Preparation method and application of needle-shaped sample for glow discharge mass spectrometry detection

A technology of glow discharge mass spectrometry and detection needle, which is applied in the field of analysis and detection, can solve the problems of easy melting of the sample tip, small contact area, and poor cooling effect, so as to widen the size range of the sample, improve the heat conduction efficiency, and improve the cooling effect. effect of effect

Pending Publication Date: 2021-03-26
安徽中飞科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the small contact area between the needle-shaped sample holder and the sample cell, and the outlet of the needle-shaped sample holder is circular, for some non-cylindrical or small-sized samples, the cooling is mainly through the two screws on the bracket, so the cooling effect Not very good, when measuring some low melting point metals (such as Ga, Cd, Te, etc.) sample

Method used

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  • Preparation method and application of needle-shaped sample for glow discharge mass spectrometry detection
  • Preparation method and application of needle-shaped sample for glow discharge mass spectrometry detection
  • Preparation method and application of needle-shaped sample for glow discharge mass spectrometry detection

Examples

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Effect test

Embodiment 1

[0021] This example provides a method for preparing a needle-shaped sample for glow discharge mass spectrometry detection. The preparation method of the needle-shaped sample used for glow discharge mass spectrometry detection in this embodiment comprises the following steps:

[0022] (1) Scrub the needle-shaped sample holder once with hydrofluoric acid, rinse it with pure water, place it in a mixed acid of nitric acid and hydrochloric acid (both volume ratio nitric acid: hydrochloric acid = 1:3) and heat it for 30 minutes, then use pure Wash with water for 2-3 times, then place it on a class 100 clean bench to dry;

[0023] (2) Inject 0.08mL of liquid gallium (purity: 99.9999wt%) into the needle-shaped sample holder, and then insert the gallium sample (namely Ga, specification Φ2.5*22mm) into the liquid gallium;

[0024] (3) Clamp the sample holder with Teflon tweezers and insert the sample holder into the liquid nitrogen cup filled with liquid nitrogen, keep the sample port ...

Embodiment 2

[0030] This example provides a method for preparing a needle-shaped sample for glow discharge mass spectrometry detection. The preparation method of the needle-shaped sample used for glow discharge mass spectrometry detection in this embodiment comprises the following steps:

[0031] (1) Scrub the needle-shaped sample holder once with hydrofluoric acid, rinse it with pure water, place it in a mixed acid of nitric acid and hydrochloric acid (both volume ratio nitric acid: hydrochloric acid = 1:3) and heat it for 30 minutes, then use pure Wash with water for 2-3 times, then place it on a class 100 clean bench to dry;

[0032] (2) Inject 0.08mL of liquid gallium (purity: 99.9999wt%) into the needle-shaped sample holder, and then insert the tellurium sample (i.e. Te, specification 2mm*2mm*18mm) into the liquid gallium;

[0033] (3) Clamp the sample holder with Teflon tweezers and insert the sample holder into the liquid nitrogen cup filled with liquid nitrogen, keep the sample po...

Embodiment 3

[0039] This example provides a method for preparing a needle-shaped sample for glow discharge mass spectrometry detection. The preparation method of the needle-shaped sample used for glow discharge mass spectrometry detection in this embodiment comprises the following steps:

[0040] (1) Scrub the needle-shaped sample holder once with hydrofluoric acid, rinse it with pure water, place it in a mixed acid of nitric acid and hydrochloric acid (both volume ratio nitric acid: hydrochloric acid = 1:3) and heat it for 30 minutes, then use pure Wash with water for 2-3 times, then place it on a class 100 clean bench to dry;

[0041] (2) Inject 0.08mL of liquid gallium (purity: 99.9999wt%) into the needle-shaped sample holder, and then insert the antimony sample (i.e. Sb, specification 1mm*2mm*8mm) into the liquid gallium;

[0042] (3) Clamp the sample holder with Teflon tweezers and insert the sample holder into the liquid nitrogen cup filled with liquid nitrogen, keep the sample port...

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Abstract

The invention provides a preparation method and application of a needle-shaped sample for glow discharge mass spectrometry detection, and belongs to the technical field of analysis and detection. Theliquid gallium is injected into a needle-shaped sample holder, a sample to be detected is inserted into the liquid gallium, then the sample holder is inserted into the liquid nitrogen to be cooled, and after the liquid gallium is solidified, the sample holder is taken out to obtain the needle-shaped sample, so that when the obtained needle-shaped sample is used for glow discharge mass spectrometrydetection, a good cooling effect is achieved; the sample can be prevented from melting when the low-melting-point sample is detected, meanwhile, the size range of the sample capable of being detectedby glow discharge mass spectrometry is widened, and a conductor and a semiconductor with the size of 0-3 mm*0-3 mm*8-22 mm can be directly measured.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a method for preparing a needle-like sample used for glow discharge mass spectrometry detection and an application thereof. Background technique [0002] In recent decades, glow discharge mass spectrometry has become the most commonly used technique for the analysis of trace or ultra-trace impurities in high-purity materials. Currently commercialized glow discharge mass spectrometers are equipped with needle-shaped and sheet-shaped sample cells, so they can directly measure conductor and semiconductor samples that meet the size requirements, such as the Astrum glow discharge mass spectrometer produced by Nu Instruments Ltd. The discharge mass spectrometer can directly measure flake samples of 12-40×12-40×1-20mm and needle samples of 0.5-3×0.5-3×18-22mm. In actual detection, different detection methods can be selected according to the type of sample and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/64
CPCG01N27/64
Inventor 谭秀珍李瑶李江霖邓育宁朱刘
Owner 安徽中飞科技有限公司
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