Method for clearing and detecting vanadic oxide

A vanadium pentoxide and detection method technology, which is applied in the detection field of plasma mass spectrometry, can solve problems such as component corrosion, influence on measurement results, pollution, etc., and achieve the effects of avoiding volatilization loss and pollution, high precision, and simple solution

Inactive Publication Date: 2009-09-16
PANGANG GROUP VANADIUM TITANIUM & RESOURCES +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

Method used

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  • Method for clearing and detecting vanadic oxide
  • Method for clearing and detecting vanadic oxide
  • Method for clearing and detecting vanadic oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The nitric acid, hydrofluoric acid and water used in this example are of ultra-pure grade, the microwave digestion system used is Mars5 produced by CEM Company of the United States, and the ICP-MS is an inductively coupled plasma mass spectrometer of Elan9000 of PE Company of the United States.

[0037] V 2 O 5 Sample digestion

[0038] Weigh 0.1000g of high-purity V with grade ≥99.999% 2 o 5 The sample (incoming product packaging) (hereinafter referred to as sample No. 1) is placed in the microwave digestion inner tank, and 3.0 mL of nitric acid with a concentration of 65% to 68% by mass is added dropwise along the tank wall, and placed at room temperature for 3 minutes , then add 0.2mL of hydrofluoric acid with a mass percentage concentration of 40% to 47%, 2.0mL of 500ng / mL Rh standard solution, and 2.0mL of 500ng / mL Sc standard solution into the inner tank, and wash the tank wall with about 4.0mL of water Then put the outer tank on, cover the lid and tigh...

Embodiment 2

[0051] V to be digested 2 o 5 The sample is 0.1000g grade ≥ 99.99% high-purity V 2 o 5 Sample (Shanghai Reagent No. 1 Factory) (hereinafter referred to as sample No. 2), using 3.0mL nitric acid, 0.5mL hydrofluoric acid, 2.5mL of 500ng / mL Rh standard solution and 2.5mL of 500ng / mL Sc standard solution, in addition Outside, digest V according to the same method as the method of Example 1 2 o 5 samples and tested.

Embodiment 3

[0053] V to be digested 2 o 5 The sample is 0.1000g grade ≥ 99.999% high-purity V 2 o 5 Sample (repacking of imported products) (hereinafter referred to as sample No. 3), using 3.0mL nitric acid, 0.3mL hydrofluoric acid, 2.0mL of 500ng / mL Rh standard solution and 2.0mL of 500ng / mL Sc standard solution, in addition Outside, digest V according to the same method as the method of Example 1 2 o 5 samples and tested.

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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...

Claims

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Application Information

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IPC IPC(8): G01N1/44G01N27/64G01N21/73G01N21/31
Inventor 成勇
Owner PANGANG GROUP VANADIUM TITANIUM & RESOURCES
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