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A method for simultaneous determination of phenol and bht in hot melt adhesives

A hot-melt adhesive and phenol technology, applied in the field of analytical chemistry, can solve the problems of not measuring phenol and BHT at the same time, affecting the accurate determination of the determination results, and incomplete extraction of BHT, etc., and achieves accurate and reliable determination, low detection limit and quantification limit. , the effect of matrix interference reduction

Active Publication Date: 2018-08-21
CHINA TOBACCO YUNNAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

BHT (2,6-di-tert-butyl-4-methylphenol) is an antioxidant widely used in hot melt adhesives, but its usage is regulated and cannot be used in excess or abused
Therefore, both phenol and BHT are important indicators for the quality control of hot melt adhesives. At present, a single method is used to measure phenol and BHT separately, which is inefficient and consumes manpower and material resources. There is no literature report on the simultaneous determination of phenol and BHT in hot melt adhesives.
[0003] At present, there are only reports on the determination of phenol in hot melt adhesives by headspace-gas chromatography-mass spectrometry, but this method cannot Determination of BHT with a higher boiling point, and the sample needs to be heated to 130-150°C in the headspace bottle, which may accelerate the oxidation of phenol and affect the accuracy of the measurement result. In addition, high temperature may cause the decomposition of the hot melt adhesive matrix and release phenol. can also affect the accuracy of the determination
[0004] At the same time, although it is also reported that ultrasonic extraction and gas chromatography-mass spectrometry are used to measure BHT in hot melt adhesives, this method has the following defects: (1) the extraction efficiency is low, and the extraction of BHT is not complete; (2) there is dissolved in the extract A large amount of hot melt adhesive matrix, direct sample analysis will seriously pollute the instrument, and the matrix will interfere with the measurement; (3) The use of external standard method leads to poor accuracy

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  • A method for simultaneous determination of phenol and bht in hot melt adhesives
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  • A method for simultaneous determination of phenol and bht in hot melt adhesives

Examples

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Effect test

Embodiment 1

[0034] A method for simultaneous extraction, purification and determination of phenol and BHT in hot melt adhesive, including the following steps:

[0035] (1) Sample extraction: accurately weigh 0.5 hot melt adhesive sample, add 5 mL deuterated-phenol-d6 with a concentration of 10 mg / L and deuterated 2,3,6-trimethylphenol with a concentration of 20 mg / L -d11 cyclohexane solvent, heating and refluxing extraction at 55 ℃ for 20 min, and cooling to room temperature after extraction;

[0036] (2) Sample purification: Add 20 mL of methanol to the sample extract, centrifuge at 8000 rpm for 5 minutes, remove the matrix, and take the supernatant to obtain the sample purification solution;

[0037] (3) Determination: Pass the purification solution obtained in step (2) through a 0.22 μm microporous membrane, the filtrate is analyzed by gas chromatography-mass spectrometry, and the double internal standard method is used for quantification. The content of the target substance is calculated acc...

Embodiment 2

[0049] A method for simultaneous extraction, purification and determination of phenol and BHT in hot melt adhesive, including the following steps:

[0050] (1) Sample extraction: Weigh 2.0 hot melt adhesive samples accurately, and add 40 mL of 2-fluorophenol with a concentration of 2 mg / L and deuterated 2,3,6-trimethylphenol-d11 with a concentration of 5 mg / L. Tetrahydrofuran solvent, ultrasonic extraction at 60℃ for 3min, after extraction, cool to room temperature;

[0051] (2) Sample purification: Add 260 mL of methanol to the sample extract, centrifuge at 5000 rpm for 10 minutes, remove the matrix, and take the supernatant to obtain the sample purification solution;

[0052] (3) Determination: Pass the purification solution obtained in step (2) through a 0.22 μm microporous membrane, the filtrate is analyzed by gas chromatography-mass spectrometry, and the double internal standard method is used for quantification. The content of the target substance is calculated according to the...

Embodiment 3

[0062] A method for simultaneous extraction, purification and determination of phenol and BHT in hot melt adhesive, including the following steps:

[0063] (1) Sample extraction: accurately weigh the 0.05 hot melt adhesive sample, add 2.5 mL of 2-fluorophenol with a concentration of 0.02 mg / L and deuterated o-cresol-d7 with a concentration of 0.05 mg / L in n-hexane, Shake and extract for 30 min at 70°C, and cool to room temperature after extraction;

[0064] (2) Sample purification: Add 20 mL of methanol to the sample extract, centrifuge at 10000 rpm for 10 min, remove the matrix, and take the supernatant to obtain the sample purification solution;

[0065] (3) Determination: Pass the purification solution obtained in step (2) through a 0.22 μm microporous membrane, the filtrate is analyzed by gas chromatography-mass spectrometry, and the double internal standard method is used for quantification. The content of the target substance is calculated according to the standard curve;

[006...

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Abstract

The invention relates to a method for simultaneously extracting, purifying, and measuring phenol and BHT in a hot melt adhesive, and belongs to the technical field of analysis chemistry. According to the method, under a heating condition, a solvent is used to extract a sample, a poor solvent is added to remove substrate to carry out purification, and finally GC-MS (Gas Chromatography-Mass Spectrometer) is used to measure phenol and BHT in a hot melt adhesive. The method comprises the following steps: step a, adding an extraction solvent containing dual internal standard substances into a hot melt adhesive sample so as to extract the sample under a heating condition; step b, adding a poor solvent into the sample extract, carrying out high speed centrifugation to remove substrate to obtain a purified sample solution; and step c, making the purified sample solution go through a microfiltration membrane, measuring the sample by GC-MS, drawing a standard curve, carrying out quantitation through an internal standard method, and calculating the contents of targets according to the standard curve. The method can effectively and simultaneously extracting, purifying, and measuring phenol and BHT in a hot melt adhesive, the extraction efficiency is high, the purification effect is good, the substrate interference is little, the measuring is accurate and reliable, and the method is worthy to promote and use.

Description

Technical field [0001] The invention belongs to the technical field of analytical chemistry, and specifically relates to a method dedicated to simultaneous extraction, purification and determination of phenol and BHT in hot melt adhesives. Background technique [0002] Phenol is a pollutant in hot melt adhesives, which may cause pollution to human health and the environment. It is one of the hazardous components that hot melt adhesive products need to pay attention to. BHT (2,6-di-tert-butyl-4-methylphenol) is an antioxidant widely used in hot-melt adhesives, but there are regulations on its usage and it cannot be used in excess or abused. Therefore, both phenol and BHT are important indicators for the quality control of hot melt adhesives. At present, a single method is used to measure phenol and BHT separately, which is less efficient and consumes manpower and material resources. There is no literature report on the simultaneous determination of phenol and BHT in hot melt adhes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 司晓喜牛佳佳刘志华张凤梅朱瑞芝朱琴申钦鹏刘春波何沛王昆淼王晋尤俊衡苏钟璧
Owner CHINA TOBACCO YUNNAN IND