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Method for detecting vanadium valence in vanadium oxide

A detection method, vanadium oxide technology, applied in the direction of measuring devices, test sample preparation, instruments, etc., can solve the problems of inaccurate detection results, complicated operation, etc., and achieve high dissolution efficiency, simple operation, and no particle size effect Effect

Inactive Publication Date: 2018-06-12
四川星明能源环保科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to provide a method for detecting the valence state of vanadium in vanadium oxide, aiming to improve the problems of complicated operation and inaccurate detection results when detecting the valence state of vanadium in vanadium oxide

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  • Method for detecting vanadium valence in vanadium oxide

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Embodiment 1

[0026] A method for detecting the valence state of vanadium in vanadium oxide provided in this embodiment, a method for detecting the valence state of vanadium in vanadium oxide, comprising:

[0027] After mixing the analyte and the solvent, use the high-pressure microwave digestion method to isolate the air and dissolve to obtain the sample solution; microwave heating for 15 minutes.

[0028] Next, the starch was compressed under a pressure of 300 MPa. Wherein, the weight ratio of the analyte to the starch is 0.1:2.

[0029] Next, drop 450 μL of the sample solution onto a filter paper with a diameter of 24 mm, and dry it at 40° C.

[0030] Put the filter paper in the center of the base holder, and press it with a pressure of 300MPa to form a 250-mesh sample to be tested.

[0031] Finally, the samples to be tested were measured by XRF. Excited under the conditions of voltage 40kV and current 40mA, the instrument uses a 28mm aperture.

Embodiment 2

[0033] A method for detecting the valence state of vanadium in vanadium oxide provided in this embodiment, a method for detecting the valence state of vanadium in vanadium oxide, comprising:

[0034] After mixing the analyte and the solvent, use the high-pressure microwave digestion method to isolate the air and dissolve to obtain the sample solution; microwave heating for 20min.

[0035] Next, the starch was compressed under a pressure of 500 MPa. Wherein, the weight ratio of the analyte to the starch is 0.8:10.

[0036] Next, drop 600 μL of the sample solution onto a filter paper with a diameter of 24 mm, and dry it at 60° C.

[0037] Put the filter paper in the center of the base holder, and press it with a pressure of 450MPa to form a 350-mesh sample to be tested.

[0038] Finally, the samples to be tested were measured by XRF. Excited under the conditions of voltage 55kV and current 60mA, the instrument uses a 30mm aperture.

Embodiment 3

[0040] A method for detecting the valence state of vanadium in vanadium oxide provided in this embodiment, a method for detecting the valence state of vanadium in vanadium oxide, comprising:

[0041] After mixing the analyte and the solvent, use the high-pressure microwave digestion method to isolate the air and dissolve to obtain the sample solution; microwave heating for 15 minutes.

[0042] Next, the starch was pressed under a pressure of 4 MPa. Wherein, the weight ratio of the analyte to the starch is 0.2:3.

[0043] Next, drop 280 μL of the sample solution onto a filter paper with a diameter of 24 mm, and dry it at 40-60° C.

[0044] Put the filter paper in the center of the bottom holder, and press it with a pressure of 420MPa to form a 320-mesh sample to be tested.

[0045]Finally, the samples to be tested were measured by XRF. Excited under the conditions of voltage 48kV and current 58mA, the instrument uses a 29mm aperture.

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Abstract

The invention provides a method for detecting vanadium valence in vanadium oxide and relates to the field of element detection. The method includes: using a high-pressure microwave digestion method todissolve a to-be-detected object in an air isolated manner to obtain a sample solution; pressing starch under the pressure of 300-500MPa, and acquiring a bottom surface after forming and demoulding,wherein the weight ratio of the to-be-detected object to the starch is (0.1-0.8):(2-10); dropwise adding 450-600 microliter of sample solution to filter paper, and drying; placing the filter paper atthe center of the bottom support, pressing with pressure of 300-450MPa to obtain a to-be-measured sample, and measuring the to-be-measured sample with an X-ray fluorescent method. The method is capable of achieving even element distribution, free of granularity effects, free of risks of leakage and volatilization, simple to operate, fast, and accurate in detection result after X-ray fluorescent method measuring.

Description

technical field [0001] The invention relates to the field of element detection, and in particular to a method for detecting the valence state of vanadium in vanadium oxide. Background technique [0002] In many industrial production processes, vanadium plays an important role. In the steel industry and petrochemical industry, vanadium and its compounds have a wide range of uses. Vanadium has different valence states: trivalent, tetravalent and pentavalent. Trivalent and tetravalent vanadium can be easily oxidized to pentavalent. In the production process of vanadium pentoxide and vanadium trioxide, trivalent vanadium, tetravalent vanadium and pentavalent vanadium can be transformed into each other. Therefore for the vanadium oxide (V x o y ) The analysis of valence state vanadium in materials is particularly important. At present, the analysis of the valence state in vanadium oxide usually adopts chemical analysis method, such as volumetric method. The operation proces...

Claims

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Application Information

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IPC IPC(8): G01N23/223G01N1/28
CPCG01N23/2202G01N23/223
Inventor 廖继安王方文邱锦荣
Owner 四川星明能源环保科技有限公司
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