CN104483444A - Method for measuring content of vanadium in nitrided ferrovanadium by oxidization and reduction - Google Patents
Method for measuring content of vanadium in nitrided ferrovanadium by oxidization and reduction Download PDFInfo
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- CN104483444A CN104483444A CN201410751332.3A CN201410751332A CN104483444A CN 104483444 A CN104483444 A CN 104483444A CN 201410751332 A CN201410751332 A CN 201410751332A CN 104483444 A CN104483444 A CN 104483444A
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Abstract
The invention relates to a method for measuring content of vanadium in nitrided ferrovanadium by oxidization and reduction. The method comprises the following steps: getting a nitrided ferrovanadium test sample, dissolving the test sample in nitric acid, smoking with phosphoric acid, quickly adding ammonium nitrate to oxidize low valent vanadium after smoking; after eliminating the interferences of manganese by sodium nitrite, performing oxidization-reduction titration by taking ammonium ferrous sulfate as a standard solution, thereby calculating the content of vanadium in ferrovanadium. The method disclosed by the invention has the advantages of greatly shortening the smoking time by adopting phosphoric acid to smoke, reducing the adding types of reagents, simplifying the operation, ensuring the accuracy while increasing the speed, reducing the reagent adding types and the sulfuric acid adding amount, saving the reagent cost, shortening the time for heating and dissolving the sample and the smoking time, and lowering energy consumption.
Description
Technical field
The present invention relates to a kind of method that redox measures content of vanadium in ferrovanadium nitride, belong to ferroalloy analysis technical field in metallurgical chemistry.
background technology
At present, the vanadium many employings potassium permanganate oxidation method in ferrovanadium nitride is measured.Adopt nitric acid decomposition samples, sulfuric acid is smoldered, and under suitable acidity of sulfuric acid, with potassium permanganate, vanadium is oxidizing to pentavalent, with the potassium permanganate of sodium nitrite decomposing excessive, and excessive sodium nitrite urea decomposition.Benzene is indicator for ortho-aminobenzoic acid, carries out redox titration with iron ammonium sulfate standard solution.Is that sulfuric acid is smoldered due to what adopt, usually will add a large amount of high-concentration sulfuric acid, sulfuric acid temperature of being fuming is high, needs the time more grown to play cigarette, needs calculating to smolder the time simultaneously, comparatively loaded down with trivial details.The kind that medicine adds is also many, and addition is large, long flow path, and operation is slow.
Summary of the invention
The object of the invention is to solve medicine when existing method measures vanadium in ferrovanadium nitride that to add kind many, consumption is large, flow process, operate slow problem, speed operations speed simultaneously, reduces costs, provide a kind of more fast, measure the method for content of vanadium in ferrovanadium nitride accurately and efficiently.
Technical scheme of the present invention is as follows:
The present invention is a kind of for content of vanadium method for measuring in ferrovanadium nitride, is specifically completed by following steps:
Get ferrovanadium nitride sample, sample is through Dissolving Simple with Nitric Acid, phosphoric acid is smoldered, add rapidly ammonium nitrate after playing cigarette to be oxidized Low Valent Vanadium, eliminate the interference of manganese with sodium nitrite after, use iron ammonium sulfate to carry out redox titration as standard solution, calculate the content of vanadium in vanadium iron thus, computing formula is as follows:
In formula: M (V): the atomic weight of vanadium, 50.94g/moL,
C: the concentration of iron ammonium sulfate standard solution, 0.05000mol/L,
M: the sample weighting amount of ferrovanadium nitride sample, 0.1000g,
V: the volume of the iron ammonium sulfate standard solution consumed during titration sample, mL,
V
01: the volume of the iron ammonium sulfate standard solution consumed when titration companion is blank, mL.
Advantage of the present invention is:
1) fast, accurately: adopt phosphoric acid to smolder, can greatly shorten the time used of smoldering, reduce medicine and add kind, operation is simplified, while improving speed, also ensure that accuracy.
2) energy-conservation, efficient: to reduce the addition that medicine adds kind and sulfuric acid, saved drug cost, shorten and add the thermosol sample time and be fuming the time, reduce energy consumption.Thus this method has efficient, energy-conservation advantage.
Embodiment
1. method summary:
Sample, through Dissolving Simple with Nitric Acid, adds phosphoric acid and is heated to smolder, add rapidly ammonium nitrate and be oxidized Low Valent Vanadium, and eliminating the interference of manganese with sodium nitrite, is that standard solution carries out titration with iron ammonium sulfate.
2. reagent:
2.1 salpeter solutions (nitric acid of density 1.42g/mL mixes with isopyknic water)
2.2 phosphoric acid (density 1.68g/mL)
2.3 ammonium nitrate (solid)
2.4 sulfuric acid (50g/L)
2.5 urea (100g/L)
2.6 sodium nitrites (10g/L)
2.7 N-phenylanthranilic acids (2g/L): take 0.2g N-benzene and to be dissolved in sodium carbonate liquor (2g/L) for ortho-aminobenzoic acid and to be diluted to 100mL.
2.8 iron ammonium sulfate standard solution: 0.05000mol/L
3. sampling and sample preparation
4. sample size
Take sample 0.1000g.
5. analytical procedure
Take ferrovanadium nitride sample 0.1000g in 300mL triangular flask, add 20mL nitric acid (nitric acid of density 1.42g/mL mixes with isopyknic water), dissolved samples on electric hot plate, after sample dissolves, take off slightly cold, add 15mL phosphoric acid (density 1.68g/mL), be heated to emit phosphoric acid cigarette, start to smolder and namely take off, add 3g ammonium nitrate immediately, blow off nitrogen, slightly cold, add 50mL sulfuric acid (50g/L), shake up, be cooled to room temperature.Add 10mL urea (100g/L), be reduced to stable yellow and excessive 2 with sodium nitrite (10g/L), add 3 N-phenylanthranilic acid indicator, with iron ammonium sulfate (0.05000mol/L)
Carry out redox titration as standard solution, calculate the content of vanadium in vanadium iron thus.
6. Analysis result calculation:
In formula: M (V): the atomic weight of vanadium, 50.94g/moL.
C: the concentration of iron ammonium sulfate, 0.05000mol/L.
M: the sample weighting amount of ferrovanadium nitride sample, 0.1000g.
V: the volume of the iron ammonium sulfate standard solution consumed during titration sample, mL,
V
01: the volume of the iron ammonium sulfate standard solution consumed when titration companion is blank, mL.
7. sample analysis contrast
As can be seen from the above table, use the ammonium nitrate oxidation method content of vanadium measured in ferrovanadium nitride to have fast, feature accurately and efficiently.
8. conclusion
By this method, the content of vanadium in ferrovanadium nitride can be determined accurately.That has saved medicine adds kind and addition, shortens the running time, has saved cost of drugs, has reduced energy consumption.Be applicable to being applied to the Fast Measurement of vanadium in ferrovanadium nitride in the middle of producing.
Claims (1)
1. a redox measures the method for content of vanadium in ferrovanadium nitride, it is characterized in that: get ferrovanadium nitride sample, sample is through Dissolving Simple with Nitric Acid, phosphoric acid is smoldered, add rapidly ammonium nitrate after playing cigarette to be oxidized Low Valent Vanadium, eliminate the interference of manganese with sodium nitrite after, use iron ammonium sulfate to carry out redox titration as standard solution, calculate the content of vanadium in vanadium iron thus, computing formula is as follows:
In formula: M (V): the atomic weight of vanadium, 50.94g/moL,
C: the concentration of iron ammonium sulfate standard solution, 0.05000mol/L,
M: the sample weighting amount of ferrovanadium nitride sample, 0.1000g,
V: the volume of the iron ammonium sulfate standard solution consumed during titration sample, mL,
V
01: the volume of the iron ammonium sulfate standard solution consumed when titration companion is blank, mL.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410751332.3A CN104483444A (en) | 2014-12-10 | 2014-12-10 | Method for measuring content of vanadium in nitrided ferrovanadium by oxidization and reduction |
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| CN201410751332.3A CN104483444A (en) | 2014-12-10 | 2014-12-10 | Method for measuring content of vanadium in nitrided ferrovanadium by oxidization and reduction |
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Citations (6)
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|---|---|---|---|---|
| SU1330139A1 (en) * | 1985-07-05 | 1987-08-15 | Всесоюзный Научно-Исследовательский Институт Водоснабжения,Канализации,Гидротехнических Сооружений,Инженерной Гидрогеологии | 3-sulfo-5-nitro-4ъ-diethylamino-2,2ъ-dioxybenzene as agent for photometric determination of gallium,indium,molybdenum and vanadium |
| JPS62198737A (en) * | 1986-02-26 | 1987-09-02 | Babcock Hitachi Kk | Analysis of vanadium |
| CN101666789A (en) * | 2009-10-14 | 2010-03-10 | 湘潭大学 | Method for quickly determining vanadium in coal mine containing scherbinaite |
| 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 |
| CN102507556A (en) * | 2011-10-31 | 2012-06-20 | 攀钢集团江油长城特殊钢有限公司 | Method for measuring vanadium content of silicon ferrovanadium |
| CN102565039A (en) * | 2010-12-21 | 2012-07-11 | 湖南晟通科技集团有限公司 | Method for measuring and analyzing content of vanadium (V) in carbon material |
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2014
- 2014-12-10 CN CN201410751332.3A patent/CN104483444A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1330139A1 (en) * | 1985-07-05 | 1987-08-15 | Всесоюзный Научно-Исследовательский Институт Водоснабжения,Канализации,Гидротехнических Сооружений,Инженерной Гидрогеологии | 3-sulfo-5-nitro-4ъ-diethylamino-2,2ъ-dioxybenzene as agent for photometric determination of gallium,indium,molybdenum and vanadium |
| JPS62198737A (en) * | 1986-02-26 | 1987-09-02 | Babcock Hitachi Kk | Analysis of vanadium |
| CN101666789A (en) * | 2009-10-14 | 2010-03-10 | 湘潭大学 | Method for quickly determining vanadium in coal mine containing scherbinaite |
| CN102565039A (en) * | 2010-12-21 | 2012-07-11 | 湖南晟通科技集团有限公司 | Method for measuring and analyzing content of vanadium (V) in carbon material |
| 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 |
| CN102507556A (en) * | 2011-10-31 | 2012-06-20 | 攀钢集团江油长城特殊钢有限公司 | Method for measuring vanadium content of silicon ferrovanadium |
Non-Patent Citations (1)
| Title |
|---|
| 张根平等: "硝酸铵氧化还原滴定法快速测定钢铁中钒", 《理化检验－化学分册》 * |
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Application publication date: 20150401 |