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Gas chromatography-mass spectrometry determination method of (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide

A technology of trimethylbenzoyl and diphenylphosphine oxide, which is applied in the field of chemical detection, can solve the problems of rare reports on TPO detection, and achieve the effects of low detection limit, low matrix interference, and high recovery rate of standard addition

Active Publication Date: 2020-04-10
广州广电计量检测(上海)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current research on it is concentrated in the field of synthesis and application, and there are few reports on the detection of TPO residues in products.

Method used

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  • Gas chromatography-mass spectrometry determination method of (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide
  • Gas chromatography-mass spectrometry determination method of (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide
  • Gas chromatography-mass spectrometry determination method of (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0044] 1. Selection of extraction solvent

[0045] In the experiment, toluene, dichloromethane, n-hexane, methanol, acetonitrile and acetone were used as extraction solvents to compare the extraction efficiency. The result is as figure 1 As shown, the extraction efficiencies of n-hexane, methanol, acetone and acetonitrile are all lower than 60%, which cannot meet the test requirements. The extraction effect of dichloromethane and toluene is better, wherein the extraction efficiency of dichloromethane is greater than 70%, and the extraction rate of toluene is even closer to 90%. Therefore, toluene is selected as the extraction solvent after comprehensive consideration.

[0046] 2. Optimization of gas phase split mode

[0047] In order to effectively separate (2,4,6-trimethylbenzoyl)diphenylphosphine oxide, the condition of the split mode was studied in the experiment: when using the splitless mode, although the low concentration (2,4 ,6-trimethylbenzoyl)diphenylphosphine oxi...

Embodiment 2

[0055] 1, a kind of GC-MS method measures the analytical testing method of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide in the plastic product, comprises the steps:

[0056] Preparation of standard solution: Accurately weigh 10 mg (accurate to 0.1 mg) (2,4,6-trimethylbenzoyl) diphenylphosphine oxide standard substance with a precision electronic analytical balance, add it to a 10 mL small beaker, and use a small amount of Dissolve the toluene, transfer it to a 10mL volumetric flask, wash the beaker twice with a small amount of toluene and transfer it to the volumetric flask, and dilute to the mark with toluene to obtain a high-concentration stock solution of 1000 mg / L, and then gradually dilute to prepare a standard working curve , the concentration points are 1, 2, 5, 10, 20mg / L respectively.

[0057] Sample pretreatment: Take a representative plastic sample, cut it into pieces, the size is not more than 2mm×2mm, weigh 1.0g (accurate to 0.1mg) sample, put it into a 60mL ...

Embodiment 3

[0075] A kind of GC-MS method measures the analytical testing method of (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide in plastic product, comprises the steps:

[0076] Sample pretreatment: Take a representative plastic sample, cut it into pieces, the size is not more than 2mm×2mm, weigh 1.0g (accurate to 0.1mg) sample, put it into a 60mL reaction bottle, add 10mL of dichloromethane, cover tightly and put The (2,4,6-trimethylbenzoyl)diphenylphosphine oxide in the sample was extracted with an ultrasonic cleaner, the ultrasonic power was 400W, the set temperature was 60°C, and the extraction time was 60min. Take it out and cool it to room temperature, take the extraction solution and centrifuge it at 10000r / min for 1min, then filter the centrifuged extract with a 0.22μm filter membrane, put it into a sample injection vial, and wait for analysis.

[0077] The gas chromatography-mass spectrometer was used to perform qualitative and quantitative tests on the above-mentioned samp...

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Abstract

The invention relates to the field of chemical detection, and particularly discloses a gas chromatography-mass spectrometry determination method of (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide.The gas chromatography-mass spectrometry determination method comprises the steps of: (1) carrying out extraction treatment on a to-be-detected sample by using toluene or dichloromethane as an extraction solvent, performing centrifugal treatment on the obtained extraction solution, and filtering the extraction solution by using a filter membrane to obtain an extracting solution; and (2) carryingout gas chromatography-mass spectrometry detection on the extracting solution. Through optimal setting of instrument analysis parameters, the (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide can obtain symmetrical chromatographic separation peaks within 9 minutes. Meanwhile, the gas chromatography-mass spectrometry determination method disclosed by the invention is low in detection limit, goodin precision and high in sample labeling recovery rate, and meets the test requirements of (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide in plastic products.

Description

technical field [0001] The invention relates to the field of chemical detection, in particular to a gas chromatography-mass spectrometry determination method for (2,4,6-trimethylbenzoyl)diphenylphosphine oxide. Background technique [0002] (2,4,6-Trimethylbenzoyl)diphenylphosphine oxide (TPO), is a white or cream powder, easily soluble in acetone, methanol, acetonitrile, ether and other organic solvents, its basic information see Table 1. (2,4,6-Trimethylbenzoyl)diphenylphosphine oxide is a free radical photoinitiator, which has light absorption in the wavelength range of 350-400nm, and can generate benzoyl and Both phosphono groups are free radicals that can initiate polymerization, so the photocuring speed is fast. As an important intermediate, (2,4,6-trimethylbenzoyl)diphenylphosphine oxide is often used in UV-curable coatings, printing inks, light-curable resins, plastic light stabilizers, optical fiber coatings, etc. . Although it has the advantages of good perform...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/7206G01N30/8637G01N30/8679G01N2030/047G01N2030/062
Inventor 严洪连张兰兰李支薇钟琳杨文宇王华林炼锋
Owner 广州广电计量检测(上海)有限公司
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