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Method for determining lead, zinc and cadmium from mixed lead-zinc-cadmium concentrate

A concentrate, lead-zinc technology, applied in the fields of cadmium, lead and zinc determination, can solve the problems of excessive zinc content and inability to detect accurately, and achieve the effect of reducing systematic errors and shortening detection and analysis time.

Active Publication Date: 2020-07-28
西安西北有色地质研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] But there are following problems in this method: 1, this method points out, when lead amount is greater than 4%, should add sulfuric acid precipitation separation, and filter removal; "There is no corresponding determination method for lead content greater than 4%; 2. The calculation formula of zinc content has cadmium content as a supplementary amount to correct, but "Cadmium content determination method (GB / T8151.8-2012)" only The flame determination method with less than 2% cadmium content, when the cadmium content in the sample exceeds 2%, there is no corresponding method for accurate determination to supplement the zinc content; 3. The separation of zinc in the national standard is based on ammonium chloride, ammonium persulfate, ammonia water and interference However, according to the separation technology of zinc ore in Chapter 42 of "Rock and Mineral Analysis", in the presence of a large amount of ammonium chloride and ammonium hydroxide, zinc and iron, aluminum, vanadium, tin, copper, Lead, cadmium, manganese, etc. can be separated. After a large number of experiments, it has been proved that at least 20% of the cadmium is precipitated and separated from the zinc solution during the separation of zinc. That is to say, when the zinc content is 30%, the cadmium content When the value is 2%, the value of the zinc content calculated according to the national standard method has exceeded the error and cannot be accurately detected

Method used

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  • Method for determining lead, zinc and cadmium from mixed lead-zinc-cadmium concentrate
  • Method for determining lead, zinc and cadmium from mixed lead-zinc-cadmium concentrate

Examples

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Embodiment 1

[0063] A method for simultaneously measuring lead content, zinc content, and cadmium content in a mixed lead-zinc-cadmium concentrate, the measurement steps of which are:

[0064] Step 1: Accurately weigh two parts of 0.2000g sample, put them into 300mL beakers respectively, add 2g of potassium chlorate and 15mL of nitric acid, cover with a watch glass, heat until the sample has no black residue, take it off, add 5mL of hydrochloric acid, 20mL of sulfuric acid (1+ 1), heat to smoke for 15 minutes, take it off, wash the tableware and cup wall, add 100mL deionized water, boil for 10 minutes, take it off, and let it stand overnight. Then filter, and the filtrate is reserved for the second step, the precipitate is washed with 2% sulfuric acid solution, and the precipitate is used for titrating the lead content in the sample. Add 30mL of acetic acid-sodium acetate buffer solution, add 0.2g of ascorbic acid, add 2 drops of xylenol orange indicator, and titrate with EDTA (0.02000mol / ...

Embodiment 2

[0070] A method for simultaneously measuring lead content, zinc content, and cadmium content in a mixed lead-zinc-cadmium concentrate, the measurement steps of which are:

[0071] Step 1: Accurately weigh two samples of 0.3g (±0.0003g), put them into 300mL beakers respectively, add 2g (±0.1g) of potassium chlorate and 15mL of nitric acid, cover with a watch glass, heat until the sample has no black residue, remove , add 5mL hydrochloric acid, 20mL sulfuric acid (1+1), heat to smoke for 15 minutes, take it off, wash the glass and cup wall, add 100mL deionized water, boil for 10min, take it off, and let it stand overnight. Then filter, and the filtrate is reserved for the second step, the precipitate is washed with 2% sulfuric acid solution, and the precipitate is used for titrating the lead content in the sample. Add 30mL of acetic acid-sodium acetate buffer solution, add 0.2g of ascorbic acid, add 2 drops of xylenol orange indicator, and titrate with EDTA (0.02000mol / L), the s...

Embodiment 3

[0076] A method for simultaneously measuring lead content, zinc content, and cadmium content in a mixed lead-zinc-cadmium concentrate, the measurement steps of which are:

[0077] Step 1: Accurately weigh two samples of 0.4g (±0.0003g), put them into 300mL beakers, add 2g of potassium chlorate and 15mL of nitric acid, cover with a watch glass, heat until the sample has no black residue, remove it, and add 5mL of hydrochloric acid , 20mL of sulfuric acid (1+1), heated to smoke for 15 minutes, take it off, wash the tableware and cup wall, add 100mL of deionized water, boil for 10min, take it off, and let it stand overnight. Then filter, and the filtrate is reserved for the second step, the precipitate is washed with 2% sulfuric acid solution, and the precipitate is used for titrating the lead content in the sample. Add 30mL of acetic acid-sodium acetate buffer solution, add 0.2g of ascorbic acid, add 2 drops of xylenol orange indicator, and titrate with EDTA (0.02000mol / L), the ...

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Abstract

The invention belongs to the field of mineral metal element detection, and particularly discloses a method for determining lead, zinc and cadmium from mixed lead-zinc-cadmium concentrate, which comprises the following steps: pretreating a concentrate sample to obtain a precipitate and a filtrate, wherein the precipitate is used for determining the lead content, and the filtrate is standby; addinga precipitant into the filtrate to obtain a first precipitate and a first filtrate, the first filtrate comprising a sample first filtrate and a comparison first filtrate, adding a cadmium masking agent into the comparison first filtrate to determine the zinc content, the sample first filtrate being directly used for determining the sum of the zinc content and the cadmium content in the solution, and the first precipitate being spare, wherein the first precipitate is used for measuring the content of cadmium in the precipitate, the final cadmium content is the zinc content in the solution, andafter the zinc content is subtracted from the sum of the cadmium content, the cadmium content in the precipitate is added. According to the method, the lead content, the zinc content and the cadmium content can be accurately measured at a time, the analysis time is shortened, and the detection efficiency is improved.

Description

technical field [0001] The invention belongs to the field of detection of mineral metal elements, and specifically invents a method for measuring lead, zinc and cadmium from mixed lead-zinc-cadmium concentrates. Background technique [0002] The current determination method of zinc content in zinc concentrate is tested according to "GB / T8151.1-2012". This part includes two methods, 1 is precipitation separation method, 2 is extraction separation method, and method 1 is arbitration method. Therefore, the measurement range of method 1, the exclusion of various interfering elements and the accuracy are very important. [0003] But there are following problems in this method: 1, this method points out, when lead amount is greater than 4%, should add sulfuric acid precipitation separation, and filter removal; "There is no corresponding determination method for lead content greater than 4%; 2. The calculation formula of zinc content has cadmium content as a supplementary amount t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/79G01N31/16
CPCG01N21/79G01N31/16Y02P10/20
Inventor 马熠罡张尼冯玉怀吴随周王奎展向娟张浏波高翔宇李皓高航
Owner 西安西北有色地质研究院有限公司