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Method for determining content of vanadium

A content and mass percentage technology, applied in the direction of material excitation analysis, thermal excitation analysis, etc., can solve the problems of long detection cycle, slow analysis speed, and high technical quality requirements of operators

Active Publication Date: 2013-04-17
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, according to the determination method of vanadium content in the prior art, the technical quality of the operator is high, and the analysis speed is slow, and the detection cycle is long.

Method used

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  • Method for determining content of vanadium

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Experimental program
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Embodiment 1

[0026] In an embodiment of the present invention, the ICP-OES is an iCAP6300 inductively coupled plasma atomic emission spectrometer from Thermo Fisher Corporation of the United States.

[0027] 1. Sodium metavanadate sample digestion preparation

[0028] Weigh 0.1g of sodium metavanadate sample into a container, first wash the container wall with 10mL of water and shake to suspend and disperse the sample, add 3mL of concentrated hydrochloric acid with a mass percentage concentration of 36% to 38%, and heat the reaction until the sample is completely digested , keep the solution boiling for 2 minutes, then cool the solution to room temperature, dilute with water to a 200mL volumetric flask, and mix well.

[0029] 2. Calibration curve series standard solutions

[0030] The standard curve series standard solution only digests high-purity vanadium pentoxide (V 2 o 5 >99.99%), composed of vanadium standard solution at 8 concentration gradient points, the content of vanadium con...

Embodiment 2

[0036] Except following difference, all the other adopt the same method as embodiment 1 to measure the sodium metavanadate sample of embodiment 2: sodium metavanadate sample takes 0.2g, and 25mL water rinses and disperses sample, concentrated hydrochloric acid consumption 10mL, keep boiling for 3 minutes, dilute and constant volume 500mL volumetric flask; the calibration curve is composed of vanadium standard solution at 8 concentration gradient points, and the vanadium element content contained in the standard solution corresponds to the mass percentage of vanadium in the sample to be tested as follows: 10.0%, 30.0%, 35.0%, 40.0%, 41.0%, 42.0%, 43.0%, 45.0%. The working parameters of the ICP spectrometer are RF power 1200W, peristaltic pump speed 60r / min, observation height 12.5mm, atomizer pressure 0.24MPa, and measurement integration time 15s.

Embodiment 3

[0038] Except following difference, all the other adopt the same method as embodiment 1 to measure the sodium metavanadate sample of embodiment 3: sodium metavanadate sample takes by weighing 0.15g, and 20mL water rinses and disperses sample, concentrated hydrochloric acid consumption 7mL, keep boiling for 2 minutes, dilute and constant volume 250mL volumetric flask; the calibration curve is composed of vanadium standard solution at 7 concentration gradient points, and the vanadium element content contained in the standard solution corresponds to the mass percentage of vanadium in the sample to be tested as follows: 10.0%, 20.0%, 40.0%, 41.0%, 42.0%, 43.0%, 45.0%. The working parameters of the ICP spectrometer are RF power 1100W, peristaltic pump speed 50r / min, observation height 12.0mm, atomizer pressure 0.21MPa, and measurement integration time 12s.

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Abstract

The invention provides a method for determining content of vanadium. The method for determining content of vanadium comprises the following steps: digesting a vanadium-containing sample with hydrochloric acid to obtain a vanadium-containing solution, and determining the content of vanadium in the vanadium-containing solution using an inductively coupled plasma atomic emission spectrometer. According to the method, the content of vanadium in sodium metavanadate can be determined fast and accurately.

Description

technical field [0001] This application relates to a method for determining vanadium content, more specifically, this application relates to a method for determining the concentration range of sodium metavanadate, ammonium metavanadate, potassium metavanadate, etc., which can reach 10wt%-45wt% The method of the content of vanadium element. Background technique [0002] Sodium metavanadate (chemical formula NaVO 3 or VNaO 3 ) is an important vanadium fine chemical product, which can be mainly used as chemical reagent, catalyst, drier, mordant, etc. Basic raw materials, among which, the content of vanadium element is a key technical index to measure the quality level of products. [0003] At present, the mainstream technology for the determination of high-concentration vanadium is the redox titration method in the traditional chemical analysis method. The ferrous ammonium sulfate titration method is a classic method for the determination of vanadium content. Products conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/71
Inventor 成勇彭慧仙李千文彭一村袁金红吴刘柱胡金荣
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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