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External standard measurement method for benzene and benzene series in glyceryl triacetate by adopting headspace-gas phase mass spectrometry

A technique for the determination of glyceryl acetate and its application in measuring devices, instruments, scientific instruments, etc., which can solve the problems of complicated and time-consuming sample processing, and achieve the effects of simplifying pre-processing steps, reducing processing time, and simple operation

Active Publication Date: 2015-02-04
CHINA TOBACCO GUANGDONG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses the internal standard method, and the sample processing is cumbersome and time-consuming

Method used

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  • External standard measurement method for benzene and benzene series in glyceryl triacetate by adopting headspace-gas phase mass spectrometry
  • External standard measurement method for benzene and benzene series in glyceryl triacetate by adopting headspace-gas phase mass spectrometry
  • External standard measurement method for benzene and benzene series in glyceryl triacetate by adopting headspace-gas phase mass spectrometry

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: Establish the external standard determination method of benzene and benzene series in the glycerol triacetate of headspace-gas chromatography mass spectrometry

[0032] S1. Preparation of standard working solution: Accurately weigh 100mg of benzene, toluene, ethylbenzene, o-xylene, m-xylene, and p-xylene standard products respectively, place them in the same 100mL volumetric flask, and use chromatographically pure triacetin Dilute to volume with ester to obtain a primary mixed standard stock solution with the concentration of each component being 1mg / mL; accurately pipette 1mL of primary mixed standard stock solution, place it in a 100ml volumetric flask, and dilute to volume with chromatographically pure glycerol triacetate , to obtain the secondary mixed standard stock solution with the concentration of each component being 10ug / mL; accurately pipette 0.01, 0.02, 0.05, 0.1, 0.2, 0.5mL secondary mixed standard stock solution, place them in 10mL volumetric ...

Embodiment 2

[0043] Embodiment 2 Practical application example

[0044] Other operations and conditions were the same as those in the examples, and 5 triacetin samples were randomly selected as detection and analysis objects, and 1.0 mL triacetin samples were accurately pipetted each time into 10 mL headspace bottles, which were immediately sealed for testing. The test results are shown in Table 3:

[0045] Table 3 Test results of benzene and benzene series in samples

[0046]

[0047] Repeatability and recovery experiment results are shown in Table 4:

[0048] Table 4 Test results

[0049] compound

[0050] The present invention determines the scientific headspace processing conditions, completes the processing of the sample solution, and after the sample is scientifically and reasonably processed by the headspace instrument of the present invention, it is directly introduced into the gas chromatography mass spectrometry analysis, which effectively reduces the detection bro...

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Abstract

The invention discloses an external standard measurement method for benzene and benzene series in glyceryl triacetate by adopting headspace-gas phase mass spectrometry. Benzene and benzene series in glyceryl triacetate are determined by using a headspace-gas phase mass spectrometry method; the quantity is fixed by adopting the external standard method, in combination with optimization measures such as taking chromatographic pure glyceryl triacetate as a solvent and a matrix correction agent, and a sample pretreatment method, the detection chromatographic condition is specifically determined, relatively good chromatographic peak separation effects of benzene, methylbenzene, ethylbenzene, o-xylene, m-xylene and paraxylene are ensured, and the external standard measurement method has relatively good linear dependence. The detection limit of benzene and benzene series is 0.01-0.02mug / mL; the relative standard deviation is 1.1%-4.8%; the recovery rate is 89.9%-97.1%; the error and complicated operation caused by sample pretreatment are effectively reduced; and the treatment time is also greatly reduced.

Description

technical field [0001] The invention relates to the technical field of detection, and more specifically relates to an external standard determination method for benzene and benzene series in glycerol triacetate by using headspace-gas mass spectrometry. Background technique [0002] Glycerin triacetate is applied to the tow to prepare a filter rod, which is tipped and packed into a cigarette. The quality of glycerol triacetate not only affects the production and processing of filter rods and the physical indicators of filter rods, but also affects the quality and taste of cigarettes and the health of consumers. [0003] At present, the industrial production of glycerol triacetate usually adopts an acid-catalyzed synthesis method. In order to move the reaction to the direction of producing glycerol triacetate, benzene and benzene series are added. The determination of benzene and benzene series content in triacetin is of great significance to the quality of triacetin, the qua...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 穆小丽梅丹丹杜瑞华孙兆东
Owner CHINA TOBACCO GUANGDONG IND
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