Method of determination of content of palladium and platinum in ores
FIELD: methods of determination of content of palladium and platinum in ores containing considerable amount of iron, copper, zinc and other metals.
SUBSTANCE: proposed method includes decomposition of ore by hydrofluoric and nitric acids followed by further decomposition by aqua regia, boiling-off to moist salts, dissolving of them in hydrochloric acid and extraction. Determination of content of palladium is carried out in organic phase thus obtained and that of platinum is carried out in hydrochloric acid phase. Extractants used for such determination are s-alkylisothiouronium halides and alcohols of C5-C8 fractions, as well as kerosene, benzene, toluene and xylols used as diluents. Used as s-alkylisothiouronium halides are chlorides, bromides and iodides from C7 to C14 and their fractions.
EFFECT: extended range of reagents and inert diluents.
2 cl, 2 ex
The invention relates to the determination of palladium and platinum ores containing large amounts of iron, copper, zinc and other metals by atomic absorption spectrometry with electrothermal atomization.
There is a method of determining the content of palladium and platinum ores, including their translation into solution, for example, by decomposition in Aqua Regia, evaporation and dissolution in hydrochloric acid and further determination by atomic absorption spectrometry with electrothermal atomization (Ginzburg SR and other Guidance on chemical analysis of platinum metals and gold. M., Nauka, 1965, p.205, 272-273).
The closest analogue to the present invention is a method of determination of palladium and platinum ores, including the decomposition of the ore hydrofluoric and nitric acids, further decomposition of the Royal vodka), evaporation to wet salts, their dissolution in hydrochloric acid, and subsequent extraction, stirring, settling the mixture for half an hour and the determination of the content of palladium in the organic phase, and the content of platinum in hydrochloric acid phase. As extractant used undecalactone chloride in a mixture of toluene and isoamyl alcohol in the ratio of 80% and 20%, and the concentration of the extractant 0,5-2,5% (RF patent No. 2226224, With 22 In 4/03, 2004).
Lack of oksanapopova is the limited range of extractants and inert diluents (mixture of toluene and ISO-amyl alcohol).
An object of the invention is the expansion of the range of extractants and inert diluents.
The technical result is achieved in that in the method of determining the content of palladium and platinum ores, including the decomposition of the ore hydrofluoric and nitric acids, further decomposition of the Royal vodka), evaporation to wet salts, their dissolution in hydrochloric acid, and subsequent extraction with an extractant in an inert diluent, stirring, settling the mixture for half an hour and the determination of the content of palladium in the organic phase, and platinum in hydrochloric acid phase, as extractants used s-alkalization halides from C7to C14(chlorides, bromides, iodides), and as an inert diluent - alcohols fraction5-C8and kerosene, benzene, toluene, xylenes.
The method is as follows. The sample at 1-2 grams pour a mixture of 10 ml HF and 1 ml of nitric acid, the solution evaporated at 160-200°to wet salts, the remainder of the double-pour 15 ml of Aqua Regia and both times evaporated to moist salts at the same temperature. Then the residue is dissolved in 4 M hydrochloric acid, transferred to a flask and bring to the mark with hydrochloric acid. Then spend the extraction of palladium from hydrochloric acid solution. The volume of solenoidoperated palladium is mixed with an equal volume of extractant solution in an inert diluent. Stirred or shaken, after which the mixture is allowed to stand for 0.5 to 2 hours, after which the organic phase define palladium, and from hydrochloric phase - platinum by atomic absorption spectrometry with electrothermal atomization "quantum-Z.". As extractants used s-alkalization halides from C7to C14or their fractions. As inert diluents used alcohols fraction C5-C8(amyl, hexyl, p), as well as kerosene, benzene, toluene, xylenes or mixtures thereof.
When using s-alkalization halides from hydrocarbon radical, a smaller 7 decreases their solubility in the inert diluent and they are poorly extracted precious metals from hydrochloric acid solution. S-alkalization halides from hydrocarbon radical, a large 14, reduced solubility in hydrochloric acid solution, and this also leads to deterioration of the extraction of noble metals from solutions.
The invention is illustrated by examples.
Example 1. Carry out analysis of samples No. 4330-2 (depth 284,8-287,3 m, composition: carbon slate with striated silicification, the content of graphite 7-20%). A sample of 1.2 grams treated with acid, then with 5 ml of hydrochloric acid solution is extracted with palladium 2% solution of s-captilization chloride in 5 ml Attila is on alcohol. The concentration of palladium on the peak of 50.2 ág/l, the integral of 50.2 ág/L. Data without extraction: peak 27,1 µg/l, the integral 28.5 ug/l
Example 2. Carry out analysis of samples No. 33035 (depth 270,6-271,8 m, composition: carbonaceous shale with pyrite content to 20%, the content of graphite 7-20%). 1.8 g of the sample is treated with acid, then with 5 ml of hydrochloric acid solution is extracted with platinum a 2.5% solution of s-tetradecylammonium chloride. From hydrochloric acid solution determine platinum. The value of concentration: peak of 11.6 µg/l, the integral of 12.2 ág/L. Data analysis without extraction: at the peak of 29.4 ág/l is integral to 26.2 ág/L.
1. The method of determining the content of platinum and palladium in ores, including the decomposition of the ore hydrofluoric and nitric acids, further decomposition of the Royal vodka), evaporation to wet salts, their dissolution in hydrochloric acid, and subsequent extraction with an extractant in an inert diluent, stirring, settling the mixture for half an hour and the determination of the content of palladium in the organic phase, and platinum in hydrochloric acid phase, characterized in that as extractants for the extraction using s-alkalization halides from hydrocarbon radical from C7to C14or their fractions, as well as inert solvents - alcohols fraction C5-C8and kerosene, benzene, toluene, xylenes./p>
2. The method according to claim 1, characterized in that as s-alkalization halides using chlorides, bromides, iodides.
FIELD: mechanical engineering; manufacture of Northern design articles and analysis of causes of low impact viscosity of welded joints and prevention of them.
SUBSTANCE: proposed method consists in finding-out dependence of grain size of microstructure and presence of ferrite net, as wells as marks on bearing faces of tested specimens for products of the same type made from steel of definite quality during analysis of causes of low impact viscosity recommended standards are established for these parameters and dependences thus found are compared with the data of specimens of low (below standard norm) impact viscosity and these data are estimated for compliance with the recommended standards. Dependences thus found are used repeatedly and constantly.
EFFECT: operative determination of causes of low impact viscosity; possibility of excluding these causes.
4 dwg, 1 tbl
FIELD: nonferrous metallurgy; methods of detection of the noble metals in the mineral raw materials.
SUBSTANCE: the invention is pertaining to nonferrous metallurgy, in particular, to the methods of detection of the noble metals in the mineral raw materials. The technical result of the invention is an increased trustworthiness to the results of the testing crucible melt analysis. The method is conducted in the following way. From the material of the laboratory test sample take out the analytical part of the filler, mix it with the calculated amount of the charge and the mixture is smelt according to the standard method. During the smelt visually control the height of the boiling layer of the melt slag and lead. On completion of the smelt measure the mass of the slag and lead and calculate an admissible height of the boiling layer of the melt according to the following formula:0,9·Hm≥Hc≥[1,9/tg2α/2·(Mш/ρш+Mc/ρc)]1/3, whereHcr - depth of the crucible in meters(m);Hsl - the height of the boiling gas-slag layer, m; α - an angle at the apex of the cone of the inner surface of the crucible, in degrees;Msl, Mla - masses of the slag and mass of the lead alloy accordingly, kg;ρsl, ρla - density of the slag and density of the lead accordingly, kg/m3. If the visual estimation of the height of the boiling layer of the melt exceeds the limits of admissible values, them one may draw a conclusion about the low quality of the testing smelt, make corrections in the composition of the charge and repeat the test analysis.
EFFECT: the invention ensures an increased trustworthiness to the results of the testing crucible melt analysis.
FIELD: investigating and analyzing materials.
SUBSTANCE: method comprises sampling initial material, producing and analyzing group samples before assessing representative mass of analytical samples, estimating representative mass of analytical samples, and calculating the value of the coefficient that characterizes the type of gold-bearing material from the formula proposed.
EFFECT: enhanced reliability.
FIELD: measuring equipment.
SUBSTANCE: method includes subjecting samples of steel to preliminary plastic deformation and on basis of wear test results of pre-deformed samples, graph of change of hardness limit of σ-1 samples is built dependent on their level of pre-deformation. Weighed samples are made with same deformation level and value of magnetic tear force Pmag is determined for each weighed sample. Graph of change of magnetic tear force Pmag is built for samples on basis of their pre-deformation level, graph with adjusting curve in coordinates Pmag - σ-1, setting a connection between Pmag and σ-1 dependent on level of pre-deformation. Hardness limit of σ-1 samples is determined by adjusting curve in coordinates Pmag - σ-1.
EFFECT: lower laboriousness, lower costs, higher efficiency.
FIELD: testing of strength properties of metals.
SUBSTANCE: method can be used for estimation of deformation-strength properties due to applying load as well as for determining damages by means of X-ray diffraction analysis. Values of structural-sensitive parameter of crystal lattice of tested material are determined by X-ray diffraction analysis in initial and post-deformation states. Deformation-strength characteristics of metal are determined by calculation from changes in structural-sensitive parameter. Serviceability is judged by comparing really achieved characteristics with admissible ones. Width of X-ray line β is used as structural-sensitive parameters. Strength of deformation P, deformation Δl provided by the deformation and corresponding values of structural-sensitive parameter β are registered during testing. Dependence of true stresses S and structural-sensitive parameter β on degree of relative residual deformation δ are calculated on the basis of P and Δl. Destruction diagram (S-δ½) and linearized diagram (β½-δ½) are built to show inflection points. Deformation-strength characteristics SD and δD corresponding to inflection point at destruction diagram (destruction point D) is taken as criterion of admissible surface strength which provides maximal serviceability of metal. Factor of merit η and factor of destruction Δ can be also taken as criteria of serviceability of metal.
EFFECT: improved precision of estimation.
3 cl, 3 dwg
FIELD: the invention refers to the field of quality control of materials and manufacture goods for assessment of resistibility of rails to destruction due to contact weariness.
SUBSTANCE: contact weariness is induced by high-frequency dynamic components of interaction of wheels and rails, which become apparent at moving at high speed. The mode of testing railway rails on contact weariness is in that tested samples of rail steel are rolled by pinch rolls in longitudinal direction until appearance on the surface of the sample of dents and also deep indents. As samples test rails are used. The diameter of a pinch roll is chosen under condition of equality of reduction ratio of linear size of the site of contact of the pinch roll with the rail along the axis of the last in comparison with corresponding size responsible to conditions of exploitation and speed reduction ratio of rolling motion of the pinch roll along exploited rail.
EFFECT: the invention allows to increase reliability of test rails' control at danger of resulting defects from contact weariness caused by contribution of high frequency components in dynamic interaction of wheels and rails which becomes apparent at the moving of trains at high speed.
FIELD: material for production of assay stone, in particular standard determination.
SUBSTANCE: assay stone is made from oxide ceramic comprising BeO-TiO2. Material affords the ability to obtain assay stone of regular geometric form with surface, electrical and mechanical properties meeting the requirement for material used in assaying control. Claimed material in useful in standard determination followed by electrochemical recovery of precision metals from solution after assaying control.
EFFECT: material of homogeneous structure; decreased time of precision metal recovery after assaying control.
FIELD: hydrometallurgy; ore concentrates processing.
SUBSTANCE: the invention is pertaining to the field of hydrometallurgy, in particular, to processing of the loparite concentrate. The method includes a decomposing of the loparite concentrate at the temperatures of 103-105°C and the concentration of hydrofluoric acid of 38-42 mass % with production of the pulp containing fluorides of titanium, rare earth elements (REE), niobium, tantalum and sodium. The pulp is filtered at the temperature of 90-95°C with extraction into the fluorotitanium solution of fluorides of niobium and tantalum and no less than 58 % of sodium in terms ofNa2O and separation of the sediment containing fluorides of rare earth elements (REE) and a residual sodium. The produced solution is cooled down to 18-24°C with separation of the second sediment of sodium fluorotitanate. After that they extract niobium and a tantalum from the solution by octanol-1 extraction at a ratio of the organic and water phases as 1.1 : 1. The sediment of REE fluorides is washed from fluorotitanate by sodium water in a single phase at the temperature of 90-95°C and at the solid :liquid ratio = 1:2-2.5. The cleansing solution is separated and evaporated with extraction of the additional sediment of sodium fluorotitanate. After extraction of niobium and tantalum the fluorotitanium solution is evaporated and filtered with separation of the first sediment of sodium fluorotitanate from the concentrated solution of fluorotitanium acid, which is directed to extraction of titanium. The gained first, second and additional sediments of sodium fluorotitanate are combined and subjected to conversion with production of sodium fluorosilicate and the conversional fluorotitanium acid added to fluorotitanium solution before its evaporation. The technical result of the invention is a decrease in 2.0-2.5 times of the volume of the cleansing solutions at provision of a high degree of extraction of compounds of titanium and other target products. The produced sodium fluorotitanate contains the decreased amount of the impurity ingredients of calcium and strontium.
EFFECT: the invention ensures a decrease in two-two and a half times of the volume of the used cleansing solutions at provision of a high degree of extraction of compounds of titanium and other target products and a decreased amount of impurities of calcium and strontium in the sodium fluorotitanate.
7 cl, 1 dwg, 1 tbl, 3 ex
FIELD: metallurgy of rare and dispersed metals, chemical technology.
SUBSTANCE: invention relates to a method for extraction separation of tantalum and niobium. Method involves extraction separation of tantalum from niobium with organic solvent. As an organic solvent method involves using a mixture of methyl isobutyl ketone taken in the amount 40-80 vol.% with aliphatic (C7-C9)-alcohol taken in the amount 20-60 vol.%. At the extraction process tantalum transfers into organic phase and niobium - into aqueous phase. Then organic and aqueous phases are separated. Invention provides enhancing the extraction degree of tantalum into organic phase and to enhance the separation degree of tantalum and niobium in extraction.
EFFECT: improved separating method.
5 tbl, 5 ex
FIELD: non-ferrous metallurgy, processing of manganese-containing materials, namely hydraulic metallurgical processing of mixed manganese-containing materials or similar manganese ores for obtaining manganese concentrate possibly used in metallurgical, electrical engineering, chemical industry branches.
SUBSTANCE: method comprises steps of converting manganese and related impurities to solution by two-stage treatment of initial manganese containing material with mineral acid. At first stage hydrochloric or sulfuric acid is used for treatment. At second stage hydrochloric acid is used for treating insoluble residue at relation of acid concentration for first stage to its concentration for second stage 1 : (1.0 - 6.6) and simultaneously providing absorption of separated chlorine by alkali solution. After second treatment stage pH of pulp is reduced till 3.5 - 4.5 due to adding carbonate manganese ore. Manganese salt solution is separated from deposit of impurities by filtering. Manganese concentrate is extracted out of filtrate by mixing solution of its salt with solution after chlorine absorption for setting pH 9.5 - 10.5. Value pH is corrected, if necessary by means of milk of lime or sodium hydroxide solution containing excess of sodium chloride. Then concentrate is filtered, washed and dried. Produced manganese concentrate contains at least 60 % of manganese and phosphorus no more than 0.08%. Extraction degree of manganese to concentrate is no less than 92.8%. Invention provides possibility of producing for one technological cycle manganese concentrate including at least 60 % of manganese and no more than 3% of impurities from manganese-containing materials containing manganese less than 30 % and phosphorus 0.1 - 1.0.
EFFECT: enhanced efficiency of method.
4 cl, 2 tbl, 5 ex