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A method for measuring 1,6-hexanediol diacrylate content

A technology of hexanediol diacrylate and content, applied in the field of analysis and detection, can solve the problems of inability to meet detection requirements, loss of production enterprises, inability to accurately quantify and other problems, achieve high recovery rate and precision, meet detection needs, and quantitatively accurate Effect

Active Publication Date: 2018-08-07
DALIAN PONY TESTING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

1,6-Hexanediol diacrylate is physically added to various industrial products, involving a wide variety and different matrices. Simple processing methods cannot meet the detection needs of all types of samples, especially coating addition or solvent matrices samples, the current relevant research is more focused on the synthesis and application of 1,6-hexanediol diacrylate, and the detection of its content has not received much attention
At the same time, a single chromatographic separation method will face serious matrix interference and other problems when detecting samples of different matrices, resulting in inaccurate quantification, and more seriously, false positive samples may occur, resulting in huge losses for manufacturers
Therefore, the detection of the content of 1,6-hexanediol diacrylate needs to adopt a more accurate method of chromatography-mass spectrometry. However, gas chromatography-mass spectrometry has not yet been given in the published literature In order to better prevent the harm of this substance to humans and the environment, it is necessary to establish a reliable detection method for the content of 1,6-hexanediol diacrylate

Method used

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  • A method for measuring 1,6-hexanediol diacrylate content
  • A method for measuring 1,6-hexanediol diacrylate content
  • A method for measuring 1,6-hexanediol diacrylate content

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The mensuration of 1,6-hexanediol diacrylate content in the plastic sample of embodiment 1

[0030] (1) Analysis steps

[0031] Take 50g of plastic samples, first crush them into 1cmx1cmx1cm particles, then use a high-efficiency cutting pulverizer for coarse powder, and then use a high-efficiency cutting pulverizer for low-temperature fine powder. The samples were crushed twice, the first sample was discarded, and the second sample was taken. The pulverized sample powder passed through a standard sieve of 80 or 100 mesh. Weigh 1.0028g and 1.0012g samples respectively in a Soxhlet extractor, add 20mL of dichloromethane-n-hexane mixed solution with a volume ratio of 1:2, perform Soxhlet extraction and reflux at 50°C for more than 4 hours, and after cooling the extract to room temperature, Filtered through a 0.22 μm nylon filter membrane, and the filtrate was analyzed by gas chromatography-mass spectrometry;

[0032] (2) Chromatography and mass spectrometry parameters ...

Embodiment 2

[0039] Embodiment 2 plastic sample 1, the standard substance of 6-hexanediol diacrylate adds and measures

[0040] (1) Analysis steps

[0041] Take the 1,6-hexanediol diacrylate negative sample in Example 1. Weigh six samples of about 1g into a 50mL glass colorimetric tube or Soxhlet extractor, add 0.1mL each of 1000μg / mL 1,6-hexanediol diacrylate standard stock solution, after standing for a period of time, add 20mL volume Dichloromethane-n-hexane mixed solution with a ratio of 1:2, Soxhlet extraction and reflux at 50°C for more than 4 hours, after the extract was cooled to room temperature, filtered through a 0.22 μm nylon filter membrane, and the filtrate was analyzed by gas chromatography-mass spectrometry;

[0042] (2) Chromatography and mass spectrometry parameters

[0043] Gas chromatographic conditions, adopt chromatographic column DB-5MS, 30m×0.25mm×0.25μm, take 60℃ as the initial temperature of the column oven, raise the temperature to 130℃ at a rate of 10℃ / min, ke...

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Abstract

The invention discloses a method for measuring the content of 1,6-hexanediol diacrylate, belongs to the field of analysis and detection, and particularly discloses a method for measuring the content of the 1,6-hexanediol diacrylate through gas chromatography-mass spectrography. The method comprises the following steps that an appropriate amount of a uniform sample is taken to be added into a soxhlet extractor, dichloromethane and n-hexane mixed solvent with the volume ratio of 1:(1-3) is added for soxhlet extraction, reflux is performed for 4 hours or above at 50 DEG C, an extracting solution is cooled to the room temperature and then filtered through a nylon filter membrane, filtrate is analyzed through a gas chromatograph-mass spectrometer, and quantifying is performed through an external standard method. The method is simple, rapid and accurate in qualitative analysis and quantification, has the higher recovery rate and can meet the detection requirement.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and relates to a method for measuring the content of 1,6-hexanediol diacrylate, in particular to a method for measuring the content of 1,6-hexanediol diacrylate by gas chromatography-mass spectrometry . Background technique [0002] 1,6-Hexamethylene diacrylate (Hexaethylene diacrylate, HDDA) is a bifunctional special acrylate prepared by esterification of 1,6-hexanediol and acrylic acid. It has good flexibility, hydrolysis resistance, heat resistance, chemical resistance, etc., and is widely used in light-curing coatings, inks, sealants, injection molding products and other fields. 1,6-Hexanediol diacrylate is a colorless or light yellow liquid under normal conditions, insoluble in water, soluble in aromatic organic solvents, boiling point not less than 200°C, molecular formula C12H18O4, CAS number 13048-33-4 . The structural formula is as follows: [0003] [0004] 1,6-Hexanediol di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
CPCG01N30/06G01N2030/062
Inventor 宋薇高俊海
Owner DALIAN PONY TESTING TECH CO LTD
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