Microwave plasma atomic emission spectrometry directly analyzing solid sample and system thereof

A technology of microwave plasma and atomic emission spectroscopy, applied in the field of plasma atomic emission spectrometer, can solve the problems of increasing the complexity of the device, and achieve the effects of fast testing speed, easy portability, and avoiding the use of chemical reagents

Active Publication Date: 2018-02-06
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used solid sampling methods include laser ablation, electrothermal evaporation sampling, and electric spark ablation. These indirect sampling methods usuall...

Method used

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  • Microwave plasma atomic emission spectrometry directly analyzing solid sample and system thereof
  • Microwave plasma atomic emission spectrometry directly analyzing solid sample and system thereof
  • Microwave plasma atomic emission spectrometry directly analyzing solid sample and system thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Embodiment 1 Microwave plasma spectrometer of the present invention

[0074] figure 1 Implementing device for direct analysis of solid samples based on microwave plasma. The implementing device is composed of a microwave plasma system, a gas transmission system, a sample carrying system, a signal collection system, and a data analysis system. The microwave plasma system includes a microwave power source 7, a coaxial cable 9, and a microwave cavity 6. The coaxial cable 9 connects the microwave cavity 6 and the interface 8 on the microwave power source 7 to realize the transmission of microwave energy. The gas discharge tube 5 used is a quartz tube with an inner diameter of 1 mm, an outer diameter of 6 mm, and a length of 200 mm. The gas transmission system consists of a gas cylinder 1, a pressure gauge 2, a mass flow controller 3, and a gas pipeline 4, which can provide a working gas with a speed of 0-1L / min for the plasma system. In this example, the working gas is ar...

Embodiment 2

[0076] Embodiment 2 The microwave plasma spectrometer of the present invention detects the element type and content in the standard product

[0077] Specifically, the job analysis conditions in this implementation case are as follows:

[0078] (1) Sample preparation: Take 0.8g standard soil sample (GSS-2, GSS-3, GSS-4, GSS-5, GSS-6, GSS-7, GSS-14) or CuSO 4 , Pb(NO 3 ) 2 , CrCl 3 Analytical pure, maintained at 4MPa pressure for 2min, made into discs of samples to be analyzed with a diameter of 13mm and a thickness of 2mm, and placed in a desiccator for testing.

[0079] (2) The microwave plasma system is used to directly detect and analyze the samples.

[0080] The plasma working gas used is argon with a purity of 99.999%, the gas flow rate is set to 200mL / min, the microwave power source outputs 2450MHz microwave in the form of continuous wave, and the output power is set to 120W; the coaxial cable is 50Ω impedance matching Coaxial cable; the microwave cavity is a Surfatr...

Embodiment 3

[0086] Embodiment 3 Verification of the method of the present invention——test element content in GBW07408 (GSS-8) sample

[0087] (1) sample preparation

[0088] Take 0.8g GBW07408 (GSS-8) sample, maintain it under 4MPa pressure for 2min, make a disc of the sample to be analyzed with a diameter of 13mm and a thickness of 2mm, and place it in a desiccator for testing.

[0089] (2) Using microwave plasma system to directly detect and analyze samples

[0090] The plasma working gas used is argon with a purity of 99.999%, the gas flow rate is set to 200mL / min, the microwave power source outputs 2450MHz microwave in the form of continuous wave, and the output power is set to 120W; the coaxial cable is 50Ω impedance matching Coaxial cable; the microwave cavity is a Surfatron cavity based on surface waves; the sample stage is three-dimensionally adjustable, which can easily adjust the test position of the sample and the relative height between the sample and the plasma; the signal col...

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Abstract

The invention discloses a microwave plasma atomic emission spectrometry and system allowing solid sampling. The method comprises the following steps of (1) using a standard solid sample with element content known as a reference substance directly or tableting the standard solid sample to obtain the reference substance; (2) using a to-be-tested solid sample as a reference substance directly or tableting the to-be-tested solid sample to obtain a test article; and (3) detecting the reference substance and the test article by the microwave plasma spectrometer, selecting an element characteristic spectrum according to a detection result of the reference substance, drawing a standard curve, and calculating according to a position and/or strength of each spectrum in the test article so as to obtain the type and/or content of each element in the test article. The invention further discloses a microwave plasma atomic emission spectrometer that comprises a microwave plasma system, an air transmission system, a sample bearing system, a signal collection system and a data analysis system. The test method is easy to operate, has high analysis speed, uses no chemical reagents, and is environment-friendly.

Description

technical field [0001] The invention relates to the field of direct analysis of solid samples, in particular to the field of element analysis on the surface and inside of solid samples, in particular to a microwave plasma atomic emission spectrometer for directly analyzing solid samples and its application. Background technique [0002] At present, the analysis of solid samples is often carried out by wet digestion, that is, before the instrumental analysis, the solid sample must be crushed, ground and digested. Due to the complexity and tediousness of the pretreatment process, the uncertainty of the analysis and test is often introduced. Factors increase the uncertainty of the method, which in turn affects the accuracy and stability of the test method. In addition, the digestion process of samples often requires the use of dangerous chemical reagents such as perchloric acid, concentrated nitric acid or caustic soda, which cannot meet the development requirements of green an...

Claims

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Application Information

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IPC IPC(8): G01N21/71
CPCG01N21/71
Inventor 段忆翔牛广辉
Owner SICHUAN UNIV
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