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Two-dimensional back flush gas chromatograph gas circuit and analysis method thereof

A technology of backflushing gas and chromatography, which is applied in the field of gas chromatography analysis, can solve the problems of low detection ability and long analysis time, and achieve the effects of strong detection ability, improved analysis efficiency and cost saving

Inactive Publication Date: 2016-11-09
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the problems of long analysis time and low detection ability of the traditional industrial analysis method for the mixture of aniline and water system in the diaminodiphenylmethane product, and to provide a two-dimensional backflushing gas chromatography gas circuit and analysis method

Method used

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  • Two-dimensional back flush gas chromatograph gas circuit and analysis method thereof

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specific Embodiment approach 1

[0017] Specific implementation mode one: the following combination figure 1 Describe this embodiment, the two-dimensional backflushing gas chromatography gas path described in this embodiment includes a vaporization chamber 1, and it also includes No. 1 six-way valve 2, No. 2 six-way valve 3, No. 1 cone valve 4, No. 2 No. 5 cone valve, No. 1 packed column 6, No. 2 packed column 7, thermal conductivity detector 8 and hydrogen flame detector 9,

[0018] The six interfaces of No. 1 six-way valve 2 and No. 2 six-way valve 3 are arranged clockwise;

[0019] The inlet A of the carrier gas source is connected to the inlet of the vaporization chamber 1, the outlet of the vaporization chamber 1 is connected to the ① port of the No. 1 six-way valve 2, and the ② port of the No. 1 six-way valve 2 is connected to the inlet of the No. 1 packed column 6. The No. 1 packed column The outlet of 6 is connected to the ⑥ interface of the No. 1 six-way valve 2, and the ⑤ interface of the No. 1 six...

specific Embodiment approach 2

[0025] Specific implementation mode two: the following combination figure 1 Describe this embodiment, a two-dimensional backflush gas chromatography analysis method described in this embodiment, the analysis method is realized based on the two-dimensional backflush gas chromatography gas path described in the first specific embodiment,

[0026] Connect the ① port of the No. 1 six-way valve 2 with the ② port, the ③ port with the ④ port, and the ⑤ port with the ⑥ port; , ⑤ interface and ⑥ interface are connected to form the initial state of No. 1 six-way valve 2 and No. 2 six-way valve 3;

[0027] The diaminodiphenylmethane product solution enters from the inlet A of the carrier gas source, and is vaporized into a gas through the vaporization chamber 1. Driven by the carrier gas A, it flows through the No. 1 six-way valve 2 and the No. 1 packed column 6, and then enters the thermal Conducting detector 8 carries out moisture analysis;

[0028] When the water peak is finished, s...

example 1

[0033] Example 1: Detection ability experiment

[0034] Using dried acetone as a solvent, prepare 7 standard samples of water with different concentrations and aniline standard samples with different concentrations, and label them. Inject and analyze 7 standard samples in sequence, record the peak height of the water peak in the TCD thermal conductivity detector, and the peak height of aniline in the FID hydrogen flame detector, and take the water / aniline content in the sample as the X-axis, the water / aniline peak The peak height signal value was used as the Y axis, and the standard curve was drawn respectively and its sensitivity, detection limit and lower limit of quantification were calculated.

[0035]The results show that: the water content is between 0.696mg / mL~4.667mg / mL, the linear correlation is good, the correlation coefficient is 0.9953, the sensitivity is 1250.8μV / mg·mL-1, and the detection limit of water is 14.42μg / mL, the lower limit of quantification is 52.23 ...

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Abstract

The invention relates to a two-dimensional back flush gas chromatograph gas circuit and an analysis method thereof, and belongs to the technical field of gas chromatography in order to solve the problems of long analysis time and low detection ability of traditional analysis methods of an aniline and water blend system mixture in a diaminodiphenylmethane product. The gas circuit adopts a thermal conduction cell back flush system as a primary chromatograph and a hydrogen flame back flush system as a secondary chromatograph in order to obtain a two-dimensional back flush chromatograph. The analysis method realizes simultaneous analysis of tiny amounts of water and aniline in the diaminodiphenylmethane product through switching the connection state of a six-way valve 1 and a six-way valve 2. The gas circuit adopts a gas phase back flush technology in order to back flush impurities, so the analysis time is saved, and the sample size is increased in the same time, thereby the detection ability is improved. The gas circuit and the method are used for gas chromatography.

Description

technical field [0001] The invention relates to a two-dimensional backflushing gas chromatography gas circuit and an analysis method, belonging to the technical field of gas chromatography analysis. Background technique [0002] Diaminodiphenylmethane is one of the raw materials for synthesizing isocyanate. It is widely used in the polyurethane industry. In industrial production, after the synthesis of diaminodiphenylmethane products, it has the characteristics of high boiling point, many components, and high viscosity. Water and aniline will affect the quality and preservation of the downstream product isocyanate. In industrial analysis, gas chromatography is commonly used, using a hydrogen flame detector to analyze trace aniline in the product, and using a thermal conductivity cell detector to analyze water in the product. Because the diaminodiphenylmethane product contains a lot of components, its retention time in the chromatographic column varies greatly, and the tradi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/42G01N30/46
CPCG01N30/02G01N30/42G01N30/463G01N2030/025
Inventor 郑永杰田景芝裴迅荆涛崔宝君郭冠楠张洪瑞李郁吕键尤里
Owner QIQIHAR UNIVERSITY
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