Method of a quality control over the test crucible melting

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·(Mшш+Mcc)]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.

3 ex

 

The method relates to analytical chemistry and can be used for determination of noble metals in mineral raw materials.

The known method [1, s] quality control of melting, including cleaning of the crucible with melt them in charge of approximate composition: 60 g Na2CO3, 20 g of Na2B4O7·10H2O, 50 g of PbO, 3 g of reducing agent (starch, flour) and analysis of lead alloys, obtained in the process of "purification" of the crucibles.

This method increases the reliability of the assay results of the analysis, but has the following disadvantages:

- increases the cost of assay analysis;

- reduces expressnet assay analysis.

Closest to the proposed method is a method [2, p.124] quality control assay crucible for melting determination of noble metals in mineral raw materials, including smelting of the charge with the extraction of precious metals in lead alloy and visual inspection of the color obtained lead alloy and otdelimosti it from slag, homogeneity and degree of acidity of the slag.

This method does not allow to control the surface tension of the slag and hydrodynamic regime of melting depends on the degree of extraction of precious metals from molten slag in the lead alloy.

The technical result of the invention is to increase the reliability of the results is the ATA assay analysis. The technical result is achieved in that in the method of quality control assay crucible for melting determination of noble metals in mineral raw materials, including smelting of the charge with the extraction of precious metals in lead alloy and visual inspection of the color obtained lead alloy and otdelimosti it from slag, homogeneity and degree of acidity of the slag according to the invention, the quality control visually the height of the fluidized bed of molten slag and lead to a valid value which is calculated by the formula:

where Nm- the depth of the crucible, m;

Hc- the height of the fluidized bed of molten slag and lead, m;

α - the angle at the vertex of the cone inner surface of the crucible, C;

MW, Mwith- the mass of the slag and weight of the lead, respectively, kg;

ρWthat ρwiththe density of the slag and the density of lead, respectively, kg/m

The essential difference is the use for visual quality control of crucible smelting of new technological parameter, the height of the fluidized bed of molten slag and lead. Another difference is the use of formulas (1) to establish an acceptable height of the fluidized bed of molten slag and lead.

The method is as follows. Of material laboratory test OTB is given the analytical sample, mix it with a design quantity of the mixture, the mixture is melted by a standard method. During melting visually control the characteristics of the fluidized bed of molten slag and lead. When choosing the right charge the molten slag and lead boils rapidly, the maximum height of the fluidized bed corresponds to the design condition (1). When the deviation of the height of the fluidized bed of molten slag and lead from the allowed value decreases the degree of extraction of precious metals in lead alloy. In this case, adjust the composition of the charge and perform sample analysis again.

The invention is illustrated by the following examples.

Example 1. Analyzing a control sample of quartz ore, containing finely dispersed gold in the amount of 15 g/so Selected analytical sample mass 50 g and mix it with the mixture composition, g: lead oxide - 80, soda ash fused - 35, dehydrated borax - 15, starch and 2.5. Spend crucible melting the mixture of the sample and the charge in the crucible PT-3. During melting visually estimate the height of the layer of the melt, which is equal to 8·10-2m In the melting receive lead alloy mass of 32.5 g and slag mass 95, Lead alloy is light, easily separated from the slag. Slag homogeneous core. Calculate the maximum height hatslacha layer by the formula (1), receive 1,6·10-1m ≥Nwith≥1·10-1m Affairs shall have the conclusion of the what height hatslacha melt is outside the range of allowable values. Therefore, gold is not fully extracted from the molten slag in the lead alloy. Sample analysis should be repeated. Next, determine the gold content in the lead alloy and calculate the gold content in the sample. Estimated gold content of the sample is 13.5 g/T. the Degree of extraction of gold in the smelting process - 90%. Thus, the result of the analysis of a control sample confirms the conclusion made on the basis of visual monitoring of the heat.

Example 2. Analyze the same control sample. Selected analytical sample mass 50 g and mixed with the charge stock, g: lead oxide - 80, soda ash - 35, borax - 15, starch and 2.5. Spend crucible melting the mixture of the sample and the charge in the crucible PT-3. During melting visually estimate the height hatslacha layer, which is 1.2·10-1m In the melting receive a lead alloy with a mass of 32.0 g and slag mass 89, Lead alloy is light, easily separated from the slag. Slag homogeneous core. Calculate the maximum height hatslacha layer by the formula (1) and conclude that the height hatslacha melt does not extend beyond the interval of acceptable values, as 1,6·10-1m ≥Nwith>0,9·10-1m Therefore, the quality of operation of Tegelen what I'm melting" high. Next, determine the gold content in the lead alloy and calculate the gold content in the sample - 15.0 g/t (the degree of extraction of gold in the smelting process - 100%). Thus, the result of the analysis of a control sample confirms the conclusion made on the basis of visual monitoring of the heat.

Example 3. Analyze the same control sample. Selected analytical sample mass 50 g and mixed with the charge stock, g: lead oxide - 50, soda ash - 60, borax - 20, starch - 3. Spend crucible melting the mixture of the sample and the charge in the crucible PT-3. During melting visually estimate the height hatslacha layer. Note that the height hatslacha layer exceeded the depth of the crucible, 1.8·10-1m and part of the melt has flowed out from the crucible. Therefore, gold is not fully extracted from the molten slag in the lead alloy and the sample analysis should be repeated, pre-adjust the composition of the charge. Next, determine the gold content in the lead alloy and calculate the gold content in the sample - 14.2 g/t (the degree of extraction of gold in the smelting process - 94,7%). Thus, the result of the analysis of a control sample confirms the conclusion made on the basis of visual monitoring of the heat.

According to the experimental verification of the proposed method in comparison with the prototype provides a higher reliability of results VI the issue of quality control operations assay analysis crucible melting.

Sources of information:

1. Shvetsov V., Pakhomov CENTURIES, Chichewa V.P. Journal of analytical chemistry. T.XLIV. Issue 6. 1988. S-1068.

2. Baryshnikov IVAN, Popova N.A., Orobinskaya VA Probootborniki and analysis of noble metals. M.: metallurgy, 1978, p.123-125.

Method of quality control assay crucible for melting determination of noble metals in mineral raw materials, including smelting of the charge with the extraction of precious metals in lead alloy and visual inspection of the color obtained lead alloy and otdelimosti it from slag, homogeneity and degree of acidity of the slag, wherein the quality control visually the height of the fluidized bed of molten slag and lead to a valid value which is calculated by the formula

where Hm- the depth of the crucible, m;

Hc- the height of the fluidized bed of molten slag and lead, m;

α - the angle at the vertex of the cone inner surface of the crucible, C;

MW, Mc- the mass of the slag and weight of the lead, respectively, kg;

ρWthat ρwiththe density of the slag and the density of lead, respectively, kg/m3.



 

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