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Silane sampling system adopting gas chromatography and method thereof

A technology of sampling system and sampling system, which is applied in the analysis field of industrial production of silane, achieves the effects of short analysis period, fulfillment of analysis requirements, and safe and easy operation

Active Publication Date: 2014-04-09
ZHEJIANG ZHONGNING SILICON IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the sampling problem of gas chromatography analysis of silane, the invention provides a sampling system and method for gas chromatography analysis of silane

Method used

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  • Silane sampling system adopting gas chromatography and method thereof
  • Silane sampling system adopting gas chromatography and method thereof
  • Silane sampling system adopting gas chromatography and method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Implementation example 1: design and installation of silane sampling system

[0047] 1. Use 316L stainless steel pipes to connect multiple detection points in the process with the sampling pipeline of the sampling system. Pipelines are connected by welding, and pipelines, valves and filters are connected by gold-plated ferrules.

[0048] 2. Connect cylinder helium gas at the front end of the sampling pipeline, which can purge the whole pipeline. The purity of helium is required to be greater than 99.999% in volume percentage.

[0049] 3. Install a helium purge valve at the back end of the injection line, and adjust the injection pressure to stabilize at 0.05MPa.

[0050] 4. Connect a venting bypass at the end of the sampling line, use a needle valve to adjust the venting flow rate, which is required to reach 300-500ml / min venting flow rate, and quickly replace the residual sample between the sampling point and the sampling system to extract to a representative sample...

Embodiment 2

[0053] Implementation Example 2: Using the sampling system to sample and analyze silane standard gas

[0054] 1. Silane standard gas 1 component: nitrogen: 50.1ppm; silane balance gas;

[0055] 2. Connect the silane standard gas cylinder to the sampling system from the inlet of sample 1, open the second vacuum valve 9 to vacuum the sampling system for 30 seconds, close the second vacuum valve 9, open the helium purge valve 1, and use high Purging with pure helium for 3 minutes. Repeat the above operation 3 times.

[0056] 3. Open the sample injection valve 2, let the silane standard gas 1 enter the sampling system, adjust the silane injection pressure to 0.05MPa, adjust the silane injection flow rate to 50ml / min, use the six-way quantitative valve 14 to quantify, and control the injection volume to 1ml into the gas chromatographic analysis, the analysis spectrum is as follows image 3 .

Embodiment 3

[0057] Implementation example 3: Connect another bottle of silane standard gas to verify the purging and replacement effect of the sampling system during switching analysis.

[0058] 1. Silane standard gas 2 components: Nitrogen: 2.9ppm; Silane balance gas;

[0059] 2. Connect the silane standard gas cylinder to the sampling system from the sample 2 inlet, open the second vacuum valve 9 and vacuum the sampling system for 30 seconds, close the second vacuum valve 9, and open the helium purge valve 1 to purge 3 minutes, with helium purge. Repeat the above operation 3 times. The previously analyzed silane standard gas 1 is purged and replaced.

[0060] 3. Open the sampling valve of sample 2, let the silane standard gas 2 enter the sampling system, adjust the silane sampling pressure to 0.05MPa, adjust the silane sampling flow rate to 50ml / min, open the inlet gas chromatography needle valve 13, and make the silane standard gas 2 enter the sampling system. Gas 2 enters the gas c...

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Abstract

The invention discloses a silane sampling system adopting gas chromatography and a method thereof. The system comprises a sample introduction system, a high-purity helium scavenging line, a quick sample replacement pipeline, a venturi tube vacuum generation device and an alkali absorption cell, wherein the sample introduction system comprises a plurality of sample introduction pipelines, the high-purity helium scavenging line comprises a helium scavenging valve, a second filter, a pressure regulating valve, a second pressure gauge, a gas chromatography needle valve and a six-way proportional valve, which are connected in sequence, the quick sample replacement pipeline comprises an air release needle valve and a float flowmeter, and the venturi tube vacuum generation device comprises a nitrogen valve, a first pressure gauge, a first vacuumizing valve, a second vacuumizing valve and a venturi tube. The silane sampling system disclosed by the invention can be used for quickly scavenging and completely replacing the whole sample introduction system to avoid interference of residues in dead corners on analysis when switching samples on various detection points for analysis; and the system and the method disclosed by the invention are short in analysis period, safe, simple and convenient to operate and capable of meeting high frequency analysis requirements of industrial production.

Description

technical field [0001] The invention relates to the analysis field of industrially produced silane, in particular to a sampling system and method for analyzing silane by using gas chromatography. Background technique [0002] Silane, the molecular formula is SiH 4 , is a colorless poisonous gas with extremely active chemical properties. It can spontaneously ignite when it encounters air, producing very thick white fumes of amorphous silica. Silane is often used in solar cell manufacturing, integrated circuit manufacturing, coated reflective glass manufacturing and other industries. When used, the impurity gas (H 2 , N 2 、CH 4 etc.) are strictly required. [0003] The impurity gas in silane is often analyzed by gas chromatography. Due to the active nature of silane, it is easy to decompose and generate dust to block the sampling pipeline. How to achieve safe and accurate injection of silane has always been a difficult problem to solve. [0004] At present, there is no f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/22G01N30/20
Inventor 陈德伟高平洲张鹏飞郑安雄
Owner ZHEJIANG ZHONGNING SILICON IND
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