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A microwave plasma atomic emission spectrometry and system for directly analyzing solid samples

A technology of microwave plasma and data analysis system, applied in the field of plasma atomic emission spectrometer, can solve problems such as increasing the complexity of the device, and achieve the effects of shortening detection time, simple device and easy operation

Active Publication Date: 2021-10-22
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 usually require additional components such as lasers and electric heating components to be added to the experimental device, which increases the complexity of the device. degree

Method used

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  • A microwave plasma atomic emission spectrometry and system for directly analyzing solid samples
  • A microwave plasma atomic emission spectrometry and system for directly analyzing solid samples
  • A microwave plasma atomic emission spectrometry and system for directly analyzing solid samples

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 50 Ω impedance Matching coaxial cables; the microwave cavity is a Surfa...

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 a system capable of injecting solid samples. The steps of the method of the present invention are: (1) get the standard solid sample of known element content, obtain reference substance directly as reference substance or after tableting; (2) get the solid sample to be measured, according to the same method of step (1), Obtain test article; (3) reference substance and test article are detected with microwave plasma spectrometer of the present invention respectively; According to reference substance detection result, select element characteristic spectral line; And draw standard curve, and according to each in test article Spectral line position and / or intensity are calculated to obtain the type and / or content of each element in the test product. The invention also discloses a microwave plasma atomic emission spectrometer, which includes a microwave plasma system, a gas transmission system, a sample carrying system, a signal collection system and a data analysis system. The test method of the invention is simple in operation, fast in analysis speed, avoids the use of chemical reagents, and is environmentally 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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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/71
CPCG01N21/71
Inventor 段忆翔牛广辉
Owner SICHUAN UNIV
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