CN104390945A - Element content fluorescence analysis method of iron-base alloy - Google Patents
Element content fluorescence analysis method of iron-base alloy Download PDFInfo
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- CN104390945A CN104390945A CN201410624241.3A CN201410624241A CN104390945A CN 104390945 A CN104390945 A CN 104390945A CN 201410624241 A CN201410624241 A CN 201410624241A CN 104390945 A CN104390945 A CN 104390945A
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 78
- 239000000956 alloy Substances 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000012921 fluorescence analysis Methods 0.000 title claims abstract description 13
- 238000005259 measurement Methods 0.000 claims abstract description 13
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 68
- 230000015572 biosynthetic process Effects 0.000 claims description 17
- 238000003786 synthesis reaction Methods 0.000 claims description 16
- 239000000470 constituent Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 9
- 230000003595 spectral effect Effects 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 4
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 12
- 239000000126 substance Substances 0.000 description 8
- 238000012937 correction Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000013507 mapping Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000007704 wet chemistry method Methods 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention relates to an analysis method of the content of alloy elements, in particular to an element content fluorescence analysis method of iron-base alloy. According to the technical scheme, the method comprises the following steps: (1) measuring an iron-base alloy standard sample, and drawing a comprehensive standard curve; (2) determining an optimum measurement parameter of a fluorescence spectrometer; (3) analyzing the comprehensive standard curve, and determining a linear relation between the element characteristic X-ray intensity and the element content; (4) setting the content of each element in an iron-base alloy virtual synthesized standard sample; (5) drawing a single element virtual working curve; and (6) measuring the content of each element in the iron-base alloy to be detected by utilizing the single element virtual working curve. According to the element content fluorescence analysis method of the iron-base alloy, the intensity of the characteristic X rays of the element to be detected in the iron-base alloy sample is measured to obtain the content of the element in the iron-base alloy to be detected.
Description
Technical field
The present invention relates to a kind of analytical approach of alloying element content, be specifically related to a kind of constituent content fluorescence analysis method of ferrous alloy.
Background technology
Current normal employing wet chemistry method, induced coupled plasma atomic emission spectrometry and fluorescent spectrometry etc. analyze the chemical composition in ferrous alloy.Wet chemistry method need select the element of diverse ways to ferrous alloy to analyze one by one for different elements; Need to carry out chemical pre-treatment to ferrous alloy sample according to induced coupled plasma atomic emission spectrometry, recycling ICP spectrometer is measured, therefore these two schemes all have analytical cycle length, complex operation, the high deficiency of experimentation cost.
Fluorescent spectrometry analysis is quick, analytical cycle is short, but this method strictly relies on the standard sample for spectrochemical analysis of corresponding trade mark ferrous alloy, development due to ferrous alloy standard sample for spectrochemical analysis lags behind the production of metal material far away, so the widespread use of fluorescence method receives the restriction of same trade mark ferrous alloy standard sample for spectrochemical analysis.If the problem of ferrous alloy standard sample for spectrochemical analysis can be solved, the application of fluorescence spectrophotometer will be expanded widely, avoid analytical cycle length, complex operation, the high deficiency of experimentation cost, the chemical composition in various ferrous alloy can be analyzed rapidly, solve the composition detection problem of new grades ferrous alloy.
Summary of the invention
The invention provides a kind of constituent content fluorescence analysis method of ferrous alloy, by measuring the intensity of the characteristic X-ray of element to be measured in ferrous alloy sample, drawing the element component content of ferrous alloy to be measured.
Technical scheme of the present invention is as follows:
A constituent content fluorescence analysis method for ferrous alloy, comprises the steps:
(1) measure ferrous alloy standard specimen, utilize fluorescence spectrophotometer to measure existing various ferrous alloy standard specimen, utilize the basic parameter FP working software of fluorescence spectrophotometer to draw out the comprehensive standard curve of these ferrous alloys;
(2) contrast described comprehensive standard curve, to determine the optimum measurement parameter of fluorescence spectrophotometer for the various elements of ferrous alloy, comprise and excite angle, pulsating sphere, exciting voltage and excitation current;
(3) described comprehensive standard curve is analyzed, determine the interference of element spectral line overlap, measure the intensity of background interference and the interference of Measurement channel material, deduct these interference, utilize the basic parameter FP working software of fluorescence spectrophotometer to draw out the linear relationship of each elemental characteristic X-ray intensity in ferrous alloy and its constituent content;
(4) content of each element in ferrous alloy dummy synthesis standard specimen is set, existing various ferrous alloy element content range is come out, high-load element gets the content of intermediate value as this element in dummy synthesis standard specimen of scope, and low micro content element gets 1.2 ~ 1.5 times of content as this element in dummy synthesis standard specimen of the intermediate value of scope;
(5) the single element virtual work curve of ferrous alloy dummy synthesis standard specimen is drawn, according to the content of each element in described ferrous alloy dummy synthesis standard specimen, fluorescence spectrophotometer is set, with described optimum measurement parameter, fluorescence spectrophotometer is set again, according to each elemental characteristic X-ray intensity, the basic parameter FP working software of fluorescence spectrophotometer is utilized to draw out the single element virtual work curve of each element;
(6) ferrous alloy sample to be measured is put into sample box, utilize described single element virtual work curve to measure ferrous alloy sample to be measured, measure the content of each element in this ferrous alloy to be measured.
The constituent content fluorescence analysis method of described ferrous alloy, wherein said single element virtual work curve is the single-point straight line of zero crossing.
The constituent content fluorescence analysis method of described ferrous alloy, wherein said fluorescence spectrophotometer is Shimadzu XRF-1800 type sequential spectrometer.
Beneficial effect of the present invention is as follows:
1, the present invention adopts excitation of X-rays ferrous alloy series standard specimen, optimize the measuring condition of ferrous alloy element, find out linear relationship formed by elemental characteristic X-ray intensity and each constituent content, thus determine the content of virtual standard specimen and the clean intensity of each element, draw out single element virtual work curve; Range site element virtual work curve only both can carry out quantitative test to the chemical composition of ferrous alloy with several minutes, thus controlled the quality of material; Present invention greatly enhances the detection efficiency of ferrous alloy, shorten analytical cycle, be more applicable to the Production requirement of modern enterprise; Releasing standard substance to the restriction of ferrous alloy, is solved a composition detection difficult problem for new grades ferrous alloy, achieves the alloy examination of unknown trade mark ferrous alloy by analytical technology of the present invention.
2, fluorescence spectrophotometer of the present invention is Shimadzu XRF-1800 type sequential spectrometer, and utilize basic parameter FP working software wherein, analyst coverage is full of forgiveness.Its analyst coverage by the virtual impact of giving value size of ferrous alloy element, is not also subject to the restriction of the ferrous alloy standard specimen upper limit; Value of drafting as nickel is 15.0%, and in standard specimen GH2132, the most high-load of nickel is 30.1%, and the minimum content of analysis verification is 0.017%, and most high-load is 39.86%.
3, in the present invention, because constituent content is virtual given, there is not any error, the theoretical strength therefore calculated is entirely accurate.The unit that the single element virtual work curve of synthesis comprises have 26, can be used for all trades mark analyzed in ferrous alloy.
4, adopt other method of Comparison Method to verify feasibility of the present invention, through the analysis verification of the domestic and international standard specimen of more than 100, prove that the accuracy of analysis of single element virtual work curve can compare favourably with wet-chemical analysis.
5, the present invention saves the buying expenses of ferrous alloy standard substance; Remove without the restriction with trade mark ferrous alloy mark steel; Solve an analysis difficult problem for new grades ferrous alloy chemical composition, reduce expending of chemical reagent, shorten analytical cycle.
Accompanying drawing explanation
Fig. 1 is single element virtual work curve map.
Embodiment
A constituent content fluorescence analysis method for ferrous alloy, comprises the steps:
(1) ferrous alloy standard specimen is measured, fluorescence spectrophotometer used is Shimadzu XRF-1800 type sequential spectrometer, utilize fluorescence spectrophotometer to measure existing various ferrous alloy standard specimen, utilize the basic parameter FP working software of fluorescence spectrophotometer to draw out the comprehensive standard curve of these ferrous alloys;
(2) described comprehensive standard curve is contrasted, to determine the optimum measurement parameter of fluorescence spectrophotometer for the various elements of ferrous alloy, comprise and excite angle, pulsating sphere, exciting voltage and excitation current etc., its face shield diameter 20mm, the element that titanium and atomic number are greater than it selects voltage 60kV, electric current 55mA, and the element that scandium and atomic number are less than it selects voltage 30kV, electric current 110mA, other measurement parameter is in table 1;
(3) described comprehensive standard curve is analyzed, determine the interference of element spectral line overlap, measure the intensity of background interference and the interference of Measurement channel material, deduct these interference, utilize the basic parameter FP working software of fluorescence spectrophotometer to draw out the linear relationship of each elemental characteristic X-ray intensity in ferrous alloy and its constituent content;
(4) content of each element in ferrous alloy dummy synthesis standard specimen is set, existing various ferrous alloy element content range is come out, high-load element gets the content of intermediate value as this element in dummy synthesis standard specimen of scope, and low micro content element gets 1.2 ~ 1.5 times of content as this element in dummy synthesis standard specimen of the intermediate value of scope;
(5) the single element virtual work curve of ferrous alloy dummy synthesis standard specimen is drawn, according to the content of each element in described ferrous alloy dummy synthesis standard specimen, fluorescence spectrophotometer is set, with described optimum measurement parameter, fluorescence spectrophotometer is set again, according to each elemental characteristic X-ray intensity, the basic parameter FP working software of fluorescence spectrophotometer is utilized to draw out the single element virtual work curve of each element;
(6) ferrous alloy sample to be measured is put into sample box, utilize described single element virtual work curve to measure ferrous alloy sample to be measured, measure the content of each element in this ferrous alloy to be measured.
As shown in Figure 1, described single element virtual work curve is the single-point straight line of zero crossing.
In above-mentioned steps (3), the bearing calibration of element spectral line overlap interference is as follows: have in the present invention between 8 elements and there is overlapping interference, the overlapping correction coefficient between them is measured by standard method, iron is measured to cobalt with 1Cr18Ni9Ti stainless steel 7 standard specimens, plumbous to arsenic, chromium is to the overlapping correction coefficient of manganese, nickel is measured to copper with GH2132 high-alloy steel 4 standard specimens, titanium is to the overlapping correction coefficient of vanadium, molybdenum and tungsten is determined to phosphorus overlapping correction coefficient respectively by daily output austenitic stainless steel ST21-28 series cover mark and W18Cr4V cover mapping, overlap mapping with W18Cr4V and determine tungsten to silicon overlapping correction coefficient, the overlapping correction coefficient of nickel to tantalum is determined by daily output austenitic stainless steel ST21-28 series cover mapping, the overlapping interference coefficient K value of each element recorded is in table 2.
In above-mentioned steps (3), utilize Rayleigh scattering cableties except background intensity and the impact eliminating channel material: the X-ray intensity that basic parameter FP method is used for unknown element cubage must be clean intensity, utilize the Rayleigh scattering line of rhodium target as line of reference, deduct as the method for deduction element spectral line overlap interference, which reduce the Measuring Time analyzing this element at least half, and decrease the error brought because measuring background intensity.The simple X ray launched from target after irradiation surface under measurement, scattering and the fluorescent X-ray that excites will through restriction light hurdle and collimating apparatus (slit).Under radiation exposure, they also can inspire the characteristic ray of each element in this material, the characteristic ray of each element that final and detected materials inspires mixes and arrives detecting device through light splitting, formation channel material disturbs, channel material is made up of stainless steel, and affected is iron, nickel, chromium 3 elements.By the method for deduction element spectral line overlap interference, with the Rayleigh scattering line of rhodium target for line of reference is deducted, make the analysis result of low content nickel, chromium in ferrous alloy very desirable.
Table 1: elements are contained parameter list
Table 2: element drafts the measurement range of content and checking
Claims (3)
1. a constituent content fluorescence analysis method for ferrous alloy, is characterized in that, described method comprises the steps:
(1) measure ferrous alloy standard specimen, utilize fluorescence spectrophotometer to measure existing various ferrous alloy standard specimen, utilize the basic parameter FP working software of fluorescence spectrophotometer to draw out the comprehensive standard curve of these ferrous alloys;
(2) contrast described comprehensive standard curve, to determine the optimum measurement parameter of fluorescence spectrophotometer for the various elements of ferrous alloy, comprise and excite angle, pulsating sphere, exciting voltage and excitation current;
(3) described comprehensive standard curve is analyzed, determine the interference of element spectral line overlap, measure the intensity of background interference and the interference of Measurement channel material, deduct these interference, utilize the basic parameter FP working software of fluorescence spectrophotometer to draw out the linear relationship of each elemental characteristic X-ray intensity in ferrous alloy and its constituent content;
(4) content of each element in ferrous alloy dummy synthesis standard specimen is set, existing various ferrous alloy element content range is come out, high-load element gets the content of intermediate value as this element in dummy synthesis standard specimen of scope, and low micro content element gets 1.2 ~ 1.5 times of content as this element in dummy synthesis standard specimen of the intermediate value of scope;
(5) the single element virtual work curve of ferrous alloy dummy synthesis standard specimen is drawn, according to the content of each element in described ferrous alloy dummy synthesis standard specimen, fluorescence spectrophotometer is set, with described optimum measurement parameter, fluorescence spectrophotometer is set again, according to each elemental characteristic X-ray intensity, the basic parameter FP working software of fluorescence spectrophotometer is utilized to draw out the single element virtual work curve of each element;
(6) ferrous alloy sample to be measured is put into sample box, utilize described single element virtual work curve to measure ferrous alloy sample to be measured, measure the content of each element in this ferrous alloy to be measured.
2. the constituent content fluorescence analysis method of ferrous alloy according to claim 1, is characterized in that, described single element virtual work curve is the single-point straight line of zero crossing.
3. the constituent content fluorescence analysis method of ferrous alloy according to claim 1, is characterized in that, described fluorescence spectrophotometer is Shimadzu XRF-1800 type sequential spectrometer.
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| CN105486707A (en) * | 2015-11-20 | 2016-04-13 | 沈阳黎明航空发动机(集团)有限责任公司 | Quantitative fluorescence analysis method for cobalt-based alloy |
| CN108663389A (en) * | 2017-03-29 | 2018-10-16 | 上海宝钢工业技术服务有限公司 | The x-ray fluorescence assay method of lead and rapid determination of content of cadmium element in aluminium alloy |
| CN108918567A (en) * | 2018-07-19 | 2018-11-30 | 三明惊石农业科技有限公司 | A kind of detection method for bamboo shoots |
| 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 |
| CN111323445A (en) * | 2020-04-02 | 2020-06-23 | 平湖旗滨玻璃有限公司 | Method for detecting tin penetration amount of glass |
| CN113109395A (en) * | 2021-04-20 | 2021-07-13 | 南昌大学 | Nondestructive testing method for measuring content of magnetic components in magnetic composite material |
| CN118225826A (en) * | 2024-05-24 | 2024-06-21 | 苏州佳谱科技有限公司 | A light element detection method and system |
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| CN105259196A (en) * | 2014-07-08 | 2016-01-20 | 日本株式会社日立高新技术科学 | Sample Plate for X-Ray Analysis and X-Ray Fluorescent Analyzer |
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| CN105486707B (en) * | 2015-11-20 | 2018-01-09 | 沈阳黎明航空发动机(集团)有限责任公司 | A kind of quantitative fluorescence analysis method of cobalt-base alloys |
| CN108663389A (en) * | 2017-03-29 | 2018-10-16 | 上海宝钢工业技术服务有限公司 | The x-ray fluorescence assay method of lead and rapid determination of content of cadmium element in aluminium alloy |
| CN108918567A (en) * | 2018-07-19 | 2018-11-30 | 三明惊石农业科技有限公司 | A kind of detection method for bamboo shoots |
| 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 |
| CN111323445A (en) * | 2020-04-02 | 2020-06-23 | 平湖旗滨玻璃有限公司 | Method for detecting tin penetration amount of glass |
| CN111323445B (en) * | 2020-04-02 | 2023-07-07 | 平湖旗滨玻璃有限公司 | Method for detecting tin penetration amount of glass |
| CN113109395A (en) * | 2021-04-20 | 2021-07-13 | 南昌大学 | Nondestructive testing method for measuring content of magnetic components in magnetic composite material |
| CN118225826A (en) * | 2024-05-24 | 2024-06-21 | 苏州佳谱科技有限公司 | A light element detection method and system |
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