CN1431484A - Method for measuring silicon content on surfaces of steel plates - Google Patents
Method for measuring silicon content on surfaces of steel plates Download PDFInfo
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- CN1431484A CN1431484A CN 03112810 CN03112810A CN1431484A CN 1431484 A CN1431484 A CN 1431484A CN 03112810 CN03112810 CN 03112810 CN 03112810 A CN03112810 A CN 03112810A CN 1431484 A CN1431484 A CN 1431484A
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- steel plate
- silicone content
- liquid parting
- deionized water
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Abstract
Under room temperature, azotic strong oxidizing property acid as the stripping fluid is contacted to the surface of steel sample sheets. Thus, silicon on the surface is peeled off into the reagent through the chemical reaction. The operation of constant volume is carried out for the peeling reagent. The concentration of silicon in the reagent is measured by using ICP spectrograph. Finally, the silicon content of the surface of the steel sample sheet is calculated out. The features of the invention are as follows. (1) The stripping fluid contains relative fewer iron ions so as to insure the high accuracy of the measured data. (2) The azotic strong oxidizing property acid is common reagent, harming spectrograph lightly. (3) The heating process is not needed in the measuring procedure so as to reduce the generation of the corrosion gas and mask the operation simple fast and accuracy.
Description
Technical field
The present invention relates to a kind of assay method of silicone content, be specifically related to a kind of assay method of surface of steel plate silicone content.This method is used to measure the silicone content that electrolytic cleaned is coated with the surface of steel plate absorption behind the silicon, such as being used for cold-strip steel after degreasing is coated with silicon, measures the silicone content that adsorbs on its surface of steel plate unit area.
Background technology
Cold-strip steel is when carrying out batch annealing, owing to batch the acting in conjunction of tension stress and thermal stress, be easy to generate band steel bonding, this bonding influences strip surface quality, it is a kind of defective of process for producing cold rolled strip steel, also be a difficult problem of cold rolled strip steel production in the world, do not find desirable solution so far as yet.
The seventies not, the people such as Guinomct of West Germany He Shi iron company add 0.1～5% silicasol in ROLLING OIL, the result has played positive role to the phenomenon that prevents to bond in band steel annealing process.Also mention the degreasing unit in Japan's " iron and steel brief guide " book and use sodium silicate, can effectively reduce the peel stress of band coil of strip interlayer, reduce the bonding phenomenon in the band steel annealing process as clean-out system.
Although domestic and international many iron and steel enterprises and research unit are for having made very big effort in this respect at present, once some application achievements had been obtained, also delivering surface of steel plate is coated with the too high meeting of silicon amount and causes steel plate when moving back to technology, make surface of steel plate white snakelike defective occur, in addition, cause also that adhesion reduces when zinc-plated, zinc-plated, influence following process.When if surface of steel plate is coated with the certain inadequately value of silicon, still can not effectively prevent to be with the steel phenomenon that when annealing process, prevents to bond to take place.Therefore, the scope of its silicon on surface of control seems very important in band steel production run.
In order to address the above problem,, must emphasize the silicone content of surface of steel plate is measured, with the situation (silicone content that adsorbs on the surface of steel plate unit area) of accurate grasp surface of steel plate silicone content except that the research belt steel surface is coated with the silicon weight range.It is introduced that at present applied surface of steel plate silica test method has two kinds in the domestic and international production:
First kind is the liquid parting that adopts the sulfuric acid of hydrofluorite+0.75% concentration of 0.75% concentration to mix, with the boric acid of 55g/l concentration and the hydrogen peroxide of 30% concentration is adjuvant, behind heating, evaporation, process for cooling, use the ionized water constant volume, use the silicon concentration in the ICP spectrophotometer solution again, calculate the silicone content on the surface of steel plate unit area then.
Second kind is that employing 10% hydrochloric acid is liquid parting, the liquid parting heating is carried out demoulding to surface of steel plate handle, and uses the deionized water constant volume, uses the silicon concentration in the ICP spectrophotometer solution again, calculates the silicone content on the surface of steel plate unit area then.
Although above-mentioned two kinds of assay methods are applied aborning, weak point is:
1, adopt hydrofluorite to add sulfuric acid as liquid parting and boric acid during as adjuvant, because reagent can generate BF63-in this process, the accuracy of influence effect of peeling off and follow-up ICP spectrometer measurement.
When 2, adopting hydrochloric acid as liquid parting, surface of steel plate is subjected to acid corrosion easily, and a large amount of ferric ions are entered in the solution to be measured, influences the accuracy of follow-up ICP spectroscopy measurements.
3, hydrofluorite toxicity is bigger, and especially volatilization easily in heating process damages human body easily.
4, above-mentioned two kinds of methods all need solution is heated in the mensuration process, the time that whole like this mensuration process need is long, and operation steps complexity, loaded down with trivial details.
5, because boric acid, hydrofluorite, sulfuric acid corrosion resistance are stronger, bigger when adopting the ICP spectroscopic methodology to measure to spectrometer corrosivity, directly influence serviceable life of device instrument.
In view of this, the object of the invention provides a kind of quick, simple, and accurate test result surface of steel plate silica test method, to overcome above-mentioned deficiency, for the production of band steel provides better surface silicon content assaying method.
Summary of the invention
For achieving the above object, the technical solution used in the present invention is: a kind of assay method of surface of steel plate silicone content, it is characterized in that: the silicon on steel plate print surface is peeled off with nitrogenous acid with strong oxidizing property, adopt the ICP spectrometer that the silicon concentration in the liquid parting is measured then, calculate the surface of steel plate silicone content according to measurement result again, its step comprises:
(1), adopts nitrogenous acid with strong oxidizing property, with the volumetric ratio preparation liquid parting of deionized water with 3～15 times;
(2), get a plastic beaker or container, add an amount of liquid parting, then the steel plate print is immersed in this demoulding solution, and fully contacts the steel plate print at ambient temperature;
(3), then take out with rinsed with deionized water steel plate print, and rinsing liquid is retained in above-mentioned beaker or the container;
(4), then the solution in above-mentioned beaker or the container all is transferred to and adds deionized water in the volumetric flask and carry out constant volume;
(5), measure silicon concentration in the above-mentioned constant volume test solution and the silicon concentration in the blank liquid parting respectively with the ICP spectrometer;
(6), utilize measured constant volume test solution silicon concentration value and blank liquid parting silicon concentration value, calculate the silicone content that deposits on the surface of steel plate unit area as follows:
Silicone content (μ g/m
2)=
In the following formula: steel plate print area is the surface area of single face.
The related content and the change interpretation of technique scheme are as follows:
1, in the such scheme, described plastic beaker or container generally adopt polytetrafluoroethylene beaker or container, and can not adopt glass beaker, because siliceous in the glass material.
2, " adding an amount of liquid parting " is meant that the amount that adds liquid parting is a principle can soak last steel plate print fully in above-mentioned second step.
3, nitrogenous acid with strong oxidizing property described in the above-mentioned first step is prepared liquid parting with deionized water by 5～10 multiple proportions example.
4, room temperature condition is preferable with 15～25 ℃ described in above-mentioned second step.
5, steel plate print described in above-mentioned second step fully contacts in liquid parting and is: can adopt plastics to take the photograph in the sub-gripping steel plate print immersion liquid parting and stir, also can adopt alternate manner, rock by beaker such as hand etc.The essence of this operation is that the steel plate print is soaking the liquid parting stirring relatively of end while, and the print surface is fully contacted with liquid parting.
6, comprise following dual mode with rinsed with deionized water described in above-mentioned the 3rd step:
(1), takes out the back directly with deionized water lavage specimens sheet two sides.
(2), take out the back and scrub steel plate print two sides with brush earlier, use deionized water washout and steel plate print then.This operation is to the better effects if of peeling off of surface silicon.
7, in the such scheme, described steel plate print is to be cut into the simple geometric shape lattice of establishing rules really in advance, such as being cut into 50mm * 50mm specification, can operate with a slice print in the mensuration, also can be with operation successively more than two or two.Can in same liquid parting, successively operate twice during such as two prints of employing, measure with the ICP spectrometer then.
Principle of work of the present invention is: utilize nitrogenous acid with strong oxidizing property as liquid parting, fully contact with steel plate print surface at ambient temperature, be stripped in the reagent by the silicon of chemical reaction surface of steel plate, carry out constant volume to peeling off reagent then, and utilize the ICP spectrometer to measure silicon concentration in the reagent, calculate the silicone content on print surface at last on this basis.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1, the present invention adopts nitrogenous acid with strong oxidizing property as liquid parting, easily form oxide film at steel surface, thereby and impel steel surface to be subjected to passivation to alleviate acid corrosion, ferric ion is not easy to enter in the test fluid like this, simultaneously, this passivation does not influence peeling off of surface silicon again, and just the ferric ion in the test fluid is less relatively, has therefore influenced following adopted ICP spectrophotometer precision.
2, need not heating in the mensuration process of the present invention, comparatively speaking, reduced the volatilization of corrosive gas on the one hand, make operation simpler on the other hand.
3, to adopt nitrogenous acid with strong oxidizing property also be the common agents of ICP spectroscopic methodology in the present invention, lighter to the spectrometer infringement.
4, the present invention's operation steps letter joint compared with prior art, the time, short speed was fast, practical, and measurement result is more accurate, so its improvement has conspicuousness.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment: a kind of assay method of surface of steel plate silicone content, its particular content and step are as follows:
One, reagent and utensil
Nitrogenous acid with strong oxidizing property deionized water
The plastics volumetric flask of the polytetrafluoroethylene beaker 250ml of 500ml
Teflon brush teflon is taken the photograph son
Stopwatch ICP spectrometer
Two, sample
Adopt 5cm * 5cm steel plate print
Three, step
1, adopt nitrogenous acid with strong oxidizing property and deionized water to prepare liquid parting by 1: 12 volumetric ratio;
2, get a 500ml polytetrafluoroethylene beaker, add the 180ml liquid parting, take the photograph sub-gripping steel plate print with teflon then and immerse in this reagent solution, and under 15～25 ℃ of room temperature conditions, stirred the steel plate print 10 seconds;
3, take out elder generation then and scrub steel plate print two sides, use rinsed with deionized water brush and steel plate print then, and rinsing liquid is retained in the above-mentioned plastic beaker with brush;
4, the solution in the above-mentioned beaker all is transferred to adds deionized water in the volumetric flask of 250ml and carry out constant volume to 250ml;
5, measure silicon concentration in the above-mentioned constant volume test solution and the silicon concentration in the blank liquid parting respectively with the ICP spectrometer;
6, utilize measured constant volume test solution silicon concentration value and blank liquid parting silicon concentration value, calculate the silicone content that deposits on the surface of steel plate unit area as follows:
Silicone content (μ g/m
2)=
In the following formula: steel plate print area is the surface area of single face.
Measure the band steel after Shanghai iron company electrolytic cleaned is coated with silicon as stated above, record surface of steel plate at last and be coated with silicon amount mean value and be:
Si(μg/m
2)＝3.260(μg/m
2)
Claims (5)
1, a kind of assay method of surface of steel plate silicone content, it is characterized in that: the silicon on steel plate print surface is peeled off with nitrogenous acid with strong oxidizing property, adopt the ICP spectrometer that the silicon concentration in the liquid parting is measured then, calculate the surface of steel plate silicone content according to measurement result again, its step comprises:
(1), adopts nitrogenous acid with strong oxidizing property, with the volumetric ratio preparation liquid parting of deionized water with 3～15 times;
(2), get a plastic beaker or container, add an amount of liquid parting, then the steel plate print is immersed in this demoulding solution, and fully contacts the steel plate print at ambient temperature;
(3), then take out with rinsed with deionized water steel plate print, and rinsing liquid is retained in above-mentioned beaker or the container;
(4), then the solution in above-mentioned beaker or the container all is transferred to and adds deionized water in the volumetric flask and carry out constant volume;
(5), measure silicon concentration in the above-mentioned constant volume test solution and the silicon concentration in the blank liquid parting respectively with the ICP spectrometer;
(6), utilize measured constant volume test solution silicon concentration value and blank liquid parting silicon concentration value, calculate the silicone content that deposits on the surface of steel plate unit area as follows:
Silicone content (μ g/m
2)=
In the following formula: steel plate print area is the surface area of single face.
2, the assay method of surface of steel plate silicone content according to claim 1 is characterized in that: nitrogenous acid with strong oxidizing property described in the first step is prepared liquid parting with deionized water by 5～10 multiple proportions example.
3, the assay method of surface of steel plate silicone content according to claim 1 is characterized in that: steel plate print described in second step fully contacts in liquid parting and is: adopt plastics to take the photograph in the sub-gripping steel plate print immersion liquid parting and stirred 5～15 seconds.
4, the assay method of surface of steel plate silicone content according to claim 1 is characterized in that: described in the 3rd step with rinsed with deionized water be: scrub steel plate print two sides with brush earlier, use rinsed with deionized water brush and steel plate print then.
5, the assay method of surface of steel plate silicone content according to claim 1 is characterized in that: described steel plate print is cut into the simple geometric shape lattice of establishing rules really in advance, adopts a slice in the mensuration or operation successively more than two.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03112810 CN1431484A (en) | 2003-01-30 | 2003-01-30 | Method for measuring silicon content on surfaces of steel plates |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03112810 CN1431484A (en) | 2003-01-30 | 2003-01-30 | Method for measuring silicon content on surfaces of steel plates |
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| CN1431484A true CN1431484A (en) | 2003-07-23 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101865848A (en) * | 2010-05-21 | 2010-10-20 | 北京泰科诺科技有限公司 | Method and device for measuring monobromethane concentration in fumigation tank by plasma emission spectroscopy |
| CN102706859A (en) * | 2012-06-15 | 2012-10-03 | 武汉钢铁(集团)公司 | Method for determining silica in silicon steel surface oxidation layer |
| CN110736763A (en) * | 2019-10-29 | 2020-01-31 | 东莞捷邦实业有限公司 | Silicon transfer rapid detection method for silicon-containing release films |
| CN112683621A (en) * | 2020-12-28 | 2021-04-20 | 唐山钢铁集团有限责任公司 | Method for detecting content of silicon element in manganese-silicon alloy |
-
2003
- 2003-01-30 CN CN 03112810 patent/CN1431484A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101865848A (en) * | 2010-05-21 | 2010-10-20 | 北京泰科诺科技有限公司 | Method and device for measuring monobromethane concentration in fumigation tank by plasma emission spectroscopy |
| CN101865848B (en) * | 2010-05-21 | 2012-05-30 | 北京泰科诺科技有限公司 | Method and device for measuring monobromethane concentration in fumigation tank by plasma emission spectroscopy |
| CN102706859A (en) * | 2012-06-15 | 2012-10-03 | 武汉钢铁(集团)公司 | Method for determining silica in silicon steel surface oxidation layer |
| CN110736763A (en) * | 2019-10-29 | 2020-01-31 | 东莞捷邦实业有限公司 | Silicon transfer rapid detection method for silicon-containing release films |
| CN112683621A (en) * | 2020-12-28 | 2021-04-20 | 唐山钢铁集团有限责任公司 | Method for detecting content of silicon element in manganese-silicon alloy |
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