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Method of improving precision of quantitative analysis of overlapping peak of laser induced breakdown spectrometry

A technology of laser-induced breakdown and quantitative analysis, which is applied in thermal excitation analysis, material excitation analysis, and material analysis through optical means, etc. It can solve the problem of low accuracy, low accuracy, and inability to accurately remove overlapping peaks in quantitative analysis, etc. problem, to achieve the effect of simplifying the process of interference correction, reducing hardware cost and important application value

Active Publication Date: 2017-06-09
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the above defects or improvement needs of the prior art, the present invention provides a method for improving the quantitative analysis accuracy of laser-induced breakdown spectrum overlapping peaks, which uses the optimized integral area factor W obtained from the corresponding calibration sample 1 and W 2 , overlapping interference factor α opt , decomposition layer number L, wavelet function F and continuous background subtraction scaling factor γ opt Correct the spectrum, and finally use the univariate linear regression model to predict the content of the analytical elements in the sample to be tested, which can effectively solve the existing problems of quantitative analysis accuracy of overlapping peaks caused by the low accuracy of overlapping peak decomposition and the inability to accurately remove continuous background interference. It has the advantages of convenient and accurate analysis, and is suitable for occasions such as quantitative analysis of overlapping peaks of materials with complex matrices, especially steel, plastic, and petroleum.

Method used

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  • Method of improving precision of quantitative analysis of overlapping peak of laser induced breakdown spectrometry
  • Method of improving precision of quantitative analysis of overlapping peak of laser induced breakdown spectrometry
  • Method of improving precision of quantitative analysis of overlapping peak of laser induced breakdown spectrometry

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Experimental program
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Effect test

Embodiment 1

[0088] (1) LIBS spectral data acquisition of samples

[0089] The experimental samples were selected from 6 kinds of microalloy steel standard samples (No. GSB03-2453-2008, developed by the Institute of Analysis and Testing of the General Iron and Steel Research Institute and Maanshan Iron and Steel Co., Ltd.). Table 1 shows.

[0090] Table 1

[0091]

[0092]The experimental device is an ordinary laser-induced breakdown spectroscopy device. The experiment is carried out in an air environment. A Q-switched Nd:YAG pulsed laser (Beamtech Nimma 400, wavelength 532nm, repetition frequency 3Hz, pulse width 8ns) is used, and the laser energy is 80mJ / pulse. The laser is focused onto the sample surface through a mirror and a plano-convex lens (focal length 15 cm). To prevent air breakdown, the focal point is 4 mm below the sample surface. The acquisition delay time was set to 2 μs, the gate width was set to 10 μs, the excited plasma radiation was collected by the light collect...

Embodiment 2

[0108] (1) LIBS spectral data acquisition of samples

[0109] The experimental samples were selected from 6 kinds of microalloy steel standard samples (No. GSB03-2453-2008, developed by the Institute of Analysis and Testing of the General Iron and Steel Research Institute and Maanshan Iron and Steel Co., Ltd.). 4. The sample LIBS spectral data was collected under the same experimental conditions, and each sample was collected 6 times, and 30 pulses were accumulated for each spectrum.

[0110] Table 4

[0111]

[0112] (2) Acquisition of overlapping spectral line parameters, decomposition layer number l, spectral line integration range w 1 、w 2 and the optimization of the overlapping interference factor α

[0113] Query the NIST standard atomic spectrum database, combined with the actual spectrum, to determine the central wavelength of the analytical element line V and the interference line Fe are 292.40nm and 292.38nm, respectively. In the wavelet function, take db1, t...

Embodiment 3

[0127] (1) LIBS spectral data acquisition of samples

[0128] The experimental samples were selected from 6 kinds of microalloy steel standard samples (No. GSB03-2453-2008, developed by the Institute of Analysis and Testing of the General Iron and Steel Research Institute and Maanshan Iron and Steel Co., Ltd.). The contents of trace metal elements Mn and Cr in the samples are shown in Table 7. . The sample LIBS spectral data was collected under the same experimental conditions, and each sample was collected 6 times, and 30 pulses were accumulated for each spectrum.

[0129] Table 7

[0130]

[0131](2) Acquisition of overlapping spectral line parameters, decomposition layer number l, spectral line integration range w 1 、w 2 and the optimization of the overlapping interference factor α

[0132] Query the NIST standard atomic spectrum database, combined with the actual spectrum, determine the central wavelength of the analytical element line Mn and the interference line C...

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Abstract

The invention discloses a method of improving the precision of quantitative analysis of an overlapping peak of laser induced breakdown spectrometry. The method comprises the following steps: detecting a calibrated sample with known element content by means of an LIBS technology to obtain a spectrogram of the calibrated sample; then correcting overlapping interference and continuous background interference by means of integral strength combined with small wave transformation, establishing a univariate linear regression model by separately taking the corrected characteristic spectral line integral strength and the content of analysis element as an independent variable and a dependent variable, and optimizing integral region factors w1 and w2, an overlapping interference factor alpha, a decomposing layer number l, and a wavelet function and continuous background deduction scale factor gamma according to a root-mean-square error of the calibrated sample; and finally, correcting the spectrum of a to-be-detected sample by employing the optimized parameters of the corresponding calibrated sample, and predicting the content of the analysis element in the to-be-detected sample by means of the univariate linear regression model. The method disclosed by the invention can remove interference of overlapping and continuous background on the spectral line, so that the precision of quantitative analysis of the overlapping peak in a complicated sample of a base body can be effectively improved.

Description

technical field [0001] The invention belongs to the technical field of material component detection, and more specifically relates to a method for improving the quantitative analysis accuracy of laser-induced breakdown spectrum overlapping peaks. Background technique [0002] Laser Induced Breakdown Spectroscopy (LIBS for short) focuses a high-energy-density pulsed laser on the surface of the substance to be measured, ablates it to generate a high-temperature plasma, and then determines the measured substance by collecting and analyzing the emission spectrum in the plasma. Material composition analysis technology for the composition and content of each element in a substance. Due to the advantages of fast speed, no sample preparation, multi-element, long-distance and online simultaneous detection, LIBS technology has broad application prospects in many fields such as industrial production, environmental monitoring, biomedicine and space exploration. [0003] However, the ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/71
CPCG01N21/718
Inventor 郭连波郭阳敏杨新艳朱志豪李阔湖李祥友曾晓雁陆永枫
Owner HUAZHONG UNIV OF SCI & TECH
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