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Method for determining antimony in lead bullion by precipitation separation-carbon reduction cerium sulfate volumetric method

A technology of precipitation separation and cerium sulfate, which is applied in the direction of chemical analysis by titration, can solve the problems of narrow linear range, difficult to distinguish titration end point, high matrix, etc., and achieve the effect of improving accuracy and precision

Inactive Publication Date: 2020-09-18
NORTHWEST RES INST OF MINING & METALLURGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0028] The purpose of the present invention is to provide a method for the determination of antimony in crude lead by precipitation separation-carbon reduction cerium sulfate volumetric method, to solve the problem of narrow linear range, high matrix and large loss of instruments caused by traditional determination methods in the process of separation and enrichment of antimony , the problem that the titration endpoint is difficult to distinguish

Method used

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  • Method for determining antimony in lead bullion by precipitation separation-carbon reduction cerium sulfate volumetric method
  • Method for determining antimony in lead bullion by precipitation separation-carbon reduction cerium sulfate volumetric method
  • Method for determining antimony in lead bullion by precipitation separation-carbon reduction cerium sulfate volumetric method

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Embodiment 1

[0047] A method for the determination of antimony in crude lead by precipitation separation-carbon reduction cerium sulfate volumetric method, it comprises the following steps:

[0048] Step 1. Preparation of cerium sulfate standard solution: Weigh 10g of cerium sulfate and place it in a 1000mL beaker, add 30mL of sulfuric acid, mix well, and gradually heat up on the electric furnace until the cerium sulfate dissolves into a paste and gradually emits white smoke of sulfuric acid for about 30min. Remove and cool slightly, add 140mL of sulfuric acid solution with a concentration of 50% by volume, then slowly add 400mL of water, stir and dissolve until the solution is clear, cool, and dilute to a 1000mL volumetric flask with water to obtain a molar concentration of 0.025mol / L of cerium sulfate standard solution;

[0049] Step 2. Calibration of metal antimony by cerium sulfate standard solution: Weigh 4 parts of 0.060g metal antimony, the mass percentage of metal antimony is ≥99....

Embodiment 2

[0074] A method for the determination of antimony in crude lead by precipitation separation-carbon reduction cerium sulfate volumetric method, it comprises the following steps:

[0075]Step 1. Preparation of cerium sulfate standard solution: Weigh 10g of cerium sulfate and place it in a 1000mL beaker, add 30mL of sulfuric acid, mix well, and gradually heat up on the electric furnace until the cerium sulfate dissolves into a paste and gradually emits white smoke of sulfuric acid for about 30min. Remove and cool slightly, add 140mL of sulfuric acid solution with a concentration of 50% by volume, then slowly add 400mL of water, stir and dissolve until the solution is clear, cool, and dilute to a 1000mL volumetric flask with water to obtain a molar concentration of 0.025mol / L of cerium sulfate standard solution;

[0076] Step 2. Calibration of metal antimony by cerium sulfate standard solution: Weigh 4 parts of 0.060g metal antimony, the mass percentage of metal antimony is ≥99.9...

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Abstract

The invention discloses a method for determining antimony in crude lead by a precipitation separation-carbon reduction cerium sulfate volumetric method, which comprises the following steps: dissolvinga sample with dilute nitric acid, selecting ammonia water or sodium carbonate as a precipitant, slowly dropwise adding the precipitant, regulating the pH value of the solution to 3-5, boiling for 5 minutes, and filtering after complete precipitation; dissolving the filter residues and filter paper with sulfuric acid, carbonizing the filter paper, directly reducing Sb < 5 + > into Sb < 3 + >, andtitrating antimony with a cerium sulfate standard solution in a sulfuric acid-hydrochloric acid medium. Ammonia water with the volume percentage concentration of 50% or a sodium carbonate solution with the mass-volume ratio of 200 g / L is adopted as a precipitator; antimony precipitates in the solution are completely separated from other interference elements; excessive precipitant reacts with sulfuric acid or hydrochloric acid to generate water or carbon dioxide, antimony precipitate and filter paper are dissolved in concentrated sulfuric acid together after filtration and can be directly usedfor reducing antimony after being carbonized by the concentrated sulfuric acid, loss caused in the ashing or precipitate redissolving process is avoided, and the detection accuracy and precision aregreatly improved.

Description

technical field [0001] The invention relates to the technical field of chemical analysis after metal smelting, in particular to a method for determining antimony in crude lead by precipitation separation-carbon reduction cerium sulfate volumetric method. Background technique [0002] The separation and enrichment methods of antimony mainly include precipitation method, extraction method, ion exchange method and distillation method, among which the most commonly used method is precipitation method and extraction method. [0003] (1) Precipitation method: [0004] In 1-2mol / L sulfuric acid solution or 0.5-1mol / L hydrochloric acid solution, antimony and S 2- Generate sulfide precipitates, separate from Al, Fe, Co, Ni, Mn(II), Zn, Ca, Mg, alkali metals and rare earths, etc., sulfide precipitates are soluble in excess alkali sulfide, and can be combined with Ag, Cu, Bi, Pb etc. separation. [0005] In the slightly acidic nitric acid or sulfuric acid solution containing Mn(II),...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 齐白羽王丁路军兵刘静静卢昌祥金龙王卓侯雪杨卓融张文强赵坤邓永怀赵中源
Owner NORTHWEST RES INST OF MINING & METALLURGY INST
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