CN107132192A - The rapid colorimetric determination method of phosphorus in silicon steel - Google Patents
The rapid colorimetric determination method of phosphorus in silicon steel Download PDFInfo
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- CN107132192A CN107132192A CN201710382998.XA CN201710382998A CN107132192A CN 107132192 A CN107132192 A CN 107132192A CN 201710382998 A CN201710382998 A CN 201710382998A CN 107132192 A CN107132192 A CN 107132192A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The invention discloses a kind of rapid colorimetric determination method of phosphorus in silicon steel, including：A certain amount of silicon steel sample is weighed in beaker in tall form, hydrochloric acid, nitric acid, hydrofluoric acid mixed-acid dissolution silicon steel sample, perchloric acid smoked to most, dissolved salts is taken；With ammonium molybdate color development, the reduction of sodium fluoride stannous chloride mixed liquor determines the absorbance of phosphorus；With the percentage composition that content is similar, the identical standard specimen of kind obtains phosphorus in silicon steel sample.The present invention can avoid interference of the silicon to developing the color and determining, and colorimetric process stabilization, measurement result is accurate.
Description
Technical field
The present invention relates to a kind of quantitative analysis method, specifically, it is related to a kind of rapid colorimetric determination method of phosphorus in silicon steel.
Background technology
Silicon steel is low-carbon ferrosilicon alloy of the silicon content 0.5% to 5% or so.It is mainly used as various motors, generator, pressure
The iron core of contracting machine, motor and transformer, is the indispensable raw material product of the industries such as electric power, household electrical appliances.
Phosphorus can make weld seam produce cold short phenomenon, with the increase of phosphorus content, will cause weld seam as harmful element in steel
The toughness of metal, particularly low-temperature impact toughness decline.Thus the content of phosphorus and carry out technology controlling and process and be in Accurate Determining silicon steel
It is very necessary.
The analysis of phosphorus content is more using ammonium persulfate oxidation, ammonium vanadate, molybdic acid currently without standard method is formed in silicon steel
Ammonium colorimetric method.Because sample silicon content is high, the later stage, which is developed the color, and determined certain interference.
The content of the invention
Technical problem solved by the invention is to provide a kind of rapid colorimetric determination method of phosphorus in silicon steel, can avoid silicon
Interference to developing the color and determining, colorimetric process stabilization, measurement result is accurate.
Technical scheme is as follows：
A kind of rapid colorimetric determination method of phosphorus in silicon steel, including：
A certain amount of silicon steel sample is weighed in beaker in tall form, hydrochloric acid, nitric acid, the examination of hydrofluoric acid mixed-acid dissolution silicon steel is taken
Sample, perchloric acid smoked to most, dissolved salts；
With ammonium molybdate color development, sodium fluoride-stannous chloride mixed liquor reduction determines the absorbance of phosphorus；
With the percentage composition that content is similar, the identical standard specimen of kind obtains phosphorus in silicon steel sample,
Calculation formula：W in formulaMarkFor the percentage composition of phosphorus in standard sample, ASurvey
For the absorbance measurements of sample, AMarkFor the absorbance measurements of standard specimen.
Further：0.0500g samples are weighed in 150mL beakers in tall form, plus 10mL hydrochloric acid, 10mL nitric acid, 10 drop hydrogen fluorine
Acid, dissolve by heating, then add 20mL perchloric acid, heating smoke to the greatest extent, plus 10mL volume ratios be 2:5 nitric acid, is heated to boiling, takes
Under, 5mL ammonium molybdates-sodium potassium tartrate tetrahydrate mixed solution is added, is shaken 10 seconds, 35mL sodium fluorides-stannous chloride mixed liquor is added, with
Water is reference, chooses 2cm cuvettes, and Red lightscreening plate determines the absorbance of phosphorus, and the percentage for calculating phosphorus in silicon steel sample contains
Amount.
Further：In ammonium molybdate-sodium potassium tartrate tetrahydrate mixed solution, ammonium molybdate, the mass percent concentration of sodium potassium tartrate tetrahydrate
For 18%, and mixing is produced and obtained in equal volume；Sodium fluoride-stannous chloride mixed liquor is used per mass per liter percent concentration
Addition 2g stannous chloride shakes up obtained in 2.4% sodium fluoride aqueous solution.
Compared with prior art, the technology of the present invention effect includes：
1st, it is quick, efficient.This method is quick colorimetric method, and without placing color development, colorimetric process speed is fast.Operating process
Short, medicine usage amount is small, and production cost is low.Compared to large-scale instrument method, this method is low to equipment, environmental requirement, equipment into
This is small.
2nd, accurately, stably.This method can be such that sample dissolves rapidly using the molten sample of a variety of acid mixing.Disappeared using screening agent
Except interference, color stability, it is ensured that the Accurate Determining of phosphorus content.
3rd, due to the silicon containing high level in sample, the conventional sour dissolution velocity of molten sample is slow and easily dissolves incomplete；This
Method is combined by adding hydrofluoric acid with silicon, and smoke is eliminated so that sample can dissolve rapidly, it is to avoid silicon participates in follow-up aobvious
Color influence is determined；This method is quickly determined suitable for stokehold, quick to determine without placing colour developing, is easily mastered.
Embodiment
Technical solution of the present invention is elaborated below with reference to example embodiment.However, example embodiment can
Implement in a variety of forms, and be not understood as limited to embodiment set forth herein；On the contrary, thesing embodiments are provided so that
The design of example embodiment more comprehensively and completely, and is comprehensively conveyed to those skilled in the art by the present invention.
The rapid colorimetric determination method of phosphorus, specifically includes following steps in silicon steel：
Step 1：A certain amount of silicon steel sample is weighed in beaker in tall form, hydrochloric acid, nitric acid, hydrofluoric acid mixed-acid dissolution silicon is taken
Steel curved beam, perchloric acid smoked to most, dissolved salts；
Step 2：With ammonium molybdate color development, sodium fluoride-stannous chloride mixed liquor reduction determines the absorbance of phosphorus.
Step 3：Similar with content, the identical standard specimen of kind obtains the percentage composition of phosphorus in silicon steel sample.
Calculation formula：
In formula：
WMark：The percentage composition of phosphorus, % in standard sample；
ASurvey：The absorbance measurements of sample；
AMark：The absorbance measurements of standard specimen.
Embodiment 1
0.0500g samples are weighed in 150mL beakers in tall form, plus 10mL hydrochloric acid, 10mL nitric acid, 10 drop hydrofluoric acid, heating
Dissolving, then add 20mL perchloric acid, heating smoke is to the greatest extent, plus 10mL nitric acid (2+5, concentrated nitric acid and water volume ratio 2:5), it is heated to
Boiling, is removed, and 5mL ammonium molybdates-sodium potassium tartrate tetrahydrate mixed solution (each 18% to mix in equal volume) is added immediately, is shaken 10 seconds, plus
Enter 35mL sodium fluorides-stannous chloride mixed liquor (2g stannous chloride shakes up in every liter of sodium fluoride (2.4% aqueous solution)), using water as ginseng
Than choosing 2cm cuvettes, Red lightscreening plate determines the absorbance of phosphorus.Calculate the percentage composition of phosphorus in silicon steel sample.
Sample analysis is compareed
As can be seen from the above table, the rate of recovery determined using this method in silicon steel obtained by phosphorus content is higher, determines accurate.
This method uses a variety of sour mixed dissolution silicon steel samples, passes through the addition of hydrofluoric acid so that silicon is combined with fluorine, quickly
Dissolving；By adding screening agent, colorimetric interference is eliminated, colorimetric process stabilization, measurement result is accurate.Operating process is shorter, method
Easily grasp, quickly, efficiently.
Term used herein is explanation and exemplary and nonrestrictive term.Because the present invention can be with a variety of
Form specific implementation without departing from the spiritual or substantive of invention, it should therefore be appreciated that above-described embodiment be not limited to it is any foregoing
Details, and should widely being explained in the spirit and scope that appended claims are limited, thus fall into claim or its etc.
Whole changes and remodeling in the range of effect all should be appended claims and covered.
Claims (3)
1. a kind of rapid colorimetric determination method of phosphorus in silicon steel, including：
A certain amount of silicon steel sample is weighed in beaker in tall form, hydrochloric acid, nitric acid, hydrofluoric acid mixed-acid dissolution silicon steel sample is taken, it is high
Chloric acid is smoldered to most, dissolved salts；
With ammonium molybdate color development, sodium fluoride-stannous chloride mixed liquor reduction determines the absorbance of phosphorus；
With the percentage composition that content is similar, the identical standard specimen of kind obtains phosphorus in silicon steel sample,
Calculation formula：W in formulaMarkFor the percentage composition of phosphorus in standard sample, ASurveyFor examination
The absorbance measurements of sample, AMarkFor the absorbance measurements of standard specimen.
2. the rapid colorimetric determination method of phosphorus in silicon steel as claimed in claim 1, it is characterised in that：Weigh 0.0500g samples in
In 150mL beakers in tall form, plus 10mL hydrochloric acid, 10mL nitric acid, 10 drop hydrofluoric acid, dissolve by heating, then add 20mL perchloric acid, heating hair
Cigarette to the greatest extent, plus 10mL volume ratios be 2:5 nitric acid, is heated to boiling, removes, and adds 5mL ammonium molybdates-sodium potassium tartrate tetrahydrate mixing molten
Liquid, shakes 10 seconds, adds 35mL sodium fluorides-stannous chloride mixed liquor, using water as reference, chooses 2cm cuvettes, red filter
Piece, determines the absorbance of phosphorus, calculates the percentage composition of phosphorus in silicon steel sample.
3. the rapid colorimetric determination method of phosphorus in silicon steel as claimed in claim 2, it is characterised in that：Ammonium molybdate-sodium potassium tartrate tetrahydrate
In mixed solution, ammonium molybdate, the mass percent concentration of sodium potassium tartrate tetrahydrate are 18%, and mixing is produced and obtained in equal volume；Fluorine
Change sodium-stannous chloride mixed liquor using addition 2g stannous chloride in the sodium fluoride aqueous solution per mass per liter percent concentration 2.4%
Shake up obtained.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108593630A (en) * | 2018-04-25 | 2018-09-28 | 长春黄金研究院有限公司 | A kind of phosphorus yield method in the ore of efficiently and accurately |
| CN110346352A (en) * | 2019-07-20 | 2019-10-18 | 武钢集团昆明钢铁股份有限公司 | The measuring method of phosphorus pentoxide content in a kind of half steel slag former |
| CN112697732A (en) * | 2020-12-18 | 2021-04-23 | 攀钢集团江油长城特殊钢有限公司 | Method for detecting niobium content in alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103398963A (en) * | 2013-08-12 | 2013-11-20 | 攀枝花学院 | Method for analyzing phosphorus in silicon iron |
| CN104390924A (en) * | 2014-12-17 | 2015-03-04 | 内蒙古包钢钢联股份有限公司 | Method for determining phosphorus in high-carbon silicon aluminum alloy by using photometric method |
| CN104458623A (en) * | 2014-12-17 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for measuring phosphorus in silicon iron by using photometric method |
| CN105004691A (en) * | 2015-08-21 | 2015-10-28 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of phosphorus in steel through spectrophotometry |
-
2017
- 2017-05-26 CN CN201710382998.XA patent/CN107132192A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103398963A (en) * | 2013-08-12 | 2013-11-20 | 攀枝花学院 | Method for analyzing phosphorus in silicon iron |
| CN104390924A (en) * | 2014-12-17 | 2015-03-04 | 内蒙古包钢钢联股份有限公司 | Method for determining phosphorus in high-carbon silicon aluminum alloy by using photometric method |
| CN104458623A (en) * | 2014-12-17 | 2015-03-25 | 内蒙古包钢钢联股份有限公司 | Method for measuring phosphorus in silicon iron by using photometric method |
| CN105004691A (en) * | 2015-08-21 | 2015-10-28 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of phosphorus in steel through spectrophotometry |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108593630A (en) * | 2018-04-25 | 2018-09-28 | 长春黄金研究院有限公司 | A kind of phosphorus yield method in the ore of efficiently and accurately |
| CN110346352A (en) * | 2019-07-20 | 2019-10-18 | 武钢集团昆明钢铁股份有限公司 | The measuring method of phosphorus pentoxide content in a kind of half steel slag former |
| CN112697732A (en) * | 2020-12-18 | 2021-04-23 | 攀钢集团江油长城特殊钢有限公司 | Method for detecting niobium content in alloy |
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