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Method for eliminating error when measuring vanadium by ferrous ammonium sulfate capacitance method

A ferrous ammonium sulfate, volumetric method, applied in chemical analysis by titration, material analysis by observing the effect of chemical indicators, and analysis by chemical reaction of materials, etc., can solve mistakes, rework, Burette overflow titration and other problems, to achieve the effect of expanding the scope of adaptation, reducing the rework rate, and making up for mistakes

Inactive Publication Date: 2010-01-13
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the existing national standard, only a fixed concentration of ferrous ammonium sulfate standard solution can be applied to each specific sample, and it cannot be applied to steel slag, electric furnace slag, corundum slag, desulfurization slag, slag samples of unknown origin or various raw materials, Analysis and Determination of Vanadium in Alloy
[0003] In actual production, the components of the samples to be tested are usually very complex, especially for the raw materials, intermediate products and products prepared according to the special needs of some scientific research projects, it is difficult to accurately predict the vanadium content in the samples to be tested range, so it is difficult to accurately select the appropriate concentration of ferrous ammonium sulfate standard solution for redox titration
Therefore, in the titration process, it is very easy to cause excessive titration endpoints, the concentration of the selected ferrous ammonium sulfate solution does not match the vanadium content, resulting in too much standard solution before reaching the endpoint, or the titration caused by misjudgment of the titration endpoint, burette overflow, etc. mistake
The above-mentioned mistakes occur from time to time in the actual measurement of production inspection, resulting in frequent rework and wasting a lot of manpower and material resources
[0004] Therefore, according to the existing standard methods (GB6730.32-86: Determination of vanadium in iron ore, sinter, and pellets; GB223.13-89: Determination of vanadium in steel and alloys; GB7315.1-87: Determination of vanadium in vanadium oxide; YB / T547.1-1995: Determination of vanadium in vanadium slag) to detect the content of vanadium in the sample, which cannot well meet the needs of actual production

Method used

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  • Method for eliminating error when measuring vanadium by ferrous ammonium sulfate capacitance method
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  • Method for eliminating error when measuring vanadium by ferrous ammonium sulfate capacitance method

Examples

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Embodiment 1

[0016] Example 1 Titration Excessive Mistake Remedial Method

[0017] Two standard samples of converter slag were used for titration operation, and the same sample was subjected to two parallel titrations respectively. The results obtained are shown in Table 1. The standard value is the value given on the standard sample of converter slag.

[0018] Table 1

[0019]

[0020] When there are operational errors such as excessive titration of the solution to be tested, mismatch between the selected ferrous ammonium sulfate concentration and the vanadium content, burette overflow, etc., use 20g / L potassium permanganate solution to adjust the solution to be tested to have a stable dimanganese When manganese precipitate appears, let it stand for 3 minutes; add 0.8 g of urea, adjust it with 20g / L sodium nitrite solution until the manganese dioxide precipitate disappears, add 1-2 drops in excess, let stand for 2 minutes; then add 2g / L N-phenyl-o-amino Benzoic acid is an indicator, a...

Embodiment 2

[0024] Embodiment 2 is beyond the titration method of national standard measuring range sample

[0025] The national standard (GS / T8704.5-94) method uses the potentiometric titration method for the determination of vanadium in ferrovanadium. If the vanadium in ferrovanadium or vanadium nitride is determined by the ferrous ammonium sulfate volumetric method, it is very difficult to It is difficult to judge the concentration range that the standard solution should be selected, so it is usually wrong to choose, which is time-consuming and inaccurate. In this case, take the following remedial measures to ensure the accuracy of the results.

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Abstract

The invention relates to a remedy method for the mistakes in vanadium content determination with ammonium ferrous sulfate volumetric analysis, which comprises the following steps: the vanadium in the solution to be test that is over-titrated or is titrated insufficiently is oxidized to be V5+ with potassium permanganate, while the chromium in the solution is not oxidized; the excessive potassium permanganate is deoxidized with sodium nitrite with the existence of urea; meanwhile, the excessive sodium nitrite is also decomposed with the existence of urea, thus the interference of excessive sodium nitrite to titration is eliminated; then n-phenylanthranilic acid is used as indicator and the vanadium is re-titrated with ammonium ferrous sulfate standard solution. The invention corrects the titration mistakes in vanadium content analysis operation, wherein, the mistakes results from the concentration of the chosen ammonium ferrous sulfate titrating solution does not matched with the vanadium content in the sample, or titration end-point is judged inaccurately, or other reasons. Compared with the prior international standard, the invention has the advantages of enlarged determination range, reduced reworking rate in operation, and better service for scientific research and production. The invention is suitable for vanadium content determination in sample of total vanadium content more than 1.00% and chromium content less than 1.00%.

Description

Technical field [0001] The present invention relates to a method for measuring vanadium content by volumetric method, and in particular, to a method for eliminating errors in measuring vanadium content by volumetric method. Background technique [0002] At present, the ferrous ammonium sulfate volumetric method is generally used to determine the vanadium content in samples such as iron ore, sinter, pellets, vanadium slag, and vanadium pentoxide. However, in the existing national standards, only a fixed concentration of ferrous ammonium sulfate standard solution can be applied to each specific sample, and it cannot be applied to steel slag, electric furnace slag, corundum slag, desulfurization slag, slag samples from unknown sources or various raw materials, Analytical determination of vanadium in alloys. [0003] In actual production, the components of the sample to be tested are usually very complex, especially the raw materials, intermediates and products prepared accordi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/16G01N21/83
Inventor 冯向琴
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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