CN102928425B - Method for determining vanadium in silicon-vanadium alloy - Google Patents
Method for determining vanadium in silicon-vanadium alloy Download PDFInfo
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- CN102928425B CN102928425B CN201210428259.7A CN201210428259A CN102928425B CN 102928425 B CN102928425 B CN 102928425B CN 201210428259 A CN201210428259 A CN 201210428259A CN 102928425 B CN102928425 B CN 102928425B
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Abstract
The invention belongs to the field of analytical chemistry, and particularly relates to a method for determining vanadium in a silicon-vanadium alloy. According to the method for determining vanadium in a silicon-vanadium alloy, the vanadium is determined by a steel and alloy chemical analysis method-ammonium ferrous sulfate titration method, and hydrofluoric acid is added after concentrated hydrochloric acid is added. Through the invention, the defect of relatively low determination result is overcome, and an accurate method for determining vanadium in a silicon-vanadium alloy is obtained.
Description
Technical field
The invention belongs to analytical chemistry field, be specifically related to the assay method of vanadium in silicon vanadium alloy.
Background technology
Silicon in silicon vanadium alloy, vanadium mainly exist with the form of simple substance, wherein containing a small amount of silicon vanadium eutectic; During chemical analysis, silicon, the v element of simple substance are soluble in acid, but silicon vanadium eutectic is then difficult to dissolve with acid solution, causes the analysis deviation of content of vanadium.
Summary of the invention
For above-mentioned defect, the invention provides the assay method of vanadium in a kind of silicon vanadium alloy, utilize the method can the content of vanadium in Accurate Determining silicon vanadium alloy.
Technical scheme of the present invention is:
The assay method of vanadium in silicon vanadium alloy, according to steel and alloy chemical analysis method-ferrous ammonium sulfate titration, and adds hydrofluorite after adding concentrated hydrochloric acid.
The assay method of vanadium in above-mentioned silicon vanadium alloy, concrete steps are:
1) detection sample comminution is made its granularity < 180 order, take 0.15g sample in acid-resistant container, add 8 ~ 10ml water and make sample soak disperse, add 8 ~ 10ml red fuming nitric acid (RFNA) successively again, 4 ~ 5ml concentrated hydrochloric acid, 5 ~ 6ml hydrofluorite, sample dissolution under room temperature; Then, add 35 ~ 40ml sulfuric acid, be heated to sulfuric acid and smolder 2-3min, take off, cooling; Add 8 ~ 10ml phosphoric acid and 70 ~ 80ml water afterwards, heating for dissolving salt, is cooled to room temperature after boiling;
2) in sample, add the mixing of 5 ~ 6ml l ferrous ammonium sulfate solution, the stable aubergine that presents direct dropping liquor potassic permanganate to test solution after shake does not take off, and excessive 1-2 drips, abundant shake also leaves standstill 5 minutes, add urea 0.5 ~ 1.0g, drip sodium nitrite solution again to disappear to aubergine, and excessive 1-2 drips, place and add 3-5 after 2-3 minute and drip benzene for adjacent aminobenzene potassium acid solution, being titrated to solution with iron ammonium sulfate standard solution again, to become bright green from aubergine be terminal, according to the volume of consumed iron ammonium sulfate standard solution, the content calculating vanadium in sample is carried out by following formula:
In formula, the massfraction of W-vanadium, %; The concentration of C-iron ammonium sulfate standard solution, mol/L; The volume of V-iron ammonium sulfate standard solution, mL; M-takes sample mass, g; The molal weight of 50.94-vanadium, g/mol.
Preferably, the concentration of described sulfuric acid is 18mol/L, and density is 1.84g/L; The concentration of hydrochloric acid is 12mol/L, and density is 1.19g/L; The concentration of nitric acid is 16mol/L, and density is 1.42g/L; The concentration of phosphoric acid is 15mol/L, and density is 1.69g/L.
Preferably, the concentration of described iron ammonium sulfate standard solution is 0.05mol/L, and the concentration of liquor potassic permanganate is 3g/L, and the concentration of urea is 200g/l, and the concentration of sodium nitrite solution is 20g/L, and benzene is 2g/L for the concentration of adjacent aminobenzene potassium acid solution.
Beneficial effect of the present invention:
The invention solves the technical matters of the assay method of vanadium in silicon vanadium alloy, fill up the blank in the assay method field of vanadium in silicon vanadium alloy.Solve the defect that measurement result is on the low side, obtain a kind of assay method reliably.
Embodiment
The assay method of vanadium in silicon vanadium alloy, measures according to steel and alloy chemical analysis method-ferrous ammonium sulfate titration (GB/T223.13-2000), and add hydrofluorite after adding concentrated hydrochloric acid.
The assay method of vanadium in silicon vanadium alloy, concrete steps are:
1) detection sample comminution is made its granularity < 180 order, take 0.15g sample in acid-resistant container, add 8 ~ 10ml water and make sample soak disperse, add 8 ~ 10ml red fuming nitric acid (RFNA) successively again, 4 ~ 5ml concentrated hydrochloric acid, 5 ~ 6ml hydrofluorite, sample dissolution under room temperature; Then, add 35 ~ 40ml sulfuric acid, be heated to sulfuric acid and smolder 2-3min, take off, cooling; Add 8 ~ 10ml phosphoric acid and 70 ~ 80ml water afterwards, heating for dissolving salt, is cooled to room temperature after boiling;
2) in sample, add the mixing of 5 ~ 6ml l ferrous ammonium sulfate solution, the stable aubergine that presents direct dropping liquor potassic permanganate to test solution after shake does not take off, and excessive 1-2 drips, abundant shake also leaves standstill 5 minutes, add urea 0.5 ~ 1.0g, drip sodium nitrite solution again to disappear to aubergine, and excessive 1-2 drips, place and add 3-5 after 2-3 minute and drip benzene for adjacent aminobenzene potassium acid solution, being titrated to solution with iron ammonium sulfate standard solution again, to become bright green from aubergine be terminal, according to the volume of consumed iron ammonium sulfate standard solution, the content calculating vanadium in sample is carried out by following formula:
In formula, the massfraction of W-vanadium, %; The concentration of C-iron ammonium sulfate standard solution, mol/L; The volume of V-iron ammonium sulfate standard solution, mL; M-takes sample mass, g; The molal weight of 50.94-vanadium, g/mol.
In the inventive method, because various acid effect is in the reaction different, must progressively add various acid according to said sequence.Wherein, nitric acid: be that the nitrate that strong oxidizer and metal reaction generate is soluble in water; Hydrochloric acid: form acid mixture with nitric acid effect, promotes that sample dissolves; Hydrofluorite: be a kind of weak acid, has very strong mating reaction, mixes as solvent with nitric acid, sulfuric acid etc., removing SiO
2, to measure other components.
In the inventive method, in sulfuric-phosphoric medium, use potassium permanganate oxidation vanadium, excessive potassium permanganate reduces with sodium nitrite, excessive sodium nitrite urea decomposition, sour for indicator for adjacent aminobenzene potassium with benzene.
In order to understand the present invention better, further illustrate the present invention below in conjunction with embodiment.
Embodiment 1
Take 0.1500g silicon vanadium alloy standard specimen (model SL25--09) and be placed in 500mL conical flask, add about 10 ml waters and soak sample, add 10 milliliters of red fuming nitric acid (RFNA)s, 5 milliliters of concentrated hydrochloric acids add 5ml hydrofluorite, sample dissolution under room temperature, then add 40 milliliters of sulfuric acid (1:1) to be placed in and electric furnace to be heated to sample and to dissolve to be evaporated to completely and emit sulfuric acid cigarette within 2-3 minute, to take off, cool, add phosphoric acid (1:1) 10 milliliters and 80 ml waters, heating for dissolving salt, take off after boiling and be cooled to room temperature;
5 milliliters of iron ammonium sulfate mixings are added in sample, after direct dropping liquor potassic permanganate to shake, solution presents micro-aubergine and not to disappear and excessive 1-2 drips and fully shakes and leave standstill 5 minutes, add urea 1g, drip sodium nitrite solution to aubergine more just to disappear and excessive 1-2 drips, place and add 3-5 after 2-3 minute and drip benzene for adjacent aminobenzene potassium acid solution, being titrated to solution with iron ammonium sulfate standard solution, to become bright green from aubergine be terminal;
According to the volume of consumed iron ammonium sulfate standard solution, carry out result calculating by following formula, obtain the content of vanadium in standard specimen:
In formula, the massfraction of W-vanadium, %; The concentration of C-iron ammonium sulfate standard solution, mol/L; The volume of V-iron ammonium sulfate standard solution, mL; M-takes sample mass, g; The molal weight of 50.94-vanadium, g/mol; The results are shown in Table 1.
Embodiment 2: take the method for testing that 0.1500g silicon vanadium alloy standard specimen (model SL25--09) adopts embodiment 1, be only not add hydrofluorite with the difference of embodiment 1, acquired results is as shown in table 1.
Embodiment 3: take the method test that 0.1500g silicon vanadium alloy 1# sample adopts embodiment 1, acquired results is as shown in table 1.
Embodiment 4: take the method test that 0.1500g silicon vanadium alloy 1# sample adopts embodiment 1, be only not add hydrofluorite with the difference of embodiment 1, acquired results is as shown in table 1.
In the present invention, because iron ammonium sulfate standard solution to place in air easily deliquescence, for making test result more accurate, generally standard specimen and sample synchronously carried out, also can convert with the content of vanadium of standard specimen during calculating, reduction formula is:
The measured value of the vanadium of table 1 standard specimen and sample
| Sample | Standard value, (%) | Measured value, (%) | Remarks |
| Embodiment 1 | 37.63 | 37.51 | Add hydrofluorite |
| Embodiment 2 | 37.63 | 37.21 | Do not add hydrofluorite |
| Embodiment 3 | / | 36.91 | Add hydrofluorite |
| Embodiment 4 | / | 34.46 | Do not add hydrofluorite |
Claims (3)
1. the assay method of vanadium in silicon vanadium alloy, is characterized in that, comprise the following steps:
1) silicon vanadium alloy sample comminution is made its granularity < 180 order, take 0.15g sample in acid-resistant container, add 8 ~ 10ml water and make sample soak disperse, add 8 ~ 10ml red fuming nitric acid (RFNA) successively again, 4 ~ 5ml concentrated hydrochloric acid, 5 ~ 6ml hydrofluorite, sample dissolution under room temperature; Then, add 35 ~ 40ml sulfuric acid, be heated to sulfuric acid and smolder 2-3min, take off, cooling; Add 8 ~ 10ml phosphoric acid and 70 ~ 80ml water afterwards, heating for dissolving salt, is cooled to room temperature after boiling;
2) in silicon vanadium alloy sample, add the mixing of 5 ~ 6ml l ferrous ammonium sulfate solution, the stable aubergine that presents direct dropping liquor potassic permanganate to test solution after shake does not take off, and excessive 1-2 drips, abundant shake also leaves standstill 5 minutes, add urea 0.5 ~ 1.0g, drip sodium nitrite solution again to disappear to aubergine, and excessive 1-2 drips, place and add 3-5 after 2-3 minute and drip benzene for adjacent aminobenzene potassium acid solution, being titrated to solution with iron ammonium sulfate standard solution again, to become bright green from aubergine be terminal, according to the volume of consumed iron ammonium sulfate standard solution, the content calculating vanadium in sample is carried out by following formula:
In formula, the massfraction of W-vanadium, %; The concentration of C-iron ammonium sulfate standard solution, mol/L; The volume of V-iron ammonium sulfate standard solution, ml; M-takes sample mass, g; The molal weight of 50.94-vanadium, g/mol.
2. the assay method of vanadium in silicon vanadium alloy according to claim 1, is characterized in that: the concentration of described sulfuric acid is 18mol/L, and density is 1.84g/L; The concentration of hydrochloric acid is 12mol/L, and density is 1.19g/L; The concentration of nitric acid is 16mol/L, and density is 1.42g/L; The concentration of phosphoric acid is 15mol/L, and density is 1.69g/L.
3. the assay method of vanadium in silicon vanadium alloy according to claim 1, it is characterized in that: the concentration of described iron ammonium sulfate standard solution is 0.05mol/L, the concentration of liquor potassic permanganate is 3g/L, the concentration of urea is 200g/l, the concentration of sodium nitrite solution is 20g/L, and benzene is 2g/L for the concentration of adjacent aminobenzene potassium acid solution.
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| CN103439330B (en) * | 2013-08-30 | 2016-05-18 | 天津长芦华信化工股份有限公司 | The detection method of vanadium pentafluoride product purity |
| CN105424685A (en) * | 2015-11-07 | 2016-03-23 | 武钢集团昆明钢铁股份有限公司 | Method for detecting content of manganese in manganous-rich slag |
| CN107121426B (en) * | 2017-04-27 | 2019-12-03 | 攀钢集团研究院有限公司 | Clear up the method for vanadium chromium titanium alloy and the detection method of digestion solution |
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| CN102507556B (en) * | 2011-10-31 | 2013-05-08 | 攀钢集团江油长城特殊钢有限公司 | Method for measuring vanadium content of silicon ferrovanadium |
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