Method for clearing and detecting vanadic oxide

Abstract

The invention discloses a method for clearing and detecting vanadic oxide which includes steps as follows: taking vanadic oxide to a container, adding nitric acid to the container, processing pre-action under the normal temperature, then closing the container, processing microwave clearing. The detecting method includes steps as follows: using one or many methods of an inductively coupled plasma mass spectrometry, an inductively coupled plasma atomic emission spectrometry, a flame atomic absorption spectrometry and a graphite furnace atomic absorption spectrometry for analyzing the cleared vanadic oxide, accordingly, obtaining elementary content of vanadic oxide sample.

Description

technical field [0001] The present invention relates to a kind of vanadium pentoxide (V 2 o 5 ) digestion and detection method, more specifically, the present invention relates to a V 2 o 5 The method of microwave digestion and the method of detection by inductively coupled plasma mass spectrometry (ICP-MS). Background technique [0002] V 2 o 5 It is widely used in metallurgy, chemical industry, national defense and military industry and other technical fields. In recent years, V 2 o 5 The production industry is developing rapidly. Especially high-purity V with a purity of more than 99.5% 2 o 5 , because of its excellent performance and won the favor of users. [0003] In order to meet the high purity V 2 o 5 Technical development and improvement of production process, optimization of equipment operating parameters, control of the content of impurity elements in raw materials and products, so as to increase V 2 o 5 Grade and other requirements, there is an urg...

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Problems solved by technology

[0008] Specifically, at present, traditional chemical analysis methods such as national standards often use alkali fusion digestion at a high temperature of nearly 1,000 degrees. 2 o 5 approach, although able to convert V 2 o 5 The matrix and the impurity elements to be measured are completely digested, but various interference factors such as reagent blank, background influence, matrix effect, salt concentration, acidity, element loss and pollution, and mass spectrometry interference of polyatomic ions greatly exceed the capabilities of ICP-MS. range of tolerance

At present, ICP-AES mostly uses large doses of hydrochloric acid and nitric acid for a long time to heat and boil slowly to digest V 2 o 5 , but this kind of method also has many defects: ① Although many indicators are better than the alkali fusion method, it has not fully met the requirements of ICP-MS for low acid and low salt in the test solution. Cone, turbomolecular pump and other components are severely corroded, and the influence of matrix effect and blank background is increased; ②, during the long acid medium digestion process in an open system, impurity elements such as As, Hg, Cd, Pb are easily volatile and lost or contaminated, especially if Al 2 o 3 , SiO 2 Such impurity elements cannot be completely digested, seriously affecting the measurement results; ③, H 2 SO 4 It will have a great adverse effect on the determination of ICP-MS, so it is not suitable to detect elements such as Nb and Zr that need to be digested with sulfuric acid and can be stored stably in organic media such as citric acid; ④, ICP-MS has strict requirements on the digestion solvent. with H 2 SO 4 , HCl digestion V 2 o 5 The sample has increased mass spectrometry interference such as polyatomic ions, and it is not suitable for the determination of As, Ti, Cr, Zn, Cu and other elements, such as 40 Ar 35 Cl + interference 75 As + , 32 S 16 o 7 + interference 65 Zn + , 32 S 16 o + interference 48 Ti + , 32 S 16 o 2 h + interference 65 Cu + Wait

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