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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 metavanadate and sodium metavanadate. -6 Literature Reports on Analytical Methods for Trace Mercury Detection at Concentration Levels

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
Effect test

Embodiment 1

[0044] Digestion of ammonium metavanadate samples

[0045] Take by weighing sample 0.2000g ammonium metavanadate sample (hereinafter referred to as No. 1 sample) in Erlenmeyer flask, add 12mL water to rinse bottle wall, disperse sample and accelerate dissolving sample by shaking or vibrating action under room temperature environment; Then in Add 6mL nitric acid and 6mL hydrogen peroxide to the solution, heat the metavanadate solution to 65°C by direct heating on a low-temperature electric heating plate or indirect heating in a hot water bath, and keep at this temperature for 3 minutes. After the digestion test solution is cooled to room temperature, dilute with water to volume and mix in a 100mL volumetric flask.

[0046] Determination of Mercury Content in Ammonium Metavanadate Sample Solution by ICP-MS

[0047] Inductively coupled plasma mass spectrometry (ICP-MS) was used as the detection method, and through the connection mode of the online internal standard mixer, the...

Embodiment 2

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

[0052] Besides, the potassium metavanadate sample was digested in the same manner as in Example 1 and the solution was detected by ICP-MS.

Embodiment 3

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

[0055] Besides, the sodium metavanadate sample was digested in the same manner 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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