SU1642303A1 - Method of determination of tungsten in ores and related products - Google Patents

Abstract

The invention relates to methods for preparing samples of concentrates for the subsequent photometric determination of tungsten and allows increasing the reproducibility and reducing the time of analysis of tungsten in the enterprises of Mincolmetmet. The method consists in processing the sample by boiling for 1 h in 3 to 4 M hydrochloric acid solution in the presence of diode , j-- antsa, vzdgom h, corresponds to ncc (2-5}: x triolgndu solfr; g; l i. subsequent, "the calculation of P; and anodnogo go mm-lol in oi razukchtso with filter he-1 ha Sol

Description

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The invention relates to a training proc ester for C. for a: aliza t. It can be used to refine; 1 tungsten grades of ores & pr etc.; ; - so their processing

The purpose of the invention is to increase reproducibility and reduce analysis time.

The goal is achieved by treating tungsten-containing samples with hydrochloric acid with a concentration of 3-4 mol / l in the extract: manganese dioxide with a ratio of manganpe dioxide and tungsten trioxide equal to (2-5;: 1

Example 1 (prototype) A portion of a sample containing 0.15% W05, weighing 1 g, is treated with 100 cm of concentrated (14 mol.) / L hydrochloric acid for 1 hour while boiling the solution3. After cooling, the solution is filtered, the filtrate is evaporated to dryness and dissolved in eO cm2 co, I am acidic, centering 4 mol / l (, 1 1) “Sediment i: a filter-tre, amount in the form of iseiil g, / l lirimy of tungsten acid, processing L MICP ICTBOP - Gll, sodium roxide with co-filter I can / l, boiled to dryness and the residue after dissolving it in bo ml of irlh; and, 4 moles / liter spot added by adding 1 to the filtrate 1 ° C. Add 5 cm3 of a solution of i rodan — ammonia with a concentration of mol / j and dropwise titanium chloride of titanium to the solution; then the disappearance of the red color of iron rhodanide and zatech 1 smh its excess

After 15 mip, the optical density of the solution was measured on a fscscorlmeter and the concentration of tungsten trioxide was calculated by the Gramir – Gram: Gram:

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fiku built on standard tungsten trioxide solutions0

The analysis time is 8 h, the relative standard deviation is 0.2 „II p and m 2 (the proposed method) g A sample of 0.15% W05 containing a mass of 1.0 g is treated with 50 ml of 3 mol / l hydrochloric acid in the presence of 3 mg of manganese dioxide, the ratio Mn02:: WO 2: 1), slightly boiled for 1 Co. After cooling, the solution is filtered. HC1 (3 mol / L) is added to an aliquot portion of the filtrate (10 cm3)

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to a volume of 50 cm, add 2.5 cm of a solution of rhodium ammonium with a concentration of J mol / l and a solution of titanium trichloride is added dropwise until the red color of iron rhodanide disappears, then I cm e, th excess, in the resulting solution tungsten trioxide on a photocolorimeter using a calibration curve based on standard tungsten trioxide solutions

The analysis time was 3 hours, the relative standard deviation of Sr was 0.05 °.

II p and me r zo A sample of a sample containing 0.15% W03 and a mass of 1.0 g is treated with 50 cm of hydrochloric acid with a concentration of 4 mol / l in the presence of 7.5 mg of manganese dioxide (ratio W0g 5g1) and slightly boil for 1 h. After cooling, the solution is filtered. HC1 (4 mol / L) is added to an aliquot portion of the filtrate (10 cm) to a volume of 50 cm, and 2.5 cm of ammonium rhodium-containing solution is added. and dropwise a solution of titanium trichloride until the red color of iron rhodanide disappears, then 1 cm of its excess. In the resulting solution, the trioxide in frama on photocolorimeter using a calibration curve constructed with standard solutions volframao oxide

The duration of the analysis is 3 hours, the relative standard deviation of Sr is 0.05 °.

To select the optimal interval, similar experiments were carried out at a ratio of manganese dioxide and tungsten trioxide of 1: 1, 3: 1, b: 1 „

The results of the experiments are presented in

the table

From the data presented in the table, it follows that the optimal parameters of the proposed method are the ratio of manganese dioxide and tungsten trioxide 2-5: I and the concentration of hydrochloric acid 3-4 mol / l. At a concentration of hydrochloric acid below 3 mol / l and the ratio x manganese dioxide and tungsten trioxide less than 2: 1, partial loss of wolfram in the form of insoluble tungsten acid is observed, which results in an underestimate of analysis results. At a concentration of hydrochloric acid above 4 mol / l and ratios of manganese dioxide and thr tungsten oxide and more than 5: 1 is a need for dilution hydrochloride solutions prior fotokolorimetrirovaniem tungsten, resulting in the additional consumption of titanium trichloride to restore Jr. (IV) to Mn (II) of these circumstance prolong the analysis and reduce its accuracy

The proposed method of refining the tungsten content in comparison with the prototype allows speeding up the analysis by 2 times and increasing the reproducibility of parallel definitions of tungsten (Sr) „by 2 times.

Claims (1)

Invention Formula The method for determining tungsten in ores and products of their processing, including the decomposition of a sample with hydrochloric acid at boiling, filtration, transfer of tungsten into a complex compound with ammonium rohanide in the presence of titanium trichloride and subsequent quantitative registration by photometry, differing in that in order to increase the reproducibility and reduce the time of analysis, the decomposition of the sample is carried out with 3.0-4.0 M hydrochloric acid solution in the presence of manganese dioxide with a weight ratio of it and trioxide wolf Ama 2-5: 1 ,, manganese dioxide: tungsten trioxide ratio 1: 1 tungstic acid precipitate A white precipitate of tungstic acid is observed.