CN102539426A - Method for determining phosphorus in silicon-manganese alloy - Google Patents
Method for determining phosphorus in silicon-manganese alloy Download PDFInfo
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- CN102539426A CN102539426A CN201210003800XA CN201210003800A CN102539426A CN 102539426 A CN102539426 A CN 102539426A CN 201210003800X A CN201210003800X A CN 201210003800XA CN 201210003800 A CN201210003800 A CN 201210003800A CN 102539426 A CN102539426 A CN 102539426A
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Abstract
The invention discloses a method for determining phosphorus in silicon-manganese alloy, which comprises the steps of: dissolving a test sample by using nitric acid and hydrofluoric acid and adding perchloric acid to convert phosphorus in the test sample into orthophosphoric acid to obtain fist mixed solution; adding sodium sulfite into the first mixed solution to reduce manganese in the silicon-manganese alloy to obtain second mixed solution; and adding bismuth nitrate solution, ammonium molybdate solution, potassium sodium tartrate solution, sodium fluoride and stannous chloride into the second mixed solution, wherein ammonium molybdate can convert the orthophosphoric acid in the first mixed solution into phosphorus-molybdenum heteropoly acid, using stannous chloride to reduce the formed phosphorus-molybdenum heteropoly acid into blue phosphomolybdenum blue and finally using a spectrophotometric method to determine the content of the phosphorus. Compared with the prior art, by using the stannous chloride as the reducing agent, since the stannous chloride has the characteristics of high reducing speed, good reducing effect and the like, the analysis time of the determination method is shorter, the accuracy and the stability of the determination result are improved and the method is suitable for field mass production analysis.
Description
Technical field
The present invention relates to the silicomangan technical field, more particularly, relate to the assay method of phosphorus in a kind of silicomangan.
Background technology
The alloy that silicomangan is made up of manganese, silicon, iron, carbon and other element is the primary raw material that alloy smelting steel and low alloy steel are produced, and the quality of its quality directly influences the quality of steel and the machining property of steel.Impurity element phosphorus in the manganese-silicon is a kind of harmful element, can make steel produce cold short phenomenon, and therefore, the content of measuring phosphorus in the manganese-silicon is significant for instructing STEELMAKING PRODUCTION.Further, because phosphorus content can obviously descend greater than the performance of 0.25% silicomangan, so the mensuration result's of phosphorus content accuracy is significant equally.
The existing national standard analytical approach of the mensuration of phosphorus is seen GB/T5686.4-1998 in the manganese-silicon.In addition, common method is in the presence of bismuth salt at present, and adopting anhydrous sodium sulfite, sodium thiosulfate and ascorbic acid to mix colour developing liquid is reductive agent; In sample, add ammonium molybdate and generate phosphato-molybdic heteropolyacid; Is that reductive agent is reduced to the phosphorus molybdenum blue with the phosphato-molybdic heteropolyacid that forms with the ascorbic acid, measures its absorbance then, concrete steps are: taking by weighing sample, to place material be the beaker of teflon; Add nitric acid; Drip hydrofluorite then with sample dissolution, add perchloric acid heating again and smolder phosphorus oxidation to be orthophosphoric acid, to be dissolved in surely in the 100ml volumetric flask; Draw mother liquor 10ml in the volumetric flask of 100ml; Add the 5ml mass concentration and be 3% bismuth nitrate solution and 5ml mass concentration and be 4% ammonium molybdate solution; The mixing developer that adds sodium thiosulfate, sodium sulphite and ascorbic acid heats in boiling water after as reductive agent, and with 7504 type spectrophotometers, wavelength is 680nm after 10 minutes; The cuvette of 2cm carries out colorimetric estimation, thereby measures the content that obtains phosphorus in the manganese-silicon.
The assay method of the phosphorus of prior art report is reductive agent with the ascorbic acid; Needing to wait for 10 minutes after the colour developing just stablizes and less stable; Therefore, there is long, the unsettled shortcoming of analysis result analysis time in this assay method, is not suitable for the on-the-spot analysis of producing in enormous quantities.The inventor considers, the assay method of phosphorus in a kind of silicomangan is provided, and shortens analysis time, increases analytical accuracy.
Summary of the invention
In view of this, the technical matters that the present invention will solve is to provide the assay method of phosphorus in a kind of silicomangan, and this assay method is shorter analysis time, and the accuracy of measuring the result is higher.
In order to solve above technical matters, the present invention provides the assay method of phosphorus in a kind of silicomangan, may further comprise the steps:
Silicomangan sample, nitric acid, hydrofluorite and perchloric acid are mixed, and the reaction back forms first mixed solution;
In said first mixed solution, add sodium sulphite, obtain second mixed solution after the reaction;
In said second mixed solution, add bismuth nitrate solution, ammonium molybdate solution, potassium sodium tartrate solution, Fluorinse and stannous chloride, obtain the 3rd mixed solution after the reaction;
Utilize the absorbance of said the 3rd mixed solution of spectrophotometry, obtain the phosphorus content in the silicomangan at 680～700nm place.
Preferably, the mass and size concentration of said bismuth nitrate solution is 5g/L.
Preferably, the mass concentration of said ammonium molybdate solution is 9%.
Preferably, the mass concentration of said potassium sodium tartrate solution is 9%.
Preferably, the volume ratio of said ammonium molybdate solution and said potassium sodium tartrate solution is 1: 1.
Preferably, the mass concentration of said Fluorinse is 2%.
Preferably, said Fluorinse is 100ml: 0.5g with the volume mass ratio of stannous chloride.
Preferably, the acidity of said the 3rd mixed solution is 0.6～1.0mol/L.
Preferably, utilize the absorbance of said second mixed solution of spectrophotometry at the 690nm place.
Preferably, the said step that obtains the 3rd mixed solution is specially:
Step a) adds bismuth nitrate solution, ammonium molybdate solution and potassium sodium tartrate solution in said second mixed solution, heat in boiling water bath the vibration back;
Step b) adds Fluorinse and stannous chloride in the mixed solution that said step a) obtains, obtain the 3rd mixed solution after the reaction.
The present invention provides the assay method of phosphorus in a kind of silicomangan, utilize nitric acid and hydrofluorite with sample dissolution after, add perchloric acid the phosphorus in the sample be converted into orthophosphoric acid, obtain first mixed solution; In said first mixed solution, add sodium sulphite,, obtain second mixed solution the reduction of the manganese in the silicomangan; In said second mixed solution, add bismuth nitrate solution, ammonium molybdate solution, potassium sodium tartrate solution, Fluorinse and stannous chloride; Wherein ammonium molybdate makes the orthophosphoric acid in first mixed solution be converted into phosphato-molybdic heteropolyacid; And utilize stannous chloride that the phosphato-molybdic heteropolyacid that forms is reduced to blue phosphorus molybdenum blue, utilize spectrophotometry to obtain the content of phosphorus then.Compared with prior art; The present invention is reductive agent with the stannous chloride, and reduction rate is fast, reduction effect good because it has, thereby makes this assay method shorter analysis time; And increased accuracy and the stability of measuring the result, be fit to the on-the-spot analysis of producing in enormous quantities.
Embodiment
Carry out clear, intactly description in the face of the technical scheme in the embodiment of the invention down, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills are not making the every other embodiment that is obtained under the creative work prerequisite, all belong to the scope of the present invention's protection.
The invention discloses the assay method of phosphorus in a kind of silicomangan, may further comprise the steps:
Silicomangan sample, nitric acid, hydrofluorite and perchloric acid are mixed, and the reaction back forms first mixed solution;
In said first mixed solution, add sodium sulphite, obtain second mixed solution after the reaction;
In said second mixed solution, add bismuth nitrate solution, ammonium molybdate solution, potassium sodium tartrate solution, Fluorinse and stannous chloride, obtain the 3rd mixed solution after the reaction;
Utilize the absorbance of said the 3rd mixed solution of spectrophotometry, obtain the phosphorus content in the silicomangan at 680～700nm place.
In above-mentioned preparation process, the present invention utilizes nitric acid and hydrofluorite with sample dissolution, and perchloric acid is converted into orthophosphoric acid with the phosphorus in the sample simultaneously; Manganese in the silicomangan is reduced second mixed solution that obtains clarifying through the sodium sulphite that adds then; Ammonium molybdate makes the orthophosphoric acid in second mixed solution be converted into phosphato-molybdic heteropolyacid, and utilizes stannous chloride that the phosphato-molybdic heteropolyacid that forms is reduced to blue phosphorus molybdenum blue, thereby obtains the content of phosphorus in the manganese alloy through spectrophotometry.
The said step that obtains first mixed solution is specially: it is the container of teflon that the silicomangan sample is placed material, in said container, adds nitric acid and hydrofluorite successively, and said hydrofluorite preferably adopts the mode of dropping; In said container, add perchloric acid and heating then, obtain first mixed solution after concentrating.In above-mentioned steps, said nitric acid and hydrofluorite are used for said sample dissolution, and the dropping mode that said hydrofluorite preferably adopts helps fully contacting between hydrofluorite and the sample.Nitric acid, hydrofluorite and perchloric acid that the present invention adopts are respectively commercial red fuming nitric acid (RFNA), dense hydrofluorite and dense perchloric acid, and density is respectively 1.40g/ml, 1.3g/ml and 1.68g/ml.Because the hot strong solution of perchloric acid has stronger oxidisability, therefore, perchloric acid is converted into orthophosphoric acid with the phosphorus in the sample, and reaction as follows takes place:
10HClO
4(dense)+14P+16H
2The O==Δ==14H3PO
4+ 5Cl
2Individual
After obtaining first mixed solution, in said first mixed solution, add sodium sulphite, the manganese reaction in sodium sulphite and the silicomangan makes the state of second mixed solution for clarifying that obtains.The sodium sulphite that the present invention adopts is preferably anhydrous sodium sulfite, and mass and size concentration is preferably 100g/L.
In addition; The present invention also comprises the step that in said second mixed solution, adds bismuth nitrate solution, ammonium molybdate solution, potassium sodium tartrate solution, Fluorinse and stannous chloride; This step is specially: step a) adds bismuth nitrate solution, ammonium molybdate solution and potassium sodium tartrate solution in said second mixed solution, and heat in boiling water bath the vibration back; Step b) adds Fluorinse and stannous chloride in the mixed solution that said step a) obtains, obtain the 3rd mixed solution after the reaction.
Wherein, bismuth nitrate preferably adopts nitric acid 1+3 preparation, bismuth nitrate act as the acidity in the regulator solution, the existence of bismuth nitrate can make the bismuth phosphorus molybdenum blue stability of generation better down.The mass and size concentration of the bismuth nitrate that the present invention adopts is preferably 4.8～5.2g/L, more preferably 5g/L.The bismuth nitrate that the present invention adopts preferably adopts the salpeter solution preparation, and this salpeter solution is nitric acid 1+3, and promptly this salpeter solution is preparation in 1: 3 by red fuming nitric acid (RFNA) and water according to volume ratio.The present invention utilizes the bismuth nitrate with nitric acid 1+3 preparation that solution is carried out acidity adjustment; Make the acidity of second mixed solution that obtains be preferably 0.6～1.0mol/L; 0.7～0.9mol/L more preferably; This acidity has guaranteed the stable of phosphorus molybdenum blue color, thereby has improved the mensuration result's of phosphorus accuracy in the alloy.
Said ammonium molybdate has the effect that the orthophosphoric acid that makes in first mixed solution is converted into phosphato-molybdic heteropolyacid, generates phosphato-molybdic heteropolyacid (being that the phosphorus molybdenum is yellow) with phosphorus reaction.The mass concentration of said ammonium molybdate solution is preferably 8～10%, and more preferably 9%.The mass concentration of said ammonium molybdate solution is preferably 8～10%, and more preferably 9%.In addition, the sodium potassium tartrate tetrahydrate of the present invention's employing has the effect of the interference of eliminating low silicon.The volume ratio of said ammonium molybdate solution and said potassium sodium tartrate solution is preferably (0.8～1.2): (0.8～1.2), more preferably 1: 1.In the preparation process of the 3rd mixed solution; Said ammonium molybdate solution and potassium sodium tartrate solution preferably add with the form of mixed solution; After being about to ammonium molybdate solution and potassium sodium tartrate solution mixing in 1: 1 by volume; Obtain ammonium molybdate-potassium sodium tartrate solution, then said ammonium molybdate-potassium sodium tartrate solution is added in said second mixed solution.
In addition, the effect of sodium fluoride is to shelter small amounts of iron, and the mass concentration of said Fluorinse is preferably 0.8～2.2%, and more preferably 2%.Stannous chloride is the stronger reductive agent of a kind of reductibility, can the phosphato-molybdic heteropolyacid that form be reduced to blue phosphorus molybdenum blue.The present invention is reductive agent with the stannous chloride, and reduction rate is fast, reduction effect good because it has, thereby makes this assay method shorter analysis time, and has increased accuracy and the stability of measuring the result, is fit to on-the-spot production in enormous quantities and analyzes.Said Fluorinse is preferably 100ml with the volume mass ratio of stannous chloride: (0.40～0.60) g, more preferably 100ml: 0.5g.In this step; Said Fluorinse and stannous chloride preferably add with the form of mixed solution; That is: in Fluorinse, add stannous chloride and form sodium fluoride-stannous chloride solution, then said sodium fluoride-stannous chloride is added in said second mixed solution.
Obtaining the 3rd mixed solution, utilizing the absorbance of said the 3rd mixed solution of spectrophotometry, more preferably measuring its absorbance at 690nm at 680～700nm place.Be specially: utilize 2cm cuvette and 7504 type spectrophotometers,, record absorbance, obtain phosphorus content according to typical curve in 690nm wavelength colorimetric.
Because the present invention utilizes the phosphorus content in the spectrophotometry silicomangan, therefore, need pre-rendered typical curve, obtain the phosphorus content in the silicomangan according to typical curve then.3～5 in the same breed standard sample of different content is preferably adopted in the drafting of typical curve; After sample synchronous operation; With the absorbance is ordinate, is horizontal ordinate with the percentage composition of phosphorus, curve plotting on coordinate paper; Thereby after measuring the absorbance of sample, obtain the percentage composition of phosphorus according to typical curve.
The colorimetric experiment that the present invention utilizes AAS to carry out need be accomplished in 30 seconds, otherwise solution is prone to the phenomenon of fading, and the result is measured in influence.
In order to further specify technical scheme of the present invention; Below in conjunction with embodiment the preferred embodiment of the invention is described; Describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
The chemical reagent that the embodiment of the invention and comparative example adopt is commercial.
Embodiment 1
Take by weighing No. 1 silicomangan sample 0.0600 gram and place the 150ml polytetrafluoroethylene beaker; Add 10ml nitric acid; Dropwise 5 ml hydrofluoric acid dissolution adds 5ml perchloric acid heating again and smolders and be concentrated into 2ml, obtains first mixed solution; Said No. 1 silicomangan sample is the GSB03-1947-2005 standard specimen, and P content is 0.078wt%;
Said first mixed solution is taken off cold slightly, add the 10ml temperature and be 60～70 ℃ distilled water, use the distilled water flushing walls of beaker; Heating drips anhydrous sodium sulfite reduction manganese, boil treat that solution is limpid after; Be chilled to room temperature, change in the 100ml volumetric flask, be diluted to scale; Shake up, obtain second mixed solution;
Accurately pipette 10.00ml second mixed solution in the 50ml volumetric flask, add the bismuth nitrate solution of 5ml by the salpeter solution configuration, said salpeter solution is preparation in 1: 3 by red fuming nitric acid (RFNA) and water according to volume ratio; Adding the 5ml mass concentration is 9% ammonium molybdate-potassium sodium tartrate solution, and said ammonium molybdate-potassium sodium tartrate solution is by the potassium sodium tartrate solution preparation in 1: 1 by volume of 9% ammonium molybdate solution and 9%, and heated 30 seconds in boiling water bath the vibration back; Add 0.5% sodium fluoride-stannous chloride solution immediately; Said 0.5% sodium fluoride-stannous chloride solution is preferably 100ml by the mass ratio by volume of Fluorinse and stannous chloride: the 0.5g preparation obtains, and fully vibration is with the 2cm cuvette; 7504 type spectrophotometers; 690nm wavelength colorimetric records absorbance, obtains phosphorus content according to typical curve.
The drafting of typical curve: with 3～5 in the same breed standard sample of different content, after sample synchronous operation, being ordinate with the absorbance, is horizontal ordinate with the percentage composition of phosphorus, curve plotting on coordinate paper.
The calculating of analysis result: after measuring the test absorbance, check in the percentage composition of phosphorus from working curve.
Adopt said method that the phosphorus content in this silicomangan sample is carried out 6 replicate determinations, the result is as shown in table 1.
Embodiment 2～4
Get No. 2 silicomangan samples, No. 3 silicomangan samples and No. 4 silicomangan samples respectively, adopt the method for embodiment 1 that the phosphorus content in the silicomangan is carried out 6 replicate determinations, the result is as shown in table 1.No. 1 silicomangan sample is the GSB03-1947-2005 standard specimen, and P content is 0.078wt%; No. 2 silicomangan samples are the GSB03-1359-2001 standard specimen, and P content is 0.104wt%; No. 3 silicomangan samples are the 09-100 standard specimen, and P content is 0.137wt%; No. 4 silicomangan samples are the YSBC37645-02 standard specimen, and P content is 0.178wt%.
Phosphorus content in the silicomangan that table 1 embodiment 1～4 measures
To above interpretation of result: stipulate according to " guaranteeing the testing result quality procedure ": regularly use certified reference material (reference material) or secondary standard material (examining material) to compare.When the result who compares satisfies condition: when
, it is qualified to declare.Wherein
Be the average of measurement result, S (x) is the standard deviation of measurement result, X
MarkBe the standard substance reference value.
Standard specimen 1: it is qualified that
declares.
Standard specimen 2: it is qualified that
declares.
Standard specimen 3: it is qualified that
declares.
Standard specimen 4: it is qualified that
declares.
Utilize same sample to carry out duplicate test.When the result who checks satisfies: | u
1-u
2|≤R
dThe time, it is qualified to declare.Wherein | u
1-u
2| be the poor of twice measurement result; R
dBe permissible error in the laboratory of stipulating in the detection method.GB GB/T5686.4-1998 only provides permissible error between the chamber, does not provide indoor permissible error, but indoor permissible error is less than permissible error between the chamber.
Standard specimen 1:|u
1-u
2|=0.005 less than permissible error between the chamber (0.008)
Standard specimen 1:|u
1-u
2|=0.007 less than permissible error between the chamber (0.010)
Standard specimen 1:|u
1-u
2|=0.008 less than permissible error between the chamber (0.010)
Standard specimen 1:|u
1-u
2|=0.006 less than permissible error between the chamber (0.015)
As seen from the above analysis: the method precision is higher, and accuracy is better, and 4 samples are all qualified.Reach re-set target:
Embodiment 5～7
Get No. 2 silicomangan samples, No. 3 silicomangan samples, No. 4 silicomangan samples respectively, adopt the method for embodiment 1 that the phosphorus content in each silicomangan sample is measured, each sample measures twice, and it is as shown in table 4 to measure the result.
Comparative example 1
Take by weighing No. 1 silicomangan sample 0.0600 and restrain in the 150ml polytetrafluoroethylene beaker, add 10ml nitric acid, Dropwise 5 ml hydrofluoric acid dissolution adds 5ml perchloric acid heating again and smolders and be concentrated into 2ml; Take off coldly slightly, add 10ml Water dissolve salt type, use the distilled water flushing walls of beaker, heat; Drip sodium sulphite reduction manganese, boil treat that solution is limpid after, be chilled to room temperature; Change in the 100ml volumetric flask, be diluted to scale, shake up;
Accurately pipette the above-mentioned analysis test solution of 10.00ml in the 100ml volumetric flask, add 50ml water, 10ml bismuth nitrate, 20ml mix colour developing liquid, the 5ml ammonium molybdate, and heating is 1 minute in the water-bath, surveys its absorbance after 10 minutes.Use wavelength 680nm, the 2cm cuvette is measured.
The drafting of typical curve: with the same breed standard sample 3-5 of different content, after sample synchronous operation, being ordinate with the absorbance, is horizontal ordinate with the percentage composition of phosphorus, curve plotting on coordinate paper.
The calculating of analysis result: after measuring the test absorbance, obtain the percentage composition of phosphorus from working curve.
Adopt said method that the phosphorus content in this silicomangan sample is carried out 6 replicate determinations, the result is as shown in table 2.
Comparative example 2～4
Get No. 2 silicomangan samples, No. 3 silicomangan samples and No. 4 silicomangan samples respectively, adopt the method for comparative example 1 that the phosphorus content in the silicomangan is carried out 6 replicate determinations, the result is as shown in table 2.
Phosphorus content in the silicomangan that table 2 comparative example 1～4 is measured
According to the regulation of GB GB/T5686.4-1998 silicomangan chemical analysis method phosphorus molybdenum blue spectrophotometric method mensuration phosphorus amount, the tolerance between the chamber is as shown in table 3:
Analysis result tolerance (%) between table 3:GB/T5686.4-1998 chamber
From above interpretation of result: stipulate according to " guaranteeing the testing result quality procedure ": regularly use certified reference material (reference material) or secondary standard material (examining material) to compare.When the result who compares satisfies condition: when
, it is qualified to declare.Wherein
Be the average of measurement result, S (x) is the standard deviation of measurement result, X
MarkBe the standard substance reference value.
Standard specimen 1:
declares defective.
Standard specimen 2: it is qualified that
declares.
Standard specimen 3: it is qualified that
declares.
Standard specimen 4: it is qualified that
declares.
Utilize same sample to carry out duplicate test.When the result who checks satisfies: | u
1-u
2|≤R
dThe time, it is qualified to declare.Wherein | u
1-u
2| be the poor of twice measurement result; R
dBe permissible error in the laboratory of stipulating in the detection method.GB GB/T5686.4-1998 only provides permissible error between the chamber, does not provide indoor permissible error, is less than permissible error between the chamber but go out indoor permissible error.
Standard specimen 1:|u
1-u
2|=0.017 greater than permissible error between the chamber (0.008), declares defective.
Standard specimen 1:|u
1-u
2|=0.018 greater than permissible error between the chamber (0.010), declares defective.
Standard specimen 1:|u
1-u
2|=0.020 greater than permissible error between the chamber (0.010), declares defective.
Standard specimen 1:|u
1-u
2|=0.022 greater than permissible error between the chamber (0.015), declares defective.
As seen from the above analysis: the method precision that comparative example adopts is relatively poor, and all greater than permissible error between the chamber of GB regulation, 4 samples are all defective for the repeatability of 4 standard specimens; It is defective at the mensuration result precision below 0.10% to measure phosphorus content; It is qualified at 0.10% above 3 result precisions to measure phosphorus content.
Comparative example 5～7
Getting No. 2 silicomangan samples, No. 3 silicomangan samples, No. 4 silicomangan samples respectively adopts the method for embodiment 1 and the methods of comparative example 1 that the phosphorus content in each silicomangan sample is measured; Each sample measures twice, and it is as shown in table 4 to measure the result.
The mensuration result of table 4 embodiment of the invention 5～7 and comparative example 5～7 phosphorus
Above data can be found out: the assay method that the embodiment of the invention adopts is measured the stable relatively good of phosphorus in the silicomangan, and maximum deviation is 0.007%, and colorimetric immediately after developing the color in the analytic process, has shortened analysis time.And the assay method that comparative example of the present invention adopts less stable as a result approximately need 120 minutes analysis time, so detection time is longer.Compare with comparative example, the methods analyst time that the embodiment of the invention adopts shortens 10～20 minutes, and the large-scale production analysis is had important and practical meanings.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (10)
1. the assay method of phosphorus in the silicomangan may further comprise the steps:
Silicomangan sample, nitric acid, hydrofluorite and perchloric acid are mixed, and the reaction back forms first mixed solution;
In said first mixed solution, add sodium sulphite, obtain second mixed solution after the reaction;
In said second mixed solution, add bismuth nitrate solution, ammonium molybdate solution, potassium sodium tartrate solution, Fluorinse and stannous chloride, obtain the 3rd mixed solution after the reaction;
Utilize the absorbance of said the 3rd mixed solution of spectrophotometry, obtain the phosphorus content in the silicomangan at 680～700nm place.
2. assay method according to claim 1 is characterized in that, the mass and size concentration of said bismuth nitrate solution is 5g/L.
3. assay method according to claim 1 is characterized in that, the mass concentration of said ammonium molybdate solution is 9%.
4. assay method according to claim 1 is characterized in that, the mass concentration of said potassium sodium tartrate solution is 9%.
5. assay method according to claim 1 is characterized in that, the volume ratio of said ammonium molybdate solution and said potassium sodium tartrate solution is 1: 1.
6. assay method according to claim 1 is characterized in that, the mass concentration of said Fluorinse is 2%.
7. assay method according to claim 1 is characterized in that, said Fluorinse is 100ml: 0.5g with the volume mass ratio of stannous chloride.
8. assay method according to claim 1 is characterized in that, the acidity of said the 3rd mixed solution is 0.6～1.0mol/L.
9. assay method according to claim 1 is characterized in that, utilizes the absorbance of said second mixed solution of spectrophotometry at the 690nm place.
10. assay method according to claim 1 is characterized in that, the said step that obtains the 3rd mixed solution is specially:
Step a) adds bismuth nitrate solution, ammonium molybdate solution and potassium sodium tartrate solution in said second mixed solution, heat in boiling water bath the vibration back;
Step b) adds Fluorinse and stannous chloride in the mixed solution that said step a) obtains, obtain the 3rd mixed solution after the reaction.
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| CN102879345B (en) * | 2012-09-26 | 2015-02-25 | 攀钢集团江油长城特殊钢有限公司 | Method for determining phosphorus content of silicon ferrovanadium |
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| CN110873714A (en) * | 2019-12-19 | 2020-03-10 | 攀钢集团江油长城特殊钢有限公司 | Method for determining phosphorus content in tungsten-free niobium steel |
| CN110873714B (en) * | 2019-12-19 | 2022-09-06 | 攀钢集团江油长城特殊钢有限公司 | Method for determining phosphorus content in tungsten-free niobium steel |
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