Two-column separation detection system and detection method based on heart cutting

Abstract

The invention provides a heart-cutting-based double-column separation detection system and detection method, including a first venting column, a second venting column, a first separation column and a second separation column; the two ports of the ten-way valve are respectively the sample inlet and the sample Outlet, 2 ports are carrier gas inlets, 1 port is connected to the first vent column, 1 port is connected to the second vent column, 1 port of the first four-way valve is connected to the first vent column, 1 port is connected to the first vent column The first separation column is connected, one port of the second four-way valve is connected to the second vent column, one port is connected to the second separation column, and one port is the fourth carrier gas inlet; one port of the six-way valve is connected to the The detector is connected, one port is connected to the second separation column, and one port is connected to the first separation column. The main component is vented through valve cutting and the front-stage chromatographic column, and the residual main peak carrying impurities is further separated and detected through the post-stage chromatographic column, which significantly improves the detection limit of the traditional single-stage chromatographic column and maximizes the performance of the pulsed helium ionization detector.

Description

technical field [0001] The invention relates to the technical field of analysis and detection of impurities in high-purity electronic special gases, especially for the analysis and detection of ppb-level trace impurities covered by main components, and is an indispensable detection and analysis equipment for the development of the electronic special gas industry. Background technique [0002] With the large-scale production and application of high-purity electronic special gases, the quantitative detection of ppb-level impurities has become an important means of quality control of special gases. This detection limit makes the application of helium ionization detectors a key point. Initially, the helium ionization detector used the radioactive tritium source as the excitation energy source, and the β ions radiated by it collided with helium atoms under the action of a strong electric field, causing the helium to transition from the ground state to a high-energy excited state, ...

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Problems solved by technology

If the cut is too early, the main peak of phosphine will cover the peak of the arsine impurity, and the detection limit will be too high; if the cut is too late, the arsine impurity may also be cut

Therefore, the above-mentioned single-column system is difficult to guarantee the 100ppb impurity detection limit of main peak interference, such as image 3 , Figure 4 shown

[0004] Therefore, when using PDHID detectors in the field of special electronic gas analysis, the detection limits of the impurities separated by the chromatographic column before the main peak all meet the linear relationship of the PDHID detector and the detection limit standard of 10ppb; The corresponding detection limit is difficult to meet the 100ppb standard

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