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Chemical analysis method for determining nickel in nickel catalyst by changing complex anions

A technology of nickel catalyst and anion, applied in the field of chemical analysis, can solve the problems of inconspicuous end point phenomenon, tailing of titration end point, difficult to grasp, etc., and achieve the effect of stable, accurate and reliable titration results, obvious sudden changes, and sharp changes

Pending Publication Date: 2020-03-24
NORTHWEST RES INST OF MINING & METALLURGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The titration of high-content nickel already has a national analysis standard for nickel in nickel concentrate. This method uses hydrochloric acid to dissolve the precipitation of dimethylglyoxime nickel. Since this method does not destroy the chemical structure of dimethylglyoxime in the solution, it will lead to subsequent EDTA During the titration process, the end point of the titration is tailed, and the end point phenomenon is not obvious, so the error is relatively large. Many chemical analysis practitioners said that this method is difficult to master

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Accurately weigh 0.4000g of nickel standard sample in a 30mL corundum crucible, cover the top and bottom with 3g of sodium peroxide (burn carbon in advance if there is carbon), put it into a muffle furnace, raise from low temperature to 680°C, and melt for 20 minutes , take out and cool;

[0023] (2) Put the crucible cooled in (1) into a 1# 300mL beaker and add 100mL distilled water to heat and leach the melt. After the melt is completely leached, boil for 5 minutes to decompose the peroxide, take it out and cool it. Filter with fast filter paper, wash the precipitate and the beaker with 1% sodium hydroxide solution 5 times each, and discard the filtrate.

[0024] (3) Put the precipitate filtered in (2) together with the filter paper into the 1# original beaker, add 25mL of concentrated nitric acid, 15mL of 1:1 dilute sulfuric acid to nitrate the precipitate, steam until wet salt, add 5mL of concentrated hydrochloric acid, rinse Water to about 50mL, heat to dissolv...

Embodiment 2

[0031] (1) Accurately weigh 0.2000g of nickel catalyst sample into a 30mL corundum crucible, cover the top and bottom with 2g of sodium peroxide (if there is carbon, burn the carbon in advance), put it into the muffle furnace, raise it from low temperature to 680°C, and melt for 20 minutes , take out and cool;

[0032] (2) Put the crucible cooled in (1) into a 1# 300mL beaker and add 100mL distilled water to heat and leach the melt. After the melt is completely leached, boil for 5 minutes to decompose the peroxide, take it out and cool it. Filter with fast filter paper, wash the precipitate and the beaker with 1% sodium hydroxide solution 5 times each, and discard the filtrate.

[0033] (3) Put the precipitate filtered in (2) together with the filter paper into the 1# original beaker, add 25mL of concentrated nitric acid, 15mL of 1:1 dilute sulfuric acid to nitrate the precipitate, steam until wet salt, add 5mL of concentrated hydrochloric acid, rinse Water to about 50mL, hea...

Embodiment 3

[0040] (1) Accurately pipette an appropriate amount (see Table 3 for the pipetted volume) of a nickel-copper electrolyte in a 300mL beaker, flush to about 100mL, add 4g ammonium citrate, 4g ammonium chloride and boil for 5min, adjust the solution with concentrated ammonia water PH to 8-9, add 20mL of 1% dimethylglyoxime solution, incubate at 75°C for 40min, filter with medium-speed filter paper, wash the beaker and precipitate with ammonia-ammonium chloride solution 4 times, discard the filtrate.

[0041] (2) Put the precipitate filtered in (1) together with the filter paper into the original beaker, add 25mL of concentrated nitric acid, 15mL of 1:1 dilute sulfuric acid to nitrate the precipitate, and after the sulfuric acid smoke is exhausted, add 10mL of concentrated hydrochloric acid and heat to dissolve Salt and steamed at low temperature until wet salt, so repeated twice.

[0042] (3) Add 50mL of distilled water to the sample that was steamed twice in (2) to a wet salt st...

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Abstract

The invention provides a chemical analysis method for determining nickel in a nickel catalyst by changing complex anions, which comprises the following steps: digesting nickel dimethylglyoxime precipitate and filter paper by using nitric-sulfuric acid mixture, and respectively carrying out complex anion conversion treatment on salts twice by using 10mL of concentrated hydrochloric acid after sulfuric acid smoke is exhausted; dissolving salts with distilled water, adjusting the pH value with ammonia water, taking ammonium urinate as an indicator, and titrating with EDTA (Ethylene Diamine Tetraacetic Acid). The method has the advantages that the end point color is obviously protruded, the operation is simple, the speed is high, and the accuracy is high.

Description

technical field [0001] The invention belongs to the field of chemical analysis and relates to a method for determining nickel with a nickel catalyst. Background technique [0002] Nickel is a silver-white metal with magnetism, good plasticity and good corrosion resistance. Nickel A silvery-white, hard, malleable, ferromagnetic metallic element that is highly polishable and corrosion-resistant. Mainly used in alloys (such as nickel steel and nickel silver) and as catalysts (such as Raney nickel, especially for hydrogenation catalysts). [0003] According to literature review, there are many analytical methods for nickel in ores, beneficiation materials, and metallurgical materials, and there are relevant national standards; there are few chemical analysis and testing methods for nickel in nickel catalysts; the current nickel analysis and testing methods mainly include titration. method, gravimetric method, absorbance photometry, etc.; the separation and enrichment method of...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N1/28
CPCG01N31/16G01N1/28
Inventor 张彦翠路军兵郑省政王红燕展之旺王源瑞杨扬鹿伟
Owner NORTHWEST RES INST OF MINING & METALLURGY INST
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