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
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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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