Method for determining content of elemental mercury in metavanadate, and preparation method for sample solution

A metavanadate, sample solution technology, applied in the preparation of test samples, thermal excitation analysis, material excitation analysis and other directions, can solve the problems such as not seen, achieve less reagent consumption, low blank, low detection limit Effect

Inactive Publication Date: 2016-08-10
PANGANG GROUP RESEARCH INSTITUTE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there is no use of ICP-MS for the determination of 10 in metavanadates such as ammonium metavanadate, potassium m

Method used

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  • Method for determining content of elemental mercury in metavanadate, and preparation method for sample solution
  • Method for determining content of elemental mercury in metavanadate, and preparation method for sample solution

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0043] Example 1

[0044] Digestion of ammonium metavanadate sample

[0045] Weigh 0.2000g sample of ammonium metavanadate sample (hereinafter referred to as sample No. 1) in an Erlenmeyer flask, add 12mL of water to rinse the bottle wall, disperse the sample, and accelerate the dissolution of the sample by shaking or shaking at room temperature; then Add 6 mL of nitric acid and 6 mL of hydrogen peroxide to the solution, heat the metavanadate solution to 65°C by placing it on a low-temperature electric hot plate or indirectly heating it in a hot water bath, and keep it at this temperature for 3 minutes. After the digestion test solution is cooled to room temperature, it is diluted with water to a constant volume in a 100mL volumetric flask and mixed.

[0046] Determination of mercury element content in ammonium metavanadate sample solution by ICP-MS

[0047] Inductively coupled plasma mass spectrometry (ICP-MS) is used as the detection method, and the sample solution prepared by di...

Example Embodiment

[0050] Example 2

[0051] The sample to be digested is 0.1000g potassium metavanadate sample (hereinafter referred to as sample No. 2), the amount of water is 6mL, the amount of concentrated nitric acid is 3mL, the amount of hydrogen peroxide is 3mL, the temperature and time of the solution heating reaction are respectively 60℃ and 2min, the final dilution volume is 50mL, and the concentration of the rhodium Rh internal standard calibration standard solution used is 1ng / mL.

[0052] Otherwise, the potassium metavanadate sample was digested in the same way as the method of Example 1, and the solution was detected by ICP-MS.

Example Embodiment

[0053] Example 3

[0054] The sample to be digested is 0.1500g sodium metavanadate sample (hereinafter referred to as sample No. 3), the amount of water is 9mL, the amount of concentrated nitric acid is 4.5mL, the amount of hydrogen peroxide is 4.5mL, the temperature and time of the solution heating reaction Respectively 63℃ and 2.5min, the final dilution volume is 100mL, and the concentration of the rhodium Rh internal standard calibration standard solution used is 3ng / mL.

[0055] Otherwise, the sodium metavanadate sample was digested according to the same method as in Example 1, and the solution was detected by ICP-MS.

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Abstract

The invention relates to a method for determining the content of elemental mercury in metavanadate and a preparation method for a sample solution, belonging to the technical field of element detection. To overcome a technical problem, the invention provides the preparation method for the sample solution used for determination of the content of elemental mercury in metavanadate. The preparation method comprises the following successive steps: dissolving a metavanadate sample with water; adding nitric acid and hydrogen peroxide and carrying out heating to 60 to 65 DEG C for digestion; and after completion of digestion, carrying out cooling to room temperature and then carrying out diluting with water until a volume is fixed so as to obtain a sample detection solution. According to the invention, an ICP-MS determination method is established for determination of the trace impurity element mercury with a content in a range of 0.0001 to 0.1000% in metavanadate, and performance indexes of the method are that quantitative determination lower limit is 0.0001%, the degree of precision is less than 10% and a recovery rate is 80 to 120%. The determination method has the characteristics of easy and fast operation, short analysis time, small usage amount of reagents, low blank, few influence factors, low detection lower limit, high precision, high accuracy, etc.

Description

technical field [0001] The invention relates to a method for measuring mercury element content in metavanadate and a sample solution preparation method, belonging to the technical field of element detection. Background technique [0002] Ammonium metavanadate, potassium metavanadate, sodium metavanadate and other metavanadate products with alkali metals, alkaline earth metals or ammonium ions as cationic components are not only intermediate products in the vanadium extraction process, but also mainly used in It is used to prepare vanadium pentoxide or metal vanadium, and then produce vanadium-iron, vanadium-aluminum, vanadium-titanium-aluminum, vanadium-nitrogen and other vanadium-based alloy materials; at the same time, metavanadate is also a chemical reagent, catalyst, and drier , mordant and ceramic industry glaze and other widely used vanadium fine chemicals. Since the content of impurity elements not only affects the grade of the product, but also seriously affects the...

Claims

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Application Information

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IPC IPC(8): G01N1/44G01N1/38G01N21/73
CPCG01N1/38G01N1/44G01N21/73
Inventor 成勇
Owner PANGANG GROUP RESEARCH INSTITUTE CO LTD
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