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CN-121978082-A - Spark source atomic emission spectrometry method for acid-soluble aluminum and aluminum inclusion

CN121978082ACN 121978082 ACN121978082 ACN 121978082ACN-121978082-A

Abstract

The application provides a spark source atomic emission spectrometry method for acid-soluble aluminum and aluminum inclusion, belonging to the technical field of steel inclusion evaluation. The method for measuring the atomic emission spectra of the spark source of the acid-soluble aluminum and the aluminum inclusion comprises the following steps of establishing a calibration curve of all aluminum, measuring integral intensities of the aluminum inclusion in a sample, all aluminum and the acid-soluble aluminum under corresponding conditions, calculating the intensity of the aluminum inclusion by using the difference value of the two, calculating a calibration coefficient K according to 2 adjacent standard samples of the intensity selection of the aluminum inclusion in the sample, and calculating an excitation rate F according to the peak integral intensity of the aluminum inclusion in the standard sample with the aluminum content Al% <0.0007% and the integral intensity of the aluminum inclusion in the sample, wherein the aluminum inclusion content Al ins %=K×F×(I Alt -I Als ), and the aluminum inclusion content in the acid-soluble aluminum is equal to the difference between the aluminum inclusion and the aluminum inclusion. The application effectively improves the accuracy of the measurement result while ensuring high analysis speed, low cost and simple operation.

Inventors

  • SU HONGMEI
  • LIANG LIANG
  • SHAN QINGHUA
  • LIU ZHAO

Assignees

  • 湖南华菱涟源钢铁有限公司

Dates

Publication Date
20260505
Application Date
20260202

Claims (9)

  1. 1. A method for measuring the atomic emission spectrum of a spark source of acid-soluble aluminum and aluminum inclusion, which is characterized by comprising the following steps: s1, establishing a calibration curve of total aluminum content and spectral intensity; S2, measuring a sample to be measured to obtain total aluminum integral intensity I Alt and acid-soluble aluminum integral intensity I Als of the sample to be measured, and determining impurity aluminum integral intensity I Alins of the sample to be measured based on the total aluminum integral intensity I Alt and the acid-soluble aluminum integral intensity I Als ; s3, determining an impurity aluminum content calibration coefficient K based on the calibration curve and the total aluminum integral intensity I Alt of the sample to be tested; s4, determining an excitation coefficient F of the aluminum inclusion based on measurement data of a low-aluminum content standard sample; S5, calculating to obtain the aluminum inclusion content Alins% of the sample to be detected according to the integral intensity I Alins of the aluminum inclusion, the calibration coefficient K of the aluminum inclusion content and the excitation coefficient F of the aluminum inclusion, and calculating to obtain the acid-soluble aluminum content Als% according to the total aluminum content Alt% of the sample to be detected and the aluminum inclusion content Alins%.
  2. 2. The method for determining atomic emission spectra of acid-soluble aluminum and aluminum-occluded spark source according to claim 1 wherein the integrated intensity I Alins of aluminum-occluded in step S2 is calculated by the formula (1): I Alins = I Alt - I Als (1) Wherein, I Alt is the total aluminum integral intensity, and I Als is the acid-soluble aluminum integral intensity.
  3. 3. The method of claim 1, wherein the set of standard samples used to create the calibration curve in step S1 comprises at least one low aluminum standard sample having an aluminum content alt% of less than 0.0007%.
  4. 4. The method of claim 1, wherein determining the calibration factor K for the content of aluminum inclusions in step S3 comprises: Selecting two standard samples S1 and S2 with total aluminum integral intensity adjacent to the total aluminum integral intensity I Alt of the sample to be tested from the standard samples used by the calibration curve, and meeting the formula (2); S1I Alt <I Alt <S2I Alt (2) calculating the calibration coefficient K according to formula (3); K = (S2Alt%-S1Alt%)/(S2I Alt -S1I Alt )(3) Wherein S1I Alt is the integral intensity of the total aluminum of the S1 standard sample, S2I Alt is the integral intensity of the total aluminum of the S2 standard sample, K is the impurity aluminum calibration coefficient, S1Alt% is the total aluminum content of the S1 standard sample, and S2Alt% is the total aluminum content of the S2 standard sample.
  5. 5. The method according to claim 1, wherein in step S4, the excitation coefficient F of aluminum inclusion is calculated from the measured data of the low aluminum content standard sample by the formula (4); F = SdI ins / SdI Alt (4) Wherein SdI ins is the peak integral intensity of the aluminum inclusion of the low-aluminum content standard sample, and SdI Alt is the total aluminum integral intensity of the low-aluminum content standard sample.
  6. 6. The method of claim 1, wherein in step S5, the content of aluminum inclusions is calculated by the formula (5): Alins% = K ×F× IA lins (5) wherein K is an aluminum inclusion calibration coefficient, F is an aluminum inclusion excitation coefficient, and IA lins is an aluminum inclusion integral intensity.
  7. 7. The method for determining atomic emission spectra of acid-soluble aluminum and aluminum-occluded spark source according to claim 1, wherein in step S5, the acid-soluble aluminum content is calculated by the formula (6): Als% = Alt%-Alins%(6) Wherein Alt% is the total aluminum content, which is obtained by the calibration curve according to the total aluminum integral intensity I Alt , and Alins% is the inclusion aluminum content.
  8. 8. The method for determining the atomic emission spectrum of an acid-soluble aluminum and aluminum-doped spark source according to claim 1, wherein the method uses a spark source atomic emission spectrometer which meets the requirements of national metrology verification code JJG 768 on the emission spectrometer.
  9. 9. The method of atomic emission spectrometry of acid soluble aluminum and aluminum-occluded spark source of claim 1 wherein the total aluminum is the sum calculated as elemental aluminum, including solid solution aluminum, aluminum nitride and aluminum from a variety of aluminum compounds.

Description

Spark source atomic emission spectrometry method for acid-soluble aluminum and aluminum inclusion Technical Field The application relates to the technical field of inclusion evaluation in steel, in particular to a spark source atomic emission spectrometry method for acid-soluble aluminum and inclusion aluminum. Background At present, the determination of aluminum inclusion and acid-soluble aluminum in steel mainly comprises wet analysis, spark spectrum pulse distribution analysis PDA method and spark spectrum peak value integral analysis PIMS method. Document 1 (Sun Qing. Determination of acid-insoluble aluminum in steel [ J ] physical and chemical examination. Chemical division, 1986,22 (05): 286-288) considers that the silicon content is high, acid-insoluble aluminum is stable complex nitrogen oxides formed by Si3N4 and AlN, the traceability of the measurement results is doubtful, the dissolution rate of aluminum inclusions in steel is closely related to the dissolution method, and the concept of acid-soluble aluminum cannot be clearly described. Document 2 (Sun, wang Haizhou. Acid decomposition behavior study of aluminum in different states [ J ]. Metallurgical analysis, 2002, (05): 15-16.) acid decomposition behavior of aluminum in different states (metallic aluminum, alumina, aluminum nitride) was studied. The result shows that the dissolution rate of the aluminum inclusion in the steel is closely related to the dissolution method, the characterization of the acid-soluble aluminum and the acid-insoluble aluminum is related to the specified dissolution conditions, and the influence factors of the wet analysis on the determination of the acid-soluble aluminum show that the accuracy of the standard value of the acid-soluble aluminum in the standard sample is not high. The PDA method is one of the best analysis methods for analyzing aluminum inclusions, and document 3 (Zhao Lanji, xu Hongying, li Zhiguo, etc. photoelectric direct-reading spectrometry is used for determining physical and chemical tests (chemical division) of aluminum in different forms in steel, 2011,47 (03): 355-356.) it is considered that the PDA method can analyze the particle size of inclusions in addition to the content of acid-soluble aluminum-acid-insoluble aluminum. The application of the spark source atomic emission spectrometry to analysis of the state of inclusions in steel [ J ]. Metallurgical analysis 2011,31 (05): 20-26.) in document 4 (Li Dongling, li Meiling, gu Yunhai, et Al) is considered that the PDA method can realize the respective measurement of solid-solution Al, alN and Al 2O 3 by further analyzing the pulse distribution by a separate analysis method. PDA methods require hardware improvements involving the instrument. The PIMS method receives a lot of attention because it can perform aluminum state analysis by only changing the calculation method without additional hardware investment. The PI M method is to analyze the relation between the initial peak and the inclusion content and convert the relation to obtain the inclusion content when the sample is excited by the spark light source and the peak higher than the stable intensity appears in the earlier stage of the combustion curve. The common practice is to establish 2 independent calibration curves of acid-soluble aluminum and full aluminum, and directly read out the contents of the acid-soluble aluminum and the full aluminum after measuring a sample to be measured. And 2 independent calibration curves of all aluminum and aluminum inclusions or acid-soluble aluminum inclusions can be established to finish the measurement. The problem with this method is that it requires the use of standard samples with acid soluble aluminium and all aluminium with accurate and reliable values. That is, the measurement results of acid-soluble aluminum and aluminum inclusions depend on the accuracy of the fixed value of acid-soluble aluminum. Therefore, the acid-soluble aluminum concept in the current wet analysis is not clear and reliable, so that the accuracy of the standard sample fixed value is not high, the speed of the wet analysis is low, the equipment hardware improvement is required for the acid-soluble aluminum and the aluminum inclusion in the spark spectrum PDA method, and the accuracy of the acid-soluble aluminum standard sample fixed value is depended on. The method for measuring the content of the acid-soluble aluminum and the aluminum inclusion is lack of a measuring method which is high in measuring speed without wet analysis, does not need improvement of spark spectrometer hardware, and is high in analyzing speed without depending on the accuracy of the standard sample acid-soluble aluminum constant value. Disclosure of Invention The application is made in view of the above problems, and has an object to provide a method for measuring an atomic emission spectrum of an acid-soluble aluminum and an aluminum-doped spark source, which comprises the steps of firstly est