Method for detecting volatile organic chlorides in resin by using headspace gas chromatography

A headspace gas chromatography and volatile organic technology, which is used in measuring devices, instruments, scientific instruments, etc., can solve the problems of chromatographic column pollution, detection errors, cumbersome and time-consuming preprocessing steps, etc. The effect of good precision

Active Publication Date: 2017-08-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although GC or HPLC has good selectivity and detection sensitivity, the pretreatment steps are cumbersome and time-consuming, and due to the volatility of the analyte, it will cause detection errors d

Method used

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  • Method for detecting volatile organic chlorides in resin by using headspace gas chromatography
  • Method for detecting volatile organic chlorides in resin by using headspace gas chromatography
  • Method for detecting volatile organic chlorides in resin by using headspace gas chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Sample preparation and determination

[0038] 1. Sample preparation

[0039] First, add 5mL of PAE sample and 1.5g of sodium chloride into two 20mL headspace bottles in parallel; then add 10μL of ECH (1%) and 30μL of pure DCP into the second headspace bottle quickly sealed after

[0040] 2. Determination of samples

[0041] Put the headspace sample vial in the headspace autosampler, under the given conditions, after equilibrium, detect by gas chromatography, and record the gas phase signal values ​​of ECH and DCP.

Embodiment 2

[0043] Chromatographic separation effect of ECH and DCP

[0044] figure 1 It is the chromatographic separation peak of a typical commercially available PAE sample under the given GC conditions. It can be seen from the figure that despite the miscellaneous peaks of other volatile substances, ECH and DCP can be well separated from the polymer and will not be affected by the miscellaneous peaks. The peak times are 1.2 and 4.0 respectively about min. The separation results also showed that the gas phase signal (corresponding to the gas phase concentration) of DCP was much higher than the ECH signal in HS-GC detection.

Embodiment 3

[0046] headspace equilibrium condition

[0047] For resin solution samples, it is necessary to achieve gas-liquid phase equilibrium of the analyte before GC detection. Figure 2 is the effect of different temperatures on the equilibration time of ECH and DCP in PAE samples. It can be seen from Figure 2 that DCP can reach phase equilibrium within 10 min, however, it takes longer time for ECH to reach phase equilibrium at high temperature. This anomaly is due to the gelation of PAE, which can seriously affect the equilibration time of ECH, especially at low levels.

[0048] Relatively short phase equilibration time can improve the analytical efficiency of the instrument, therefore, this study suggests to choose the phase equilibration time at low temperature. However, as shown in Figure 2, low temperature will affect the detection sensitivity of HS-GC. Considering all the factors, 60°C and 30 min were selected as the headspace equilibrium temperature and time in the subsequent ...

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Abstract

The invention discloses a method for detecting volatile organic chlorides in resin by using headspace gas chromatography. The method specifically is a headspace gas chromatography (HS-GC) method for detecting residual epichlorohydrin (ECH) and a by-product, 1,3-dichloro-2-propanol (DCP), in a polyamide polyamine epichlorohydrin (PAE) solution. The method is based on a phase balance achieved by a closed headspace bottle before GC detection under the headspace conditions of 60 DEG C and 30 minutes. An experiment proves that a PAE matrix solution affects the phase balance of a to-be-detected substance. Therefore, the accuracy of the method is tested by adopting a standard addition method. The result shows that the method has relatively good precision (RSD is smaller than 2.90%) and accuracy (the recovery rate range is 93.6%-105%). Therefore, the method is suitable for analysis of volatile organic chlorides in a PAE resin solution.

Description

technical field [0001] The invention relates to the detection of organic chlorides, in particular to a method for detecting volatile organic chlorides in resin (polyamide polyamine epichlorohydrin) by headspace gas chromatography. Background technique [0002] Polyamide polyamine epichlorohydrin (PAE) is a water-soluble, cationic, thermosetting resin, which has been widely used as a wet strength agent in the paper industry due to its excellent properties. PAE is a solution formed by the reaction of adipic acid (AA), diethylenetriamine (DETA) and epichlorohydrin (ECH). The reaction is as follows: [0003] AA+DETA→PPC (1) [0004] PPC+ECH→PAE (2) [0005] Among them, polyamide polyamine (PPC) is an intermediate produced by the reaction of AA and DETA, which can further react with ECH to generate PAE resin. At the same time, the excess epichlorohydrin remaining in the system will undergo acidolysis to generate 1,3-dichloro-2-propanol (DCP). Studies have shown that DCP can c...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 闫宁柴欣生
Owner SOUTH CHINA UNIV OF TECH
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