CN102507556A - Method for measuring vanadium content of silicon ferrovanadium - Google Patents
Method for measuring vanadium content of silicon ferrovanadium Download PDFInfo
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Abstract
The invention provides a method for measuring the vanadium content of silicon ferrovanadium, which includes the steps: (a) mixing silicon ferrovanadium and nitric acid, adding hydrofluoric acid into mixture, heating the mixture to completely dissolve the silicon ferrovanadium, adding sulfuric acid into the mixture, heating the mixture until the moment of smoking, and afterwards cooling the mixture; (b) adding phosphoric acid into the mixture, heating the mixture until smoking, keeping smoking for a period of time and cooling the mixture; (c) adding sulfuric acid into the mixture, cooling the mixture, adding potassium permanganate solution into the mixture until appearing of stable red and allowing the mixture to stand for a period of time; (d) adding urea solution into the mixture, dripping sodium nitrite solution into the mixture to reduce excessive potassium permanganate, excessively adding 1-3 drops of sodium nitrite solution and then allowing the mixture to stand for a period of time; (e) adding N-phenyl o-aminobenzoic acid indicators into the mixture and then dripping ammonium ferrous sulfate standard solution into the mixture to obtain a titration endpoint when the mixture is light green; and (f) computing the vanadium content according to the formula.
Description
Technical field
The present invention relates to a kind of method of measuring the content of vanadium of vanadium alloy, particularly a kind of method of measuring the content of vanadium of silicon vanadium iron.
Background technology
Along with the continuous increase that contains the vanadium steel demand, steel industry is smelted the demand that contains the used vanadium iron of vanadium steel to be increased thereupon in recent years.But supply falls short of demand for vanadium iron on the market, and price is comparatively expensive.Therefore seek the target that the vanadium iron substitute becomes enterprise.The silicon vanadium iron is exactly a kind of economic and practical vanadium iron substitute.
The content of vanadium scope is 25%～50% in the silicon vanadium iron, and the silicone content scope is 10%～40%, does not have the analytical approach and the corresponding standard material of the maturation of silicon vanadium iron at present.Vanadium iron and silicon vanadium iron component difference are very big, particularly owing to silicone content in the sample is very high, make sample handle very difficulty, and silicon is to the mensuration serious interference of vanadium, so have the analysis that the analytical approach of vanadium in the vanadium iron is not suitable for vanadium in the silicon vanadium iron now.
Summary of the invention
One object of the present invention is to provide a kind of method of measuring the content of vanadium of silicon vanadium iron, and this method has been eliminated the interference of silicon to the mensuration of vanadium.
Another object of the present invention is to provide a kind of method of measuring the content of vanadium of silicon vanadium iron, this method can be measured the content of the vanadium in the silicon vanadium iron quickly and accurately.
Comprise the steps: that according to the method for the content of vanadium of mensuration silicon vanadium iron of the present invention (a) is that 60%～68% nitric acid mixes with silicon vanadium iron and concentration; With concentration is that 35%～40% hydrofluorite adds potpourri, and heating blends makes the dissolving of silicon vanadium iron fully, is that 90%～98% sulfuric acid adds potpourri with concentration then; Heating blends is to just smoldering; With the potpourri cooling, wherein, the milliliter number of nitric acid is 60～100 with the ratio of the gram number of silicon vanadium iron afterwards; The milliliter number of sulfuric acid is 27.5～32.5 with the ratio of the gram number of silicon vanadium iron, and the milliliter number of hydrofluorite is 15～30 with the ratio of the gram number of silicon vanadium iron; (b) be that 80%～85% phosphoric acid adds potpourri with concentration, heating blends is to smoldering and keeping 1 minute to 2 minutes, and with the potpourri cooling, wherein, the milliliter number of phosphoric acid is 45～55 with the ratio of the gram number of silicon vanadium iron; (c) be that 13%～15% sulfuric acid adds potpourri with concentration; And be cooled to below 45 ℃; Adding concentration to potpourri then is that the liquor potassic permanganate of 20g/L～50g/L is until there being stable redness to occur; Placed 2 minutes～5 minutes, wherein, the milliliter number of sulfuric acid is 325～375 with the ratio of the gram number of silicon vanadium iron; (d) with concentration be the urea liquid adding potpourri of 90g/L～110g/L; Drip the excessive potassium permanganate of sodium nitrite solution reduction that concentration is 8g/L～12g/L to potpourri; And make excessive 1 to 3 of sodium nitrite solution; Potpourri was placed 1 minute～3 minutes, and wherein, the milliliter number of urea liquid is 45～60 with the ratio of the gram number of silicon vanadium iron; (e) the N-phenyl is added potpourri for the ortho-aminobenzoic acid indicator, the iron ammonium sulfate standard solution with 0.020～0.025mol/L carries out titration to potpourri then, is titration end-point when the potpourri color becomes bright green; (f) according to the content of vanadium W of computes silicon vanadium iron
V:
Wherein, C representes the amount of substance concentration of iron ammonium sulfate standard solution, and unit is mol/L; V representes the volume of the iron ammonium sulfate standard solution that titration consumes, and unit is mL; M representes the quality of silicon vanadium iron, and unit is g.
The N-phenyl can be 1.5g/L～2.5g/L for the concentration of ortho-aminobenzoic acid indicator, and the N-phenyl can be 20～30: 1 for the ratio that drips number and the gram number of silicon vanadium iron of ortho-aminobenzoic acid indicator.
Available sulfuric acid dissolution six ferrous sulfate hydrate ammoniums also are diluted to standard volume and prepare the iron ammonium sulfate standard solution.
This method also can comprise uses the potassium dichromate standard solution that the concentration of iron ammonium sulfate standard solution is demarcated.
This method can be used for measuring the content of vanadium of silicon vanadium iron of Fe of V and the 10wt%～60wt% of the Si that comprises 10wt%～40wt%, 25wt%～50wt%.
Embodiment
Method according to the content of vanadium of mensuration silicon vanadium iron of the present invention comprises the following step of carrying out successively (a)～(f).Method of the present invention can be used for measuring that silicone content is 10%～40%, content of vanadium be 25%～50% and iron content be the content of vanadium of 10%～60% silicon vanadium iron; Yet, be not limited to have the silicon vanadium iron of above-mentioned content range according to the method for the content of vanadium of mensuration silicon vanadium iron of the present invention.Content as herein described is weight percent content.
Step (a):
With silicon vanadium iron and concentration is that 60%～68% nitric acid mixes, and is that 35%～40% hydrofluorite adds potpourri with concentration, and heating blends makes the dissolving of silicon vanadium iron fully.Be that 90%～98% sulfuric acid adds potpourri with concentration then, heating blends cools off potpourri to just smoldering.Wherein, the milliliter number of nitric acid is 60～100 with the ratio of the gram number of silicon vanadium iron, and the milliliter number of sulfuric acid is 27.5～32.5 with the ratio of the gram number of silicon vanadium iron.The milliliter number of hydrofluorite is 15～30 with the ratio of the gram number of silicon vanadium iron.
In step (a), hydrofluorite is added potpourri, make that silicon and the hydrofluorite reaction generation in the silicon vanadium iron has volatile SiF
4Through sulfuric acid being added potpourri and heating, make at least a portion volatilization of nitric acid and hydrofluorite to reduce the influence that nitric acid and hydrofluorite are measured the back; In addition, through sulfuric acid being added potpourri and heating, the SiF that makes generation
4At least a portion volatilization, reduce or eliminate the influence of Si the mensuration of V.
Step (b):
With concentration is that 80%～85% phosphoric acid adds potpourri, and heating blends cools off potpourri to smoldering and keeping 1 minute to 2 minutes.Wherein, the milliliter number of phosphoric acid is 45～55 with the ratio of the gram number of silicon vanadium iron.
In this step, phosphoric acid is added potpourri and smolders, make nitric acid, hydrofluorite and SiF in the potpourri
4Volatilization is complete, thereby eliminates nitric acid, hydrofluorite and SiF
4Influence to back mensuration.In addition, phosphoric acid has complexing, separates out thereby produce a large amount of salts when avoiding smoldering.
Step (c):
With concentration is that 13%～15% sulfuric acid adds potpourri, and is cooled to below 45 ℃, then to potpourri add concentration be the liquor potassic permanganate of 20g/L～50g/L until there being stable redness to occur, placed 2 minutes～5 minutes.Wherein, the milliliter number of sulfuric acid is 325～375 with the ratio of the gram number of silicon vanadium iron.
In this step, add sulfuric acid as stated and make the sulfuric acid concentration of potpourri acquire a certain degree, in the sulphuric acid environment of this concentration, potassium permanganate could be oxidized to the pentavalent vanadium with the tetravalence vanadium.
Step (d):
With concentration is the urea liquid adding potpourri of 90g/L～110g/L, drips the excessive potassium permanganate of sodium nitrite solution reduction that concentration is 8g/L～12g/L to potpourri, and makes excessive 1 to 3 of sodium nitrite solution, and potpourri was placed 1 minute～3 minutes.Wherein, the milliliter number of urea liquid is 45～60 with the ratio of the gram number of silicon vanadium iron.
In this step, as stated urea liquid is added potpourri, come the sodium nitrite of decomposing excessive with this, thereby avoid the influence of nitrite anions subsequent measurements.
Step (e):
The N-phenyl is added potpourri for the ortho-aminobenzoic acid indicator, and the iron ammonium sulfate standard solution with 0.020～0.025mol/L carries out titration to potpourri then, is titration end-point when the potpourri color becomes bright green.In one embodiment, the N-phenyl can be 1.5g/L～2.5g/L for the concentration of ortho-aminobenzoic acid indicator, and the N-phenyl can be 20～30: 1 for the ratio that drips number and the gram number of silicon vanadium iron of ortho-aminobenzoic acid indicator.
In this step, as stated the N-phenyl is added potpourri with the indication titration end-point for the ortho-aminobenzoic acid indicator.In titration process, the iron ammonium sulfate standard solution is reduced to the tetravalence vanadium with the pentavalent vanadium.
In one embodiment, can be through with sulfuric acid dissolution six ferrous sulfate hydrate ammoniums and be diluted to standard volume and prepare the iron ammonium sulfate standard solution.In one embodiment, can use the potassium dichromate standard solution that the concentration of iron ammonium sulfate standard solution is demarcated.
Step (f):
Content of vanadium W according to computes silicon vanadium iron
V:
Wherein, C representes the amount of substance concentration of iron ammonium sulfate standard solution, and unit is mol/L; V representes the volume of the iron ammonium sulfate standard solution that titration consumes, and unit is mL; M is the quality of silicon vanadium iron, and unit is g.
Be described in more detail below in conjunction with the method for concrete example the content of vanadium of mensuration silicon vanadium iron according to the present invention.
Example 1:
Take by weighing 0.20g (being accurate to 0.0001g) test with silicon vanadium iron sample in polytetrafluoroethylene beaker (for synthetic standard sample; Take by weighing a certain amount of vanadium iron standard specimen and the synthetic standard specimen of a certain amount of ferrosilicon standard specimen work by table 1); Add 15mL concentration and be 66% nitric acid, dropwise drip concentration and be 40% hydrofluorite 5mL, heating makes sample dissolution complete; Add 6mL concentration and be 98% sulfuric acid, be heated to just and smolder.Take off polytetrafluoroethylene beaker from heating arrangement, cooling changes solution in the 500mL conical flask over to; Add 10mL concentration and be 85% phosphoric acid, be heated to and smolder 1 to 2 minute, take off polytetrafluoroethylene beaker from heating arrangement; Cool to room temperature adds 70mL concentration and is 14% sulfuric acid, shakes up; Be cooled to below 45 ℃, the liquor potassic permanganate that drips concentration and be 40g/L is to there being stable redness to occur, placement 3min; Add the urea liquid that 10mL concentration is 100g/L, with the excessive potassium permanganate of sodium nitrite solution reduction of 10g/L, and excessive 1; Place 1min, add 5 N-phenyl, be titrated to iron ammonium sulfate standard solution (0.02308mol/L) that to be bright green be terminal point for the ortho-aminobenzoic acid indicator.Calculate content of vanadium by the aforementioned calculation formula.
The N-phenyl that uses in this example prepares according to following method for the ortho-aminobenzoic acid indicator: take by weighing 0.2g N-phenyl for ortho-aminobenzoic acid in the 300mL beaker; Add 0.2 gram natrium carbonicum calcinatum, add 20mL water, heating for dissolving; Cooling; Constant volume 100mL, mixing, the N-phenyl that obtains concentration and be 2g/L is for the ortho-aminobenzoic acid indicator.
The iron ammonium sulfate standard solution that uses in this example prepares according to following method: take by weighing 9.05g six ferrous sulfate hydrate ammoniums, dissolve and be diluted to 1000mL, mixing with sulfuric acid (5+95).Adopt following method that the iron ammonium sulfate standard solution is demarcated: to pipette concentration C (1/6K respectively
2Cr
2O
7Three parts of the 25.00mL potassium dichromate standard solution of)=0.02308mol/L are in the 250mL conical flask; Use the iron ammonium sulfate standard solution titration to yellow green respectively, adding 3 above-mentioned N-phenyl is terminal point for ortho-aminobenzoic acid continuation titration by rose to bright green.The concentration of iron ammonium sulfate standard solution is by computes:
Wherein, C representes the amount of substance concentration of iron ammonium sulfate standard solution, mol/L; C
1The amount of substance concentration of expression potassium dichromate standard solution, mol/L; V
0Represent that 3 parts of potassium dichromate standard solution consume the mean value of the volume of iron ammonium sulfate standard solution, mL.
The potassium dichromate standard solution that uses in this example prepares according to following method: take by weighing 1.1316g in advance through 150 ℃ of bakings after 1 hour and in exsiccator, be cooled to the base weight potassium chromate of room temperature; Place the 300mL beaker, the water dissolving moves into the 1000mL volumetric flask; Be diluted with water to scale, mixing.
Mensuration result according to example 1 is illustrated in the following table 1.
Table 1
Wherein, It is 54.20% that FeV50-A-1 vanadium iron standard specimen contains the vanadium standard value; BH0301-5 ferrosilicon standard specimen contains vanadium and hangs down very much and can ignore; It is 52.82% that FeV50-A-2 vanadium iron standard specimen contains the vanadium standard value, and GBW01422 ferrosilicon standard specimen contains vanadium and hangs down very much and can ignore, and it is 81.12% that GSBH42005-92 vanadium iron standard specimen contains the vanadium standard value.
Visible by table 1, have very high accuracy and precision according to the method for the content of vanadium of the mensuration silicon vanadium iron of example 1.
Example 2:
Take by weighing 0.20g (being accurate to 0.0001g) test with silicon vanadium iron sample in polytetrafluoroethylene beaker (for synthetic standard sample; Take by weighing a certain amount of vanadium iron standard specimen and the synthetic standard specimen of a certain amount of ferrosilicon standard specimen work by table 2); Add 12mL concentration and be 60% nitric acid, dropwise drip concentration and be 36% hydrofluorite 3mL, heating makes sample dissolution complete; Add 5.5mL concentration and be 91% sulfuric acid, be heated to just and smolder.Take off polytetrafluoroethylene beaker from heating arrangement, cooling changes solution in the 500mL conical flask over to; Add 9mL concentration and be 80% phosphoric acid, be heated to and smolder 1 to 2 minute, take off polytetrafluoroethylene beaker from heating arrangement; Cool to room temperature adds 75mL concentration and is 13% sulfuric acid, shakes up; Be cooled to below 45 ℃, the liquor potassic permanganate that drips concentration and be 20g/L is to there being stable redness to occur, placement 2min; Add the urea liquid that 12mL concentration is 90g/L, with the excessive potassium permanganate of sodium nitrite solution reduction of 12g/L, and excessive 1; Place 2min, add 4 N-phenyl, be titrated to iron ammonium sulfate standard solution (0.02308mol/L) that to be bright green be terminal point for the ortho-aminobenzoic acid indicator.Calculate content of vanadium by the aforementioned calculation formula.
The N-phenyl that uses in this example is identical with the iron ammonium sulfate standard solution for the ortho-aminobenzoic acid indicator for the N-phenyl that uses in ortho-aminobenzoic acid indicator and iron ammonium sulfate standard solution and the example 1.
Mensuration result according to example 2 is illustrated in the following table 2.
Table 2
Wherein, It is 54.20% that FeV50-A-1 vanadium iron standard specimen contains the vanadium standard value; BH0301-5 ferrosilicon standard specimen contains vanadium and hangs down very much and can ignore; It is 52.82% that FeV50-A-2 vanadium iron standard specimen contains the vanadium standard value, and GBW01422 ferrosilicon standard specimen contains vanadium and hangs down very much and can ignore, and it is 81.12% that GSBH42005-92 vanadium iron standard specimen contains the vanadium standard value.
Visible by table 2, have very high accuracy and precision according to the method for the content of vanadium of the mensuration silicon vanadium iron of example 2.
Example 3:
Take by weighing 0.20g (being accurate to 0.0001g) test with silicon vanadium iron sample in polytetrafluoroethylene beaker (for synthetic standard sample; Take by weighing a certain amount of vanadium iron standard specimen and the synthetic standard specimen of a certain amount of ferrosilicon standard specimen work by table 3); Add 20mL concentration and be 68% nitric acid, dropwise drip concentration and be 38% hydrofluorite 6mL, heating makes sample dissolution complete; Add 6.5mL concentration and be 95% sulfuric acid, be heated to just and smolder.Take off polytetrafluoroethylene beaker from heating arrangement, cooling changes solution in the 500mL conical flask over to; Add 11mL concentration and be 82% phosphoric acid, be heated to and smolder 1 to 2 minute, take off polytetrafluoroethylene beaker from heating arrangement; Cool to room temperature adds 65mL concentration and is 15% sulfuric acid, shakes up; Be cooled to below 45 ℃, the liquor potassic permanganate that drips concentration and be 50g/L is to there being stable redness to occur, placement 5min; Add the urea liquid that 9mL concentration is 110g/L, with the excessive potassium permanganate of sodium nitrite solution reduction of 8g/L, and excessive 3; Place 3min, add 6 N-phenyl, be titrated to iron ammonium sulfate standard solution (0.02308mol/L) that to be bright green be terminal point for the ortho-aminobenzoic acid indicator.Calculate content of vanadium by the aforementioned calculation formula.
The N-phenyl that uses in this example is identical with the iron ammonium sulfate standard solution for the ortho-aminobenzoic acid indicator for the N-phenyl that uses in ortho-aminobenzoic acid indicator and iron ammonium sulfate standard solution and the example 1.
Mensuration result according to example 3 is illustrated in the following table 3.
Table 3
Wherein, It is 54.20% that FeV50-A-1 vanadium iron standard specimen contains the vanadium standard value; BH0301-5 ferrosilicon standard specimen contains vanadium and hangs down very much and can ignore; It is 52.82% that FeV50-A-2 vanadium iron standard specimen contains the vanadium standard value, and GBW01422 ferrosilicon standard specimen contains vanadium and hangs down very much and can ignore, and it is 81.12% that GSBH42005-92 vanadium iron standard specimen contains the vanadium standard value.
Visible by table 3, have very high accuracy and precision according to the method for the content of vanadium of the mensuration silicon vanadium iron of example 3.
According to the method for the content of vanadium of mensuration silicon vanadium iron of the present invention, can remove the interference that the existence of silicon is measured vanadium.In addition, can measure the content of the vanadium in the silicon vanadium iron quickly and accurately according to the method for the content of vanadium of mensuration silicon vanadium iron of the present invention.
Claims (5)
1. method of measuring the content of vanadium of silicon vanadium iron, said method comprises the steps:
(a) be that 60%～68% nitric acid mixes with silicon vanadium iron and concentration; With concentration is that 35%～40% hydrofluorite adds potpourri, and heating blends makes the dissolving of silicon vanadium iron fully, is that 90%～98% sulfuric acid adds potpourri with concentration then; Heating blends is to just smoldering; With the potpourri cooling, wherein, the milliliter number of nitric acid is 60～100 with the ratio of the gram number of silicon vanadium iron afterwards; The milliliter number of sulfuric acid is 27.5～32.5 with the ratio of the gram number of silicon vanadium iron, and the milliliter number of hydrofluorite is 15～30 with the ratio of the gram number of silicon vanadium iron;
(b) be that 80%～85% phosphoric acid adds potpourri with concentration, heating blends is to smoldering and keeping 1 minute to 2 minutes, and with the potpourri cooling, wherein, the milliliter number of phosphoric acid is 45～55 with the ratio of the gram number of silicon vanadium iron;
(c) be that 13%～15% sulfuric acid adds potpourri with concentration; And be cooled to below 45 ℃; Adding concentration to potpourri then is that the liquor potassic permanganate of 20g/L～50g/L is until there being stable redness to occur; Placed 2 minutes～5 minutes, wherein, the milliliter number of sulfuric acid is 325～375 with the ratio of the gram number of silicon vanadium iron;
(d) with concentration be the urea liquid adding potpourri of 90g/L～110g/L; Drip the excessive potassium permanganate of sodium nitrite solution reduction that concentration is 8g/L～12g/L to potpourri; And make excessive 1 to 3 of sodium nitrite solution; Potpourri was placed 1 minute～3 minutes, and wherein, the milliliter number of urea liquid is 45～60 with the ratio of the gram number of silicon vanadium iron;
(e) the N-phenyl is added potpourri for the ortho-aminobenzoic acid indicator, the iron ammonium sulfate standard solution with 0.020～0.025mol/L carries out titration to potpourri then, is titration end-point when the potpourri color becomes bright green;
(f) according to the content of vanadium W of computes silicon vanadium iron
V:
Wherein, C representes the amount of substance concentration of iron ammonium sulfate standard solution, and unit is mol/L,
V representes the volume of the iron ammonium sulfate standard solution that titration consumes, and unit is mL,
M representes the quality of silicon vanadium iron, and unit is g.
2. method according to claim 1, wherein, the N-phenyl is 1.5g/L～2.5g/L for the concentration of ortho-aminobenzoic acid indicator, the N-phenyl is 20～30 for the ratio that drips number and the gram number of silicon vanadium iron of ortho-aminobenzoic acid indicator: 1.
3. method according to claim 1, wherein, said method also comprises: with sulfuric acid dissolution six ferrous sulfate hydrate ammoniums and be diluted to standard volume and prepare the iron ammonium sulfate standard solution.
4. method according to claim 3, wherein, said method also comprises: use the potassium dichromate standard solution that the concentration of iron ammonium sulfate standard solution is demarcated.
5. method according to claim 1, wherein, said silicon vanadium iron comprises the Si of 10wt%～40wt%, the V of 25wt%～50wt% and the Fe of 10wt%～60wt%.
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| CN104483444A (en) * | 2014-12-10 | 2015-04-01 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of vanadium in nitrided ferrovanadium by oxidization and reduction |
| CN104515827A (en) * | 2014-12-10 | 2015-04-15 | 内蒙古包钢钢联股份有限公司 | Method for determination of vanadium in ferrovanadium by redox |
| CN105548164A (en) * | 2015-12-25 | 2016-05-04 | 北京有色金属研究总院 | Measuring method for content of titanium in titanium silicon |
| CN109655577A (en) * | 2018-12-25 | 2019-04-19 | 河钢股份有限公司承德分公司 | In sub-molten salt vanadium extracting process in sodium vanadate solution vanadium concentration detection method |
| CN109991362A (en) * | 2019-03-26 | 2019-07-09 | 南京钢铁股份有限公司 | The measuring method of silicone content in a kind of silicon vanadium iron |
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