CN104390924A - Method for determining phosphorus in high-carbon silicon aluminum alloy by using photometric method - Google Patents
Method for determining phosphorus in high-carbon silicon aluminum alloy by using photometric method Download PDFInfo
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Abstract
The invention relates to a method for determining phosphorus in high-carbon silicon aluminum alloy by using a photometric method. The method comprises a control experiment and a sample determination test, wherein the control experiment comprises the following steps: respectively putting phosphorus standard solutions with same concentrations and gradient volumes in a beaker added with quantitative pure iron powder in advance and a beaker added with quantitative pure aluminum foil or pure aluminum powder in advance; adopting nitric acid-hydrofluoric acid to dissolve a sample to be detected, using perchloric acid to oxidize to orthophosphoric acid, and smoking until hydrofluoric acid is removed; transferring to a high beaker, immediately adding nitric acid, and then adding sodium nitrite until brown sediments disappear; boiling for 10S, adding ammonium molybdate and tartaric acid for shaking, adding ferric fluoride, and using stannous chloride to reduce into phosphomolybdenum blue, taking water as reference, and respectively measuring absorbance, drawing a working curve or calculating a regression equation at 680nm in a spectrophotometer; the sample determination test comprises the following steps: after carrying out the experimental procedures same with the control experiment in the beaker, measuring the absorbance at 680nm in the spectrophotometer, and contrasting the working curve or the regression equation of the control experiment to obtain the content of phosphorus.
Description
Technical field
The present invention relates to ferroalloy analysis field, particularly relate to the method for phosphorus in a kind of spectrphotometric method for measuring high-carbon silicon-aluminium alloy.
Background technology
High-carbon silicon-aluminium alloy is composite alloy, uses this kind of ferroalloy can add deoxidation and alloying element simultaneously, is namely deoxidizer, is also the adjuvant of alloy, is widely used in STEELMAKING PRODUCTION.Various ferroalloy, again according to the needs of steel-making, specifies many grades by the content of alloying element or carbon containing height, and considered critical impurity content.
Be mingled with some harmful elements in high-carbon silicon-aluminium alloy, be also brought in steel simultaneously, as: phosphorus.The too high levels of phosphorus, will affect plasticity and the toughness of steel, and easily occur cold short, in condensation process, the content of phosphorus is greatly important, high to the content requirement of phosphorus when high-carbon silicon-aluminium alloy is produced, and the content of phosphorus also determines grade, the price of high-carbon silicon-aluminium alloy simultaneously.Therefore the Accurate Determining carrying out phosphorus in high-carbon silicon-aluminium alloy is significant.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of fast, measure the method for phosphorus content in high-carbon silicon-aluminium alloy accurately and efficiently.
For reaching above-mentioned purpose, a kind of method utilizing phosphorus in spectrphotometric method for measuring high-carbon silicon-aluminium alloy of the present invention, it comprises the following steps:
Control test: get same concentrations respectively, the phosphorus mark liquid of gradient volume has added in the beaker of quantitative straight iron powder and quantitative fine aluminium pool or pure aluminium powder in advance, nitrate acid and hydrofluoric acid is adopted to dissolve sample to be tested, with perchloric acid oxidation to orthophosphoric acid, smolder to hydrofluorite and only do, transfer in beaker in tall form, add nitric acid immediately, add sodium nitrite again to disappear to tan precipitate, boil 10S, add ammonium molybdate and tartrate shake, add ferric flouride, and become P-Mo blue with Reduction with Stannous Chloride, take water as reference, absorbance is measured respectively in 680nm in spectrophotometer, drawing curve or calculating regression equation,
Sample determination is tested: in beaker, adopt nitrate acid and hydrofluoric acid to dissolve sample to be tested, with perchloric acid oxidation to orthophosphoric acid, smolder to hydrofluorite and only do, transfer in beaker in tall form, add nitric acid immediately, add sodium nitrite again to disappear to tan precipitate, boil 10S, add ammonium molybdate and tartrate shake, adding ferric flouride, and become P-Mo blue with Reduction with Stannous Chloride, take water as reference, in spectrophotometer in 680nm measure absorbance, contrast described control experiment working curve or regression equation contrast draw phosphorus content.
Comprise the following steps as the preferred wherein said method of phosphorus in spectrphotometric method for measuring high-carbon silicon-aluminium alloy that utilizes:
Control test: get 5ug/ml phosphorus mark liquid 0.00ml respectively, 0.50ml, 1.00ml, 1.50ml, 2.00ml, 2.50ml, 3.00ml is in the beaker having added 0.02500g straight iron powder and 0.02500g fine aluminium pool or pure aluminium powder in advance, add 10mL nitric acid, add 2-3mL hydrofluorite, dissolved samples on electric hot plate, after sample dissolves, add 5mL perchloric acid, continue to be heated to perchloric acid smoked, during perchloric acid smoked, temperature reaches 230 DEG C, hydrofluorite is caught up with and only removes hydrofluorite, take off, with the washing bottle that intermediate water is housed, solution is washed in 150mL beaker in tall form, wash 3-4 time, electric hot plate continues be heated to perchloric acid smoked, emit to clean dry, take off, add nitric acid 10mL immediately, add 3 sodium nitrites, boil 10S, add 5mL ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor immediately, shake 10S, adding 35mL sodium fluoride-stannous chloride mixed liquor, shake up, take water as reference, absorbance is measured respectively in 680nm place, drawing curve or calculating regression equation with spectrophotometer,
Sample determination is tested: take high-carbon silicon-aluminium alloy sample 0.0500g in polytetrafluoroethylene beaker, add 10mL nitric acid, add 2-3mL hydrofluorite, dissolved samples on electric hot plate, after sample dissolves, add 5mL perchloric acid, continue to be heated to perchloric acid smoked, during perchloric acid smoked, temperature reaches 230 DEG C, hydrofluorite is caught up with and only removes hydrofluorite, take off, with the washing bottle that intermediate water is housed, solution is washed in 150mL beaker in tall form, wash 3-4 time.Electric hot plate continues be heated to perchloric acid smoked, emit to clean dry, take off, add nitric acid 10mL immediately, add 3 sodium nitrites, boil 10S, add 5mL ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor immediately, shake 10S, adding 35mL sodium fluoride-stannous chloride mixed liquor, shake up, take water as reference, with spectrophotometer in 680nm place measure absorbance, contrast described control experiment working curve or regression equation contrast draw phosphorus content;
Wherein said concentration of nitric acid is 66.97%, described hydrofluoric acid concentration is 40%, described perchloric acid concentration is 70.15%, described sodium nitrite to be massfraction be 5% sodium nitrite in aqueous solution, described ammonium molybdate to be massfraction be 18% ammonium molybdate aqueous solution, described sodium potassium tartrate tetrahydrate to be massfraction be 18% aqueous sodium potassium tartrate, described ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor is the mixed liquor of described ammonium molybdate aqueous solution and described aqueous sodium potassium tartrate volume ratio 1:1, described sodium fluoride to be massfraction be 2.4% sodium fluoride aqueous solution, in described sodium fluoride-stannous chloride mixed liquor sodium fluoride aqueous solution belonging to often liter, add stannous chloride described in 2g and dissolve rear gained.
Wherein said ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor uses front absorbent cotton to filter.
Wherein said sodium fluoride-stannous chloride mixed liquor uses front absorbent cotton to filter.
The invention difference from existing technology is that the present invention achieves following technique effect:
The present invention establish a kind of fast, measure the method for phosphorus content in high-carbon silicon-aluminium alloy accurately and efficiently, can be used for production testing, Instructing manufacture technique.
Embodiment
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
1. method: adopt nitrate acid and hydrofluoric acid dissolved samples in vinyon beaker, with perchloric acid oxidation to orthophosphoric acid, smolders to clean dry, take off, transfer in 100mL beaker in tall form, add nitric acid immediately, add 3 sodium nitrites again to disappear to tan precipitate, boil 10S, removing oxides of nitrogen.Add ammonium molybdate, make it to generate phosphato-molybdic heteropolyacid with phosphoric acid, add the interference that silicon eliminated by tartrate, add sodium fluoride coordination iron, become P-Mo blue with Reduction with Stannous Chloride, measure absorbance in the hope of phosphorus amount.
2. reagent:
2.1 nitric acid (concentration is 66.97%);
2.2 hydrofluorite (concentration is 40%);
2.3 perchloric acid (concentration is 70.15%);
2.4 sodium nitrites (5%);
2.5 ammonium molybdates (18%);
2.6 sodium potassium tartrate tetrahydrates (18%);
2.7 ammonium molybdates-sodium potassium tartrate tetrahydrate mixed liquor: both volume ratio 1:1, existing with existing mixing, and filter with absorbent cotton;
2.8 sodium fluorides (2.4%);
2.9 sodium fluorides-stannous chloride mixed liquor: in often liter of Fluorinse (2.4%), adds after stannous chloride 2g dissolves and shakes up, matching while using, and use with absorbent cotton filtration again.
3. sampling and sample preparation: get sample preparation standard according to ferroalloy and carry out sample and produce.
4. sample weighting amount: take sample 0.0500g
5. analytical procedure:
Take high-carbon silicon-aluminium alloy sample 0.0500g in polytetrafluoroethylene beaker, add 10mL nitric acid, add 2-3mL hydrofluorite, dissolved samples on electric hot plate, after sample dissolves, add 5mL perchloric acid, continue to be heated to perchloric acid smoked, during perchloric acid smoked, temperature reaches 230 DEG C, hydrofluorite is caught up with and only removes hydrofluorite, take off, with the washing bottle that intermediate water is housed, solution is washed in 150mL beaker in tall form, wash 3-4 time.Electric hot plate continues be heated to perchloric acid smoked, emit to clean dry, take off, add nitric acid 10mL immediately, add 3 sodium nitrites, boil 10S, add 5mL ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor immediately, shake 10S, adding 35mL sodium fluoride-stannous chloride mixed liquor, shake up, take water as reference, measure in 680nm place with spectrophotometer, measurement result sees the following form.
Working curve is drawn:
(1) 5ug/ml phosphorus mark liquid 0.00ml is got respectively, 0.50ml, 1.00ml, 1.50ml, 2.00ml, 2.50ml, 3.00ml is in the polytetrafluoroethylene beaker having added 0.02500g straight iron powder and 0.02500g fine aluminium pool or pure aluminium powder (purity 99.9%) in advance, add 10mL nitric acid, add 2-3mL hydrofluorite, dissolved samples on electric hot plate, after sample dissolves, add 5mL perchloric acid, continue to be heated to perchloric acid smoked, during perchloric acid smoked, temperature reaches 230 DEG C, hydrofluorite is caught up with and only removes hydrofluorite, take off, with the washing bottle that intermediate water is housed, solution is washed in 150mL beaker in tall form, wash 3-4 time.Electric hot plate continues be heated to perchloric acid smoked, emit to clean dry, take off, add nitric acid 10mL immediately, add 3 sodium nitrites, boil 10S, add 5mL ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor immediately, shake 10S, adding 35mL sodium fluoride-stannous chloride mixed liquor, shake up, take water as reference, measure respectively in 680nm place with spectrophotometer, drawing curve or calculating regression equation.
(2) the standard specimen synchronous operation that content is close can be chosen, drawing curve.Calculate with equation of linear regression.
6. Analysis result calculation: calculate with equation of linear regression
Example:
7. sample analysis contrast:
Because high-carbon silicon-aluminium alloy does not have standard specimen, therefore generally monitor with ferrosilicon standard specimen.
As can be seen from the above table: use P-Mo blue photometric method to measure phosphorus content the data obtained in ferrosilicon accurate, and operating process is shorter, fast, efficient.
By this method, phosphorus content in high-carbon silicon-aluminium alloy can be determined accurately.Determination data is accurate, is applicable to the Fast Measurement that phosphorus in medium high carbon silicon-aluminium alloy is produced in application.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (4)
1. utilize a method for phosphorus in spectrphotometric method for measuring high-carbon silicon-aluminium alloy, it is characterized in that it comprises the following steps:
Control test: get same concentrations respectively, the phosphorus mark liquid of gradient volume has added in the beaker of quantitative straight iron powder and quantitative fine aluminium pool or pure aluminium powder in advance, nitrate acid and hydrofluoric acid is adopted to dissolve sample to be tested, with perchloric acid oxidation to orthophosphoric acid, smolder to hydrofluorite and only do, transfer in beaker in tall form, add nitric acid immediately, add sodium nitrite again to disappear to tan precipitate, boil 10S, add ammonium molybdate and tartrate shake, add ferric flouride, and become P-Mo blue with Reduction with Stannous Chloride, take water as reference, absorbance is measured respectively in 680nm in spectrophotometer, drawing curve or calculating regression equation,
Sample determination is tested: in beaker, adopt nitrate acid and hydrofluoric acid to dissolve sample to be tested, with perchloric acid oxidation to orthophosphoric acid, smolder to hydrofluorite and only do, transfer in beaker in tall form, add nitric acid immediately, add sodium nitrite again to disappear to tan precipitate, boil 10S, add ammonium molybdate and tartrate shake, adding ferric flouride, and become P-Mo blue with Reduction with Stannous Chloride, take water as reference, in spectrophotometer in 680nm measure absorbance, contrast described control experiment working curve or regression equation contrast draw phosphorus content.
2. the method utilizing phosphorus in spectrphotometric method for measuring high-carbon silicon-aluminium alloy according to claim 1, is characterized in that it comprises the following steps:
Control test: get 5ug/ml phosphorus mark liquid 0.00ml respectively, 0.50ml, 1.00ml, 1.50ml, 2.00ml, 2.50ml, 3.00ml is in the beaker having added 0.02500g straight iron powder and 0.02500g fine aluminium pool or pure aluminium powder in advance, add 10mL nitric acid, add 2-3mL hydrofluorite, dissolved samples on electric hot plate, after sample dissolves, add 5mL perchloric acid, continue to be heated to perchloric acid smoked, during perchloric acid smoked, temperature reaches 230 DEG C, hydrofluorite is caught up with and only removes hydrofluorite, take off, with the washing bottle that intermediate water is housed, solution is washed in 150mL beaker in tall form, wash 3-4 time, electric hot plate continues be heated to perchloric acid smoked, emit to clean dry, take off, add nitric acid 10mL immediately, add 3 sodium nitrites, boil 10S, add 5mL ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor immediately, shake 10S, adding 35mL sodium fluoride-stannous chloride mixed liquor, shake up, take water as reference, absorbance is measured respectively in 680nm place, drawing curve or calculating regression equation with spectrophotometer,
Sample determination is tested: take high-carbon silicon-aluminium alloy sample 0.0500g in polytetrafluoroethylene beaker, add 10mL nitric acid, add 2-3mL hydrofluorite, dissolved samples on electric hot plate, after sample dissolves, add 5mL perchloric acid, continue to be heated to perchloric acid smoked, during perchloric acid smoked, temperature reaches 230 DEG C, hydrofluorite is caught up with and only removes hydrofluorite, take off, with the washing bottle that intermediate water is housed, solution is washed in 150mL beaker in tall form, wash 3-4 time.Electric hot plate continues be heated to perchloric acid smoked, emit to clean dry, take off, add nitric acid 10mL immediately, add 3 sodium nitrites, boil 10S, add 5mL ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor immediately, shake 10S, adding 35mL sodium fluoride-stannous chloride mixed liquor, shake up, take water as reference, with spectrophotometer in 680nm place measure absorbance, contrast described control experiment working curve or regression equation contrast draw phosphorus content;
Wherein said concentration of nitric acid is 66.97%, described hydrofluoric acid concentration is 40%, described perchloric acid concentration is 70.15%, described sodium nitrite to be massfraction be 5% sodium nitrite in aqueous solution, described ammonium molybdate to be massfraction be 18% ammonium molybdate aqueous solution, described sodium potassium tartrate tetrahydrate to be massfraction be 18% aqueous sodium potassium tartrate, described ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor is the mixed liquor of described ammonium molybdate aqueous solution and described aqueous sodium potassium tartrate volume ratio 1:1, described sodium fluoride to be massfraction be 2.4% sodium fluoride aqueous solution, in described sodium fluoride-stannous chloride mixed liquor sodium fluoride aqueous solution belonging to often liter, add stannous chloride described in 2g and dissolve rear gained.
3. the method utilizing phosphorus in spectrphotometric method for measuring high-carbon silicon-aluminium alloy according to claim 2, is characterized in that: described ammonium molybdate-sodium potassium tartrate tetrahydrate mixed liquor uses front absorbent cotton to filter.
4. the method utilizing phosphorus in spectrphotometric method for measuring high-carbon silicon-aluminium alloy according to claim 2, is characterized in that: described sodium fluoride-stannous chloride mixed liquor uses front absorbent cotton to filter.
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| CN107132192A (en) * | 2017-05-26 | 2017-09-05 | 内蒙古包钢钢联股份有限公司 | The rapid colorimetric determination method of phosphorus in silicon steel |
| CN113670835A (en) * | 2021-07-20 | 2021-11-19 | 包头钢铁（集团）有限责任公司 | Method for analyzing phosphorus content in serpentine |
| CN114858969A (en) * | 2022-05-11 | 2022-08-05 | 包头钢铁（集团）有限责任公司 | Method for analyzing content of phosphorus in fluorite |
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