Method for measuring content of 4,4'-bi(hydroxymethyl) biphenyl (4,4'-BHMBP)

A determination method, the technology of hydroxymethyl, which is applied in the field of chemical detection, can solve the problems such as the difficulty of quantitative work, and achieve the effects of long service life, easy operation and stable performance

Active Publication Date: 2012-12-26
BAOWU CHARCOAL MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, no relevant literature has reported the analysis method for the content of 4,4'-bis(hydroxymethyl)biphenyl, which brings great difficulty to its quantitative work

Method used

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  • Method for measuring content of 4,4'-bi(hydroxymethyl) biphenyl (4,4'-BHMBP)
  • Method for measuring content of 4,4'-bi(hydroxymethyl) biphenyl (4,4'-BHMBP)
  • Method for measuring content of 4,4'-bi(hydroxymethyl) biphenyl (4,4'-BHMBP)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Instruments and Conditions

[0034] Equipped with hydrogen flame detector, FID detection limit -10 g / S (benzene or n-hexadecane) gas chromatograph, chromatographic workstation or data processor; automatic sampler (8*2ml sample tray); 5% phenyl 95% polydimethylsiloxane as Stationary phase (VF-5MS column produced by Varian, USA, φ0.25mm×30m×0.25μm); carrier gas: nitrogen, gas: H 2 99.999%, supporting gas: Air; injection volume 0.2ul; 80℃ column initial temperature, 8℃ / min heating rate; split ratio 50:1, sample concentration is about 2154.4~10772.0ng / ul acetone; vaporization temperature 230 °C; column flow rate: 1ml / min.

[0035] Get 4,4'-bis(hydroxymethyl)biphenyl product and carry out gas chromatography analysis, record chromatogram, result retention time is that the chromatographic peak of 22.388 minutes is 4,4'-bis(chloromethyl)biphenyl, retention time The chromatographic peak at 22.768 minutes is 4,4'-bis(hydroxymethyl)biphenyl.

Embodiment 2

[0037] Instruments and Conditions

[0038] Equipped with hydrogen flame detector, FID detection limit -10 g / S (benzene or n-hexadecane) gas chromatograph, chromatographic workstation or data processor; automatic sampler (8*2ml sample tray); 5% phenyl 95% polydimethylsiloxane as Stationary phase (HP-5 column capillary gas chromatography column produced by Agilent, USA, φ0.32mm×60m×0.25μm); carrier gas: nitrogen, gas: H 2 99.999%, supporting gas: Air; injection volume 2ul; initial column temperature of 150°C, heating rate of 4°C / min; split ratio 5:1, sample concentration of about 2154.4~10772.0ng / ul acetone; vaporization temperature 270°C ; Column flow rate: 1ml / min.

[0039] Get 4,4'-bis(hydroxymethyl) biphenyl product and carry out gas chromatography analysis, record chromatogram (see figure 1 ), wherein the chromatographic peak with a retention time of 28.514 minutes is 4,4'-bis(chloromethyl)biphenyl, and the chromatographic peak with a retention time of 29.957 minutes is ...

Embodiment 3-1

[0041] Instruments and Conditions

[0042] Equipped with hydrogen flame detector, FID detection limit -10 g / S (benzene or n-hexadecane) gas chromatograph, chromatographic workstation or data processor; automatic sampler (8*2ml sample tray); 5% phenyl 95% polydimethylsiloxane as Stationary phase (HP-5 column capillary gas chromatography column produced by Agilent, USA, φ0.32mm×30m×0.25μm); carrier gas: nitrogen, gas: H 2 99.999%, supporting gas: Air; injection volume 1ul; initial column temperature of 60°C, heating rate of 10°C / min; split ratio 20:1, sample concentration of about 2154.4~10772.0ng / ul acetone; vaporization temperature of 250°C ; Column flow rate: 1ml / min.

[0043] Get 4,4'-bis(hydroxymethyl)biphenyl product and carry out gas chromatography analysis, record chromatogram, result retention time is that the chromatographic peak of 20.034 minutes is 4,4'-bis(chloromethyl)biphenyl, retention time The chromatographic peak at 20.256 minutes is 4,4'-bis(hydroxymethyl)bip...

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Abstract

The invention provides a method for measuring the content of 4,4'-bi(hydroxymethyl) biphenyl (4,4'-BHMBP). In the method, a capillary gas-phase chromatographic column is used for separating the 4,4'-bi(hydroxymethyl) biphenyl, and an automatic sample injector is used for quantifying the 4,4'-bi(hydroxymethyl) biphenyl by adopting an external standard calibration curve method. The method is characterized in that a fixed phase of the capillary gas-phase chromatographic column is 5 percent phenyl 95 percent polydimethylsiloxane, the length of the column is 15-60m, the inner diameter of the column is 0.2-0.5mm, the film thickness of the inner diameter of the column is 0.1-0.6mum, the initial temperature of the column is 60-150 DEG C, and the heating rate is 4-10 DEG C / min; and the sample size of the automatic sample injector is 0.2-5mul, the split ratio is (5:1)-(50:1), and the vaporization temperature is 230-270 DEG C. The method is simple, quick and accurate, is a more ideal qualitative and quantitative analysis method for measuring the content of the 4,4'-BHMBP and is suitable for the quality monitoring of 4,4'-BHMBP products.

Description

technical field [0001] The invention relates to the field of chemical detection, in particular, the invention relates to a method for measuring the content of 4,4'-bis(hydroxymethyl)biphenyl products by gas chromatography. Background technique [0002] 4,4'-bis(hydroxymethyl)biphenyl [4,4'-Bis(hydroxymethyl)biphenyl], also known as 4,4'-biphenyldimethanol [4,4'-Biphenyldimethanol], abbreviated as 4, 4'-BHMBP. Molecular formula: C 14 h 14 o 2 , molecular weight: 214.26, CAS number: 1667-12-5. 4,4'-BHMBP is prepared by hydrolysis of 4,4'-bis(chloromethyl)biphenyl (abbreviated as 4,4'-BCMBP) in water It is mainly used as a monomer for the synthesis of flame retardant polymers and liquid crystal polymers, and can also be used for the synthesis of other biphenyl derivatives, such as 4,4'-biphenyl dicarboxylic acid. [0003] At present, no relevant literature has reported an analysis method for the content of 4,4'-bis(hydroxymethyl)biphenyl, which brings great difficulty to i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/60G01N30/30
Inventor 朱春燕侯文杰
Owner BAOWU CHARCOAL MATERIAL TECH CO LTD
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