Method for rapidly measuring content of barium sulfate

Abstract

The invention belongs to the technical field of barium sulfate content determination, and particularly relates to a method for rapidly determining the content of barium sulfate, which comprises the following steps: S1, placing a sample in a beaker, adding sodium fluoride, adding concentrated hydrochloric acid, boiling, and adding concentrated nitric acid; s2, adding potassium sulfate, adding water to a constant volume, and boiling; s3, cooling, and filtering with filter paper; s4, washing the beaker and the precipitate with sulfuric acid, washing the beaker with water, and washing the precipitate; s5, transferring the precipitate together with the filter paper into a weighed crucible, firing to constant weight, and weighing together with the crucible; and S6, calculating the content. By means of a hydrochloric acid-nitric acid gradient acidolysis system, efficient dissolution of impurities can be achieved within a short time, and the problem that high-temperature melting consumes time is avoided; in addition, a sodium fluoride dynamic silicon removal mechanism is introduced, so that the safety is improved. And secondly, by adopting the same ion effect of potassium sulfate, the SOconcentration in the solution is improved, the Baprecipitation rate is further improved, the precipitation time is shortened, and the mine detection timeliness requirement is perfectly met.

Description

Technical Field

[0001] The invention belongs to the technical field of barium sulfate content determination, and particularly relates to a method for quickly determining barium sulfate content. Background Art

[0002] Barium sulfate, a key component of associated minerals in lead-zinc ores, is crucial for comprehensive resource utilization and beneficiation process optimization. During lead-zinc ore mining and sales, rapid assessment of the barium sulfate grade in ore samples is essential to guide flotation reagent addition, tailings treatment, and by-product recovery. However, due to the complex mineral composition of lead-zinc ores (including silicates, sulfides, and metal oxides), traditional analytical methods face the following technical bottlenecks:

[0003] (1) The conventional gravimetric method is cumbersome: The classic barium sulfate gravimetric method requires the sample to be melted in sodium carbonate, dissolved in hydrochloric acid, and separated by multiple precipitation steps, which takes up to 6-8 hours. The large amount of silicates present in lead-zinc ores will form inclusions with barium sulfate, which requires repeated filtration and washing to remove the silicate colloid, resulting in low process efficiency.

[0004] (2) Incomplete separation of interfering elements: Lead-zinc ores commonly contain interfering components such as SiO2 (quartz, feldspar), Fe³⁺ (oxidation product of pyrite), and Pb²⁺ (dissolution product of galena). Among them, silicate residues will co-precipitate with barium sulfate, and Fe³⁺ is easily hydrolyzed under acidic conditions to form Fe(OH)3 colloids that adsorb Ba²⁺, resulting in inflated measured values.

[0005] (3) Poor controllability of the precipitation process: Traditional methods rely on natural aging to completely precipitate barium sulfate, which takes up to 2-3 hours. However, lead-zinc ore processing plants need to obtain test results within 30 minutes to adjust flotation parameters, and existing technologies cannot meet the timeliness requirements. In addition, when the ore sample contains trace amounts of Sr²⁺ and Ca²⁺, sulfate co-precipitation is significant, and conventional calcination methods are difficult to distinguish the true BaSO4 content.

[0006] The information disclosed in this background technology section is only intended to enhance understanding of the overall background of the invention and should not be regarded as an admission or any form of suggestion that the information constitutes the prior art already known to a person skilled in the art. Summary of the Invention

[0007] The object of the present invention is to provide a method for quickly determining the content of barium sulfate to solve the problems existing in the prior art.

[0008] To achieve the above object, the present invention provides the following technical solutions:

[0009] A method for rapidly determining barium sulfate content comprises the following steps:

[0010] S1. Place the sample in a beaker, add sodium fluoride, and bring to a boil with concentrated hydrochloric acid. Continue boiling with concentrated nitric acid.

[0011] S2. Rinse the watch glass and beaker, add potassium sulfate, and dilute to 50 mL with water. Bring to a boil for 10 minutes.

[0012] S3. After cooling, place the beaker in running water for 30 minutes and filter with filter paper;

[0013] S4. Wash the beaker and precipitate with sulfuric acid 4-5 times each, wash the beaker with water once, and wash the precipitate;

[0014] S5. The precipitate and filter paper are transferred to a crucible weighed m1, burned to constant weight, and the crucible is weighed m2;

[0015] S6. Calculate the barium sulfate content in the sample according to the following formula

[0016] ;

[0017] Where m is the mass of the sample.

[0018] Furthermore, in step S1, the mass-to-volume ratio of the sample to concentrated hydrochloric acid is 0.3 g:15 mL, and the mass-to-volume ratio of the sample to concentrated nitric acid is 0.3 g:5 mL.

[0019] Furthermore, in step S1, concentrated hydrochloric acid is added and boiled at low temperature for 5 minutes, and concentrated nitric acid is added and boiled until the volume of the solution in the beaker is 1 / 10 of the total volume of concentrated hydrochloric acid and concentrated nitric acid.

[0020] Furthermore, in step S2, the mass ratio of potassium sulfate to sample is 1:0.3.

[0021] Furthermore, in step S4, washing is performed until there is no sulfate ion.

[0022] Furthermore, in step S5, the mixture is calcined at 800° C. to a constant weight.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] (1) The present invention uses a hydrochloric acid-nitric acid gradient acid hydrolysis system (HCl dissolves metal oxides, HNO3 oxidizes sulfides), which can achieve efficient dissolution of impurities in a relatively short time and avoid the time-consuming problem of high-temperature melting.

[0025] (2) The present invention introduces a dynamic desiliconization mechanism of sodium fluoride, which converts silicate into volatile SiF4 under acidic boiling conditions, thereby improving safety compared with the traditional hydrofluoric acid treatment method.

[0026] (3) The present invention uses the common ion effect of potassium sulfate to increase the concentration of SO4²⁻ in the solution, thereby increasing the Ba²⁺ precipitation rate and shortening the precipitation time, which perfectly meets the timeliness requirements of mine detection. DETAILED DESCRIPTION

[0027] The following is a clear and complete description of the technical solution of the present invention. Obviously, the embodiments described are part of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making any creative work are within the scope of protection of the present invention.

[0028] Example 1

[0029] A method for rapidly determining barium sulfate content comprises the following steps:

[0030] S1. Place 0.3000g of sample (denoted as m) in a 250mL beaker, add 0.5g of sodium fluoride, and then add 15mL of concentrated hydrochloric acid (38.0%). Boil for 5 minutes. Add 5mL of concentrated nitric acid (68.0%) and continue boiling until the volume of the solution in the beaker is 2mL.

[0031] S2. Rinse the watch glass and beaker, add 1 g of potassium sulfate, dilute to 50 mL with water, and boil for 10 minutes.

[0032] S3. After cooling, place the beaker in running water for 30 minutes and filter with slow quantitative filter paper;

[0033] S4. Wash the beaker and precipitate 4-5 times each with 2% sulfuric acid, then rinse the beaker once with water until the precipitate is free of sulfate ions.

[0034] S5. Transfer the precipitate and filter paper into a 30 mL porcelain crucible (m1). Incinerate at 800°C to a constant weight. Weigh the crucible and precipitate together (m2).

[0035] S6. Calculate the barium sulfate content in the sample according to the following formula

[0036] .

Claims

1. A method for rapidly determining the content of barium sulfate, characterized in that: The following steps are involved: S1. Place the sample in a beaker, add sodium fluoride, and bring to a boil with concentrated hydrochloric acid. Continue boiling with concentrated nitric acid. S2. Rinse the watch glass and beaker, add potassium sulfate, and dilute to 50 mL with water. Bring to a boil for 10 minutes. S3. After cooling, place the beaker in running water for 30 minutes and filter with filter paper; S4. Wash the beaker and precipitate with sulfuric acid 4-5 times each, wash the beaker with water once, and wash the precipitate; S5. The precipitate and filter paper are transferred to a crucible weighed m1, burned to constant weight, and the crucible is weighed m2; S6. Calculate the barium sulfate content in the sample according to the following formula ； Where m is the sample mass.

2. The method for rapidly measuring barium sulfate content according to claim 1, wherein In step S1, the mass volume ratio of the sample to concentrated hydrochloric acid is 0.3 g:15 mL, and the mass volume ratio of the sample to concentrated nitric acid is 0.3 g:5 mL.

3. The method for rapid determination of barium sulfate content according to claim 1, wherein In step S1, concentrated hydrochloric acid is added and boiled at low temperature for 5 minutes, and concentrated nitric acid is added and boiled until the volume of the solution in the beaker is 1 / 10 of the total volume of the concentrated hydrochloric acid and concentrated nitric acid.

4. The method for rapid determination of barium sulfate content according to claim 1, wherein In step S2, the mass ratio of potassium sulfate to sample is 1:0.

3.

5. The method for rapid determination of barium sulfate content according to claim 1, wherein In step S4, washing is performed until there is no sulfate ion.

6. The method for rapid determination of barium sulfate content according to claim 1, wherein: In step S5, the mixture is calcined at 800° C. to a constant weight.

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