CN103439330A - Method for detecting purity of vanadium pentafluoride product - Google Patents
Method for detecting purity of vanadium pentafluoride product Download PDFInfo
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Abstract
The invention discloses a method for detecting the purity of a vanadium pentafluoride product and belongs to the field of vanadium halides. According to the detection method, the purity of vanadium pentafluoride can be detected by analyzing the content of pentavalent vanadium of vanadium pentafluoride through conversion. The detection method specifically comprises the following steps of (i) preparing a sample, namely sampling through an anti-corrosion material sampling bag, absorbing an acidic solution, and making up the sample to volume through a volumetric flask; (ii) measuring the pentavalent vanadium through oxidation-reduction titration, and calculating the content through a formula to obtain the purity of the vanadium pentafluoride product. The method is simple, feasible, convenient to operate, high in measurement precision and particularly suitable for detection on the purity of the vanadium pentafluoride product made from fluoride and elemental vanadium.
Description
Technical field
The invention belongs to the halogenide field of vanadium, be specifically related to a kind of detection method of vanadium pentafluoride product purity.
Background technology
Vanadium pentafluoride (VF5) is a kind of very strong fluorization agent and oxygenant, is usually used in organic synthesis doing fluorization agent.
At present not yet relevant for the bibliographical information of measuring the vanadium pentafluoride purity analysis.Only have the report of measuring impurity content of vanadium in alloy, as the Spectrophotometric Determination of Vanadium amount, aas determination vanadium amount, but be all the report of measuring the low content vanadium, have no and be applicable to the detection method that purity is greater than 95% vanadium pentafluoride product.
Summary of the invention
The present invention proposes in order to overcome the shortcoming existed in prior art, its objective is that providing a kind of is applicable to take fluorine gas and elemental vanadium and prepares the detection method of purity of antimony pentafluoride products as raw material, utilization is carried out content analysis to pentavalent vanadium in vanadium pentafluoride, by conversion, realizes the detection to vanadium pentafluoride purity.
Technical scheme of the present invention is:
A kind of detection method of vanadium pentafluoride product purity comprises the following steps:
(i) prepare sample
Use corrosion-resistant material sampling bag to get 1g ~ 10g vanadium pentafluoride liquid, adding 10mL ~ 60mL quality in sampling bag is that 5% ~ 20% sulfuric acid solution absorbs than concentration, solution is proceeded in volumetric flask, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations obtains the sample hydrolyzate to 250ml ~ 1000 ml;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to be measured the 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 the 1mL quality is 0.2% than concentration, with the titration of iron ammonium sulfate standard solution, when sample solution becomes bright green by aubergine, and in 30 seconds during nondiscolouring, record is used the volume of iron ammonium sulfate standard solution, according to detecting data, calculates the content of vanadium pentafluoride by following formula (1):
In formula: c-iron ammonium sulfate concentration of standard solution, mol/L; V
3---the volume of the iron ammonium sulfate standard solution that consumes during the titration test solution, mL; V
4---blank test consumes the volume of iron ammonium sulfate standard solution, mL; γ---test solution divides gets ratio; The molal weight of M---vanadium pentafluoride, g/mL; M---the example weight taken, g.
The present invention is simple and easy to do, convenient operation, and measuring accuracy is high, is specially adapted to take the detection of vanadium pentafluoride product purity prepared as raw material by fluorine gas and elemental vanadium.
Embodiment
Below in conjunction with embodiment, the detection method of vanadium pentafluoride product purity of the present invention is elaborated:
A kind of detection method of vanadium pentafluoride product purity comprises the following steps:
(i) prepare sample
Use corrosion-resistant material sampling bag to get 1g ~ 10g vanadium pentafluoride liquid, adding 10mL ~ 60mL quality in sampling bag is that 5% ~ 20% sulfuric acid solution absorbs than concentration, solution is proceeded in volumetric flask, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations obtains the sample hydrolyzate to 250ml ~ 1000 ml;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to be measured the 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 the 1mL quality is 0.2% than concentration, with the titration of iron ammonium sulfate standard solution, when sample solution becomes bright green by aubergine, and in 30 seconds during nondiscolouring, record is used the volume of iron ammonium sulfate standard solution, according to detecting data, calculates the content of vanadium pentafluoride by following formula (1):
formula (1)
In formula: c-iron ammonium sulfate concentration of standard solution, mol/L; V
3---the volume of the iron ammonium sulfate standard solution that consumes during the titration test solution, mL; V
4---blank test consumes the volume of iron ammonium sulfate standard solution, mL; γ---test solution divides gets ratio; The molal weight of M---vanadium pentafluoride, g/mL; M---the example weight taken, g.
Blank test: the deionized water that pipettes institute's sample thief hydrolyzate equal volume in analyzing with step (II) vanadium pentafluoride product purity, the sulfuric acid that adds respectively equal volume in analyzing with step (II) vanadium pentafluoride product purity, equal in quality concentration, phosphoric acid, the phenylanthranilic acid indicator, be titrated to solution with the iron ammonium sulfate standard solution and become bright green by aubergine, record the volume of titration iron ammonium sulfate standard solution used, be the volume V that blank test consumes the iron ammonium sulfate standard solution
4.
Embodiment 1
(i) prepare sample
Use corrosion-resistant material sampling bag to get 1.0543g vanadium pentafluoride liquid, adding the 10mL quality in sampling bag is that 5% sulfuric acid solution absorbs than concentration, solution is proceeded in volumetric flask, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations obtains the sample hydrolyzate to 250 ml;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to be measured the pentavalent vanadium, pipette 100mL sample hydrolyzate, adding respectively quality is 98% sulfuric acid 5mL than concentration, the phosphatase 11 mL that quality is 85% than concentration, add again the N-phenylanthranilic acid indicator that the 1mL quality is 0.2% than concentration, with the titration of iron ammonium sulfate standard solution, when sample solution becomes bright green by aubergine, and in 30 seconds during nondiscolouring, record is used the volume of iron ammonium sulfate standard solution, the volume that consumes 0.1104 mol/L iron ammonium sulfate standard solution is 24.99mL, the volume that blank test consumes 0.1104mol/L iron ammonium sulfate standard solution is 0mL, 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, adding the 30mL quality in sampling bag is that 12% sulfuric acid solution absorbs than concentration, solution is proceeded in volumetric flask, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations obtains the sample hydrolyzate to 500 ml;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to be measured the pentavalent vanadium, pipette 50mL sample hydrolyzate, adding respectively quality is 98% sulfuric acid 12mL than concentration, the phosphoric acid 2mL that quality is 85% than concentration, add again the N-phenylanthranilic acid indicator that the 1mL quality is 0.2% than concentration, with the titration of iron ammonium sulfate standard solution, when sample solution becomes bright green by aubergine, and in 30 seconds during nondiscolouring, record is used the volume of iron ammonium sulfate standard solution, the volume that consumes 0.1082mol/L iron ammonium sulfate standard solution is 32.44mL, the volume that blank test consumes 0.1082mol/L iron ammonium sulfate standard solution is 0mL, 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, adding the 60mL quality in sampling bag is that 20% sulfuric acid solution absorbs than concentration, solution is proceeded in volumetric flask, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations obtains the sample hydrolyzate to 1000 ml;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to be measured the pentavalent vanadium, pipette 10mL sample hydrolyzate, adding respectively quality is 98% sulfuric acid 20mL than concentration, the phosphoric acid 3mL that quality is 85% than concentration, add again the N-phenylanthranilic acid indicator that the 1mL quality is 0.2% than concentration, with the titration of iron ammonium sulfate standard solution, when sample solution becomes bright green by aubergine, and in 30 seconds during nondiscolouring, record is used the volume of iron ammonium sulfate standard solution, the volume that consumes 0.1015 mol/L iron ammonium sulfate standard solution is 6.61mL, the volume that blank test consumes 0.1015mol/L iron ammonium sulfate standard solution is 0mL, 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. the detection method of a 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, adding 10mL ~ 60mL quality in sampling bag is that 5% ~ 20% sulfuric acid solution absorbs than concentration, solution is proceeded in volumetric flask, and the sulfuric acid solution constant volume of use and absorption liquid same concentrations obtains the sample hydrolyzate to 250ml ~ 1000 ml;
(II) vanadium pentafluoride product purity is analyzed
Utilize oxidimetry to be measured the 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 the 1mL quality is 0.2% than concentration, with the titration of iron ammonium sulfate standard solution, when sample solution becomes bright green by aubergine, and in 30 seconds during nondiscolouring, record is used the volume of iron ammonium sulfate standard solution, according to detecting data, calculates the content of vanadium pentafluoride by following formula (1):
In formula: c-iron ammonium sulfate concentration of standard solution, mol/L; V
3---the volume of the iron ammonium sulfate standard solution that consumes during the titration test solution, mL; V
4---blank test consumes the volume of iron ammonium sulfate standard solution, mL; γ---test solution divides gets ratio; The molal weight of M---vanadium pentafluoride, g/mL; M---the example weight taken, g.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH08311574A (en) * | 1995-05-12 | 1996-11-26 | Shinko Kagaku Kogyo Kk | Method for recovering valuable metal |
| 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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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08311574A (en) * | 1995-05-12 | 1996-11-26 | Shinko Kagaku Kogyo Kk | Method for recovering valuable metal |
| 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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