CN105223307A - A kind of detection method for element silicon volumetric method in vanadium iron - Google Patents
A kind of detection method for element silicon volumetric method in vanadium iron Download PDFInfo
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- CN105223307A CN105223307A CN201410311170.1A CN201410311170A CN105223307A CN 105223307 A CN105223307 A CN 105223307A CN 201410311170 A CN201410311170 A CN 201410311170A CN 105223307 A CN105223307 A CN 105223307A
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Abstract
The invention provides a kind of detection method for element silicon volumetric method in vanadium iron, operating process be easy, testing cost is low, measurement result accurately and reliably.Technical scheme of the present invention comprises: take vanadium iron sample in beaker; Add appropriate dissolving acid, dissolving smolders takes off cooling after silicon dioxide silicon is separated out completely; Add distilled water, dissolution in low temperature and solubility salt; Filter while hot, use distilled water washing precipitation; Precipitation is dissolved in the beaker of teflon completely, in above-mentioned solution, adds potassium fluosilicate precipitation agent successively, fully stir.Cool in cooling bath after there is precipitation; Precipitation is leached, washing precipitation 2-3 time, with in standard solution of sodium hydroxide and remnants acid, there is stable rose close to adding indicator to solution during terminal; The mass percent of element silicon in vanadium iron sample is measured by formulae discovery.
Description
Technical field
The invention belongs to chemical analysis technology field, relate to a kind of detection technique for silicone content volumetric method in vanadium iron.
Background technology
Vanadium iron is a kind of important steel-making raw and auxiliary material, as alloy addition, is mainly used in alloy smelting steel.In steelmaking process, vanadium additive adds mainly with vanadium iron form, and vanadium iron is the ferroalloy of vanadium and iron composition, is used for greatly that the oxide of carbon, ferrosilicon or aluminium reducing vanadium or vanadium slag produce.Reductive agent and can require to select according to purposes, and content of vanadium is widely used in metallurgy at 35%-80% vanadium iron usually, petrochemical complex, machinery building, Aero-Space, the new technical field of national defense industry.Usual element silicon melting, in vanadium iron, makes vanadium iron have good superconductivity.And in vanadium iron the range of control of silicone content 1%-3%.
Detection technique patent and the report of silicone content volumetric method in vanadium iron is not found through update search.At present, the determination techniques of silicone content gravimetric method in vanadium iron is only had in GB, the detecting step of its method: molten sample-dehydration-filtration-calcination-weigh-hydrofluoric acid treatment-calcination again-weigh, pure platinum crucible and high-temperature electric resistance furnace must be used during calcination, cause testing inspection cost high, energy consumption is high, complex operation step, and sense cycle is long.
Summary of the invention
The technical problem to be solved in the present invention: a kind of detection method for element silicon volumetric method in vanadium iron is provided, operating process is easy, testing cost is low, measurement result accurately and reliably.
Technical scheme of the present invention: a kind of detection method for element silicon volumetric method in vanadium iron, comprising:
Take vanadium iron sample, the described vanadium iron sample scope of weighing is that 1.0000g ± 0.1g is accurate to 0.0001g in 350 ml beakers;
Add the nitric acid of 10 milliliters of 1:1,15 milliliters of density are the hydrochloric acid of ρ 1.19g/ml, and low-temperature heat adds the sulfuric acid of 25 milliliters of 1:1, continues to be heated to emit sulfuric acid dense smoke 3 ~ 5 minutes, until silicon takes off cooling after separating out completely after decomposing;
Add 100 ml distilled waters, solubility salt is dissolved in low-temperature heat;
Filter, with 60 degrees Celsius of distilled water washing precipitations with middling speed quantitative filter paper and plastic funnel while hot; By precipitation about 3 milliliters, 40% hydrofluorite, be dissolved in completely in the beaker of teflon, blow a small amount of distilled water along wall of cup, fixing fabric structure is within 50 milliliters;
In above-mentioned solution, add 20% potassium fluoride solution 10 milliliters successively, 2 grams, potassium nitrate, stir with sticking plaster, after there is precipitation, in cooling bath, be cooled to 25 degree;
With Medium speed filter paper and plastic funnel, precipitation is leached, with the potassium nitrate solution of 5%, washing precipitation 2-3 time, precipitation is transferred in former polytetrafluoroethylene beaker together with filter paper;
Add potassium nitrate-ethanolic solution 15 milliliters, drip 0.1% phenolphthalein solution 15, with sour with remnants in 0.1mol/L standard solution of sodium hydroxide, to occurring stable rose, add boiling water 200 milliliters, with the titration of 0.1mol/L standard solution of sodium hydroxide, close to adding 0.1% phenolphthalein solution 10 during terminal, continuing to drop to solution and occurring stable rose;
Measured the mass percent of element silicon in vanadium iron sample by formulae discovery, described formula is: Si%=C × V × 0.007068 × 100/G;
In formula: the concentration of C-standard solution of sodium hydroxide, unit is mol/L; The volume of V-consumption standard solution of sodium hydroxide, unit is ml; The milligramequivalent of 0.007068-silicon; Weighing of G-vanadium iron sample, unit is g.
Beneficial effect of the present invention: this method is by twice precipitation, after making silicon form potassium fluosilicate, with the silicon in sodium hydroxide titration vanadium iron sample, without the need to the high-temperature electric resistance furnace of the pure platinum crucible and high energy consumption that use high cost, not only operating process is easy, testing cost is low, energy consumption is low, sense cycle is short simultaneously, and measurement result accurately and reliably.
Embodiment
The invention provides a kind of detection method for element silicon volumetric method in vanadium iron, comprising:
Take vanadium iron sample, the described vanadium iron sample scope of weighing is that 1.0000g ± 0.1g is accurate to 0.0001g in 350 ml beakers.
Add the nitric acid of 10 milliliters of 1:1,15 milliliters of density are the hydrochloric acid of ρ 1.19g/ml, and low-temperature heat adds the sulfuric acid of 25 milliliters of 1:1, continues to be heated to emit sulfuric acid dense smoke 3 ~ 5 minutes, until silicon takes off cooling after separating out completely after decomposing.
Add 100 ml distilled waters, solubility salt is dissolved in low-temperature heat.
Filter, with 60 degrees Celsius of distilled water washing precipitations with middling speed quantitative filter paper and plastic funnel while hot; By precipitation about 3 milliliters, 40% hydrofluorite, be dissolved in completely in the beaker of teflon, blow a small amount of distilled water along wall of cup, fixing fabric structure is within 50 milliliters.
In above-mentioned solution, add 20% potassium fluoride solution 10 milliliters successively, 2 grams, potassium nitrate, stir with sticking plaster, after there is precipitation, in cooling bath, be cooled to 25 degree.
With Medium speed filter paper and plastic funnel, precipitation is leached, with the potassium nitrate solution of 5%, washing precipitation 2-3 time, precipitation is transferred in former polytetrafluoroethylene beaker together with filter paper.
Add potassium nitrate-ethanolic solution 15 milliliters, drip 0.1% phenolphthalein solution 15, with sour with remnants in 0.1mol/L standard solution of sodium hydroxide, to occurring stable rose, add boiling water 200 milliliters, with the titration of 0.1mol/L standard solution of sodium hydroxide, close to adding 0.1% phenolphthalein solution 10 during terminal, continuing to drop to solution and occurring stable rose.
Measured the mass percent of element silicon in vanadium iron sample by formulae discovery, described formula is: Si%=C × V × 0.007068 × 100/G;
In formula: the concentration of C-standard solution of sodium hydroxide, unit is mol/L; The volume of V-consumption standard solution of sodium hydroxide, unit is ml; The milligramequivalent of 0.007068-silicon; Weighing of G-vanadium iron sample, unit is g.
Element silicon in vanadium iron is evaporated to smolder by sulfuric acid and makes silicic acid dehydration form polymeric silicicacid precipitation by this method, after filtration washing precipitation, under the condition of < 60 DEG C, pass through hydrofluoric acid dissolution, add appropriate potassium fluoride, the potassium fluosilicate making excessive potassium ion and silicon form slightly solubility precipitates, and precipitation is washed till close to neutral, utilizes the water-disintegrable of potassium fluosilicate after filtration, dissociate after hydrolysis hydrofluorite in the hot water, be indicator with phenolphthalein, sodium hydroxide titration, asks its result.
Below by embodiment, the invention will be further described:
Embodiment 1:
1. take vanadium iron standard model 1.0066g (standard model certificate si=1.31) and be accurate to 0.0001g in 350 ml beakers.
2. add 30 milliliters of nitric acid (1:1), 10 milliliters of hydrochloric acid (ρ 1.19g/ml), low-temperature heat adds 25 milliliters of sulfuric acid (1:1) after decomposing, continue to be heated to emit sulfuric acid dense smoke 3 ~ 5 minutes, until silicon takes off cooling after separating out completely.
3. add 100 ml distilled waters, solubility salt is dissolved in low-temperature heat.
4. filter, with 60 degree of distilled water washing precipitations with middling speed quantitative filter paper and plastic funnel while hot.By precipitation about 3 milliliters, 40% hydrofluorite, be dissolved in completely in the beaker of teflon, blow a small amount of distilled water along wall of cup, fixing fabric structure is within 50 milliliters.
5. in above-mentioned solution, add 15% potassium fluoride solution 10 milliliters successively, 2 grams, potassium nitrate, stir with sticking plaster, after there is precipitation, in cooling bath, be cooled to 25 degree.
6. with Medium speed filter paper and plastic funnel, precipitation is leached, with the potassium nitrate solution of 5%, washing precipitation 2-3 time, precipitation is transferred in former polytetrafluoroethylene beaker together with filter paper.
7. add potassium nitrate-ethanolic solution 15 milliliters, drip 0.1% phenolphthalein solution 15, with sour with remnants in 0.1036mol/L standard solution of sodium hydroxide, to occurring stable rose (now titration sodium hydrate content is not remembered).Add boiling water 200 milliliters, with the titration of 0.1036mol/L standard solution of sodium hydroxide, close to adding 0.1% phenolphthalein solution 10 during terminal, continuing to drop to solution and occurring stable rose.
The calculating of analysis result:
Si％＝0.1036×18.01×0.007068×100/1.0066＝1.31％
In formula: C---the concentration 0.1036mol/L of standard solution of sodium hydroxide
V---consume the volume 18.01ml of standard solution of sodium hydroxide
0.007068---the milligramequivalent of silicon
The 1.0066g that weighs of G---vanadium iron sample
Embodiment 2:
1. take vanadium iron sample 1.0035g and be accurate to 0.0001g in 350 ml beakers.
2. add 30 milliliters of nitric acid (1:1), 10 milliliters of hydrochloric acid (ρ 1.19g/ml), low-temperature heat adds 25 milliliters of sulfuric acid (1:1) after decomposing, continue to be heated to emit sulfuric acid dense smoke 3 ~ 5 minutes, until silicon takes off cooling after separating out completely.
3. add 100 ml distilled waters, solubility salt is dissolved in low-temperature heat.
4. filter, with 60 degree of distilled water washing precipitations with middling speed quantitative filter paper and plastic funnel while hot.By precipitation about 3 milliliters, 40% hydrofluorite, be dissolved in completely in the beaker of teflon, blow a small amount of distilled water along wall of cup, fixing fabric structure is within 50 milliliters.
5. in above-mentioned solution, add 15% potassium fluoride solution 10 milliliters successively, 2 grams, potassium nitrate, stir with sticking plaster, after there is precipitation, in cooling bath, be cooled to 25 degree.
6. with Medium speed filter paper and plastic funnel, precipitation is leached, with the potassium nitrate solution of 5%, washing precipitation 2-3 time, precipitation is transferred in former polytetrafluoroethylene beaker together with filter paper.
7. add potassium nitrate-ethanolic solution 15 milliliters, drip 0.1% phenolphthalein solution 15, with sour with remnants in 0.1036mol/L standard solution of sodium hydroxide, to occurring stable rose (now titration sodium hydrate content is not remembered).Add boiling water 200 milliliters, with the titration of 0.1036mol/L standard solution of sodium hydroxide, close to adding 0.1% phenolphthalein solution 10 during terminal, continuing to drop to solution and occurring stable rose.
The calculating of analysis result:
Si％＝0.1036×28.64×0.007068×100/1.0035＝2.09％
In formula: C---the concentration 0.1036mol/L of standard solution of sodium hydroxide
V---consume the volume 28.64ml of standard solution of sodium hydroxide
0.007068---the milligramequivalent of silicon
The 1.0035g that weighs of G a---vanadium iron
Embodiment 3:
1. take vanadium iron sample 1.0005g and be accurate to 0.0001g in 350 ml beakers.
2. add 30 milliliters of nitric acid (1:1), 10 milliliters of hydrochloric acid (ρ 1.19g/ml), low-temperature heat adds 25 milliliters of sulfuric acid (1:1) after decomposing, continue to be heated to emit sulfuric acid dense smoke 3 ~ 5 minutes, until silicon takes off cooling after separating out completely.
3. add 100 ml distilled waters, solubility salt is dissolved in low-temperature heat.
4. filter, with 60 degree of distilled water washing precipitations with middling speed quantitative filter paper and plastic funnel while hot.By precipitation about 3 milliliters, 40% hydrofluorite, be dissolved in completely in the beaker of teflon, blow a small amount of distilled water along wall of cup, fixing fabric structure is within 50 milliliters.
5. in above-mentioned solution, add 15% potassium fluoride solution 10 milliliters successively, 2 grams, potassium nitrate, stir with sticking plaster, after there is precipitation, in cooling bath, be cooled to 25 degree.
6. with Medium speed filter paper and plastic funnel, precipitation is leached, with the potassium nitrate solution of 5%, washing precipitation 2-3 time, precipitation is transferred in former polytetrafluoroethylene beaker together with filter paper.
7. add potassium nitrate-ethanolic solution 15 milliliters, drip 0.1% phenolphthalein solution 15, with sour with remnants in 0.1036mol/L standard solution of sodium hydroxide, to occurring stable rose (now titration sodium hydrate content is not remembered).Add boiling water 200 milliliters, with the titration of 0.1036mol/L standard solution of sodium hydroxide, close to adding 0.1% phenolphthalein solution 10 during terminal, continuing to drop to solution and occurring stable rose.
The calculating of analysis result:
Si％＝0.1036×37.98×0.007068×100/1.0005＝2.78％
In formula: C---the concentration 0.1036mol/L of standard solution of sodium hydroxide
V---consume the volume 37.98ml of standard solution of sodium hydroxide
0.007068---the milligramequivalent of silicon
The 1.0005g that weighs of G---vanadium iron
The present invention has following beneficial effect:
1. due to the silicon value in vanadium iron high (1.31), aluminum values is high (2.12) also, and aluminium ion can generate the most stable with fluorine ion is in an acidic solution AlF2+, because in solution, fluorinion concentration is high, produce fluoaluminate with aluminium to precipitate, can interference measurement be had a strong impact on, so this method adopts first precipitate and separate silicon, thoroughly can be separated with aluminium after forming silicic acid, eliminate aluminium and the mensuration of silicon value is disturbed.
2. the vanadium in vanadium iron is about 80%, so when divided silicon, adopt sulfuric acid to smolder and separate out precipitation better, perchloric acid smoked can generate vanadate, is difficult to isolated by filtration.
3. under the existence of excessive potassium ion, silicon can form secondary precipitate, generates the silicon fluoro acid potassium precipitation of slightly solubility, utilize the water-disintegrable of potassium fluosilicate, dissociate after hydrolysis hydrofluorite in the hot water, is indicator with phenolphthalein, sodium hydroxide titration, its terminal is obvious, measurement result accurate stable.
Claims (1)
1., for a detection method for element silicon volumetric method in vanadium iron, it is characterized in that, comprising:
Take vanadium iron sample, the described vanadium iron sample scope of weighing is that 1.0000g ± 0.1g is accurate to 0.0001g in 350 ml beakers;
Add the nitric acid of 10 milliliters of 1:1,15 milliliters of density are the hydrochloric acid of ρ 1.19g/ml, and low-temperature heat adds the sulfuric acid of 25 milliliters of 1:1, continues to be heated to emit sulfuric acid dense smoke 3 ~ 5 minutes, until silicon takes off cooling after separating out completely after decomposing;
Add 100 ml distilled waters, solubility salt is dissolved in low-temperature heat;
Filter, with 60 degrees Celsius of distilled water washing precipitations with middling speed quantitative filter paper and plastic funnel while hot; By precipitation about 3 milliliters, 40% hydrofluorite, be dissolved in completely in the beaker of teflon, blow a small amount of distilled water along wall of cup, fixing fabric structure is within 50 milliliters;
In above-mentioned solution, add 20% potassium fluoride solution 10 milliliters successively, 2 grams, potassium nitrate, stir with sticking plaster, after there is precipitation, in cooling bath, be cooled to 25 degree;
With Medium speed filter paper and plastic funnel, precipitation is leached, with the potassium nitrate solution of 5%, washing precipitation 2-3 time, precipitation is transferred in former polytetrafluoroethylene beaker together with filter paper;
Add potassium nitrate-ethanolic solution 15 milliliters, drip 0.1% phenolphthalein solution 15, with sour with remnants in 0.1mol/L standard solution of sodium hydroxide, to occurring stable rose, add boiling water 200 milliliters, with the titration of 0.1mol/L standard solution of sodium hydroxide, close to adding 0.1% phenolphthalein solution 10 during terminal, continuing to drop to solution and occurring stable rose;
Measured the mass percent of element silicon in vanadium iron sample by formulae discovery, described formula is: Si%=C × V × 0.007068 × 100/G;
In formula: the concentration of C-standard solution of sodium hydroxide, unit is mol/L; The volume of V-consumption standard solution of sodium hydroxide, unit is ml; The milligramequivalent of 0.007068-silicon; Weighing of G-vanadium iron sample, unit is g.
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| CN106226303A (en) * | 2016-08-23 | 2016-12-14 | 内蒙古包钢钢联股份有限公司 | A kind of assay method of silicone content in low-carbon ferrochromium |
| CN109030711A (en) * | 2018-06-28 | 2018-12-18 | 四川龙蟒钛业股份有限公司 | The measuring method of silicon in a kind of Phosphorus Slag |
| 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 |
| CN111257094A (en) * | 2020-02-28 | 2020-06-09 | 武汉科技大学 | Filter paper composite filtering method for precipitation quantitative separation |
| CN114965326A (en) * | 2022-07-28 | 2022-08-30 | 山东飞源气体有限公司 | Method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106226303A (en) * | 2016-08-23 | 2016-12-14 | 内蒙古包钢钢联股份有限公司 | A kind of assay method of silicone content in low-carbon ferrochromium |
| CN109030711A (en) * | 2018-06-28 | 2018-12-18 | 四川龙蟒钛业股份有限公司 | The measuring method of silicon in a kind of Phosphorus Slag |
| 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 |
| CN111257094A (en) * | 2020-02-28 | 2020-06-09 | 武汉科技大学 | Filter paper composite filtering method for precipitation quantitative separation |
| CN114965326A (en) * | 2022-07-28 | 2022-08-30 | 山东飞源气体有限公司 | Method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis |
| CN114965326B (en) * | 2022-07-28 | 2022-10-21 | 山东飞源气体有限公司 | Method for measuring nickel content in waste residue generated by nitrogen trifluoride electrolysis |
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