CN103335997A - Method for analyzing nitrogen components of furnace front low-nitrogen steel sample - Google Patents
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Abstract
The invention relates to the technical field of steelmaking and in particular relates to a method for analyzing nitrogen components of a furnace front low-nitrogen steel sample. The method comprises the following steps: preparing a cylindrical sample, and cutting and milling the sample; measuring the sample by employing a direct-reading spectrograph, wherein the argon pressure is set to be 0.27-0.29Mpa, the argon purging time is set to be 2-4 seconds, the pre-burning time is set to be 3-5 seconds, and the integral time is set to be 5-10 seconds; drawing an analytical curve by employing a one-step regression mode by utilizing a series of standard samples, wherein the curve slope is set to be 0.97-1.03, the curve intercept is set to be -0.003-+0.003, the interference element is silicon, and the interference removal coefficient is 0.005-0.010; and exciting the sample twice, recording results from the third analysis point to the fifth analysis point, and calculating the average value to serve as the final detection result. The provided method for analyzing nitrogen components of the furnace front low-nitrogen steel sample is high in analysis precision and high in analysis speed, the iron and steel smelting period is shortened, and the production efficiency is improved.
Description
Technical field
The present invention relates to steelmaking technical field, particularly the nitrogen component analytical approach of a kind of stokehold low nitrogen steel sample.
Background technology
The nitrogen component check employing of general smelting iron and steel stokehold steel sample is got bar-shaped sample and is adopted the thermal conductivity method analysis then through the pelletizing sample preparation, or gets the cylinder sample and adopt the thermal conductivity method analysis then through drilling cuttings system.Though the said method accuracy of analysis is produced needs before can satisfying smelting furnace, analysis time is longer, and influenced by human factor, is unfavorable for the production control of smelting iron and steel stokehold.Utilize direct reading spectrometry analyze in the steel composition have analysis speed fast, have multicomponent characteristics of simultaneous determination simultaneously, analysis time was less than 3 minutes, but at present used direct reading spectrometry is analyzed the influence that nitrogen in steel is subject to sample state, environmental baseline, instrument state, analytical approach, there are slag inclusion, trachoma in surface as sample, causes the nitrogen component lack of homogeneity.Do not have texture after the sample sample preparation, the sample temperature before analyzing is too high all can cause the analysis result distortion.The ambient temperature and humidity fluctuation is excessive, and the analytic curve drift is too fast, directly impact analysis accuracy.Analytical approach mainly be subjected to N interference element, curve linear, excite to heat etc. and influence, the influence relation is complicated, must find best of breed, could guarantee that the result's is accurate.It is bigger that instrument state is influenced by its gas circuit state and ambient atmos input state, is prone to the unstable situation of data.
Summary of the invention
It is short that the technical problem to be solved in the present invention provides a kind of analysis time, the nitrogen component analytical approach of the stokehold low nitrogen steel sample that analysis precision is high.
For solving the problems of the technologies described above, the invention provides the nitrogen component analytical approach of a kind of stokehold low nitrogen steel sample, comprising: make the sample of cylindrical shape and described sample is cut and mills sample.Utilize direct-reading capacitance meter to measure described sample, argon pressure is set to 0.27～0.29Mpa, argon purge time and is set to 2～4s, preburn time and is set to 3～5s, integral time and is set to 5～10s.Analytic curve utilizes the series standard sample to adopt the mode that once returns to draw, and rate of curve is set to 0.97～1.03, and the curve intercept is set to-0.003～+ 0.003.Interference element is silicon, disturbs to once disturbing, and disturbing coefficient of removal is 0.005～0.010.To described sample excitation twice, record the 3rd to the 5th analysis site result, and calculating mean value is final detection result.
Further, described make the sample of cylindrical shape and described sample cut and mill sample comprise: make diameter and be 39～41cm, diameter is 35～37cm, highly is the sample of the cylindrical shape of 68～70cm down.On described sample length direction, cut apart from 1/3-1/4 place, described sample upper end.Described sample after the cutting is milled sample and cooling.
Further, when the surface of described sample was cut, cutting speed was 4500～4700 commentaries on classics/min.When described sample was milled sample, to mill the sample feed velocity and be 1100～1200 commentaries on classics/min, a feed rotating speed be 300～500mm/min, mill the sample degree of depth is 15～20mm.
Further, the described sample after described will the cutting mills sample and cooling, and comprising: the described sample after will cutting mills sample, makes described sample surfaces have texture and the no sand holes in surface and shrinkage cavity.Described sample is cooled to below 35 ℃ after milling sample.
Further, direct-reading capacitance meter laboratory temperature of living in remains on 20～30 ℃.The room temperature fluctuation range is 0～2 ℃ in the residing room temperature of direct-reading capacitance meter two hours.The residing humidity control of direct-reading capacitance meter is below 70%.Direct-reading capacitance meter is analyzed the purity of used argon gas more than or equal to 99.9995%, and the steady quality of argon gas.Direct-reading capacitance meter and argon gas connection line seal, and with the high precision pressure gauge connection line are carried out leakage detection.
Further, in test sample, in the nitrogen element, can realize the joint-detection to the C in the sample, Si, Mn, P, S, Alt, N composition.
Further, the sample of described cylindrical shape is taken molten steel by the sampler of cylindrical shape and is made.
Further, take the sample that molten steel is made cylindrical shape by the sampler of cylindrical shape.
The nitrogen component analytical approach of stokehold provided by the invention low nitrogen steel sample adopts the sampler of cylindrical shape, and the easier contraction of molten steel is solidified, and the sample of formation does not have and is mingled with and pore, is conducive to obtain stable analysis result.Adopt direct reading spectrometry to carry out the analysis of nitrogen component, argon pressure is set to 0.27-0.29Mpa, argon purge time and is set to 2-4s, makes the stable higher of argon gas air-channel system, thereby has guaranteed the accuracy of the nitrogen component analysis of steel sample.
Description of drawings
The nitrogen component analytical approach process flow diagram of the stokehold low nitrogen steel sample that Fig. 1 provides for the embodiment of the invention.
Embodiment
Referring to Fig. 1, the embodiment of the invention provides the nitrogen component analytical approach of a kind of stokehold low nitrogen steel sample, comprising:
Step 10: make the sample of cylindrical shape and described sample is cut and mills sample, be specially: take molten steel by the sampler of cylindrical shape and make that diameter is 39cm～41cm, diameter is 35cm～37cm, highly is the sample of the cylindrical shape of 68cm～70cm down.1/3～1/4 place cutting on the described sample of distance top on the sample length direction, when sample was cut, cutting speed was 4500～4700 commentaries on classics/min.Sample after the cutting is milled sample, the texture and surface no sand holes and the shrinkage cavity that make sample surfaces must have certain rule, to mill the sample feed velocity and be 1100-1200 commentaries on classics/min, a feed rotating speed be 300～500mm/min, mill the sample degree of depth is 15～20mm.The sample that will mill behind the sample is cooled to below 35 ℃.
Step 20: to cutting and mill described sample behind the sample and carry out direct reading spectrometry and analyze nitrogen component, be specially: direct-reading capacitance meter laboratory temperature of living in is remained on 20～30 ℃.The room temperature fluctuation range is 0～2 ℃ in the residing room temperature of direct-reading capacitance meter two hours.The residing humidity control of direct-reading capacitance meter is below 70%.Direct-reading capacitance meter is analyzed used purity of argon more than or equal to 99.9995%, and the steady quality of argon gas.Direct-reading capacitance meter and argon gas connection line seal, and regularly carry out leakage detection with the high precision pressure gauge.When utilizing direct-reading capacitance meter to measure, argon pressure is set to 0.27～0.29Mpa, argon purge time and is set to 2～4s, preburn time and is set to 3～5s, integral time and is set to 5～10s.Analytic curve utilizes the series standard sample to adopt the mode that once returns to draw, and rate of curve is set to 0.97～1.03, and the curve intercept is set to-0.003～+ 0.003.Interference element is silicon, disturbs to once disturbing, and disturbing coefficient of removal is 0.005～0.010.After treating analytic sample and exciting twice, record the 3rd to the 5th analysis site result, and calculating mean value is final detection result.
The nitrogen component analytical approach of the stokehold low nitrogen steel sample that the embodiment of the invention provides adopts the sampler of cylindrical shape, and the easier contraction of molten steel is solidified, and the sample of formation does not have and is mingled with and pore, is conducive to the stable of analysis result.The 1/3-1/4 place of (end that diameter the is less) cutting apart from the sample top on the sample length direction, this feed position can effectively be removed sample top and be shunk incomplete part, guarantee that cutting section does not have shrinkage cavity, crackle situation, satisfy follow-up analysis requirement, improved analysis precision.The optimized parameter combination of feed velocity, a feed rotating speed can make the sample texture that makes satisfy the instrumental analysis requirement, reaches simultaneously to heat the purpose minimum, that tool bit abrasion is minimum.Learn that through test sample temperature whenever increases 5 ℃ greater than temperature after 35 ℃, analysis result upwards departs from 3-5ppm, and the temperature that guarantees to mill the sample behind the sample is lower than 35 ℃, has guaranteed the accuracy that the nitrogen component of steel sample is analyzed.Argon pressure is set to 0.27-0.29Mpa, argon purge time and is set to 2-4s, makes the stable higher of argon gas air-channel system, thereby has guaranteed the accuracy that the nitrogen component of steel sample is analyzed.In the embodiment of the invention, can satisfy the preburn time of setting and integral time the quick joint-detection of the composition such as C, Si, Mn, P, S, Alt, N of multielement in the steel.In the nitrogen component analytical approach of the stokehold low nitrogen steel sample that the embodiment of the invention provides, by the DOE design, optimum argon pressure 0.27-0.29Mpa, argon purge time 2-4s, preburn time 3-5s, four instrumental analysis parameters of 5-10s integral time have been determined.Wherein, argon pressure and argon purge time influence the most obvious owing to be related to the stable of air-channel system to analysis result.For example: when argon pressure reaches 0.31Mpa, higher 5-6ppm when the nitrogen analysis result can be 0.28Mpa than argon pressure, so the pressure of argon gas produces significant effects to analysis result.The preburn time that the present invention sets and can satisfy the quick joint-detection of the compositions such as C, Si, Mn, P, S, Alt, N of multielement in the steel integral time.Analytic curve utilizes serial nitrogenous standard model (being GBW1386-1391, GSB03-2622-2010, GSB03-1525-2002, ZRM098-1, BSLC-6 and 0.0026) to adopt the mode that once returns to draw, rate of curve is 0.97-1.03, and the curve intercept is-0.003～+ 0.003.Through with the contrast test of analysis of thermal conductivity method (being the nitrogen analysis national standard method), determine that the content of silicon has appreciable impact to the nitrogen analysis result, through the match to silicon, the interference of determining silicon is linear disturbance, it is 0.005-0.010 that silicon disturbs coefficient of removal.When the nitrogen component content of sample is 0.0008-0.015%, the accuracy that direct reading spectrometry is analyzed (namely | assay value-asserting value |/asserting value)＜5%, analytical precision RSD＜5%, analysis time＜3 minute.The embodiment of the invention has following beneficial effect:
1, analyzes the precision height, analyze linear wide ranges.When the nitrogen component content of sample is 0.0008-0.015%, the accuracy that direct reading spectrometry is analyzed (namely | assay value-asserting value |/asserting value)＜5%, analytical precision RSD＜5%,
2, analysis speed is fast, finish nitrogen analysis and only need 3 minutes, and this method is easy and simple to handle, and artifical influence factor is little, is beneficial to the practical application that the stokehold produces fast.
3, can realize the simultaneous determination of same sample multielement, make the check composition more representative, can better instruct the preceding production of converter.
4, saved the stokehold sampler, materials such as analysis of thermal conductivity method crucible, helium, standard model, and can remove the hardware of buying nitrogen analysis analysis of thermal conductivity instrument in the chamber of testing, chamber from and drop into expense, have significant tangible benefit; Shorten the proving time of the preceding sample composition of converter, shortened the smelting iron and steel cycle, reduced energy consumption, improved production efficiency, for improving and raising of steel-making smelting process, had significant benefit.
It should be noted last that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to example the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (7)
1. the nitrogen component analytical approach of a stokehold low nitrogen steel sample is characterized in that, comprising:
Make the sample of cylindrical shape and described sample is cut and mills sample;
Utilize direct-reading capacitance meter to measure described sample, argon pressure is set to 0.27～0.29Mpa, argon purge time and is set to 2～4s, preburn time and is set to 3～5s, integral time and is set to 5～10s;
Analytic curve utilizes the series standard sample to adopt the mode that once returns to draw, and rate of curve is set to 0.97～1.03, and the curve intercept is set to-0.003～+ 0.003;
Interference element is silicon, disturbs to once disturbing, and disturbing coefficient of removal is 0.005～0.010;
To described sample excitation twice, record the 3rd to the 5th analysis site result, and calculating mean value is final detection result.
2. analytical approach according to claim 1 is characterized in that, described make the sample of cylindrical shape and described sample cut and mill sample comprise:
Make diameter and be 39～41cm, diameter is 35～37cm, highly is the sample of the cylindrical shape of 68～70cm down;
On described sample length direction, cut apart from 1/3-1/4 place, described sample upper end;
Described sample after the cutting is milled sample and cooling.
3. analytical approach according to claim 2 is characterized in that:
When the surface of described sample was cut, cutting speed was 4500～4700 commentaries on classics/min;
When described sample was milled sample, to mill the sample feed velocity and be 1100～1200 commentaries on classics/min, a feed rotating speed be 300～500mm/min, mill the sample degree of depth is 15～20mm.
4. analytical approach according to claim 2 is characterized in that, the described sample after described will the cutting mills sample and cooling, comprising:
Described sample after the cutting is milled sample, make described sample surfaces have texture and the no sand holes in surface and shrinkage cavity;
Described sample is cooled to below 35 ℃ after milling sample.
5. analytical approach according to claim 1 is characterized in that, direct-reading capacitance meter laboratory temperature of living in remains on 20～30 ℃;
The room temperature fluctuation range is 0～2 ℃ in the residing room temperature of direct-reading capacitance meter two hours;
The residing humidity control of direct-reading capacitance meter is below 70%;
Direct-reading capacitance meter is analyzed the purity of used argon gas more than or equal to 99.9995%, and the steady quality of argon gas;
Direct-reading capacitance meter and argon gas connection line seal, and with the high precision pressure gauge connection line are carried out leakage detection.
6. analytical approach according to claim 5 is characterized in that, in the nitrogen element, can realize the joint-detection to the C in the sample, Si, Mn, P, S, Alt, N composition in test sample.
7. analytical approach according to claim 1 is characterized in that, takes the sample that molten steel is made cylindrical shape by the sampler of cylindrical shape.
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| CN109668872A (en) * | 2019-01-29 | 2019-04-23 | 南京钢铁股份有限公司 | A kind of direct-reading spectrometer surveys the analysis method of nitrogen in steel online |
| CN110308098A (en) * | 2019-08-13 | 2019-10-08 | 建龙北满特殊钢有限责任公司 | A kind of method of quick detection P91 nitrogen in steel content |
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| CN110308098A (en) * | 2019-08-13 | 2019-10-08 | 建龙北满特殊钢有限责任公司 | A kind of method of quick detection P91 nitrogen in steel content |
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