CN110441340A - Measuring method based on Ta element in X-ray fluorescence spectra analysis steel alloy - Google Patents
Measuring method based on Ta element in X-ray fluorescence spectra analysis steel alloy Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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Abstract
The invention discloses a kind of based on X-ray fluorescence spectra analysis to the measuring method of Ta element in steel alloy, including step 1. apparatus measures condition, 2. the preparation of sample, 3. the selection of standard sample, 4. drawing working curve, 5. Analysis on Selecting sample and the standard sample of wet process definite value carry out veracity and precision measurement.The beneficial effects of the present invention are: accurately and quickly measuring Ta constituent content in low-alloy steel；And it is easy to operate.
Description
Technical field
The invention belongs to Analysis of Metallic Materials technical field of research, more particularly to one kind based on X-ray fluorescence spectra point
Analyse the measuring method of Ta element in steel alloy.
Background technique
X-ray fluorescence spectra analysis is a kind of instrument analysis side generallyd use in the external metallurgical analysis of Now Domestic
The advantages that method has method for making sample simple, and analysis content range is wide, and accuracy is high, analyzes fast speed.
Metallurgical unit detections many at present are also analyzed frequently with X-ray fluorescence spectra.Ta is a kind of hard metal element, is had
Plasticity and ductility.It can be cold worked, the service performance that can improve steel be added in steel, therefore Ta element contains in Accurate Determining steel
Amount is significant to steel-making and technique production.
Summary of the invention
To solve the problems, such as above-mentioned technology, the object of the present invention is to provide one kind based on X-ray fluorescence spectra point
The measuring method for analysing Ta element in steel alloy, can accurately and quickly measure the content of Ta element in steel.
To achieve the above object, the technical solution adopted by the present invention is that: one kind based on X-ray fluorescence spectra analyze to alloy
The measuring method of Ta element, this method include following steps in steel:
1. apparatus measures condition
Using MAX type Xray fluorescence spectrometer, in which: power 4Kw, voltage 30Kv, electric current 110mA；
Ta element selects KA linear system, and collimator selects 300um, and optical filter selects brass copper optical filter, and crystal is
LiF200, detector select scintillation detector Scint, the operating condition of voltage 30Kv, and collimator selects 300um, no optical filtering
Piece, crystal LiF200, detector selection flow probe Flow, the operating condition of voltage 30Kv,
2. the preparation of sample:
Analysis sample grinds and to put down, no shrinkage cavity, crackle, trachoma, and grind away lines is consistent；
3. the selection of standard sample
Purchase have the sample of Ta element definite value as standard sample, standard specimen constituent content to have standard chemical analysis as a result,
Content distribution is uniform, and without segregation phenomena, no shrinkage cavity, nothing are mingled with；
4. drawing working curve
Using the operating condition of step 3., fluorescence intensity successively is measured with X-fluorescence instrument, the content of Ta element is given in the certificate
Out, it using the fluorescence intensity of five standard samples of measurement as abscissa, using the Ta content of five standard samples as ordinate, draws
Working curve.
5. selection standard sample carries out the experiment of veracity and precision accuracy of measurement: choosing several samples using this hair
Bright method carries out xrf analysis, measures Ta constituent content, compares standard value, when result is very close, then meets standard analysis
It is required that；
Precision Experiment: selection standard sample simultaneously carries out xrf analysis 10 experimental datas of measurement respectively, when Ta element
When standard deviation is all in lesser range, illustrate that this analysis method whole process is reliable and stable.
It is that drafting working curve is carried out by series standard sample that effect of the invention, which is using this analysis determining method, quasi-
Really and quickly measure Ta constituent content in low-alloy steel.Using this analysis method, analysis result is accurate and reliable, meets enterprise pair
Detect that analysis data is rapid, accurate demand.And easy to operate, favorable reproducibility, it can accurately and quickly measure steel alloy
The content of kind Ta element.Although chemical method analysis is classical analysis method, the period is tediously long, and consumes a large amount of chemistry examination
Agent saves the consumption of period and chemicals using this analysis method.
Detailed description of the invention
Fig. 1 is Ta constituent content and intensity.
Specific embodiment
It is subject to below with reference to measuring method of the example to Ta element in X-ray fluorescence spectra analysis low-alloy steel of the invention
Explanation.
The measuring method of X-ray fluorescence spectra analysis low-alloy steel Ta element of the invention is based on following design philosophy: X
Fluorescent x ray spectroscopy x is to generate incident X-rays i.e. primary X-ray, excites sample.Each element meeting in sample
Secondary x rays are radiated, and the secondary x rays that different elements is radiated have specific energy response or wavelength characteristic.
Detection system measures these energy and quantity for radiating the secondary x rays come.Information collected by detection system is converted into
The type and content of various elements in sample.The foundation of X-ray fluorescence spectra analytic approach progress quantitative analysis is the fluorescence X of element
Transmitted intensity I1With the content W of the element in sampleiIt is directly proportional: Ii=IsWi.
The measuring method of Ta element in X-ray fluorescence spectra analysis low-alloy steel of the invention, includes following steps:
1, apparatus measures condition
Apparatus measures condition
Used equipment is the MAX type Xray fluorescence spectrometer of company, Dutch pa nanogram section, power 4Kw, voltage
30Kv, electric current 110mA；
Analysis condition includes that analytical line, analyzing crystal, collimator, detector carry out selection, and this method selects MAX X-ray
The collimator of Fluorescence Spectrometer suggestion, detector, analytical line and analyzing crystal are rule of thumb to be selected.Measuring condition is seen below
Table 1.
1 element measuring condition of table
2, the preparation of sample
Standard sample and steel samples are prepared under the same terms, and standard sample and analysis sample grind and to put down, and are ground
Complete sample should not overheat, sample standing time is unsuitable too long, and otherwise specimen surface aoxidizes, and is unfavorable for exciting, and impact analysis is quasi-
Exactness.To the requirement of analysis sample, without shrinkage cavity, crackle, trachoma, otherwise testing staff can not be analyzed, and must be resampled, grind away line
Road is consistent, must not be criss-cross.High-carbon steel curved beam slow cooling occurs with Anti-cracking, forbids grinding overheat to analysis sample and cause point
Analyse result fluctuation.Analysis sample diameter cannot be less than 12mm, and thickness of sample is greater than 2mm.Standard sample is used to draw working curve,
Sample is analyzed to test for precision and accuracy.
3, the selection of standard sample
Purchase has the sample of Ta element definite value as standard sample, and each element content of standard specimen will have relatively accurate standard
Chemical analysis results.The content distribution of each element is uniform in standard specimen, without segregation phenomena.Standard specimen should be mingled with without shrinkage cavity, nothing.Standard specimen
The steel grade wanted and analyzed is identical as far as possible, all elements including analysis.The institutional framework of standard specimen will approach, analytical element in standard specimen
Content range it is wider than the content of analytical element, internal standard element content makes every effort to consistent.It is shown in Table 2.
The each standard sample Ta elemental standards value of table 2
4, working curve is drawn
Step 3. in standard sample Ta element select KA linear system, collimator select 300um, optical filter select copper
(brass) optical filter, crystal LiF200, detector select scintillation detector Scint, the operating condition of voltage 30Kv, W member
Element selection LA linear system, collimator select 300um, free of light filter, crystal LiF200, and detector selects flow probe Flow,
The operating condition of voltage 30Kv successively measures fluorescence intensity with X-fluorescence instrument, and the content of Ta element provides in the certificate, to survey
The fluorescence intensity of five fixed standard samples is abscissa, and using the Ta content of five standard samples as ordinate, it is bent to draw work
Line.
Pass through experiment, it is determined that the overlap peak and correction coefficient in each analysis channel, working curve equation are as follows:
C=D+ERM (1)
In formula: D is intercept, and E is slope, and R is counting rate, and M is matrix effect coefficient.
After corrected, the dispersion (RMS) and factor of merit (K) of curve be improved significantly, dispersion (RMS) and product
Matter coefficient (K)
N is standard specimen number, and k is linear regression related coefficient, and Cchem is that standard specimen gives standard value, and Ccak is to fit curve meter
Calculation value, Co are weighted factor (Co=0.1%), and Ta element dispersion (RMS) and factor of merit (K) value are all smaller.It is shown in Table 3.
3 analytical element calibration parameter of table
5. the precision of method, accuracy experiment
Selection standard sample carries out veracity and precision measurement.
Accuracy experiment carries out xrf analysis and wet chemical analysis, X-fluorescence point to 11# and 15# standard sample respectively
Analysis hair uses method of the invention.
The accuracy data of 4 method of table
Above-mentioned table 5 shows the analysis method and wet chemical acquired results analysis deviation very little, shows this method accuracy
It is high.
It carries out xrf analysis for 11# and 15# standard sample to measure 10 times, the result is shown in the following table 5.
The precision data of 5 method of table
Two samples are measured in table 5 and carry out 10 measurements, average value are calculated, to acquire the standard deviation of this method, from experiment
The precision of data investigates the stability of this analysis method, and upper table experimental data shows the standard deviation of Ta element all smaller
In the range of.Illustrate that this analysis method whole process is reliable and stable.
Fig. 1 is to measure the fluorescence of five standard samples of 11#, 12#, 13#, 14#, 15# respectively according to the measuring condition of table 1
Intensity, using the fluorescence intensity of five standard samples of 11#, 12#, 13#, 14#, 15# as ordinate, with 11#, 12#, 13#, 14#,
The standard value of the Ta content of five standard samples of 15# is abscissa, draws working curve, obtains Ta constituent content and intensity curve
Figure.
Using this experimental method, solve Ta element in low-alloy steel X fluorescence spectrum analysis can not accurately measure ask
Topic, easy to operate, determination data is accurate, saves the period lengthy process of wet chemical analysis and the consumption of chemicals.
Claims (3)
1. a kind of measuring method analyzed based on X-ray fluorescence spectra to Ta element in steel alloy, this method includes following step
It is rapid:
1. setting apparatus measures condition
Using MAX type Xray fluorescence spectrometer, in which: power 4Kw, voltage 30Kv, electric current 110mA；Ta element selects KA line
System, collimator select 300um, and optical filter selects brass copper optical filter, crystal LiF200, and detector selects scintillation detector
Scint, the operating condition of voltage 60Kv, collimator select 300um, free of light filter, crystal LiF200, detector selection stream
Amount detector Flow, the operating condition of voltage 30Kv,
2. the preparation of sample
Analysis sample grinds and to put down, no shrinkage cavity, crackle, trachoma, and grind away lines is consistent；
3. the selection of standard sample
Purchase has the sample of Ta element definite value as standard sample, and standard specimen constituent content to have standard chemical analysis as a result, content
It is evenly distributed, without segregation phenomena, no shrinkage cavity, nothing are mingled with；
4. drawing working curve
Using the operating condition of step 3., fluorescence intensity successively is measured with X-fluorescence instrument, the content of Ta element provides in the certificate,
Using the fluorescence intensity of five standard samples of measurement as abscissa, using the Ta content of five standard samples as ordinate, work is drawn
Make curve.
5. selection standard sample carries out veracity and precision measurement
Accuracy experiment: choosing several samples using method of the invention and carry out xrf analysis, measure Ta constituent content, than
To standard value, when result is very close, then meet standard analysis requirement；
Precision Experiment: selection standard sample simultaneously carries out xrf analysis 10 experimental datas of measurement, the standard deviation of Ta element respectively
When difference is all in lesser range, illustrate that this analysis method whole process is reliable and stable.
2. a kind of X-ray fluorescence spectra analysis according to claim 1 is to the measuring method of Ta element in steel alloy, special
Sign is: 2. the analysis specimen finish cannot be less than 12mm to step, and sample thickness is greater than 2mm.
3. a kind of X-ray fluorescence spectra analysis according to claim 1 is to the measuring method of Ta element in steel alloy, special
Sign is: the abscissa of the step 4. working curve diagram takes the fluorescence intensity of five standard samples, and ordinate takes five standard samples
The Ta content of product.
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Cited By (1)
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| CN111751395A (en) * | 2020-06-15 | 2020-10-09 | 安徽长江钢铁股份有限公司 | Method for measuring aluminum inclusion in steel |
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