Quantitative analysis method of vanadium in high chrome alloy
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A high-chromium alloy, quantitative analysis technology, applied in the field of analytical chemistry, can solve problems such as operational hazards, interference with vanadium determination, corrosion of corundum crucibles, etc., and achieve the effects of expanding the scope of application, simple operation, and easy mastery
Inactive Publication Date: 2009-04-22
PANZHIHUA UNIV
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Problems solved by technology
It is relatively easier to use sodium peroxide alkali fusion and re-acidification method than acid-dissolved slag, refer to the national standard GB / T 7315.1-1987 and the industry standard YB / T 547.1-1995 ferrous ammonium sulfate titration method for the determination of vanadium pentoxide But in the actual analysis, there are two problems: one, in the process of using sodium peroxide alkali fusion, the sample is prone to explosion, and the corrosion of the corundum crucible is very serious. It is often necessary to repeatedly melt the sample several times for one detection, and it takes several Crucible, and because it is easy to explode, the operation is very dangerous; 2. In the operation of using ferrous ammonium sulfate titration method to determine vanadium, potassium permanganate is used to oxidize vanadium, and part of chromium is also oxidized at the same time, which interferes with the determination of vanadium and affects the accuracy of determination. Due to the very similar properties of vanadium and chromium, it is difficult to separate vanadium and chromium
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Embodiment 1
[0027] The mensuration of vanadium (V%) in the hydrogen storage alloy of embodiment 1
[0028] Preparation of mixed acid: sulfuric acid: nitric acid: hydrochloric acid: water = 5: 2.5: 5: 12.5
[0029] Mix 100 mL of sulfuric acid (1+1), 50 mL of nitric acid (1+1), and 100 mL of hydrochloric acid (1+1).
[0030] Three hydrogen storage alloy samples: 1#, 2#, and 3# samples have chromium contents of 21.22%, 21.98%, and 12.95%, respectively.
[0031] Take 0.1000g of 1#, 2#, and 3# samples respectively. Use 25ml of the prepared mixed acid solution to dissolve the high vanadium chromium alloy. Then use 10mL ferrous ammonium sulfate solution with a concentration of 100g / L to reduce and place for 5min, then add potassium permanganate solution with a concentration of 20g / L to oxidize for 3-5min, until the solution turns red and then add 2 drops; add urea, and use sodium nitrite For reduction, add 10ml of ethanol masking agent and let it stand for 1 to 2 minutes, add 3 drops of 2g / L ...
Embodiment 2
[0038] Embodiment 2: the analysis of vanadium content in the iron vanadium standard sample, investigate the interference of chromium to vanadium determination
[0039] A sample similar to the hydrogen storage alloy was prepared by adding the corresponding chromium standard solution to the iron-vanadium standard sample, and analyzed in the manner of Example 1, and carried out a control test with and without adding ethanol. The results are shown in Table 2.
[0040] Analysis results of vanadium (V%) in the standard sample of vanadium iron in table 2:
[0041]
[0042] It can be seen from Table 2 that chromium interferes with the determination of vanadium to a certain extent. After adding ethanol, the measurement results are in good agreement with the standard value, indicating that the interference can be eliminated.
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Abstract
The invention relates to a method used for quantitative analysis on vanadium in high-chromium alloy, in particular to the method used for the quantitative analysis on vanadium in hydrogen storage alloy, belonging to the analytical chemistry field. The technical problem to be solved is that the interference of vanadium is eliminated and the content of the vanadium in the high-chromium alloy is exactly and quantitatively analyzed. The analysis method adopts solution mixed by sulfuric acid, nitric acid and hydrochloric acid to dissolve the high-chromium alloy, then takes ethanol as a masking agent and uses ammonium ferrous sulfate to carry out titration analysis on the content of the vanadium; wherein, the proportion of the mixed solution of sulfuric acid, nitric acid, hydrochloric acid and water is 4-6:2-3:4-6:10-15. The analysis method has simple and convenient operation, is easy to be handled, eliminates the chromium interference, enlarges the applicable range of the existing method used for measuring the content of vanadium by the ammonium ferrous sulfate volumetric method, and provides a new method for quantitatively analyzing the content of the vanadium in the high-chromium alloy, especially in the hydrogen storage alloy.
Description
technical field [0001] The invention relates to a quantitative analysis method for vanadium in high-chromium alloys, in particular to a quantitative analysis method for vanadium in hydrogen storage alloys, and belongs to the field of analytical chemistry. technical background [0002] For quantitative analysis of samples with high chromium and high vanadium content, sodium peroxide alkali fusion is generally used to decompose the sample, or acid-dissolved slag is used, and the operation is relatively cumbersome [Analysis method of copper in high chromium ore, "Ferrous Metals" 2004 November, 2004. Vol. 56. No. 4; Determination of calcium oxide and magnesium oxide in chrome ore by neutral separation of lead salts - EDTA titration. "Metallurgical Analysis". June 2004. Vol. 24. No. 3]. It is relatively easier to use sodium peroxide alkali fusion and re-acidification method than acid-dissolved slag, refer to the national standard GB / T 7315.1-1987 and the industry standard YB / T 54...
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