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Method of assay determination of content of gold in ores and in products of their processing

IPC classes for russian patent Method of assay determination of content of gold in ores and in products of their processing (RU 2288288):
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Multicomponent waste material is preliminarily impregnated with solution of salt of metal-collector in amount ensuring weight content of metal-collector in melt exceeding content of metallic components therein. Material is then calcined and melted in reductive atmosphere after addition of slag-forming flux based on metal fluorides. Melt is stirred and kept in liquid state over a period of time long enough to allow separation of slag and metallic phases. Resulting slag and metal are tapped and mechanically separated when solidified.
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Claimed method includes sampling the probe of starting material, grinding, mixing with massicot, smelting to form bullion, parting of gold-silver globule, weighting of gold sinterskin. Probe is sampled from starting natural solid organic material. Before smelting mixture is packaged in lead foil, established in full-hot scorifying dish, and padded with borax and table salt.
Gold content determination in gold-containing raw material / 2245931
Claimed method includes sampling the probe of starting material, grinding, mixing with massicot, smelting to form bullion, parting of gold-silver globule, weighting of gold sinterskin. Probe is sampled from starting natural solid organic material. Before smelting mixture is packaged in lead foil, established in full-hot scorifying dish, and padded with borax and table salt.

FIELD: analytical chemistry of noble metals; assay analysis; determination of content of gold in ores of different mineralogical composition and in products of their processing (tailings, concentrates).

SUBSTANCE: proposed method includes melting of starting material with lead oxide, soda, borax and flour for obtaining lead alloy (crude lead), its cupellation till gold-silver regulus, dissolving of silver in diluted nitric acid and determination of amount of gold by weighing or by any other instrumental method. Melting process is carried out in metal crucibles at temperature of 600-800°C for 10-30 minutes; charge per 10 g of sample contains the following components: 20-50 g of sodium or potassium hydroxide; 2-20 g of borax; 1-10 g of soda; 15-30 g of litharge and 1-3 g of flour. Method is recommended for assay of samples having mass of 10-100 g.

EFFECT: facilitated procedure and low cost of assay.

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The invention relates to the field of analytical chemistry of the noble metals (BM), namely the assay analysis, and can be used for determination of gold in ores of different mineralogical types and products of their processing.

The essence of the assay analysis consists in fusing the sample analyzed material with flux and collector. The main part of the breed (macronutrients) associated with flux and passes into the slag. Precious metals are quantitatively transferred into the collector. Hot water poured into the mold. After cooling the collector is separated from the slag and sent for further chemical processing with subsequent determination of BM.

Melting is carried out in a powerful furnaces special design (crucible furnaces) at a temperature of 1000-1200°C for 1-2 hours.

As fluxes usually use baking soda, borax, quartz.

As collectors use a variety of metals and sulfides of metals. The composition of the charge collector is introduced in the form of a metal oxide or sulfide, or metal and sulfur. For recovery of metal oxide to metal collector a necessary part of the charge is the reducing agent. Current top in most of these reducing agents is carbon (charcoal, flour, bran, starch, sugar, paper).

Scheme of chemical processing collector determines the tsya collector type.

View of the final instrumental analysis scheme determines the chemical processing of the header and content of BM in the final concentrate.

A known method of assay concentration of gold in tin Wren followed by atomic absorption determination (Navsarka, Nsamba, Towpackage and other Concentration of gold and silver in tin Wren to further their determination by atomic absorption spectrometry. Proceedings of TsNIGRI, 1981, No. 157, p.78-82). Crucible melting is carried out at a temperature of 1200-1250°within hours. The composition of the charge is tin dioxide (40 g), soda (50 g), silica (15 g), fused borax (10 g), flour (40 g). The weight ratio of the weighed sample and mixture 1:7,5. The resulting tin alloy is dissolved under heating in a mixture of hydrochloric and nitric acid (5:1), the solution evaporated several times with the addition of the same lump to remove SnCl4translate to chlorides by three-time processing of hydrochloric acid and hydrogen peroxide with an intermediate evaporation to moist salts. Further salt was dissolved in 1M HCl and sent for atomic absorption analysis. The disadvantages of this method is the high temperature fusion and complexity acid treatment, since the dissolution goes the whole tin alloy, obtained by crucible smelting.

A known method of assay concentration angry is that in copper alloy with subsequent atomic absorption determination (Diamantatos A. Fire-assay collection of gold and silver by copper. Talanta, 1987, 34, No. 8, R-738). The method includes annealing at 750°sample sample mass of 1-3 g, mixing it with flux (40 g of CuO, 25 g of borax, 60 g sodium, 10 g silica, 2 g of graphite) and melting at a temperature of 1200°C for 1.5 hours. The obtained copper alloy weighing 30 g dissolved in 300 cm3perchloric acid under heating for 2 hours, after addition of acetic acid is boiled for a further 1 hour. After cooling, the solution stand in the dark for 1.5 hours, filtered, the precipitate to the filter is dissolved in Aqua Regia boiling. The resulting solution is evaporated to dryness with sodium chloride, the salt is dissolved by boiling in hydrochloric acid with the addition of hydrogen peroxide and translated into the volume of 3M hydrochloric acid. The solution is directed to the atomic-absorption determination of gold. Disadvantages of the method are the high temperature fusing, the need for pre-roasting, small sample tests (nepredstavitelne sample) and the complexity of the acid treatment, since the dissolution goes the whole copper alloy, obtained by crucible smelting.

A known method of assay concentration of gold and platinum group metals in the copper-Nickel reservoir with subsequent atomic emission determination (Paydayloa, Ihavenolife, Ramnagaram. Assay-chemical-spectral about what the definition of platinum group metals and gold in sulfide copper-Nickel ores and products of their processing. Laboratory, 1982, 48, No. 8, p.9-10). The method developed for the analysis of sulfide copper-Nickel ores. A necessary preliminary step in the scheme of assay determination of such ores is the burning of the sample (weight of 30-100 g) at a temperature of 850°C for 7 hours. Crucible melting burned samples is carried out at a temperature of 1200°C for 1-1 .5 hours. The charge is calculated on the formation of Cu-Ni collector with a mass ratio of Cu:Ni≥2:1 (add CuO with regard to the content of copper and Nickel in the ore). Other components of the mixture per 100 g ore: anhydrous soda - 95 g of fused borax - 250 g glass - 25 g, starch - 20 was Obtained Cu-Ni alloy (translated in chips) is dissolved in 50 cm3hydrochloric acid added dropwise hydrogen peroxide, the solution is filtered. The filter residue silaut, fusion with sodium peroxide, water leached 6M HCl. All solutions combine, evaporated and transferred in 1M HCl. Platinum metals and gold adsorb from solution on activated carbon and the sorbent PVB-MP-20T and determine the content of atomic-emission method. Disadvantages of the method are the high temperature fusing, the need for pre-firing and the complexity of the acid treatment, since dissolution is sent to all Cu-Ni alloy, obtained by crucible smelting.

Known assay method concentrated the I gold and platinum group metals in Nickel matte and subsequent atomic emission inductively coupled plasma determination (instruction NSAM No. 366-s Atomic emission inductively coupled plasma determination of platinum, palladium, rhodium, iridium, ruthenium and gold in sulfide copper-Nickel ores and products of their processing with pre-concentrated in Nickel matte". M, 1995). The method developed for the analysis of sulfide copper-Nickel ores. The method includes crucible melting weighed samples (0.5 to 100 g) with the charge to produce Nickel matte, acid dissolution collector, analysis undissolved residue containing in itself all precious metals. Crucible melting is performed at a temperature of 1000-1100°C for 1 hour. In charge is injected Nickel oxide and sulfur for the formation of the collector (the calculation is performed on education matte weight of about 20 g on empirical formulas with regard to the content of sulfur in the ore and Nickel) and fluxes: soda ash 50-120 g borax 25-60 g, glass 0-60 g (compositions of fluxes depending on the mass of the weighed sample is shown in table). In order to reduce losses BM method involves melting slag flux and Nickel sulfide. United matte is crushed, selected sample (mass of a sample is selected in accordance with table and is 10-15 g), treated with concentrated hydrochloric acid (200-250 cm3) when heated, separated by filtering any insoluble sulfides BM that translate into solution by boiling in Aqua Regia and then to chlorides by mnogokrat the nd evaporation with the addition of hydrochloric acid. The resulting solution BM (on the basis of hydrochloric acid 1:5) is directed to atomic emission determination (spectrometer with plasma excitation source company FCD, model 3580. Disadvantages of the method are the high melting temperature, the need for processing of almost all of the mass obtained Stein, the complexity acid treatment.

A common disadvantage of the above methods is the need for time-consuming acid treatment all received in the process of melting the mass of the collector, which, as a rule, comparable to the mass of the sample. This drawback is devoid method of assay concentration of gold in lead collector (free), which includes (in addition to the melting crucible) operation Kopaliani free, i.e. its oxidation melting on Kabalah: the lead is oxidized to oxides, which are selectively absorbed in the molten state in the material drops - magnesite, bone meal, etc. So cupellation allows you to completely remove the lead from free to get gold-silver bead small mass.

To obtain a lead collector in the composition of the charge additionally include litharge (low-temperature modification of oxide of lead), which when heated with a reducing agent in the process of melting crucible readily gives up oxygen with formation of metallic light of the CA (melting point 327° C). Litharge is both highly basic flux and forms a fusible silicates, easily dissolving the metal oxides. In the presence of sulfur in the sample litharge is also desulfurization.

The known method of assay determination of gold and silver ion-exchange resins (Ubicare, Submicron, Waggonbau, Avenarius. "Method for determination of gold and silver ion-exchange resins". Copyright certificate №1547319, MKI 22 In 3/00, publ. 01.11.1989, priority from 11.12.1987 year). The method includes drying the saturated resin at a temperature of 60-80°its melting when 890-940°in the presence of borax, litharge, nitrate to obtain zolotopererabatyvayuschego lead alloy. While nitrate is introduced in a quantity of 0.5-0.6 by weight of the resin and litharge, taken on 20 units of mass greater than the mass of nitrate (an example is shown on a portion of the dried resin weight 24 g with a mixture of nitrate - 13 grams of litharge - 33 g of borax - 5 g). The free kapelrud to obtain gold-silver goldcrest, which weighed, razvarivat in nitric acid to Golden squat, which burn and re-weighed. The disadvantages of the method are its oncospecific direction: the composition of the charge and the melting temperature is only suitable for the analysis of resins.

The known method of assay determination of gold (ISO 10378 International Standart "Concentres de sulfures plomb - Dosage cte D'argent et de for - Methode par voie seche et spec trometrie d asorption atomique dans la flamme a partir d'une coupellation. First edition 1994-06-11. The reference number ISO 10378:1994 (E)), which includes assay crucible melting samples pre°with the charge on the basis of soda, borax, litharge, reductant to obtain lead alloy (free), cupellation to gold-silver goldcrest, dissolution of silver in dilute nitric acid and the weighting of the resulting gold squat. If the mass of the gold squatting less than 0.005 mg it is dissolved in a mixture of nitric and hydrochloric acids and determine gold by the method of flame atomic absorption spectrometry. The method developed for concentrates of copper sulfide, resulting in the charge injected additional quantity of litharge and nitrate (20 g samples of 30 g of sodium, 210 g of litharge, 25 g of silicon dioxide; the mass of nitrate calculated by the resilience of the sample and determine the control melting).

The closest analogue in essential characteristics and purpose is: Probootborniki and analysis of noble metals, edited by Iframename. M., "metallurgy", 1968, 121-132, 154 C, in which is disclosed a method of assay determination of gold in ores and products of their processing, including melting at a temperature of 1150°With the charge from the sample source material with litharge, soda, brown and flour with getting lead alloy, it cupellation to gold-silver goldcrest, dissolving the sulfur is RA in dilute nitric acid and determining the quantity of gold obtained by weighing the gold squatting or instrumental method.

The objective of the invention is to simplify and accelerate the analysis, as well as reducing its cost by reducing the duration and temperature of fusion of the sample, increasing the service life of furnace, reusable metal crucibles.

The technical result is achieved in that in the method of assay determination of gold in ores and products of their processing, including the melting of the charge from the sample source material with litharge, soda, brown and flour with getting lead alloy, it cupellation to gold-silver goldcrest, dissolution of silver in dilute nitric acid and determining the quantity of gold obtained by weighing the gold squatting or instrumental method

- in charge is injected sodium hydroxide or potassium in the composition of the mixture, 10 g of sample: 20-50 g of sodium hydroxide or potassium, 2-20 g of borax, 1-10 g soda, 15-30 g of litharge, 1-3 g of flour, and a heat conducting metal crucibles for 10-30 minutes at a temperature of 600-800°C.

The recommended method for analysis of samples by weight of 10-100 g

Technical implementation of the method

The mixture for the assay alkaline fusion is prepared by weighing the individual components on a technical scale (0.1-0.01 g) and subsequent mixing, which produces well-known methods (mixing with a spatula. then rolling the sheet to which LCI; mixing in a closed jar or plastic bag and so on), in this first mix the sample, soda, litharge, borax, flour, then add the lye and mix again.

The prepared mixture is poured into a metal crucibles (the fill factor of 0.2-0.4), which is placed in a heated to a predetermined temperature oven and leave in oven set time, take out and not cooling water, pour it into a metal mold. After cooling the mold overturn and easy to remove from her frozen water 1-2 blows on the anvil. Then the hammer is separated from the slag lead alloy. The resulting free kapelrud to gold-silver goldcrest, dissolved silver in dilute nitric acid and determine the amount of gold obtained by weighing the gold squatting or other instrumental method (for example, dissolve gold kartochka in acids and analyze the solution by atomic absorption).

One of the advantages of the inventive method is used for alkaline melting metal crucibles instead of fireclay crucibles used in the classical assay analysis, which are made on special order and re-used is usually not more than 3-5 times (with the possible contamination of the samples). Metal crucibles can be used many times: after melting (after disposing of taperapua) they are placed in a large tank of water (for example, barrel) and leave for a few hours. The solidified slag is partially dissolved and otmechaet". The crucibles are easily cleared from the wet slag. Sticking balls of lead alloy to the walls and bottom of the washed crucibles is not observed. Thus, contamination of subsequent samples of the remains of the previous does not occur. Prepared by the above method crucibles can be used for the following heats.

The main advantage of the claimed method is the use of low-melting of the charge, which reduces the melting temperature at 200-400°and the time of fusing reduced to 10-30 minutes. This significantly increases the service life of furnaces, performance analysis and, therefore, reduces the cost of analysis. For melting can be used not only special furnace designs (designed for this method of fusion), but also assay crucible and conventional muffle furnace.

The table shows the results of the analysis of the claimed method (final operation - weighing gold squatting) number of standard samples and samples Pokrovsky mine. The mineralogical composition of the samples is as follows:

- granite-porphyries with veins of quartz (sample Pokrovsky mine),

- quartz gold-silver ore RGU-6 (GSO 5806-91),

- gold sulphide ore WA-6 (CCA 283-96).

For sravneniyami Pokrovsky mine analyzed in the assay analytical laboratory OJSC Pokrovskiy Rudnik (Amur region, Blagoveschensk) certified by the method of classical assay analysis.

Thus, when verifying the claimed method was used limitedly interlaboratory experiment two independent methods, and two independent laboratories.

Table
The results of the analysis of standard samples and samples Pokrovsky mine
No. sample no experience The composition of the charge and melt conditions in the claimed method The content of Au in the sample, g/t The allowable error of determination (R=0,68), g/t
The composition of the charge, grams (10 g samples) Melting temperature, ° The melting time, min The claimed method Classical fire assay
Litharge Lye Soda Borax Flour
Sample Pokrovsky mine (granite-porphyries with veins of quartz)
1 1 20 30 0 0 2 750 33 0,3 0,2 0,1
2 2 20 40 0 0 2 750 29 7,5 7,8 0,9
3 3 20 40 0 0 2 750 19 10,0 10,0 0,8
4 4 20 40 0 0 2 750 28 4,8 5,2 0,6
5 5 20 40 0 0 2 750 30 6,7 6,6 0,8
6 20 50 0 10 2 800 20 6,8
7 20 50 0 10 2 800 20 6,4
8 20 50 10 0 2 800 17 6,7
9 20 40 0 0 2 800 17 6,7
6 10 20 50 0 10 2 800 20 to 12.0 12,4 1,0
11 20 40 0 10 2 800 23 12,9
12 20 50 0 10 2 800 20 to 12.0
13 20 40 0 0 2 800 14 11,5
14 30 30 0 10 3 800 10 to 12.0
15 20 30 0 20 2 800 13 12,2
16 30 30 0 20 2 800 13 11,9
Quartz gold-silver ore RGU-6 GSO 5806-91
17 20 30 - 20 2 70 30 12,8 12,8 1,05
18 20 40 - 20 2 750 20 11,8
19 30 30 - - 2 750 25 11,8
20 20 30 - 20 2 800 13 13,2
Gold sulfide ore WA-6 CCA 283-96
21 20 30 - - 2 750 10 4,0 4,1 0,74
22 20 30 - 10 2 800 13 4,4
23 20 30 - - 2 800 13 a 3.9
24 20 35 - - 2 800 15 5,3
25 20 30 - - 2 800 12 a 3.9

As can be seen from the table, the results of determination of gold by the claimed method differs from the classical results of assay analysis within the most stringent (P=0,68) permissible error analysis

DSS.=With·σD,r:100, g/t,

where C is the content of the component to be determined in the sample, g/t,

σDGpermissible relative standard deviation of the results of the analysis performed by the methods category III classification (standardized for OST 41-08-212-82), %.

Absolute tolerance is calculated according to the gold content in the sample, a specific certified by the method of classical assay analysis.

Method of assay determination of gold in ores and products of their processing, including the melting of the charge from the sample source material with litharge, soda, brown and flour with getting lead alloy, it cupellation to gold-silver goldcrest, dissolution of silver in dilute nitric acid and determining the quantity of gold obtained by weighing the gold squatting or instrumental method, characterized in that the charge injected sodium hydroxide or potassium in the composition of the mixture of 10 g of the sample: 20-50 g of sodium hydroxide or potassium, 2-20 g of borax, 1-10 g soda, 15-30 g of litharge, 1-3 g of flour, and melting is carried out in m is a metallic crucible for 10-30 minutes at a temperature of 600-800° C.

 

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