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A pretreatment method for improving the sensitivity of elements in solid detection samples

A technology for sample detection and pretreatment, which is used in the preparation, sampling, and measurement devices of samples for testing. Material cost, the effect of eliminating the introduction of secondary pollution

Active Publication Date: 2020-10-13
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is used for sample monitoring and can be used for laser-induced breakdown spectroscopy analysis with simple or no processing of the sample, but the detection sensitivity is not high, and the influence of the matrix effect is obvious, which makes calibration difficult.

Method used

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  • A pretreatment method for improving the sensitivity of elements in solid detection samples
  • A pretreatment method for improving the sensitivity of elements in solid detection samples
  • A pretreatment method for improving the sensitivity of elements in solid detection samples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Mix GBW-07408 national standard soil sample and nano-alumina powder evenly at a mass ratio of 1:4, press it into a disc with a diameter of 13 mm with a tablet machine, and part of the tablet will not be processed for comparison , the other part of the tablet is sintered for 30s with a 980nm continuous laser with a laser power of 100W, and the laser spot diameter is adjusted to about 10mm. The two groups of pellets were subjected to LIBS test and chromium signal comparison.

[0033] figure 2 For the comparison of the detection results of the present invention for chromium, as shown in the figure, the signal strength of chromium in the soil pretreated by the present invention is about 3 times stronger than that of the traditional direct compression test, which means that the sensitivity got improved.

Embodiment 2

[0035] Mix GBW-07408 national standard soil sample and nano-alumina powder evenly at a mass ratio of 1:4, press it into a disc with a diameter of 13 mm with a tablet machine, and part of the tablet will not be processed for comparison , the other part of the tablet was sintered with a 980nm continuous laser with a laser power of 100W for 30 s, and the laser spot diameter was adjusted to about 10 mm. The two groups of pellets were subjected to LIBS test and the signals of magnesium and silicon were compared.

[0036] image 3 For the comparison of the detection results of the present invention for magnesium and silicon, as shown in the figure, the signal strength of magnesium and silicon in the soil pretreated by the present invention is about 2 times higher than that of the traditional direct compression test. The above obvious enhancement means that the sensitivity has been improved.

Embodiment 3

[0038] Mix Pu’er tea sample 1 and nano-alumina powder evenly according to the mass ratio of 1:4, and press it into a disc with a diameter of 13 mm with a tablet machine. The surface of the chip was sintered for 30 s with a 980 nm continuous laser with a laser power of 100 W, and the laser spot diameter was adjusted to about 10 mm. The two groups of compressed tablets were subjected to LIBS test and calcium element signal comparison.

[0039] Figure 4 For the comparison of the detection results of the calcium element in tea sample 1, as shown in the figure, the signal intensity of the calcium element of the tea tablet pretreated by the present invention is about 5 times stronger than that of the traditional direct tablet test signal intensity , which means that the sensitivity has been significantly improved.

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Abstract

The invention discloses a pretreatment method of improving element sensitivity in a solid detection sample. The method comprises the steps of: a) grinding the sample to be detected into fine powder, adding a nano oxide for uniform mixing, and performing pressing and sheeting, b) heating and sintering the surface of a sample pressing sheet, and c) fixing the heated and sintered sample pressing sheet on an objective table, detecting the sample pressing sheet and calibrating target elements in the sample pressing sheet, wherein the surface of the sample pressing sheet is heated by a continuous laser or a quasi-continuous laser; the size of a laser spot is the same as that of the surface of the sample pressing sheet; and the surface of the sample pressing sheet is sintered by adjusting laser energy. The nano oxide is doped in the sample to be detected; since the nano oxide has strong adsorptive capacity on metal cations, metal elements in the sample are enriched and concentrated under a heating condition; matrices of the different samples are unified via the doping of the nano oxide; the spectral intensity of the target elements of a laser induced breakdown spectral test is improved ina sintering area finally; a matrix effect is weakened; and the element calibration is achieved.

Description

technical field [0001] The invention relates to a pretreatment method for improving the sensitivity of elements in a solid detection sample, in particular to a sample doped with nano-oxides heated by high-power continuous laser sintering, thereby realizing concentrated adsorption of target elements by nano-oxides under high temperature conditions , and the conversion of the multi-element matrix to a unified matrix, thereby improving the signal intensity of the target element in the laser-induced breakdown spectrum for sample compression, weakening the matrix effect, and realizing the method of element calibration. Background technique [0002] In recent years, there has been an increasing demand for the detection of common sample elements, such as the detection of heavy metal elements in water and soil to monitor and control heavy metal pollution, and the detection of various elements in organic matter such as vegetables and tea to evaluate their impact on The effects of ing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/40
CPCG01N1/405
Inventor 牛盛曾和平
Owner EAST CHINA NORMAL UNIV
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