盐酸溶液作为测定介质。WO3的质量浓度在0~100 ng/m L范围内与信号强度呈良好的线性关系,相关系数为0.999 9,方法检出限为0.5 ng/m L。用该方法对5个钨矿石样品和2个标准物质样品中的钨华进行测定,测定结果的相对标准偏差为2.15%~9.46%(n=12),且与经典方法极谱法测定结果的相对偏差小于10%。该方法快速、简便,精确度较高,可用于钨矿石中钨华的测定。     

Determination of lithium by boron spiking and proton irradiation

A major matrix effect that hampers nuclear analysis with charged particles is found in the range differences which charged particles experience in samples and comparators. The determination of lithium in ores was attempted by the previous determination of the ranges of protons therein. This was achieved by the homogeneous spiking of the ores with pure boron compounds of known composition and therefore known calculated ranges. Pure lithium compounds, also with known calculated ranges, were used as lithium standards. Determinations were carried out by proton-induced prompt photon spectrometry on nuclides of lithium and boron. Results obtained for standard reference ores, SRM 181 and-183, were in good agreement with the specificfied values.     

Atomic-absorption spectrometric determination of silver,bismuth and cadmium in sulfide ores by direct atomization from the solid state

Atomic absorption spectrometric determinations of silver, bismuth and cadmium in the Canadian SU-1 and the Nordic ASK reference sulfide ores and in a series of Norwegian sulfide ores of technical importance, were carried out by atomizing the elements directly from the solid state. Atomizations were made in a high-frequency induction-heated graphite furnace. For comparison purposes, samples were also decomposed, and analyses made by atomizing sample solutions in the furnace and in the flame.     

Radioactive ore analysis by optimized radioisotope X-ray fluorescence technique

A method for analyzing U and Th in radioactive ores by radioisotope excited X-ray fluorescence is described. For the proposed analysis, the theoretical and experimental factors that affect the sensitivity of the radioisotope XRF technique were investigated. Minimum detection limits of 13 ppm and 108 ppm can be achieved for U and Th, respectively, with a total counting time of 1000 s on a powdered ore sample. Results obtained in the analyses of radioactive ores from Turkey and BL-5 candidate reference uranium ores from CANMET (Canada Centre for Mineral and Energy Technology) are reported.     

Rapid method for total iron determination in iron ores, sinter and related materials without use of mercury compounds

A rapid method for determining total iron in iron ores, sinter and related materials without use of mercury compounds is described. Fusion of the sample with sodium peroxide in a zirconium crucible and subsequent treatment with acid yields total decomposition and a solution amenable to direct reduction to ferrous iron with a silver reductor and subsequent titration with dichromate. Results for NBS, BCS and ISO reference standard ores demonstrate the universal applicability of the method both for routine and referee analysis. There is no interference from vanadium and two samples can be analysed in 30 min.     

Chelatometric determination of calcium and magnesium in iron ores, slags, anorthosite, limestone, copper-nickel-lead-zinc ores and divers materials

Chelatometric methods for the determination of calcium and magnesium in iron ores, slags, anorthosite, copper-nickel-lead-zinc ores and various other materials are described. Potential interfering elements are masked with triethanolamine and potassium cyanide. In one aliquot calcium is titrated at pH > 12, with calcein and thymolphthalein mixed indicator and in another aliquot calcium and magnesium are titrated in ammonia buffer, with o-cresolphthalein complexone screened with Naphthol Green B as indicator. The results compare favourably with certified values for reference materials of diverse nature.     

Methodological information from the certification of CCRMP ores and concentrates

In the course of 90 certifications for 27 elements in 26 reference ores and concentrates, carried out by the Canadian Certified Reference Materials Project, much methodological information has been documented and is now made available to analysts for the selection of suitable methods for the analysis of specific materials. Information is presented for copper, gold, lead, silver, sodium, potassium, tin, tungsten, uranium and zinc. A relationship between the average coefficient of variation and element concentration makes it possible to make some generalizations about the precision to be expected for a given concentration of an element in ores and concentrates.     

The role of 70-80% perchloric acid as oxygen donor and the oxidation potentials made available

A study has been made of the probable oxidation potentials provided by perchloric acid in the concentration range 70-80 %. The effect of acid concentration and temperature on the oxidation of chromium, vanadium, cerium, and manganese has been investigated. Available oxidation potentials appear to be 2.0-2.1 V or higher. The monohydrate of perchloric acid, HClO(4).H(2)O, containing 84.6% of perchloric acid, has been made commercially available and authorized for distribution by common carrier. It can be diluted to give acid concentrations from 73.6% (corresponding to HClO(4).2H(2)O) upwards. Perchloric acid mixed with sulphuric acid is equivalent to high concentrations of perchloric acid and can be used for dissolution of ores and destruction of organic matter.     

Presentation of differential laser-induced fluorimetry as a reference measurement procedure for determination of total uranium content in ores and similar matrices

The metrological principle of ‘differential technique in laser-induced fluorimetry’ analysis is discussed and recommended as a reference measurement procedure for determination of total uranium content in ores and similar matrices. The estimated relative expanded uncertainty values obtained for uranium content in standard IAEA samples are, S 1, 0.04 g/kg, S 2, 0.06 g/kg, S 3, 0.04 g/kg, and for S 4, 0.10 g/kg, respectively. These low uncertainty values obtained for uranium show high metrological quality of differential technique. This reference measurement procedure guarantees the quality of an analytical result (accuracy, high precision, reliability, comparability, and traceability). Laser-induced fluorimetry will be useful for the analysis of uranium in ores, certification of reference materials, borehole core assay, and other diverse applications in nuclear fuel cycle. Differential technique in spectrophotometry/laser fluorimetry has inherent high metrological quality. In principle, laser-induced fluorimetry is an ideal technique for the very accurate determination of uranium by the use of appropriate fluorescence-enhancing reagents and methodology depending upon the concentration of uranium and sample matrices.     

蒸馏分离–电感耦合等离子体质谱法测定铜铅锌矿石中微量锗

建立蒸馏分离-电感耦合等离子体质谱法测定铜铅锌矿石中微量锗的方法。采用硝酸-磷酸混合酸消解铜铅锌矿石样品,在盐酸介质中蒸馏分离微量锗,在氦气碰撞池模式下,以103Rh为在线内标进行质谱法测定。锗的质量浓度在0~50 μg/L 范围内线性良好,相关系数为0.9995,方法检出限为0.019 μg/g。用所建方法对3个铜铅锌矿石成分国家一级标准物质进行测定,测定结果的相对标准偏差为4.58%~5.55%(n=7),样品加标回收率为93.0%~102.0%。该方法操作简便,灵敏度高,适用铜铅锌矿石中微量锗含量的测定。     

Removal of Flotation Collector O-Isopropyl-N-ethylthionocarbamate from Wastewater

Flotation collector O-isopropyl N-ethylthionocarbamate (IPETC) is widely used for separation of sulfide ores. Its removal from water by several oxidation processes was studied. Photocatalytic oxidation with air in the presence of iron salts, utilizing solar irradiation or artificial UV-A light is very efficient. Oxidation leads through the formation of O-isopropyl N-ethylcarbamate and several other reaction intermediates to total decomposition of organic compound in the final stage in 1 day. Similar results were obtained with a Fenton type oxidation with hydrogen peroxide and iron salts. Treatment with sodium hypochlorite yields mainly O-isopropyl N-ethylcarbamate. The formation of this compound in wastewaters can be of concern, since simple alkyl carbamates are cancer suspect agents.     

Quantitative Analysis of Lead Ores Using Sepharose for Sample Preparation by X-Ray Fluorescence Spectrometry

A method for the quantitative analysis of lead ores by wavelength-dispersive x-ray fluorescence spectrometry (WD-XRF) using sepharose was proposed. The sample was decomposed with aqua regia and then the solution was mixed with sepharose. The mixture was heated to boiling and became a quasi-solid gel at ambient temperature. The quasi-solid gel was detected by WD-XRF. This method was adapted in detecting high content ores, because it avoided the risk of using platinum crucible. In addition, cobalt was used as an internal standard to reduce the matrix effects caused by the loss of water in dissolving samples. Analytical characteristics of the methods used were compared, and their reliability tested against several certified geological reference materials. The results showed high precision and accuracy. This method has been applied to the determination of lead in lead concentrates successfully.