CN105259302B - Directly measure the method for trivalent vanadium content in vanadium slag - Google Patents
Directly measure the method for trivalent vanadium content in vanadium slag Download PDFInfo
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Abstract
The invention belongs to chemical analysis method, be specifically related to a kind of trivalent vanadium method Han quantitative analysis in directly mensuration vanadium slag.The present invention directly measures the method for trivalent vanadium content in vanadium slag, comprises the following steps: A, take testing sample X/g in reaction vessel；B, addition hydrochloric acid and fluoride salt sample dissolution, addition titanous chloride. is screening agent, with carbon dioxide for protection gas, is heated to the micro-boiling of solution；C, after sample is completely dissolved, add sodium sulfite, continue reaction 5～10min, stop heating, be cooled to 60～70 DEG C；D, to cooling after solution in add sulphuric acid regulation acidity, dropping ammonium thiocyanate is indicator, with ferric ammonium sulfate titer as volumetric solution, titrate, until reaction solution becomes kermesinus, stop titration, calculate the content of trivalent vanadium in vanadium slag with the ferric sulphate ammonium salt solution consumed.It is simple that the present invention measures trivalent vanadium method in vanadium slag, and accuracy rate is high.
Description
Technical field
The invention belongs to chemical analysis method, be specifically related to trivalent vanadium in a kind of directly mensuration vanadium slag and contain quantitative analysis side
Method.
Background technology
Vanadium slag is through smelting the technique Ore making vanadium be fully enriched with containing vanadium raw materials, is vanadium extraction (V2O5)
Primary raw material, has the biggest economic worth.The valence state of understanding vanadium slag and content are to determining the production technology of vanadium in process for extracting vanadium
Condition, improves and produces conversion ratio important in inhibiting.Valence state for Vanadium in Vanadium Residue is studied, domestic existing more research, wherein
" valence state of vanadium in X-ray photoelectricity energy spectrum analysis vanadium slag grog " and " Determination of Different Valence States of Vanadium in Vanadium Residue " are qualitative analysis；" sodium
The Determination of Different Valence States of Vanadium in Vanadium Residue " it is quantitative analysis, method is with ferrous ammonium sulfate titration tetravalence vanadium and pentavalent vanadium content,
Being deducted pentavalent vanadium by total vanadium and tetravalence content of vanadium obtains trivalent vanadium content, method is complex lengthy and tedious, and trivalent vanadium is indirect determination, accurate
Exactness is the highest.
Further for example, Application No. " 201210572028.3 ", invention entitled " method measuring content of vanadium ", disclose one
Plant and comprise the following steps: clear up containing vanadium sample with hydrochloric acid, obtain containing vanadium solution；By inductively coupled plasma atomic emissions light
Spectrometer measures containing the content of vanadium in vanadium solution.This patent uses ICP to measure and analyzes the content of vanadium, testing cost and inspection in solution containing vanadium
Measurement equipment is more expensive, there is also bigger test error.
Application No. " 201310030450.0 ", invention entitled " assay method of tetravalence content of vanadium in vanadium oxide ", public
Having opened a kind of determination step is: (1) measures the full content of vanadium in vanadium oxide sample；(2) alkali solution technique is used to dissolve identical oxidation
Vanadium sample, filters insoluble matter and separates, and obtains filtrate and insoluble trivalent vanadium precipitation；(3) adding sulphuric acid filtrate, dropping vanadium refers to
Pentavalent vanadium content is determined with Ferrous ammonium sulfate mark drop after showing agent；(4) in trivalent vanadium precipitates, add sulphuric acid and nitric acid post-heating is molten
Solve, be subsequently adding Ferrous ammonium sulfate and vanadium is reduced into lower valency, then drip potassium permanganate vanadium is oxidized to pentavalent；It is subsequently adding urine
Element, with the potassium permanganate of sodium nitrite solution reduction excess, determines trivalent vanadium with Ferrous ammonium sulfate mark drop after dropping vanadium indicator
Content；(5) deduct the content of trivalent vanadium and pentavalent vanadium with full content of vanadium and be tetravalence content of vanadium.This patented method is also trivalent vanadium
Indirect determination method, measures process complicated, and accuracy is the highest.
Being looked into by document, Chinese scholars thinks that Vanadium in Vanadium Residue mainly exists with trivalent, is formed containing vanadic spinel, pentavalent vanadium and
Tetravalence content of vanadium is few, and inventor thinks can directly measure trivalent vanadium content in vanadium slag, improve accuracy that trivalent vanadium measures and
Analyze speed.
Containing the elements such as substantial amounts of manganese, silicon, calcium, magnesium, ferrum, the thing phase that the fired formation of these elements is different in vanadium slag.Want
Solve a mensuration difficult problem for trivalent vanadium, first solve sample and decompose a difficult problem, vanadium thing will be contained as far as possible when decomposing sample mutually fully open；
Secondly, eliminate value Mn, at high price ferrum and the interference of high price vanadium, and ensure that in vanadium slag, tetravalence vanadium is not reduced, value Mn, height
Valency ferrum, at high price vanadium etc. and trivalent vanadium reactivity are relatively strong, in certain acid medium, it is impossible to coexist, can be oxidized to by trivalent vanadium
Tetravalence vanadium, measures trivalent vanadium and produces interference, and suitable reducing agent need to be selected preferentially to reduce high price thing and ensure not reduce four
Valency vanadium；Finally there is stronger reproducibility because of trivalent vanadium, need to ensure that trivalent vanadium is not oxidized during whole analysis.
Summary of the invention
It is simple that the technical problem to be solved is to provide a kind of method, and accuracy is high, can directly measure vanadium slag
The method of middle trivalent vanadium.
The method of trivalent vanadium content in a kind of direct mensuration vanadium slag of the present invention, comprises the following steps:
A, take the testing sample X/g of particle diameter≤0.125mm in reaction vessel；
B, adding hydrochloric acid and fluoride salt dissolve testing sample in reaction vessel, additions titanous chloride. is screening agent, addition
Reaction vessel, to produce carbon-dioxide protecting gas, is added a cover isolation air by sodium bicarbonate, is heated to the micro-boiling of solution；
Wherein, according to 0.1～0.2g testing sample meter, hydrochloric acid addition is 20～40mL, and the addition of fluoride salt is
0.5g～1.0g；
C, after testing sample is completely dissolved, add sodium sulfite, under slight boiling condition continue reaction 5～10min, stop adding
Heat, is cooled to 60～70 DEG C；
D, will step C cool down after solution in add sulphuric acid, regulation solution acidity be 6～8mol L-1, then drip sulfur cyanogen
Acid ammonium is indicator, with molar concentration for c/mol L-1Ferric ammonium sulfate titer be volumetric solution, titrate, until instead
Answer solution to become kermesinus, stop titration, the ferric ammonium sulfate liquor capacity V/mL that record consumes, measure vanadium slag according to formula I
The content of middle trivalent vanadium:
Wherein, V0Blank experiment consumes ferric ammonium sulfate standard solution volume, and unit is mL；
The relative atomic mass of 50.94 vanadium, unit is g/mol.
The method of trivalent vanadium content in direct mensuration vanadium slag described above, the hydrochloric acid used in step B is hydrochloric acid (1+1),
I.e. concentrated hydrochloric acid and water volume ratio are 1:1, and its molar concentration is 6mol L-1。
The method of trivalent vanadium content in direct mensuration vanadium slag described above, wherein in step B the concentration of titanous chloride. be 5～
15wt%.
Further, as preferred technical scheme, the method for trivalent vanadium content in direct mensuration vanadium slag described above, step
In rapid B, the concentration of titanous chloride. is preferably 10wt%.
The method of trivalent vanadium content in direct mensuration vanadium slag described above, wherein said fluoride salt is sodium fluoride or fluorination
At least one in potassium.
The method of trivalent vanadium content in direct mensuration vanadium slag described above, needs after wherein adding sodium sulfite in step C
Add sodium bicarbonate to produce carbon-dioxide protecting gas.
The method of trivalent vanadium content in direct mensuration vanadium slag described above, wherein in step D titration temperature control be 60～
70℃。
The method of trivalent vanadium content, wherein ferric ammonium sulfate mole mole in step D in direct mensuration vanadium slag described above
Concentration c is 0.01～0.03mol L-1。
Further, as preferred technical scheme, the method for trivalent vanadium content in direct mensuration vanadium slag described above, step
In rapid D, ferric ammonium sulfate molar concentration c is preferably 0.02mol L-1。
The method of trivalent vanadium content in direct mensuration vanadium slag described above, the sulphuric acid wherein used in step D is sulphuric acid (1+
1), i.e. 1 volume 98wt% concentrated sulphuric acid, add 1 volume of water formulated, its concentration is 9～9.5mol L-1, preferably 9.2mol
L-1。
The method of trivalent vanadium content in a kind of direct mensuration vanadium slag of the present invention, compared with prior art, has mensuration accurately
Property high, precision is good, and assay method is simple, has popularizing application prospect widely.Due in vanadium slag containing substantial amounts of manganese, silicon,
The elements such as calcium, magnesium, ferrum, the thing phase that the fired formation of these elements is different, the inventive method decomposes the base of a difficult problem solving sample
On plinth, eliminate again value Mn, at high price ferrum and the interference of high price vanadium, and ensure that in vanadium slag, tetravalence vanadium is not reduced, and decreases
The interference measuring trivalent vanadium, finally ensures that trivalent vanadium is not oxidized during whole analysis, decreases trivalent vanadium and measures by mistake
Difference.
Detailed description of the invention
The method of trivalent vanadium content in a kind of direct mensuration vanadium slag of the present invention, comprises the following steps:
A, take the testing sample X/g of particle diameter≤0.125mm in reaction vessel；Wherein assay sample should be by YB/T 008
Being sampled and prepare, sample should be by the sieve aperture of 0.125mm；
B, adding hydrochloric acid and fluoride salt dissolve testing sample in reaction vessel, additions titanous chloride. is screening agent, addition
Reaction vessel, to produce carbon-dioxide protecting gas, is added a cover isolation air by sodium bicarbonate, is heated to the micro-boiling of solution；
Wherein, according to 0.1～0.2g testing sample meter, hydrochloric acid addition is 20～40mL, and the addition of fluoride salt is
0.5g～1.0g；
C, after testing sample is completely dissolved, add sodium sulfite, under slight boiling condition continue reaction 5～10min, stop adding
Heat, is cooled to 60～70 DEG C；
D, will step C cool down after solution in add sulphuric acid, regulation solution acidity be 6～8mol L-1, then drip sulfur cyanogen
Acid ammonium is indicator, with molar concentration for c/mol L-1Ferric ammonium sulfate titer be volumetric solution, titrate, until instead
Answer solution to become kermesinus, stop titration, the ferric ammonium sulfate liquor capacity V/mL that record consumes, measure vanadium slag according to formula I
The content of middle trivalent vanadium:
Wherein, V0Blank experiment consumes ferric ammonium sulfate standard solution volume, and unit is mL；
The relative atomic mass of 50.94 vanadium, unit is g/mol.
The method of trivalent vanadium content in direct mensuration vanadium slag described above, the hydrochloric acid used in step B is hydrochloric acid (1+1),
I.e. concentrated hydrochloric acid and water volume ratio are 1:1, and its molar concentration is 6mol L-1, the metal being added in dissolving vanadium slag of hydrochloric acid
Oxide and carbonate.
The method of trivalent vanadium content in direct mensuration vanadium slag described above, wherein said fluoride salt is sodium fluoride or fluorination
At least one in potassium, sodium fluoride or potassium fluoride are cosolvent, add it for silicon dioxide and silicate in sample dissolution.
The method of trivalent vanadium content in direct mensuration vanadium slag described above, wherein in step B the concentration of titanous chloride. be 5～
15wt%.
Further, as preferred technical scheme, the method for trivalent vanadium content in direct mensuration vanadium slag described above, step
In rapid B, the concentration of titanous chloride. is preferably 10wt%.
The method of trivalent vanadium content in direct mensuration vanadium slag described above, needs after wherein adding sodium sulfite in step C
Add sodium bicarbonate to produce carbon-dioxide protecting gas.
The method of trivalent vanadium content in direct mensuration vanadium slag described above, wherein in step D titration temperature control be 60～
70℃。
The method of trivalent vanadium content, wherein ferric ammonium sulfate molar concentration c in step D in direct mensuration vanadium slag described above
It is 0.01～0.03mol L-1。
Further, as preferred technical scheme, the method for trivalent vanadium content in direct mensuration vanadium slag described above, step
In rapid D, ferric ammonium sulfate molar concentration c is preferably 0.02mol L-1。
The method of trivalent vanadium content in direct mensuration vanadium slag described above, the sulphuric acid wherein used in step D is sulphuric acid (1+
1), i.e. 1 volume 98wt% concentrated sulphuric acid, add 1 volume of water formulated, its concentration is 9～9.5mol L-1, preferably 9.2mol
L-1。
In step B of the present invention, add excess titanous chloride., make high price thing in sample preferential and titanous chloride. reaction, it is ensured that
Trivalent vanadium is not oxidized；Add sodium bicarbonate generate carbon dioxide with hydrochloric acid reaction or be passed directly into carbon dioxide gas
Body, completely cuts off air, it is ensured that trivalent vanadium not oxidation by air.
In step C of the present invention, adding sodium sulfite, can aoxidize the titanous chloride. of excess, the sodium sulfite of excess is micro-
Decompose under boiling state.
In step D of the present invention, reaction rate during in order to improve titration, arranging titration temperature is 60～70 DEG C, uses sulphuric acid
Trivalent vanadium in high ferro ammonium standard titration solution volumetric soiutions, finally measures trivalent in solution with ferric ammonium sulfate standard titration solution
Content of vanadium.
Detailed below measure the method for trivalent vanadium content in vanadium slag according to the present invention.
According to the present invention, the method measuring trivalent vanadium content, specially comprise the following steps:
A, weigh 0.1g～0.2g testing sample in conical flask；
B, addition 0.5g～1g sodium fluoride, 1g sodium bicarbonate, 20mL～40mL hydrochloric acid, 1.0mL～2.0mL titanous chloride.,
Pour a small amount of water, add a cover porcelain crucible lid, sample is placed in high temperature furnace and quickly boils, sample is moved into low-temperature heat dish and keeps sample
Micro-boiling；
C, sample add sodium sulfite 2.0mL～4.0mL after decomposing completely, add sodium bicarbonate 0.5g, add a cover porcelain crucible
Cover and continue to keep micro-boiling 5min～10min, decompose residue sodium sulfite；Sodium sulfite takes off after decomposing completely, is slightly cooled to
60 DEG C～70 DEG C；
D, addition 30mL～50mL sulphuric acid regulation acidity, add water 50mL, adds ammonium thiocyanate indicator, with ferric ammonium sulfate
Standard titration solution be titrated to solution be kermesinus be terminal.
In the trivalent vanadium content assaying method of the present invention, the suitable sample size of described sample is at 0.1g～0.2g；Tri-chlorination
Titanium be analytical pure and more than, mass concentration is 10%, addition 1.0mL～2.0mL；Sodium sulfite be analytical pure and with
On, mass concentration 5%, addition is 2.0mL～4.0mL.Hydrochloric acid, sulphuric acid be analytical pure and more than, concentration is (1+1)
(volume ratio)；Ammonium thiocyanate be analytical pure and more than, mass concentration 40%, addition is 5mL；Ferric ammonium sulfate is analytical pure
More than and, concentration is 0.01～0.03mol L-1；In analysis with water quality meet three grades of GB/T6682-1992 and with
Upper distilled water.
Below in conjunction with embodiment, the detailed description of the invention of the present invention is further described, the most therefore the present invention is limited
System is among described scope of embodiments.
The mensuration of trivalent vanadium in embodiment 1 vanadium slag
Weighing 5 parts of samples, every part of 0.15g, in conical flask, weighs 0.1～0.2g testing sample in conical flask, adds
1g sodium fluoride, 1g sodium bicarbonate, 30mL hydrochloric acid, 1.0mL titanous chloride., pour a small amount of water, add a cover porcelain crucible lid, be placed in by sample
High temperature furnace quickly boils, with moving into the holding micro-boiling of sample of low-temperature heat dish by sample.Sample adds sulfurous acid after decomposing completely
Sodium 2.0mL, adds sodium bicarbonate 0.5g, adds a cover porcelain crucible lid and continues to keep micro-boiling 5min to decompose residue sodium sulfite.Take off,
Being cooled to 60～70 DEG C, add water 50mL, adds sulphuric acid 40mL, adds 5mL ammonium thiocyanate indicator, molten with ferric ammonium sulfate standardized titration
Liquid be titrated to solution be kermesinus be terminal, the preparation of ferric ammonium sulfate with demarcate enter according in YB/T4392.1-2014 4.11
OK；
Blank experiment is arranged: separately takes 1 conical flask, is added without testing sample, is directly added into 1g sodium fluoride, 1g bicarbonate
Sodium, 30mL hydrochloric acid, 1.0mL titanous chloride., pour a small amount of water, add a cover porcelain crucible lid, mixed material is placed in high temperature furnace and cooks quickly soon
Boiling, with moving into the holding micro-boiling of sample of low-temperature heat dish by sample, then adds sodium sulfite 2.0mL, adds sodium bicarbonate 0.5g,
Add a cover porcelain crucible lid and continue to keep micro-boiling 5min to decompose residue sodium sulfite.Taking off, be cooled to 60～70 DEG C, add water 50mL, adds
Sulphuric acid 40mL, adds 5mL ammonium thiocyanate indicator, is titrated to solution for kermesinus as end with ferric ammonium sulfate standard titration solution
Point, the preparation of ferric ammonium sulfate is carried out according in YB/T4392.1-2014 4.11 with demarcating；
Analysis result is calculated as follows:
In formula:
The substance withdrawl syndrome of c ferric ammonium sulfate standard solution, unit is mole every liter (mol/L)；
V titration sample solution consumes ferric ammonium sulfate standard solution volume, and unit is milliliter (mL)；
V0Blank experiment consumes ferric ammonium sulfate standard solution volume, and unit is milliliter (mL)；
M test portion amount, unit is gram (g)；
The relative atomic mass of 50.94 vanadium, unit is gram every mole (g/mol).
Table 1 V3+The measurement result of content
In table 1, RSD is relative standard deviation.
The mensuration response rate of trivalent vanadium in embodiment 2 vanadium slag
Weighing 4 parts of samples, every part of 0.15g, in conical flask, weighs 0.1～0.2g testing sample in conical flask, adds
1g sodium fluoride, 1g sodium bicarbonate, 30mL hydrochloric acid, 1.0mL titanous chloride., pour a small amount of water, add trivalent vanadium standard solution (trivalent
Vanadium concentration of standard solution 4.48mg/mL) 3.0mL, 4.0mL, 5.0mL add a cover porcelain crucible lid, and sample is placed in high temperature furnace and cooks quickly soon
Boiling, with moving into the holding micro-boiling of sample of low-temperature heat dish by sample.Sample adds sodium sulfite 2.0mL, carbonic acid after decomposing completely
Hydrogen sodium 0.5g, adds a cover porcelain crucible lid and continues to keep micro-boiling 5min to decompose residue sodium sulfite.Take off, be cooled to 60～70 DEG C,
Add water 50mL, adds sulphuric acid 40mL, adds 5mL ammonium thiocyanate indicator, is titrated to solution with ferric ammonium sulfate standard titration solution
Being terminal for kermesinus, blank experiment arranges same embodiment 1, and the preparation of ferric ammonium sulfate and demarcation are according to YB/T 4392.1-
In 2014,4.11 are carried out, and analysis result is calculated as follows:
In formula:
The substance withdrawl syndrome of c ferric ammonium sulfate standard solution, unit is mole every liter (mol/L)；
V titration sample solution consumes ferric ammonium sulfate standard solution volume, and unit is milliliter (mL)；
V0Blank experiment consumes ferric ammonium sulfate standard solution volume, and unit is milliliter (mL)；
M test portion amount, unit is gram (g)；
The relative atomic mass of 50.94 vanadium, unit is gram every mole (g/mol).
Table 2 V3+Amount response rate experimental design and result thereof
| Add V3+Amount, mg | 0.0 | 13.44 | 17.92 | 22.40 |
| Record V3+Amount, mg | 13.14 | 26.42 | 30.95 | 35.14 |
| Reclaim V3+Amount, ug | / | 13.28 | 17.81 | 22.00 |
| The response rate, % | / | 98.81 | 99.39 | 98.21 |
By above example 1～2 it can be seen that according to trivalent vanadium in the mensuration vanadium slag of the present invention, accuracy is high, precision
Good, there is popularizing application prospect widely.
Claims (11)
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: comprise the following steps:A, take the testing sample X/g of particle diameter≤0.125mm in reaction vessel；B, adding hydrochloric acid and fluoride salt dissolve testing sample in reaction vessel, additions titanous chloride. is screening agent, addition carbonic acid Reaction vessel, to produce carbon-dioxide protecting gas, is added a cover isolation air by hydrogen sodium, is heated to the micro-boiling of solution；Wherein, according to 0.1～0.2g testing sample meter, hydrochloric acid addition is 20～40mL, fluoride salt addition be 0.5g～ 1.0g；C, after testing sample is completely dissolved, add sodium sulfite, under slight boiling condition continue reaction 5～10min, stop heating, It is cooled to 60～70 DEG C；D, will step C cool down after solution in add sulphuric acid, regulation solution acidity be 6～8mol L-1, then drip ammonium thiocyanate For indicator, with molar concentration for c/mol L-1Ferric ammonium sulfate titer be volumetric solution, titrate, until reacting molten Liquid becomes kermesinus, stops titration, the ferric ammonium sulfate liquor capacity V/mL that record consumes, and measures in vanadium slag three according to formula I The content of valency vanadium:Wherein, V0Blank experiment consumes ferric ammonium sulfate standard solution volume, and unit is mL；The relative atomic mass of 50.94 vanadium, unit is g/mol.
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: described fluoride salt is At least one in sodium fluoride or potassium fluoride.
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: hydrochloric acid in step B Concentration is 6mol L-1。
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: trichlorine in step B The concentration changing titanium is 5～15wt%.
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: titanous chloride. dense Degree is 10wt%.
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: step C adds Need after sodium sulfite to add sodium bicarbonate to produce carbon-dioxide protecting gas.
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: step D titrates Temperature is 60～70 DEG C.
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: sulphuric acid in step D High ferro ammonium molar concentration c is 0.01～0.03mol L-1。
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: sulphuric acid in step D High ferro ammonium molar concentration c is 0.02mol L-1。
- The most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: sulphuric acid in step D Concentration is 9～9.5mol L-1。
- 11. the most directly measure the method for trivalent vanadium content in vanadium slag, it is characterised in that: sulfuric acid concentration is 9.2mol·L-1。
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| CN102590444A (en) * | 2012-03-15 | 2012-07-18 | 河北钢铁股份有限公司承德分公司 | Determination method for vanadium valence state in vanadium-containing slag |
| CN102879391A (en) * | 2012-09-24 | 2013-01-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Device and method for measuring content of trivalent vanadium in vanadyl sulfate |
| CN102928427A (en) * | 2012-10-26 | 2013-02-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for determining pentavalent vanadium in vanadyl sulfate |
| CN102928372A (en) * | 2012-11-11 | 2013-02-13 | 山东师范大学 | Measurement method for whole vanadium in soil |
| CN104181272A (en) * | 2014-07-30 | 2014-12-03 | 武汉钢铁(集团)公司 | Method for rapidly determining content of total iron in vanadium titano-magnetite |
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- 2015-11-13 CN CN201510779514.6A patent/CN105259302B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590444A (en) * | 2012-03-15 | 2012-07-18 | 河北钢铁股份有限公司承德分公司 | Determination method for vanadium valence state in vanadium-containing slag |
| CN102879391A (en) * | 2012-09-24 | 2013-01-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Device and method for measuring content of trivalent vanadium in vanadyl sulfate |
| CN102928427A (en) * | 2012-10-26 | 2013-02-13 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for determining pentavalent vanadium in vanadyl sulfate |
| CN102928372A (en) * | 2012-11-11 | 2013-02-13 | 山东师范大学 | Measurement method for whole vanadium in soil |
| CN104181272A (en) * | 2014-07-30 | 2014-12-03 | 武汉钢铁(集团)公司 | Method for rapidly determining content of total iron in vanadium titano-magnetite |
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