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Method for determining residual methylbenzene and residual ethyl acetate in methyl vinyl ether-maleic anhydride copolymer

A technology of methyl vinyl ether and ethyl acetate, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems that are not seen and affect the quality of polymers, improve quality, avoid other interference, and have strong practicability Effect

Inactive Publication Date: 2016-05-11
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If toluene and ethyl acetate are not removed effectively, it will affect the quality of the polymer
There are certain reports on the synthesis method of this polymer in domestic and foreign literature, but there is no qualitative and quantitative determination method for quickly and accurately residual toluene and ethyl acetate in this polymer.

Method used

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  • Method for determining residual methylbenzene and residual ethyl acetate in methyl vinyl ether-maleic anhydride copolymer
  • Method for determining residual methylbenzene and residual ethyl acetate in methyl vinyl ether-maleic anhydride copolymer
  • Method for determining residual methylbenzene and residual ethyl acetate in methyl vinyl ether-maleic anhydride copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The methyl vinyl ether-maleic anhydride copolymer was weighed in parallel into two headspace vials, where m of sample 1 was 1 =0.1311g, m of sample 2 2 = 0.1219 g, then pipette 10 mL of dimethyl sulfoxide into a headspace vial, cover and shake on an air-bath shaker for 1 hour until completely dissolved, to obtain solution 1 and solution 2 to be tested.

[0037] The test solution 1 and the test solution 2 were injected through a static headspace and then measured by gas chromatography-mass spectrometry (GC-MS), and the peak positions of toluene and ethyl acetate were determined by mass spectrometry scanning. The total ion current diagram of GC-MS of solution 1 to be tested is as follows image 3 As shown, the peak retention time of ethyl acetate is 2.414min, and the peak retention time of toluene is 4.570min. Then according to the peak area of ​​the selected characteristic peak, it can be calculated by the standard equation of ethyl acetate and toluene. The concentrat...

Embodiment 2

[0040]The methyl vinyl ether-maleic anhydride copolymer was weighed in parallel into two headspace vials, where m of sample 1 was 1 =0.1514g, m of sample 2 2 = 0.1847 g, then pipette 10 mL of dimethyl sulfoxide into a headspace bottle, cover and shake on an air bath shaker for 1 hour until completely dissolved, to obtain solution 1 and solution 2 to be tested.

[0041] The test solution 1 and the test solution 2 were injected through a static headspace and then measured by gas chromatography-mass spectrometry (GC-MS), and the peak positions of toluene and ethyl acetate were determined by mass spectrometry scanning. Then according to the peak area of ​​the selected characteristic peak, it can be calculated by the standard equation of ethyl acetate and toluene. The content of ethyl ester was 9.97mg / g and 3.96mg / g, respectively. The concentrations of toluene and ethyl acetate in solution 2 to be tested are 0.17 mg / mL and 0.071 mg / mL, respectively, so the contents of toluene and...

Embodiment 3

[0043] Standard addition recovery experiment: Weigh two samples of methyl vinyl ether-maleic anhydride copolymer, respectively, the m of sample 1 1 =0.1029g, mass m of sample 2 2＝ 0.1028g. Add 3 μL of 100 mg / mL mixed standard of toluene and ethyl acetate to sample 2, then pipette 10 mL of dimethyl sulfoxide into a headspace vial, cover and shake on an air bath shaker for 1 hour to completely dissolve, and obtain Test solution 1 and test solution 2.

[0044] The test solution 1 and the test solution 2 were injected through a static headspace and then measured by gas chromatography-mass spectrometry (GC-MS), and the peak positions of toluene and ethyl acetate were determined by mass spectrometry scanning. Calculated according to the methods of Examples 1 and 2, the contents of toluene and ethyl acetate in sample 1 are 3.70 mg / g and 9.22 mg / g respectively, and the contents of toluene and ethyl acetate in sample 2 are 6.26 mg / g respectively and 1.17 mg / g, the spiked recoveries ...

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Abstract

The invention discloses a method for determining residual methylbenzene and residual ethyl acetate in a methyl vinyl ether-maleic anhydride copolymer. The method comprises the following steps of (1) dissolving a to-be-detected sample into a to-be-detected solution by using dimethyl sulfoxide; (2) dissolving the methylbenzene and the ethyl acetate by using the dimethyl sulfoxide to prepare at least three standard solutions of which the concentrations comprise the concentration of the methylbenzene and the concentration of the ethyl acetate in the to-be-detected solution; (3) carrying out GC-MS (Gas Chromatography-Mass Spectrometry) determination on the standard solutions which are in different concentrations, and respectively establishing standard curves of peak area of concentration-GC peaks of the methylbenzene and the ethyl acetate and standard equations of the methylbenzene and the ethyl acetate through regression analysis; (4) carrying out the GC-MS determination on the to-be-detected solution under the same conditions, determining out-of-peak positions and characteristic ions of the methylbenzene and the ethyl acetate through MS scanning, and obtaining the contents of the methylbenzene and the ethyl acetate in the to-be-detected solution through the peak area of characteristic ion peaks in the out-of-peak positions and regression calculation. The method disclosed by the invention has the advantages that the determining result is rapid, accurate and reliable, and the practicability is very high.

Description

technical field [0001] The invention relates to the field of determination methods in analytical chemistry, in particular to a method for determination of residual toluene and ethyl acetate in methyl vinyl ether-maleic anhydride copolymers. Background technique [0002] Methyl vinyl ether-maleic anhydride copolymer is a water-soluble electrolyte polymer, which is one of the few synthetic electrolyte polymers that are non-toxic and harmless to humans and animals. Because the polymer has good chemical stability, low toxicity, biocompatibility, adhesion, cohesion, moldability (the mold is easy to peel), complexation, chelation and other properties, so It has a wide range of uses in modern industry, and can be used as dispersant, coupling agent, stabilizer, thickener, emulsifier, film-forming agent or antistatic agent. The specific uses are mainly oral care, such as: toothpaste products, mouthwashes, dental adhesives, denture cleaners, etc. [0003] However, a certain amount o...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 杨小秋李航陈焱玲
Owner JIANGHAN UNIVERSITY
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