Method for detecting 1-vinyl imidazole in chemical product

A technology of vinylimidazole and detection method, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., to achieve the effects of simple operation, symmetrical peak shape, high accuracy and precision

Pending Publication Date: 2021-10-22
杭州科准检测科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the qualitative and quantitative detection methods of 1-vinylimidazole

Method used

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  • Method for detecting 1-vinyl imidazole in chemical product
  • Method for detecting 1-vinyl imidazole in chemical product
  • Method for detecting 1-vinyl imidazole in chemical product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment one 1-vinylimidazole standard curve

[0018] a. Reagent preparation

[0019] 50mM Potassium Dihydrogen Phosphate Buffer: Accurately weigh 6.8g of Potassium Dihydrogen Phosphate and 1g of Sodium Heptane Sulfonate into a 1L volumetric flask, add 900mL of water, adjust the pH to 3.5 with phosphoric acid, dilute to the mark with water, and mix well;

[0020] Standard stock solution: Accurately weigh an appropriate amount (accurate to 0.1mg) of the standard substance in a volumetric flask, dissolve in water and dilute to the mark, prepare a standard stock solution with a concentration of 1000μg / mL, store at 4°C, and have a validity period of 6 months ;

[0021] Standard intermediate solution: measure a certain volume of standard stock solution in a volumetric flask, dilute it with water and adjust the volume to the mark, prepare a standard intermediate solution of 100 μg / mL, store at 4°C, and have a validity period of 3 months;

[0022] Standard working solution...

Embodiment 2

[0027] The detection of 1-vinylimidazole in the sample of embodiment two

[0028] a. Sample pretreatment

[0029] Take a rubber product as a sample, cut it into small pieces below 3mm×3mm, then freeze and pulverize it to a powder sample with a particle size of no more than 1mm for use. Weigh about 1g of the sample into a 50mL centrifuge tube, add 40mL of methanol, mix well, ultrasonically extract for 20min, centrifuge at 4000r / min for 10min, take the supernatant and filter it through a filter membrane for testing.

[0030] b. Sample testing

[0031] The detection conditions are the same as in "Example 1".

[0032] c. Test results

[0033] Spectrum of the sample solution as image 3 As shown, it can be seen from the figure that the rubber sample does not detect a peak near the retention time of 1-vinylimidazole, that is, the rubber sample does not contain 1-vinylimidazole.

Embodiment 3

[0034] Embodiment three method accuracy and precision test

[0035] Select the above negative rubber sample as the matrix, and do two levels of standard addition experiments at 400mg / kg and 120mg / kg, with 6 parallels in each group. The spectrum diagram is for example Figure 4 The precision and accuracy results are shown in Table 1.

[0036] The recovery rate of this method is between 98.2-112.1%, and the RSD is 2.28-3.33%, which shows that this method has relatively good accuracy and precision.

[0037] Table 1. Accuracy and precision detection of 1-vinylimidazole spiked samples

[0038]

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Abstract

The invention belongs to the field of chemical product detection, and discloses a method for detecting 1-vinyl imidazole in a chemical product. A sample is extracted by methanol, filtered by an organic filter membrane and detected by a liquid chromatography-ultraviolet detector. The detection method is simple to operate, good in separation degree, symmetrical in peak shape and relatively high in accuracy and precision, and can realize qualitative and quantitative detection of 1-vinyl imidazole in a complex sample matrix.

Description

technical field [0001] The invention belongs to the field of detection of chemical products, and relates to a detection method of 1-vinylimidazole in chemical products, in particular to a method capable of effectively separating impurities and high in precision of 1-vinylimidazole in chemical products. Background technique [0002] 1-vinylimidazole (1-vinylimidazole) is mainly used for bonding, encapsulation, coating and lamination of instruments, meters, various electrical components, chemical machinery, vehicles and defense industries, as well as medium temperature epoxy resin Hardener. However, this substance is toxic, and it will cause great damage to mucous membrane tissue, upper respiratory tract, eyes and skin when it comes into contact, causing cough, shortness of breath, headache, nausea and other symptoms. [0003] Based on the characteristics of high boiling point and strong polarity of 1-vinylimidazole, it can be detected by liquid chromatography. However, ther...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 张雅莉
Owner 杭州科准检测科技有限公司
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