CN110455779A - Analysis method based on Ce elements in direct reading spectrometry measurement low-alloy steel - Google Patents
Analysis method based on Ce elements in direct reading spectrometry measurement low-alloy steel Download PDFInfo
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- CN110455779A CN110455779A CN201910641131.0A CN201910641131A CN110455779A CN 110455779 A CN110455779 A CN 110455779A CN 201910641131 A CN201910641131 A CN 201910641131A CN 110455779 A CN110455779 A CN 110455779A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
- G01N21/67—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence using electric arcs or discharges
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Abstract
The invention discloses the analysis methods of Ce elements in a kind of direct reading spectrometry measurement low-alloy steel, have selection instrument and setting operating condition, the preparation of sample, the selection of standard sample, analysis and result including step.The beneficial effects of the present invention are: analysis result is accurate and reliable, meet that enterprise is rapid to detection analysis data, accurate demand.And easy to operate, favorable reproducibility, it can accurately and quickly measure the content of Ce element.
Description
Technical field
The invention belongs to Analysis of Metallic Materials technical field of research, measure low-alloy steel more particularly to a kind of direct reading spectrometry
The analysis method of middle Ce elements.
Background technique
Direct-reading spectrometer is one of analysis of metallic materials common instrument, have quickly, accurate, precision is high, easy to operate etc.
Feature is that chemical analysis method is incomparable.It is a kind of method of quantitative analysis, has good, the calibration curve line of selectivity
The advantages that property range is wide, and accuracy is high.Since the analysis of low-alloy steel spark source atomic emission spectrometry needs usually to quote cerium member
Element, but there is no the method in national standard to Ce elements in existing national standard, therefore studied based on direct-reading spectrometer.
Summary of the invention
To solve the problems, such as above-mentioned technology, the object of the present invention is to provide one kind to have accurate exactness and precision
Direct reading spectrometry measurement low-alloy steel in Ce elements analysis method.
To achieve the above object, the technical solution adopted by the present invention is that: cerium member in a kind of direct reading spectrometry measurement low-alloy steel
The analysis method of element, this method includes following steps:
Step 1: selection instrument and setting operating condition
Direct-reading spectrometer, in which: vacuum degree is 16 μm of Hg, and vacuum room temperature is 38 DEG C, focal length 1m；Analysis condition are as follows:
Analytical gap 3mm, it is purity of argon >=99.999% that spark chamber, which controls atmosphere, and argon flow includes rinsing 15L/min, integral
0L/min, static 1L/min, prespark period 12s, time of integration 15s；
Step 2: the preparation of analysis sample
Analyze the size of sample: diameter is greater than 16mm, and thickness is greater than 2mm, and guarantees that sample surfaces are smooth, clean, sample
Surface zero defect；
Step 3: the selection of standard sample
Fe element: wavelength is 271.40nm or 273.07nm or 287.20nm, noiseless element；
Ce element: wavelength 399.92nm；
Step 4: the content of analysis Ce element
1) it first excites style 2-5 times, instrument is made to be in optimum Working；
2) production of standard sample working curve: 16 serial standard samples, each standard sample excitation 3 are excited one by one
Point, using 3 excitation intensity average values of Ce element of each standard sample as abscissa, the true value in each standard sample is vertical sits
Mark draws standard sample working curve；
3) according still further to the analysis condition of table 1, excitation analysis sample is found out point according to obtained intensity from working curve
Analyse the content of element.
Step 5: result:
1) accuracy is tested: is analyzed respectively GBW01673 and gbw1666 standard sample, wet chemical measures Ce member
Element, direct reading spectrometry use above-mentioned steps, GBW01673 and gbw1666 standard sample carries out the Ce constituent content point that spectrum measures
It Wei 0.127% and 0.018%；The content of wet chemical analysis measurement is respectively 0.128 and 0.018%, as a result meets standard
Analysis requires；
2) Precision Experiment: carrying out spectrum analysis respectively for GBW01673 and gbw1666 standard sample and measure 10 times, point
The standard deviation for analysing sample is respectively 0.122% and 0.127%Ce, and the standard deviation data of element shows that this law analytic process is steady
It is fixed.
Analysis sample described in step 2 is ground under the conditions of 60 mesh sand paper, consistent with standard sample lines.
Described in step 2 analysis sample will use similar steel grade, close chemical content have exhibit matter excitation analysis, and should
Sample is uniform.
Excitation standard sample described in step 4 is 16 series, and each standard sample excites at 3 points, with each standard sample
3 excitation intensity average values of Ce element be abscissa, the true value in each standard sample is ordinate, draws standard sample work
Make curve.
Effect of the invention is accurately and quickly to measure Ce constituent content using this analysis determining method.Without one's duty
When analysis method, the Ce element for measuring sample is analyzed with wet chemical, and the period is long.Using this analysis method, it is accurate to analyze result
Reliably, meet that enterprise is rapid to detection analysis data, accurate demand.And easy to operate, favorable reproducibility, it can be accurate and fast
The content of the measurement Ce element of speed.
Detailed description of the invention
Fig. 1 is Ce constituent content and intensity.
Specific embodiment
It is illustrated below with reference to measuring method of the example to Ce element in low-alloy steel of the invention.
The method of Ce elements is based on following design philosophy in direct reading spectrometry measurement low-alloy steel of the invention: Ce member at present
The analysis method of element mostly uses humid analysis, without rapid analysis method.Principle are as follows: using the bulk sample prepared as one
Electrode makes sample with light source generator and shines to exciting between electrode, and the light beam is introduced light-splitting chamber, passes through dispersion element
After spectral resolution, the intensity of selected internal standard line and analytical line is measured, the calibration curve of according to standard sample production is asked
The content of element to be measured in sample is analyzed out.
The method of Ce elements in direct reading spectrometry measurement low-alloy steel of the invention, includes following steps:
1. apparatus measures condition
Used equipment be ARL4460 direct-reading spectrometer, vacuum degree: 16 μm of Hg, vacuum room temperature: 38 DEG C, focal length 1m；
Analysis condition see the table below 1.
1 analysis condition of table
2. the preparation of sample
The diameter for analyzing sample is greater than 16mm, and thickness is greater than 2mm, and guarantees that sample surfaces are smooth, clean.Standard sample and
Analysis sample is ground under the conditions of 60 mesh sand paper, and sample lines is consistent, sample surfaces zero defect.
3. the selection of standard sample
Every time analysis sample before will use similar steel grade, close chemical content have exhibit matter excitation analysis, to ensure instrument
The normal use of device.The sample must be very uniform.The following table 2 lists the wavelength of analytical element.
2 Ce elemental analysis line wavelength of table
| Element | Wavelength |
| Ce | 399.2nm |
4. analytical procedure
4.1 analysis work before, first excite one piece sample 2-5 times, it is ensured that instrument stabilizer makes instrument be in best effort shape
State.
The production of 4.2 working curves: under operating condition as shown in Table 1, exciting 16 serial standard samples one by one,
Each standard sample excites, using 3 excitation intensity average values of Ce element of each standard sample as abscissa, each standard at 3 points
True value in sample is ordinate, draws standard sample working curve.Obtain Ce constituent content and intensity.Table 3 is mark
The true value and excitation intensity data of quasi- sample.
As shown in Figure 1, exciting 16 serial standard samples, each standard one by one under operating condition as shown in Table 1
3 points of sample excitation, using 3 excitation intensity average values of Ce element of each standard sample as abscissa, in each standard sample
True value is ordinate, draws standard sample working curve.Obtain Ce constituent content and intensity.
The true value and excitation intensity data of 3 standard sample of table
4.3 excitation control samples and analysis sample, each sample are at least excited 2-3 times, are averaged.
4.4, according to the intensity of analytical line, find out the content of analytical element from calibration curve.
5. results and discussion
Accuracy experiment: analyzing GBW01673 and GBW1666 standard sample respectively, and wet chemical measures Ce member
Element, direct reading spectrometry use above-mentioned steps, GBW01673 and GBW1666 standard sample carries out the Ce constituent content point that spectrum measures
It Wei 0.127% and 0.018%；The content of wet chemical analysis measurement is respectively 0.128% and 0.018%, as a result meets mark
Quasi- analysis requires.
Precision Experiment: carrying out spectrum analysis respectively for GBW01673 and GBW1666 standard sample and measure 10 times, analysis
The standard deviation of sample is respectively 0.122%, and the standard deviation data of 0.127%, Ce element shows that this law analytic process is stablized.
Ce element precision data is as shown in table 4:
4 sample precision data of table
Claims (4)
1. a kind of analysis method based on Ce elements in direct reading spectrometry measurement low-alloy steel, comprising the following steps:
Step 1: selection instrument and setting operating condition
Direct-reading spectrometer, in which: vacuum degree is 16 μm of Hg, and vacuum room temperature is 38 DEG C, focal length 1m；Analysis condition are as follows: analysis
Gap 3mm, it is purity of argon >=99.999% that spark chamber, which controls atmosphere, and argon flow includes rinsing 15L/min, integral 0L/
Min, static 1L/min, prespark period 12s, time of integration 15s；
Step 2: the preparation of analysis sample
Analyze the size of sample: diameter is greater than 16mm, and thickness is greater than 2mm, and guarantees that sample surfaces are smooth, clean, sample surfaces
Zero defect；
Step 3: the selection of standard sample
Fe element: wavelength is 271.40nm or 273.07nm or 287.20nm, noiseless element；
Ce element: wavelength 399.92nm；
Step 4: the content of analysis Ce element
1) instrument is made to be in optimum Working；
2) production of standard sample working curve: excitation standard sample is flat with 3 excitation intensities of Ce element of each standard sample
Mean value is abscissa, and the true value in each standard sample is ordinate, draws standard sample working curve；
3) excitation analysis sample finds out the content of analytical element according to obtained intensity from standard sample working curve；
Step 5: result:
1) accuracy is tested: GBW01673 and GBW1666 standard sample to be analyzed respectively, wet chemical measures Ce element,
Direct reading spectrometry uses above-mentioned steps, GBW01673 and GBW1666 standard sample carries out the Ce constituent content difference that spectrum measures
For 0.127% and 0.018%；The content of wet chemical analysis measurement is respectively 0.128 and 0.018%, as a result meets standard scores
Analysis requires；
2) it Precision Experiment: carries out spectrum analysis respectively for GBW01673 and GBW1666 standard sample and measures 10 times, analyze sample
The standard deviation of product is respectively 0.122% and 0.127%Ce, and the standard deviation data of element shows that this law analytic process is stablized.
2. a kind of analysis method based on Ce elements in direct reading spectrometry measurement low-alloy steel according to claim 1, special
Sign is: analysis sample described in step 2 is ground under the conditions of 60 mesh sand paper, consistent with standard sample lines.
3. a kind of analysis method based on Ce elements in direct reading spectrometry measurement low-alloy steel according to claim 1, special
Sign is: analysis sample described in step 2 will use similar steel grade, close chemical content to have the excitation analysis of exhibit matter, and the sample
Uniformly.
4. a kind of analysis method based on Ce elements in direct reading spectrometry measurement low-alloy steel according to claim 1, special
Sign is: excitation standard sample described in step 4 is 16 series, and each standard sample excites at 3 points, with each standard sample
3 excitation intensity average values of Ce element are abscissa, and the true value in each standard sample is ordinate, draw standard sample work
Curve.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113218934A (en) * | 2021-04-08 | 2021-08-06 | 江西理工大学 | Detection method for rapidly determining content of yttrium in steel by utilizing full-spectrum spark direct-reading spectrometry |
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- 2019-07-16 CN CN201910641131.0A patent/CN110455779A/en active Pending
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| CN103575707A (en) * | 2013-11-15 | 2014-02-12 | 西安航空动力股份有限公司 | Method for measuring components of nickel-based high-temperature alloy steel by using photoelectric direct reading spectrometer |
| CN107340276A (en) * | 2017-07-06 | 2017-11-10 | 钢研纳克检测技术有限公司 | A kind of method of multiple element content in quick measure rare earth metal/alloy |
| CN109540872A (en) * | 2018-11-28 | 2019-03-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Use the method for direct-reading spectrometer measurement nickel-base alloy ingredient |
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| CN113218934A (en) * | 2021-04-08 | 2021-08-06 | 江西理工大学 | Detection method for rapidly determining content of yttrium in steel by utilizing full-spectrum spark direct-reading spectrometry |
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