Method of determination of gold and silver content in sulphide ores and products of their processing
SUBSTANCE: proposed method comprises annealing of initial charge, selective leaching and analytical determination of noble metal content in produced solution. Charge annealing is performed in microwave frequency field without access of air at 550-600°C Annealed product is leached in steps by adding successive volumes of thiourea sulphide solution. Content of noble metal in obtained solutions is analytically defined to sum obtained values for determination of noble metal content in initial charge.
EFFECT: higher validity of estimation.
2 cl, 1 tbl, 2 ex
The invention relates to the field of analytical chemistry of the noble metals, and can be used to determine the gold, silver and platinum group metals in sulfide ores and products of their processing.
The known method of assay concentration of gold and platinum group metals in the copper-Nickel collector developed for the analysis of sulfide copper-Nickel ores [Danilov PI, IGOR Fedotov, Nazarenko, R.M. Assay-chemical-spectral determination of platinum group metals and gold in sulfide copper-Nickel ores and products of their processing. Laboratory, 1982, 48, 8, p.9-10.]. The known method includes oxidizing roasting weighed samples of the ore at a temperature of 850°C for 7 hours, mixing the calcine with copper oxide (CuO), sodium carbonate, sodium tetraborate, sodium silicate glass and starch, crucible, melting the mixture at 1200°C with obtaining slag and copper-Nickel alloy, followed by dissolving the alloy in hydrochloric acid, the sorption of noble metals from solution on activated carbon and the sorbent PVB-MP-20T, quantitative determination of their content atomic emission method.
The disadvantages of this method include the high cost, due to oxidative roasting of a sample of ore sample and dissolution of the entire mass of copper-Nickel alloy obtained PR the crucible smelting. In this case, if the content of the studied metals slightly, it is impossible to ensure the accuracy of the quantitative analysis due to the heterogeneity of the distribution of metals in ores that are difficult to take into account when taking the sample the sample for analysis.
There is also known a method of analysis of noble metals, in which a portion of the sample analyzed material is subjected to pre-treatment - burning or leaching in acid order decomposition of sulphides and removal of non-ferrous metals, the residue from the digestion of the sample is mixed with lead oxide, sodium carbonate, silicate glass, sodium tetraborate, sodium nitrate or potassium, calcium oxide, nitrate or chloride of silver, and the carbonaceous reducing agent to obtain a mixture, the mixture is melted at a temperature of 1100-1300°C with obtaining slag and lead alloy - free. The products of melting share, free kapelrud to silver or gold-silver goldcrest [Probootborniki and analysis of noble metals, Ed. by Baryshnikov IVAN - M.: metallurgy, 1968, p.131-134, 151-158, 316-320]. The content of noble metals in the Wren determine chemical and physico-chemical methods.
The disadvantage of this method are the high costs associated with conducting operations pre-treatment sample sample analyzed material before probem is th fuse. In addition, when a low content of noble metals, the known method does not allow to ensure the accuracy of quantitative analysis.
Closest to the proposed method is preliminary roasting of sulfide ores and their processing products containing gold and silver assay in the analysis, including the oxidation of ores oxygen in fireclay boats in a muffle furnace at two modes of firing, and the firing starts at 250-300°C and finished at a temperature of 450-500°C for 10-15 min the incomplete removal of sulfur [patent RU No. 2224805, IPC C22B 11/02, 2004].
The main disadvantage is the large values of error due to the microinhomogeneity of samples and technical limitations of sample handling large mass to minimize the impact of heterogeneity.
The objective of the invention is to increase the reliability of determination of gold and silver in sulfide ores and products of their processing.
The problem is solved in that the proposed method of determination of gold and silver in sulfide ores and products of their processing, which includes the firing of the original sample with the subsequent election of its leaching sulfuric acid timeonline solutions and the analytical determination of the content of noble metal in the obtained solution, and abrignani lead once in the microwave field of the microwave range at a temperature of 550-600°C without access of air, followed by repeated leaching of the product of firing successive volumes of sulfuric acid timeonline solutions in the obtained solutions analytically determine the content of gold and/or silver, summarize the obtained values, mathematically calculating the content of gold and/or silver in the original sample.
As sulfate timesaving solutions using 3% solution of thiourea and 3% solution of sulfuric acid, is widely known for leaching gold and silver ores (see, for example, Ladadika V.V., Panchenko A.F., Khmelnytsky OD Thiocarbamide leaching gold and silver ores // Hydrometallurgy of gold. M.: Nauka, 1980. p.26-35). Leaching are preferably within 1 hour at a ratio of t:W=1:2,5.
Using the proposed method allows to solve the problem, first of all, due to the fact that in the present method the original sample of the investigated material can be increased up to 500 grams, i.e. the representation of the traditional sample (25-50 g) increases by 10-20 times. Standard deviation from the microheterogeneity of the investigated materials is reduced in proportion to the square root of the mass of the sample, i.e. the increase in sample mass reduces the detection error that is associated with the microinhomogeneity of the material. Increase the representativeness of the sample significantly increases the reliability of the determination of gold and silver in ores low in their content or in the presence of the AI coarse grains of gold or silver. When using previously known methods of determination of gold and silver in sulfide ores is not possible to conduct research on the hinge of a large mass.
In addition, using the proposed method provides an opportunity to reduce the random component of measurement error due to repeated measurements of the concentration in the solution obtained after leaching. Measuring the concentration of the investigated component can be held in the several Parallels in various ways known to those goals.
The mechanism of extraction of gold and silver by the claimed method is that the roasting of sulfide ores and products of their processing in the microwave field without access of air at a temperature up to 550-600°C provides a flow pertinacious firing and thermolysis process, resulting in sulfur removal with the formation of pyrite pyrrhotite (Fe7S8), which has a porous structure due process expulsion (removal) of sulfur, the latter evaporates and condenses out of the reaction zone. Multiple stepwise sequential leaching sulfuric acid timeonline solutions product of the high temperature firing provides complete recovery of the original sample of noble metals, which become available for leaching only what about after high temperature processing.
The essence of the proposed method is illustrated by examples of specific performance.
Example 1. As source material for analysis using the standard sample, namely GSO 1788-80 containing CAu=33 g/t, CAg=6.2 g/t and has the following mineral composition: quartz - 9,4%, mica, feldspars, clay minerals or 14.8%; carbonates of 4.1%; pyrite - 41,5%, arsenopyrite - 26,6%; chalcopyrite - 0,2%; sphalerite is 0.2%. Taken the sample of the analyzed material weighing 50 g, which was examined on the content of gold and silver by the claimed method. The sample was subjected to high-temperature firing without air in the microwave field of the microwave range, with output power of 0.5 kW for 4 hours, the temperature of the material in the treatment area was approximately 550°C. as microwave ovens used household microwave brand Elenberg MS-1700M. To ensure the regime of firing without access of air was used sealed quartz vessel. The material obtained after microwave treatment, was subjected to consecutive four sequential leaching in sulfuric tiomochevina solution for 1 hour at a ratio of T:W 1:2,5 respectively. The slurry resulting from each leaching, filtering, separating the solution for analysis.
Determination of gold and silver in solutions for the analysis of the implementation of the conduct on the mass spectrometer ELAN 9000. The results of the mass spectrometric measurements were tabulated and counted on the content of silver and gold in the source material.
The content of gold and silver, as defined by the claimed method, amounted to: CAu=33,2 g/t, CAg=6.8 g/so
Example 2. Research used the flotation tailings dump fields in Karabash, representing the products of processing of sulfide ores. Were selected for the study hitch weight of 500, a portion of the samples were annealed without air for 4 hours in the microwave field of the microwave range when the output power 0,55 kW, the temperature of the material in the treatment zone to 600°C. as microwave ovens used household microwave brand Elenberg MS-1700M. To ensure the regime of firing without access of air was used sealed quartz vessel. The sample after microwave annealing was subjected to leaching, which was carried out in 3% sulfuric acid tiomochevina solution for 1 hour at a ratio of T:W 1:2,5, respectively.
The slurry resulting from leaching, filtering, separating the solution for analysis. The resulting solid phase was subjected to repeated leaching. The sample after microwave annealing was subjected to leaching sequentially in 4 stages. Analytical determination of gold and silver in solutions for the analysis of the implementation of the conduct on the mass spectrometer ELAN 9000. The results of the mass spectrometric measurements were tabulated and counted on the content of silver and gold in the source material.
In the result, it was obtained the following result CAu=0.1 g/t, CAg=0,67 g/T. the Results of determination of components in solutions for analysis, allocated to each stage of leaching, are presented in Table 1. The data in table 1 is presented in the form of conversion of gold extracted in the solution to the initial concentration in the ore to the sum of the previous stages of leaching.
The process of burning without air in the microwave field microwave range below 550°C can improve the accuracy of the determination of noble metals, because it does not allow to adequately disclose the access to the private gold (not achieved the completeness of the translation, in pyrrhotite).
The process of burning without air in the microwave field microwave range above 600°C leads to the melting of the material, thereby closing the access leaching agent to gold or silver.
As can be seen from the presented examples, the use of the proposed method can improve the accuracy assessment of the contents of noble metals in sulfide materials, can be the basis for an adequate assessment of the stock and tools of scientific research in the field of "hard gold".
|Microwave roasting of the original sample without access of air, followed four sequential leaching|
|Analyzed the||The content in solutions for analysis at each stage of leaching, g/t|
1. The method of determination of gold and silver in sulfide ores and products of their processing, including the firing of the original sample, the subsequent selective leaching and analytical determination of the content of noble metal in the resulting solution, characterized in that the firing sample lead once in the microwave field of the microwave range at a temperature of 550-600°C without air, and the subsequent leaching of the product of firing stage are sequentially input volume series is cislago timesaving solution, in the obtained solutions analytically determine the content of the noble metal and summarize the values obtained for the calculation of the content of noble metal in the original sample.
2. The method according to claim 1, characterized in that the number of stages of the sequential leaching is at least four.
SUBSTANCE: method includes dissolution of a sample of analysed alloy and separation of cerium from the base of the alloy and macrocomponents. At the same time the base and macrocomponents are separated from cerium by serial deposition and extraction of the alloy base and macrocomponents of the alloy from the solution. Deposition is carried out with sodium diethyldithiocarbamate, extraction - with dithizone in chloroform. After separation of the organic phase, the cerium content is detected in water phase with the spectrometric method.
EFFECT: elimination of harmful influence of high contents of iron and other components of steel and alloy base, improved quantitative analysis, higher accuracy and reproducibility of the analysis method.
1 tbl, 1 ex
SUBSTANCE: proposed device comprises gas collecting body, immersion end, gas feed line terminating nearby said immersion end, and gas discharge line. Note here that gas collecting body has face side located on immersion end, and side walls. Note here that, at least, part of gas collecting body has gastight layer. Besides, invention covers application of said device for measuring gas content in metal melt.
EFFECT: perfected design.
15 cl, 1 dwg
SUBSTANCE: lyosol contains 0.5-1 wt % nano- and microparticles of metals and/or metal oxides, 0.6-0.9 wt % sodium chloride, 4.0-4.5 glucose monohydrate and distilled water.
EFFECT: aggregate-stable lyosols for analysing powdered materials by determining their toxicological properties in vivo.
1 tbl, 1 ex
SUBSTANCE: field is created by a magnetic explosion generator based on one circular winding of an exploding wire, through whose centre the ferromagnetic metal fibre is passed, said fibre being stretched by a force close to a breaking force in the absence of a magnetic field. The plane of the winding is strictly orthogonal to the stretched fibre which is protected from the exploding winding by a piece of glass tube. The ends of the stretched ferromagnetic metal fibre are electrically connected to a measuring device, for example, a resonance amplifier or an oscilloscope, which picks up damped electric oscillations arising when the fibre breaks.
EFFECT: recording EMF which arises upon breakage of a ferromagnetic metal fibre which is stretched by a defined force, taking place under the action a localised superstrong magnetic field.
SUBSTANCE: method employs a magnetic explosion generator to generate a magnetic field based on a coil of explosive wire. A centrally-symmetrically loaded ferromagnetic fibre made from ferromagnetic material, e.g., a thin wire made from rare-earth metals or compounds thereof, which is stretched by the load applied to it, is placed inside the coil.
EFFECT: possibility of detecting breakage of ferromagnetic material in superstrong spatially localised magnetic fields, particularly breakage of a loaded fibre made from ferromagnetic material lying in such a field.
SUBSTANCE: method of determining noble metals involves drying a sample with grain size 1 mm to constant weight at temperature 105-110°C and using the dried sample for second and subsequent one-off determination of noble metals. An undried sample is used during the first one-off determination, wherein sample material is mixed with a charge mixture, the obtained mixture is molten and the amount of noble metals in the melt is determined. The sample is dried during the first determination and the weight ratio of moisture in the sample is determined. Content of noble metals in the sample is determined using the formula: where Cme is content of noble metals in the sample, g/t, Mme is mass of the noble metal detected in the melt, mg, m1 is the mass of the sample material used in the first determination, g, W is the weight ratio of moisture in the sample.
EFFECT: invention increases rapidness of determining noble metals and labour efficiency.
SUBSTANCE: invention refers to investigation of structure of high-strength steels. Method involves interaction of tube steel specimen with water solution of sulphosalts, further flushing and drying of specimen and detection of areas of bainite of rack morphology by means of optic microscope. At that, after application to specimen surface of water solution of sulphosalts, there removed is formed film, and bainitic areas are detected by means of polarised light of optic microscope; after that, obtained pictures of specimen are fixed and parameters of the detected bainitic areas of rack morphology are determined.
EFFECT: method allows detecting structure of high-strength tube steel as a result of evaluation of which the conclusion can be made on metallurgical quality of tube steel.
SUBSTANCE: method involves determination of the sum of the maximum allowable additive (MAA) of a metal/metalloid and background content thereof Cf, where content of heavy metal/metalloid and content of a reference element R in form of Zr and Ti is determined both in the epidedon A and the parent rock C, with subsequent determination of the local background content of heavy metal/metalloid Cf using the expression: Cf=MeC·RA:RC, where: MeC is content of metal/metalloid, RA is content of the reference element in the epidedon A, RC is content of reference element in the parent rock C, after which the local value of the approximate permissible concentration (APC) of heavy metal/metalloid is calculated using the expression: APC*=MAA+Cf.
EFFECT: high accuracy of analysis owing to separate calculation of the background content of the determined elements.
1 ex, 4 tbl, 1 dwg
SUBSTANCE: method for determining precious metals in ores and their derivatives involves preparation of mixture from sample of the analysed material with fluxes, lead oxide, silver nitrate or chloride and carbon-bearing reducing agent. Then, mixture is molten at temperature of 1100-1300°C so that slag and lead alloy is obtained in the form of lead bullion. After that, cupellation of lead bullion is performed till silver globule is obtained, and content of precious metals in silver globule is determined with chemical and physical-chemical methods. At that, prior to cupellation to lead bullion there added is tin metal in quantity of 0.4÷1.0% of lead bullion weight, and cupellation is performed at temperature of 880÷930°C.
EFFECT: improving the accuracy of determining the content of precious metals owing to preventing their oxidation during cupellation process.
3 tbl, 1 ex
SUBSTANCE: procedure for determination of gold in ore and concentrate consists in oxidising burning and in successive cinder melting with fluxes, oxide of lead and reducer for production of gold-lead alloy. Further, there is performed cupellation, and gold bead extraction and weighting. Also, oxidising burning is performed with addition of oxide or peroxide of calcium or barium at amount of 110-130 % of stoichiometric required for binding sulphur into sulphate of calcium or barium at temperature 400-700°C during 30-60 minutes. Produced cinder is melted for production of gold-lead alloy.
EFFECT: more accurate determination of gold.
SUBSTANCE: proposed method comprises heating the reaction mix in assembly consisting of two units composed of heaters and bubblers. Every of said unit is heated in turns to boil the solution and to direct live steam to bubbler of another unit. Proposed device represents the assembly consisting of two units composed of heaters and bubblers and integrated in a system by steam-gas pipelines. Note here that one pipeline is connected with bubblers while another one is connected with atmosphere. Shutoff valves and auxiliaries are fitted between units and pipelines. Proposed device may comprise shutoff valves automatic changer-over devices and their control unit.
EFFECT: maximum application of live steam heat, optimised thermal and hydrodynamic conditions, lower costs.
4 cl, 2 dwg, 3 ex
SUBSTANCE: method to produce metals from storages of stale wastes of polymetal ore dressing consists in trench opening of the storage, detection of layers containing easily dissolved forms of non-ferrous metals and layers containing noble metals, bulk extraction of stale wastes from the storage, fraction separation of stale wastes into a finer sulfide fraction dressed with noble metals and coarser fraction dressed with non-ferrous metals, and their separate leaching.
EFFECT: complete processing of storages of stale dressing wastes, release of areas occupied by them, complex usage of mineral materials and high environmental and economic effect.
3 cl, 1 dwg
SUBSTANCE: invention refers to metallurgy of precious metals, and namely to processing of slurries and concentrates containing elementary silicon, carbon and platinum. Similar slurries are formed namely at dilution of platinum-containing cast-iron in sulphuric acid. Slurries are mixed with sodium carbonate at consumption of 120-150% of the weight of silicon and carbon in initial material and sintered at the temperature of 500-650°C during 1-2 hours. Sintered material is leached in water so that insoluble residue containing precious metals and being a concentrate of precious metals is obtained.
EFFECT: simpler technology and higher quality of concentrate.
1 tbl, 1 ex
SUBSTANCE: method of lead extraction from lead wastes containing one or more of Pb, PbO, PbO2 and PbSO4 includes treatment with aqueous solution of citric acid with production of lead citrate. Then lead citrate is extracted from the aqeuous solution, and the extracted lead citrate is converted into Pb and/or PbO. The method for processing of lead accumulator batteries, containing or more of Pb, PbO, PbO2 and PbSO4 includes mixing of a paste of lead plates of accumulator batteries with the aqueous solution of citric acid for production of lead citrate. Then lead citrate is extracted from the aqueous solution, and lead citrate is converted into lead and/or lead oxide. Further Pb and/or PbO are included into a plate of an accumulator battery.
EFFECT: simplified process and its improved cost-effectiveness.
17 cl, 7 dwg, 8 tbl, 1 ex
SUBSTANCE: method involves crushing chemical cells, leaching, magnetic separation and electrolysis. The cells are crushed and leached with water in an atmosphere of carbon dioxide gas without access to oxygen. Light fractions are then removed from the scrap by floatation. Filtration is then carried out. The filtrate is treated with sorbents. After filtration, the scrap is washed with water, dried and fragments of ferrous and nonferrous metals are removed by electromagnetic separation, and then leached with sulphuric acid solution. Sulphuric acid pulp is filtered through a filter with an inert material, a filter with a coal medium and a filter with a cation-exchange medium. Ions of row d and row p metals sorbed by a cation-exchange resin are selectively desorbed with sulphuric acid solutions. Solutions containing ions of row d metals are subjected to electrolysis, and solutions containing ions of row p metals are neutralised to pH 3-4 and treated with clay mineral sorbents. The precipitate after sulphuric acid leaching is leached with nitric acid solution; the undissolved manganese dioxide precipitate is removed and the filtrate is neutralised and acidified to pH 3. The precipitate is filtered off. The filtrate containing mercury ions is subjected to cathode reduction and the precipitate containing lead and silver chlorides is dissolved in nitric acid and subjected to cathode reduction in an electrolysis cell with separate deposition of metals on electrodes.
EFFECT: environmental safety of recycling any type of spent chemical cells.
SUBSTANCE: proposed method comprises multistep leaching of red slag by the mix of sodium carbonate and bicarbonate on forcing annealing furnace flue gases containing carbon dioxide there through to obtained solution. Then, three-step holding of said solution at increased temperatures is performed along with selective separation of precipitates after every said step. At first step, said solution is heated to temperature not exceeding 80°C for, at least, 1 hour. Thereafter, it is settled for, at least, two hours at natural cooling. At second step, said solution is boiled and mixed for, at least, two hours. At third step, said solution is evaporated to 50% of initial volume to add 46%-solution of sodium hydroxide to concentration of Na2Ocaustic of 1.5-2.0 kg/m3. Now, it is boiled for, at least, 2 hours and precipitate containing scandium oxide is settled for 10-16 hours at natural cooling.
EFFECT: simplified process, higher yield of scandium oxide.
SUBSTANCE: method involves processing of base material during heating in water vapour atmosphere and further leaching of precious metals from processing product in solutions of reagents. Besides, processing of base material is performed in water vapour atmosphere, which is mixed with oxygen at the temperature of 300-500°C at oxygen content in gas mixture within 10-20%. Waste gases released during the processing are brought into contact with the solution that is combined with a leaching solution.
EFFECT: decrease of temperature and reduction of costs at preparation of refractory ores and concentrates to leaching.
1 tbl, 1 ex
SUBSTANCE: method involves solid-phase roasting of wastes mixed with soda to fix arsenic to a water-soluble form of sodium arsenate. Then, water leaching and deposition from arsenic solution is performed. In order to obtained the product from water leaching with low residual arsenic content of 0.7%, solid-phase roasting is performed at 850°C so that a roasted product containing 2.9% of arsenic is obtained. Water leaching of the roasted product is performed with extraction degree of 84%. Deposition from arsenic solution is performed in the form of arsenic sulphide with sodium sulphide at pH=3 with deposition degree of 99.6%, and filtrate with arsenic content of 0.02 g/l for removal of residual amount of arsenic by neutralisation and deposition with iron compounds meets the requirements of sanitary norms.
EFFECT: obtaining low-toxicity commodity product of arsenic sulphide and product of water leaching with low residual content of arsenic.
1 dwg, 1 tbl, 5 ex
SUBSTANCE: method involves crushing of raw material, its heaping in the form of a pile, pre-treatment of raw material in the pile, treatment of the pile with a leaching solution, dilution of metals and obtaining of productive solution with removal of metals from it. At that, pre-treatment is performed by supplying separate solutions or mixture of solutions containing surface active substance and hypochlorite to the pile. Treatment with the leaching solution is performed by means of the solution obtained by mixing in the pile volume at supply to it of separate solutions or mixture of solutions containing hypochlorite, surface-active substance and/or mineral acid. In the leaching solution there used are mixtures of mineral acids or in-series introduced mineral acids. Supply points of the above solutions to the pile can be different.
EFFECT: increasing the efficiency of the process cycle at reduction of costs and emission of hazardous gases.
5 cl, 9 tbl, 6 ex
SUBSTANCE: method of bath-well leaching of metals from ores includes treatment of mineral mass by solution of leaching in baths and metal winning from product solution. Baths are formed along leached mass, in the baths bottom a system of injection and extraction wells is built located above the level of bath with depth not less than the lower point of leached layer of mineral mass, and baths are filled with agglomerated mineral mass or pulp prepared in advance from extracted material, mineral mass in baths is treated by solution of leaching, and metal is extracted from product solution. Reusable solution obtained after metal extraction is strengthened or replaced with solution of another composition and is supplied to the system of injection wells for leaching of lower layers of material, then working solution is pumped off with leached metal through the system of extraction wells and metal is extracted from it; for leaching of lower layers of material solutions of environmentally safe chemicals, such as chlorides or thiosulfates, are used.
EFFECT: invention allows improving metal extraction efficiency.
SUBSTANCE: method of noble metal extraction from solid stock comprises dissolving of noble metal and base metals in acid. Noble metal is extracted with the help of substituted quaternary ammonium salts (SQAS). Noble metal can be oxidised and reduced. Said substituted quaternary ammonium salts represent the following form H0-3R4-1NX, where H= hydrogen, R= organic group, N= nitrogen and X= halogen. This method uses, for example, tetramethyl ammonium chloride. Au-SQAS is separated by flushing with solvent. Rh-SQAS is dissolved in acid and oxidised to precipitate the salts, and separated. SQAS is added to filtrate and cooled to precipitate Rh-AQAS to be separated. Rh-SQAS is cleaned before formation of final product. Other metals are separated by boiling the initial acid solution with precipitation of metal salts, cooling and separation. The pulp is separated by dissolution and separation.
EFFECT: simplified extraction.
20 cl, 4 dwg, 4 tbl, 2 ex