CN102279202A - Method for measuring chemical compositions in molten iron of blast furnace by X-ray fluorescence spectrometry - Google Patents

Method for measuring chemical compositions in molten iron of blast furnace by X-ray fluorescence spectrometry Download PDF

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Publication number
CN102279202A
CN102279202A CN2011101794508A CN201110179450A CN102279202A CN 102279202 A CN102279202 A CN 102279202A CN 2011101794508 A CN2011101794508 A CN 2011101794508A CN 201110179450 A CN201110179450 A CN 201110179450A CN 102279202 A CN102279202 A CN 102279202A
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China
Prior art keywords
ray fluorescence
sample
blast
fluorescence spectra
melted
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CN2011101794508A
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Chinese (zh)
Inventor
崔宏利
李飞
王占祥
王晓峰
李丽军
张东升
李张华
梁玉东
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JIANLONG INDUSTRIAL Co Ltd TANGSHAN CITY
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JIANLONG INDUSTRIAL Co Ltd TANGSHAN CITY
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Abstract

The invention relates to a method for measuring chemical compositions in molten iron of a blast furnace by an X-ray fluorescence spectrometry, belonging to the technical field of metallurgical chemical analysis tests. According to the technical scheme, the method comprises the following processing steps of: characterizing the chemical compositions of the molten iron of the blast furnace by using an ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) and an infrared absorption method; determining a plurality of samples as standard samples; drawing a working curve through directly using an X-ray fluorescence spectral analytical instrument for scanning after the samples are grinded by a sample-grinding machine; and calculating the content of the chemical compositions of the samples through measuring the sample strength. The method provided by the invention has the positive effects that: the method comprises scientificity, advance, applicability and popularization; the method has the characteristics of short analysis time, high accuracy, good repeatability, no pollution and the like; and indicated by the accuracy verification, the method has extremely-high accuracy and precision.

Description

Method with the blast-melted middle chemical constitution of X-ray fluorescence spectra assay
Technical field
The present invention relates to a kind of method, belong to metallurgical chemistry analytical test technical field with the blast-melted middle chemical constitution of X-ray fluorescence spectra assay.
Background technology
In iron and steel enterprise, the molten iron that blast furnace process goes out is the product of blast furnace, be again the main raw material(s) of downstream steel-making, its quality directly affects steel making working procedure and finally goes out steel quality, so it is extremely important to detect the content of the chemical constitution in blast-melted in time, accurately and rapidly.Traditional chemical analysis method complicated operation, ultimate analysis one by one, link is many, length consuming time, operation easier is big, and it is many to consume reagent, and poor repeatability is unfavorable for instructing and produces, and can not satisfy allegro production needs.
Summary of the invention
The purpose of this invention is to provide a kind of method with the blast-melted middle chemical constitution of X-ray fluorescence spectra assay, this methods analyst time is short, does not have chemical contamination, and accuracy height, good reproducibility solve the problems referred to above that background technology exists.
Technical scheme of the present invention is: with the method for the blast-melted middle chemical constitution of X-ray fluorescence spectra assay, comprise following processing step: blast-melted sample, by ICP-AES analytical approach and infrared absorption method to its chemical constitution definite value, determine several samples as standard model, after grinding by sample grinding machine, directly, calculate the wherein content of chemical constitution by working sample intensity with X-ray fluorescence spectra analyser scanning drawing curve.
The present invention has determined the analysis condition of instrument, with k α 1 line as analysis spectral line, maximum peak position is the actual detected peak position, metallic element is chosen the LiF analyzing crystal, nonmetalloid is chosen the PET analyzing crystal, the photon intensity that detecting device receives is not higher than 500kcps, analysis time in the sweep signal deviation less than 0.3% o'clock as analyzing the concluding time.
Identity element content difference in several standard models among the present invention.
The present invention adopts fixedly side reaction coefficient correction method to proofread and correct with X-ray fluorescence spectra analyser scanning standard sample.
The ICP-AES analytical approach that the present invention mentioned, infrared absorption method, calculate wherein by working sample intensity that the content of chemical constitution is public method.
The present invention adopts solid to grind sample, this method is simple to operate, analysis speed is fast, do not consume any chemical reagent, can analyze S, Si, Mn, Ti, Ni, Cr, chemical constitutions such as Cu, P in the molten iron simultaneously, by confirm that this method has science, advance, applicability, analysis time is short, accuracy is high, good reproducibility, characteristics such as pollution-free.Repeatability and Reproducibility all is better than the relevant criterion requirement.
Good effect of the present invention is: the present invention is better than the assay method of chemical constitution in the national standard molten iron, but this method has science, advance, applicability generalization, analysis time is short, accuracy is high, good reproducibility, characteristics such as pollution-free, by the correctness checking, show that the method has high accuracy and precision.
Embodiment
The present invention will be further described below by embodiment.
Method with the blast-melted middle chemical constitution of X-ray fluorescence spectra assay, comprise following processing step: the blast-melted sample of selecting our company to produce, after air chill is handled, C, S adopt the infrared absorption Par value, other element is taked ICP-AES analytical approach definite value, determine have certain gradient several samples as standard model, after grinding by sample grinding machine, directly, calculate the wherein content of chemical constitution by working sample intensity with X-ray fluorescence spectra analyser scanning drawing curve.During with X-ray fluorescence spectra analyser scanning drawing curve, with k α 1 line as analysis spectral line, maximum peak position is the actual detected peak position, metallic element is chosen the LiF analyzing crystal, nonmetalloid is chosen the PET analyzing crystal, the photon intensity that detecting device receives is not higher than 500kcps, analysis time in the sweep signal deviation less than 0.3% o'clock as analyzing the concluding time.With X-ray fluorescence spectra analyser scanning standard sample, adopt fixedly side reaction coefficient correction method to proofread and correct.
Embodiment more specifically:
1, major equipment:
A) wavelength dispersion X fluorescent x ray spectroscopy x instrument:
Detecting device is sweep type gas proportional counter and scintillation counter;
Peak power: 4kW;
B) sample making apparatus:
MY-200 type belt sander
2, the selection of standard model
In order to reduce the influence of matrix effect to measurement result, the blast-melted sample of selecting our company oneself production is as standard model, and it selects foundation is that certain gradient will be arranged, the fluctuation range that can contain actual smelting composition, the preparation of sample and air chill degree are identical.
3, standard model grinds
Sample to grind quality very big to testing result influence, therefore to guarantee that the condition of grinding is the same, and not overheated in the process of grinding, texture is clear, can not intersect, crackle and greasy dirt etc. can not be arranged.
4, the definite value of standard model
C, S adopt the infrared absorption Par value, and other element is taked ICP-AES analytical approach definite value.
5, drawing curve
A) selection of standard model
According to the content of daily test sample, select a series of standard specimens that are fit to.
  
Table 1: standard model
Sample number into spectrum Si/% P/% Mn/% Ti/% C/% S/% Ni/% Cr/% Cu/%
T1 5.760 0.072 3.52 0.320 3.546 0.0166 0.0087 0.0193 0.0041
T2 4.450 0.061 2.95 0.350 3.927 0.0223 0.0066 0.0219 0.0050
T3 3.850 0.055 2.15 0.340 4.110 0.0224 0.0074 0.0233 0.0065
T4 2.450 0.055 1.72 0.320 4.296 0.0378 0.0077 0.0239 0.0053
T5 1.190 0.053 1.24 0.260 4.682 0.0524 0.0080 0.0240 0.0054
T6 1.710 0.047 0.93 0.410 4.555 0.0142 0.0071 0.0200 0.0043
T7 0.970 0.043 0.77 0.260 4.686 0.0315 0.0080 0.0286 0.0040
T8 0.250 0.034 0.08 0.073 4.560 0.0225 0.0077 0.0253 0.0042
T9 0.230 0.038 0.07 0.068 4.360 0.0290 0.0085 0.0268 0.0041
T10 0.430 0.400 0.11 0.203 4.810 0.0120 0.0067 0.0217 0.0052
T11 0.924 0.520 0.13 0.158 4.100 0.0145 0.0007 0.0017 0.0002
T12 1.108 0.540 0.12 0.168 4.160 0.0159 0.0096 0.0310 0.0076
T13 0.660 0.530 0.12 0.170 4.296 0.0759 0.0093 0.0318 0.0079
T14 0.350 0.420 0.07 0.073 4.552 0.0198 0.0057 0.0200 0.0030
T15 0.360 0.390 0.08 0.072 4.506 0.0204 0.0058 0.0208 0.0027
T16 0.610 0.590 0.12 0.150 4.296 0.0596 0.0090 0.0388 0.0077
T17 0.290 0.500 0.11 0.120 4.501 0.0375 0.0087 0.0286 0.0065
T18 0.730 0.058 0.16 0.280 4.655 0.0135 0.0086 0.0345 0.0077
T19 0.450 0.660 0.16 0.360 4.740 0.0236 0.0660 0.0219 0.0044
T20 0.210 0.390 0.10 0.046 4.032 0.0618 0.0067 0.0190 0.0035
T21 0.593 0.870 0.47 0.087 4.487 0.0292 0.0112 0.0343 0.0190
T22 0.355 0.960 0.25 0.088 4.309 0.0319 0.0139 0.0457 0.0079
T23 0.588 0.085 0.40 0.092 4.453 0.0250 0.0098 0.0342 0.0255
T24 0.447 0.860 0.41 0.074 4.562 0.0229 0.0106 0.0376 0.0360
T25 0.495 0.104 0.37 0.083 4.417 0.0236 0.0179 0.0580 0.0480
T26 0.295 0.103 0.21 0.057 4.441 0.0395 0.0202 0.0660 0.0412
T27 0.420 0.072 0.36 0.064 4.308 0.0301 0.0095 0.0304 0.0288
T28 0.431 0.089 0.43 0.080 4.514 0.0276 0.0096 0.3430 0.0200
T29 0.596 0.098 0.38 0.116 4.399 0.0298 0.0500 0.1550 0.0350
B) scan conventional sample, determine analysis condition
Select the higher conventional sample of chemical constitution to scan, general glitch-free k α 1 line is as analysis spectral line, and maximum peak position is the actual detected peak position; The general selection principle of analyzing crystal is that LiF is fit to the most elements in Ni ~ Te scope, and PET is suitable for the element in Al ~ Cl scope, and OVO-55 is suitable for the element in O ~ Mg scope; Factors such as light pipe voltage, electric current, collimator slit will be taken all factors into consideration, and guarantee that the photon intensity that detecting device receives is not higher than 500kcps; The PHA window analysis is all in and strengthens window when not introducing other spectral line signal as far as possible; Select single-point as a setting during the general both sides of background symmetries,, can ignore background intensity, to shorten sweep time when measured signal is higher than background signal by force more than 10 times the time; Analysis time in the sweep signal deviation less than 0.3% o'clock as analyzing the concluding time.Final definite optimum analysis condition is as follows:
Table 2: analysis condition
C) scanning standard specimen intensity is made and the optimization working curve
Under fixed analysis condition, scanning standard sample, data processor are made working curve automatically, because the known component content of standard model can not be all in 95 ~ 105% scopes, so can only adopt fixedly side reaction coefficient correction in this experiment.
 
Table 3: working curve information
Test item Slope, (%/kcps) Intercept, % The range of linearity, % SD，%
S 0.06457 -0.0293 0.012~~0.076 2.68*10 -3
Ti 0.01686 -0.0027 0.046~0.41 6.2*10 -3
Cr 0.00749 -0.4529 0.023~0.066 2.6*10 -3
Mn 0.00105 -4.2423 0.07~3.52 0.019
Ni 0.02105 -1.7681 0.0058~0.020 9.3*10 -4
Cu 0.01822 -0.436 0.003~0.048 1.2*10 -3
Si 0.1341 -0.164 0.21~5.76 0.032
6, correctness experiment
A) accuracy experiment
According to above sample melting method and analysis condition existing sample is analyzed, data are as follows:
Table 4: accuracy experimental data
B) precision experiment
Same sample is scanned 10 times and analyze that can to get data as follows respectively:
Table 5: precision experimental data
Test item S,% Si,% Ti,% Mn,% P,% Ni,% Cr,% Cu,%
1 0.022 0.33 0.068 0.40 0.095 0.0071 0.024 0.011
2 0.022 0.32 0.068 0.40 0.096 0.0069 0.025 0.011
3 0.022 0.32 0.068 0.40 0.096 0.0074 0.025 0.01
4 0.021 0.33 0.069 0.40 0.097 0.0073 0.025 0.011
5 0.021 0.33 0.068 0.40 0.094 0.0074 0.025 0.011
6 0.022 0.33 0.068 0.40 0.095 0.0074 0.025 0.01
7 0.022 0.33 0.069 0.40 0.096 0.0075 0.025 0.011
8 0.022 0.33 0.068 0.40 0.097 0.0072 0.024 0.011
9 0.021 0.32 0.068 0.40 0.097 0.0073 0.025 0.011
10 0.022 0.32 0.068 0.40 0.098 0.0072 0.025 0.01
Above data show that this analytical approach has higher accuracy and precision, and Repeatability and Reproducibility all is better than national standard.
Blast-melted sample is ground, adopt above analysis condition and working curve to analyze, it is as follows to record data:
Numbering S,% Si,% Ti,% Mn,% P,% Ni,% Cr,% Cu,%
T217547 0.033 0.30 0.057 0.315 0.086 0.009 0.038 0.017

Claims (4)

  1. One kind with the X-ray fluorescence spectra assay blast-melted in the method for chemical constitution, it is characterized in that comprising following processing step: blast-melted sample, by ICP-AES analytical approach and infrared absorption method to its chemical constitution definite value, determine several samples as standard model, after grinding by sample grinding machine, directly, calculate the wherein content of chemical constitution by working sample intensity with X-ray fluorescence spectra analyser scanning drawing curve.
  2. According to the described usefulness X-ray fluorescence spectra assay of claim 1 blast-melted in the method for chemical constitution, it is characterized in that blast-melted sample needs to handle through air chill, several standard model air chill degree are identical, C, S adopts the infrared absorption Par value, other element is taked ICP-AES analytical approach definite value, during with X-ray fluorescence spectra analyser scanning drawing curve, with k α 1 line as analysis spectral line, maximum peak position is the actual detected peak position, metallic element is chosen the LiF analyzing crystal, nonmetalloid is chosen the PET analyzing crystal, the photon intensity that detecting device receives is not higher than 500kcps, analysis time in the sweep signal deviation less than 0.3% o'clock as analyzing the concluding time.
  3. According to claim 1 or 2 described usefulness X-ray fluorescence spectra assays blast-melted in the method for chemical constitution, it is characterized in that identity element content difference in several standard models.
  4. According to claim 1 or 2 described usefulness X-ray fluorescence spectra assays blast-melted in the method for chemical constitution, it is characterized in that X-ray fluorescence spectra analyser scanning standard sample, adopt fixedly side reaction coefficient correction method correction.
CN2011101794508A 2011-06-30 2011-06-30 Method for measuring chemical compositions in molten iron of blast furnace by X-ray fluorescence spectrometry Pending CN102279202A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106383136A (en) * 2016-08-23 2017-02-08 金川集团股份有限公司 A method for improving linearity of a Fe element content working curve of flash converting slag measured by X-ray fluorescence spectrometry
CN110441340A (en) * 2019-07-16 2019-11-12 天津钢管制造有限公司 Measuring method based on Ta element in X-ray fluorescence spectra analysis steel alloy
WO2020030120A1 (en) * 2018-08-10 2020-02-13 米亚索乐装备集成（福建）有限公司 Method and apparatus for detecting material composition, and computing device and storage medium
CN111380859A (en) * 2018-12-27 2020-07-07 上汽通用汽车有限公司 Sample preparation verification method and sample preparation method
CN111458363A (en) * 2020-04-21 2020-07-28 中国地质大学（武汉） Method for rapidly delineating titanium deposit based on handheld X-ray fluorescence analyzer

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* Cited by examiner, † Cited by third party
Title
BRUKER AXS: "《X射线荧光光谱分析技术》", 30 December 2001 *
吉昂: "《X射线荧光光谱分析》", 30 December 2003 *
杨剑: "用x射线荧光光谱法测定Cl、S等31个元素", 《吉林地质》 *
高建民: "X射线荧光光谱法测定生铁中10种元素", 《冶金分析》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106383136A (en) * 2016-08-23 2017-02-08 金川集团股份有限公司 A method for improving linearity of a Fe element content working curve of flash converting slag measured by X-ray fluorescence spectrometry
WO2020030120A1 (en) * 2018-08-10 2020-02-13 米亚索乐装备集成（福建）有限公司 Method and apparatus for detecting material composition, and computing device and storage medium
CN111380859A (en) * 2018-12-27 2020-07-07 上汽通用汽车有限公司 Sample preparation verification method and sample preparation method
CN110441340A (en) * 2019-07-16 2019-11-12 天津钢管制造有限公司 Measuring method based on Ta element in X-ray fluorescence spectra analysis steel alloy
CN111458363A (en) * 2020-04-21 2020-07-28 中国地质大学（武汉） Method for rapidly delineating titanium deposit based on handheld X-ray fluorescence analyzer

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Application publication date: 20111214