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Analytical method and determination method of oxalate ion content in vanadyl oxalate

A technology for the content of oxalic acid and ions in vanadyl oxalate, applied in the field of analysis and detection, can solve the problems of many reaction control conditions, high labor intensity, long inspection period, etc., and achieve the effects of excellent performance indicators, low labor consumption, and improved detection ability.

Active Publication Date: 2018-05-01
PANGANG GROUP RESEARCH INSTITUTE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be clearly seen that this type of determination method has many complicated steps, many reaction control conditions, a long test cycle, high labor intensity and low efficiency, especially multiple precipitation separations and aging reactions consume a lot of time, and the entire detection process usually takes about 8 hours. Hour

Method used

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  • Analytical method and determination method of oxalate ion content in vanadyl oxalate
  • Analytical method and determination method of oxalate ion content in vanadyl oxalate
  • Analytical method and determination method of oxalate ion content in vanadyl oxalate

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Experimental program
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Effect test

Embodiment 1

[0029] Weigh 0.5g of vanadyl oxalate sample (Sample No. 1), add 30mL of 1:4 dilute hydrochloric acid solution and heat to dissolve the sample until it is completely dissolved. After cooling, dilute with water and dilute to volume in a 100mL volumetric flask. The ICP-OES detection parameters were set as follows: RF power 1350W, auxiliary gas flow rate 1.0L / min, peristaltic pump speed 65r / min, observation height 11.2mm, atomizer pressure 0.18MPa, measurement integration time 20s. In order to ensure the reliability of the results, avoid spectral interference between elements and the sensitivity is suitable for the content in the sample, the elemental analysis line: C 194.488nm.

[0030] Use one of the above-mentioned oxalate ion determination methods for determination. That is to say, ammonium oxalate is used to prepare a series of oxalate ion standard solutions with a concentration gradient. The concentration of the oxalate ion standard solution is used as the abscissa, and the ...

Embodiment 2

[0032] Except the following difference, all the others adopt the method identical with embodiment 1 to measure the vanadyl oxalate sample of embodiment 2: the vanadyl oxalate sample (No. 2 sample) weighs 1.0 g, dilutes constant volume 200mL.

Embodiment 3

[0034] Except the following differences, all the others adopt the same method as in Example 1 to measure the vanadyl oxalate sample of embodiment 3: the vanadyl oxalate sample (No. 3 sample) weighs 0.8g, adds dilute hydrochloric acid heating to dissolve the sample After completion, continue to boil the solution and keep it for 5 minutes, dilute to a constant volume of 100mL; draw a calibration curve with an oxalate ion standard solution prepared with high-grade pure oxalic acid.

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Abstract

The invention relates to an analysis method and a determination method for the content of oxalate ions in vanadyl oxalate, belonging to the field of analysis and detection. The invention discloses that a dilute hydrochloric acid solution dissolves a vanadyl oxalate sample and dilutes it to a constant volume with water, and prepares a series of standard solutions of oxalate ion in a concentration gradient by using superior-grade pure ammonium oxalate or oxalic acid and other reagents containing oxalate, or using carbonic acid Sodium carbonate or other inorganic carbon-containing compounds prepare a series of carbon standard solutions with a concentration gradient. The concentration of oxalate ions or carbon standard solutions is used as the abscissa, and through inductively coupled plasma atomic emission spectroscopy (ICP-OES) ) Directly measure the signal intensity of the carbon element in the vanadyl oxalate sample solution to draw a calibration curve for the ordinate, and directly or indirectly obtain the detection and analysis method for the content of the oxalate ion compound. The method disclosed by the invention has high precision and accuracy, and can quickly and effectively measure the content of oxalate ions in vanadyl oxalate samples.

Description

technical field [0001] The invention relates to an analysis method and a determination method for the content of oxalate ions in vanadyl oxalate, belonging to the field of analysis and detection. Background technique [0002] Vanadyl oxalate is widely used in the industrial field. It is mostly used in the synthesis of organic chemical products, as a chemical reagent and in the preparation of high-purity vanadium compounds, nanomaterials, glazes, electroplating materials and high-energy battery materials. Lithium vanadium phosphate Wait. At present, the purity and quality of vanadyl oxalate products are mainly evaluated according to the molar ratio of vanadium (IV) to oxalate, and the content of impurity elements in the product, that is, the content of oxalate ion is the key to judge the quality of vanadyl oxalate products. A key technical performance indicator. Therefore, the analysis and detection method for determining the oxalate ion content in the vanadyl oxalate sampl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/71
Inventor 成勇杨新能袁金红
Owner PANGANG GROUP RESEARCH INSTITUTE CO LTD
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