CN103439330B - The detection method of vanadium pentafluoride product purity - Google Patents
The detection method of vanadium pentafluoride product purity Download PDFInfo
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Abstract
The invention discloses a kind of detection method of vanadium pentafluoride product purity, belong to the halide field of vanadium. Described detection method utilization is carried out content analysis to pentavalent vanadium in vanadium pentafluoride, realize the detection to vanadium pentafluoride purity by conversion, concrete steps comprise: (i) prepare sample, be wherein divided into and use corrosion-resistant material sampling bag sampling, acid solution absorbs, volumetric flask constant volume; (II) utilizes oxidimetry to measure pentavalent vanadium, and process formula calculates, thereby obtains the purity of vanadium pentafluoride product. The present invention is simple and easy to do, convenient operation, and certainty of measurement is high, is specially adapted to the detection of the vanadium pentafluoride product purity of preparing taking fluorine gas and elemental vanadium as raw material.
Description
Technical field
The invention belongs to the halide field of vanadium, be specifically related to a kind of vanadium pentafluoride product purityDetection method.
Background technology
Vanadium pentafluoride (VF5) is a kind of very strong fluorization agent and oxidant, is usually used in organic closingCheng Zhongzuo fluorization agent.
Not yet have at present about the bibliographical information of measuring vanadium pentafluoride purity analysis. Only have to measure and closeThe report of impurity content of vanadium in gold, as Spectrophotometric Determination of Vanadium amount, Atomic Absorption SpectrometryDetermine vanadium amount, but be all the report of measuring low content vanadium, have no be applicable to purity be greater than 95% fiveThe detection method of vanadium fluoride product.
Summary of the invention
The present invention proposes in order to overcome the shortcoming existing in prior art, its objective is and carriesFor a kind of detection that is applicable to prepare taking fluorine gas and elemental vanadium as raw material purity of antimony pentafluoride productsMethod, utilizes pentavalent vanadium in vanadium pentafluoride is carried out to content analysis, realizes five fluorine by conversionChange the detection of vanadium purity.
Technical scheme of the present invention is:
A detection method for vanadium pentafluoride product purity, comprises the following steps:
(i) prepare sample
Use corrosion-resistant material sampling bag to get 1g～10g vanadium pentafluoride liquid, in sampling bag, addEntering 10mL～60mL quality is the absorption liquid absorption of 5%～20% sulfuric acid solution than concentration, by moltenLiquid proceeds in volumetric flask, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations arrives250ml～1000ml, obtains sample hydrolyzate;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to measure pentavalent vanadium, pipette 10mL～100mL sampleProduct hydrolyzate, adding respectively quality is 98% sulfuric acid 5mL～20mL than concentration, mass ratio is denseDegree is phosphatase 11 mL～3mL of 85%, then adds the N-that 1mL quality is 0.2% than concentrationPhenylanthranilic acid indicator, with the titration of iron ammonium sulfate standard liquid, works as sample solutionBecome bright green from aubergine, and in 30 seconds when nondiscolouring, record uses iron ammonium sulfate markThe volume of accurate solution, calculates vanadium pentafluoride according to detecting data by following formula (1)Content:
In formula: c-iron ammonium sulfate concentration of standard solution, unit is mol/L; V3---titrationWhen test solution, consume the volume of iron ammonium sulfate standard liquid, unit is mL; V4---blankThe volume of the test iron ammonium sulfate standard liquid that consumes, unit is mL; γ---test solution divides to be gotRatio; The molal weight of M---vanadium pentafluoride, unit is g/moL; M---the sample takingWeight, unit is g;
The method of operating of described blank test is for pipetting and step (II) vanadium pentafluoride product purityThe deionized water of institute's sample thief hydrolyzate same volume in analysis, adds respectively and step (II)The sulfuric acid of same volume, equal in quality concentration in the analysis of vanadium pentafluoride product purity, phosphoric acid, benzeneBase ortho-aminobenzoic acid indicator, is titrated to solution by aubergine with iron ammonium sulfate standard liquidBecome bright green, record the volume of titration iron ammonium sulfate standard liquid used, be blank examinationTest the volume V of consumed iron ammonium sulfate standard liquid4。
The present invention is simple and easy to do, convenient operation, and certainty of measurement is high, be specially adapted to fluorine gas andElemental vanadium is the detection of the vanadium pentafluoride product purity prepared of raw material.
Detailed description of the invention
Below in conjunction with embodiment, the detection method of vanadium pentafluoride product purity of the present invention is carried out in detailDescribe in detail bright:
A detection method for vanadium pentafluoride product purity, comprises the following steps:
(i) prepare sample
Use corrosion-resistant material sampling bag to get 1g～10g vanadium pentafluoride liquid, in sampling bag, addEntering 10mL～60mL quality is the absorption liquid absorption of 5%～20% sulfuric acid solution than concentration, by moltenLiquid proceeds in volumetric flask, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations arrives250ml～1000ml, obtains sample hydrolyzate;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to measure pentavalent vanadium, pipette 10mL～100mL sampleProduct hydrolyzate, adding respectively quality is 98% sulfuric acid 5mL～20mL than concentration, mass ratio is denseDegree is phosphatase 11 mL～3mL of 85%, then adds the N-that 1mL quality is 0.2% than concentrationPhenylanthranilic acid indicator, with the titration of iron ammonium sulfate standard liquid, works as sample solutionBecome bright green from aubergine, and in 30 seconds when nondiscolouring, record uses iron ammonium sulfate markThe volume of accurate solution, calculates vanadium pentafluoride according to detecting data by following formula (1)Content:
In formula: c-iron ammonium sulfate concentration of standard solution, unit is mol/L; V3---titrationWhen test solution, consume the volume of iron ammonium sulfate standard liquid, unit is mL; V4---blankThe volume of the test iron ammonium sulfate standard liquid that consumes, unit is mL; γ---test solution divides to be gotRatio; The molal weight of M---vanadium pentafluoride, unit is g/moL; M---the sample takingWeight, unit is g.
Blank test: pipette with step (II) vanadium pentafluoride product purity analyze in institute's sample thiefThe deionized water of hydrolyzate same volume, adds respectively with step (II) vanadium pentafluoride product pureThe sulfuric acid of same volume, equal in quality concentration in degree analysis, phosphoric acid, phenylanthranilic acidIndicator, is titrated to solution with iron ammonium sulfate standard liquid and becomes bright green from aubergine, noteThe volume of record titration iron ammonium sulfate standard liquid used, is blank test and consumes sulfuric acid AsiaThe volume V of iron ammonium standard liquid4。
Embodiment 1
(i) prepare sample
Use corrosion-resistant material sampling bag to get 1.0543g vanadium pentafluoride liquid, in sampling bag, addEntering 10mL quality is the absorption liquid absorption of 5% sulfuric acid solution than concentration, and solution is proceeded to capacityIn bottle, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations is to 250ml, obtains sampleHydrolyzate;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to measure pentavalent vanadium, pipette the hydrolysis of 100mL sampleLiquid, adding respectively quality is 98% sulfuric acid 5mL than concentration, the phosphorus that quality is 85% than concentrationAcid 1mL, then add the N-phenylanthranilic acid that 1mL quality is 0.2% than concentration to refer toShow agent, with the titration of iron ammonium sulfate standard liquid, when sample solution becomes bright green from aubergine,And in 30 seconds, when nondiscolouring, record uses the volume of iron ammonium sulfate standard liquid, consumesThe volume of 0.1104mol/L iron ammonium sulfate standard liquid is 24.99mL, blank test consumptionThe volume of 0.1104mol/L iron ammonium sulfate standard liquid is 0mL, and test solution divides to be got than being 1/25,The purity of utilizing computing formula to calculate vanadium pentafluoride is 95.48%.
Embodiment 2
(i) prepare sample
Use corrosion-resistant material sampling bag to get 5.2361g vanadium pentafluoride liquid, in sampling bag, addEntering 30mL quality is the absorption liquid absorption of 12% sulfuric acid solution than concentration, and solution is proceeded to capacityIn bottle, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations is to 500ml, obtains sampleHydrolyzate;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to measure pentavalent vanadium, pipette the hydrolysis of 50mL sampleLiquid, adding respectively quality is 98% sulfuric acid 12mL than concentration, the phosphorus that quality is 85% than concentrationAcid 2mL, then add the N-phenylanthranilic acid that 1mL quality is 0.2% than concentration to refer toShow agent, with the titration of iron ammonium sulfate standard liquid, when sample solution becomes bright green from aubergine,And in 30 seconds, when nondiscolouring, record uses the volume of iron ammonium sulfate standard liquid, consumesThe volume of 0.1082mol/L iron ammonium sulfate standard liquid is 32.44mL, blank test consumptionThe volume of 0.1082mol/L iron ammonium sulfate standard liquid is 0mL, and test solution divides to be got than being 1/10,The purity of utilizing computing formula to calculate vanadium pentafluoride is 97.83%.
Embodiment 3
(i) prepare sample
Use corrosion-resistant material sampling bag to get 9.8250g vanadium pentafluoride liquid, in sampling bag, addEntering 60mL quality is the absorption liquid absorption of 20% sulfuric acid solution than concentration, and solution is proceeded to capacityIn bottle, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations is to 1000ml, obtains sampleProduct hydrolyzate;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to measure pentavalent vanadium, pipette the hydrolysis of 10mL sampleLiquid, adding respectively quality is 98% sulfuric acid 20mL than concentration, the phosphorus that quality is 85% than concentrationAcid 3mL, then add the N-phenylanthranilic acid that 1mL quality is 0.2% than concentration to refer toShow agent, with the titration of iron ammonium sulfate standard liquid, when sample solution becomes bright green from aubergine,And in 30 seconds, when nondiscolouring, record uses the volume of iron ammonium sulfate standard liquid, consumesThe volume of 0.1015mol/L iron ammonium sulfate standard liquid is 6.61mL, blank test consumptionThe volume of 0.1015mol/L iron ammonium sulfate standard liquid is 0mL, and test solution divides to be got than being 1/10,The purity of utilizing computing formula to calculate vanadium pentafluoride is 99.72%.
Claims (1)
1. a detection method for vanadium pentafluoride product purity, is characterized in that: comprise the following steps:
(i) prepare sample
Use corrosion-resistant material sampling bag to get 1g ~ 10g vanadium pentafluoride liquid, in sampling bag, add the absorption liquid that 10mL ~ 60mL quality is 5% ~ 20% sulfuric acid solution than concentration to absorb, solution is proceeded in volumetric flask, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations is to 250ml ~ 1000ml, obtains sample hydrolyzate;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to measure pentavalent vanadium, pipette 10mL ~ 100mL sample hydrolyzate, adding respectively quality is 98% sulfuric acid 5mL～20mL than concentration, phosphatase 11 mL～3mL that quality is 85% than concentration, add again the N-phenylanthranilic acid indicator that 1mL quality is 0.2% than concentration, with the titration of iron ammonium sulfate standard liquid, when sample solution becomes bright green from aubergine, and in 30 seconds when nondiscolouring, record uses the volume of iron ammonium sulfate standard liquid, calculates the content of vanadium pentafluoride according to detection data by following formula (1):
In formula: c-iron ammonium sulfate concentration of standard solution, unit is mol/L; V3---the volume of the iron ammonium sulfate standard liquid that consumes when titration test solution, unit is mL; V4---blank test consumes the volume of iron ammonium sulfate standard liquid, and unit is mL; γ---test solution divides gets ratio; The molal weight of M---vanadium pentafluoride, unit is g/moL; M---the example weight taking, unit is g;
The method of operating of described blank test for pipette analyze with step (II) vanadium pentafluoride product purity in the deionized water of institute's sample thief hydrolyzate same volume, add respectively the sulfuric acid of same volume in analyzing with step (II) vanadium pentafluoride product purity, equal in quality concentration, phosphoric acid, phenylanthranilic acid indicator, be titrated to solution with iron ammonium sulfate standard liquid and become bright green from aubergine, record the volume of titration iron ammonium sulfate standard liquid used, be blank test and consume the volume V of iron ammonium sulfate standard liquid4。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101413898A (en) * | 2008-11-25 | 2009-04-22 | 攀枝花学院 | Quantitative analysis method of vanadium in high chrome alloy |
| CN101609078A (en) * | 2009-07-16 | 2009-12-23 | 武汉钢铁(集团)公司 | The method of full iron in a kind of fast measuring sulfate slag |
| CN102288727A (en) * | 2011-07-12 | 2011-12-21 | 内蒙古包钢钢联股份有限公司 | Method for measuring vanadium in vanadium-nitrogen alloy |
| CN102928425A (en) * | 2012-10-31 | 2013-02-13 | 攀枝花钢城集团瑞钢工业有限公司 | Method for determining vanadium in silicon-vanadium alloy |
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| JP3501546B2 (en) * | 1995-05-12 | 2004-03-02 | 新興化学工業株式会社 | Collection of valuable metals |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413898A (en) * | 2008-11-25 | 2009-04-22 | 攀枝花学院 | Quantitative analysis method of vanadium in high chrome alloy |
| CN101609078A (en) * | 2009-07-16 | 2009-12-23 | 武汉钢铁(集团)公司 | The method of full iron in a kind of fast measuring sulfate slag |
| CN102288727A (en) * | 2011-07-12 | 2011-12-21 | 内蒙古包钢钢联股份有限公司 | Method for measuring vanadium in vanadium-nitrogen alloy |
| CN102928425A (en) * | 2012-10-31 | 2013-02-13 | 攀枝花钢城集团瑞钢工业有限公司 | Method for determining vanadium in silicon-vanadium alloy |
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