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Analysis method for determining potassium in potassium metavanadate and/or sodium in sodium metavanadate

A technology of sodium metavanadate and potassium metavanadate, which is applied in the field of constant element detection and analysis, can solve the problem of not finding sodium metavanadate, etc., and achieve the effect of excellent technical performance indicators, fewer steps, and strong anti-interference ability

Active Publication Date: 2013-07-24
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, there is no detection and analysis method for measuring sodium content in sodium metavanadate in the prior art

Method used

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  • Analysis method for determining potassium in potassium metavanadate and/or sodium in sodium metavanadate
  • Analysis method for determining potassium in potassium metavanadate and/or sodium in sodium metavanadate
  • Analysis method for determining potassium in potassium metavanadate and/or sodium in sodium metavanadate

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Experimental program
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example 1

[0028] In the example of the present invention, the ICP-OES is an iCAP6300 Inductively Coupled Plasma Atomic Emission Spectrometer from Thermo Fisher Corporation of the United States.

[0029] 1. Sodium metavanadate sample digestion system

[0030] Weigh 0.2g of sodium metavanadate sample and place it in a polytetrafluoroethylene beaker or other container, first rinse the container wall with 25mL of water and shake to suspend and disperse the sample, then add 10mL of concentrated hydrochloric acid and heat the reaction until the sample is basically completely digested, then Add 2mL of concentrated nitric acid and continue the reaction until the solution boils to produce uniform large bubbles and keep it for 5 minutes. After cooling, transfer to a 500mL volumetric flask to dilute to volume and mix well;

[0031] 2. Calibration curve series standard solution

[0032] The standard curve series standard solution is composed of 7 concentration points: the mass percentage concentra...

example 2

[0039] Except the following differences, all the others adopt the same method as example 1 to measure the sodium metavanadate sample of example 2: the sodium metavanadate sample takes 0.1g, 10mL water rinses and disperses the sample, concentrated hydrochloric acid consumption 3mL, The amount of concentrated nitric acid is 1mL, and it is kept for 2 minutes; the working parameters of the ICP spectrometer are RF power 850W, peristaltic pump speed 65r / min, observation height 11.5mm, atomizing gas pressure 0.23MPa, measurement times 5 times, and the integration time of each measurement is 6s .

example 3

[0041] Except the following differences, all the others adopt the same method as example 1 to measure the sodium metavanadate sample of example 3: the sodium metavanadate sample takes 0.15g, 15mL water rinses and disperses the sample, concentrated hydrochloric acid consumption 6mL, The amount of concentrated nitric acid is 1.5mL, and it is kept for 4 minutes; the working parameters of the ICP spectrometer are RF power 800W, peristaltic pump speed 60r / min, observation height 11.3mm, atomizing gas pressure 0.25MPa, number of measurements 6 times, integration time for each measurement 7s.

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Abstract

The invention provides an analysis method for determining potassium in potassium metavanadate and / or sodium in sodium metavanadate. The method comprises the following steps of: counteracting potassium metavanadate and / or sodium metavanadate so as to form a solution to be tested; preparing multiple standard solutions with different concentration values, wherein the standard solutions contain potassium and / or sodium and do not contain vanadium; sequentially determining the multiple standard solutions in a sequence that the concentration values are from low to high by using an inductively coupled plasma atomic emission spectrometer, and then drawing a calibration working curve; and determining potassium and / or sodium in the solution to be tested by using the inductively coupled plasma atomic emission spectrometer, and calculating the potassium content of the potassium metavanadate and / or the sodium content of the sodium metavanadate in combination with the calibration working curve. The method disclosed by the invention has the advantages of wide application, wide concentration detection range, strong anti-jamming capability, less man-made factors, convenient and rapid operation, short process, less steps, and excellent technical performance indexes such as accuracy, precision and recovery rate, and the like.

Description

technical field [0001] The invention relates to the field of detection and analysis of constant elements. Specifically, the invention relates to a method capable of measuring potassium content in potassium metavanadate, measuring sodium content in sodium metavanadate, or simultaneously measuring potassium content and metavanadium in potassium metavanadate. Method for the analysis of sodium content in sodium bicarbonate. Background technique [0002] Sodium metavanadate (its chemical formula NaVO 3 or VNaO 3 , also known as sodium vanadate) and potassium metavanadate (its chemical formula KVO 3 or VKO 3 , also known as potassium vanadate) are two important vanadium fine chemical products, mainly used as chemical reagents, catalysts, drier, mordant, etc. Among them, sodium metavanadate is used to manufacture ammonium metavanadate and metavanadate Basic raw materials for fine chemical products such as potassium phosphate. [0003] At present, in the prior art, there is a m...

Claims

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Application Information

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IPC IPC(8): G01N21/73
Inventor 成勇彭慧仙李千文彭一村吴刘柱袁金红胡金荣
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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