Gas chromatography detection method of isophthaloyl dichloride
A technology of isophthaloyl dichloride and gas chromatography, which is applied in the field of gas chromatography detection of isophthaloyl dichloride, can solve the problems of inability to fully represent the quality of acyl chloride and the inability to detect weakly polar small molecule organic compounds, and achieve the detection process Simple and convenient, good precision, good separation effect
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Embodiment 1
[0032] Weigh 1.0 g of crude isophthaloyl chloride sample, add 8 mL of absolute ethanol, add 10 mL of dichloromethane, control the reaction temperature on the electric furnace to 250 ° C and slowly heat esterification until no bubbles are generated, and measure the pH of the sample to be 4;
[0033] Set the detection conditions of gas chromatography: gasification temperature: gasification temperature: 240°C, detection temperature: 260°C, split ratio: 20:1, injection volume: 1.5μL, carrier gas flow rate: 25mL / min, H2 flow rate: 50mL / min, air flow rate: 400mL / min;
[0034] Put the sample on the sample tray of the gas chromatograph, call out the saved sample operation and data processing method, and inject the sample according to the set conditions and procedures.
[0035] Perform data analysis, call out the spectrum, and integrate with the area percentage method.
[0036] For the detection spectrum of crude product isophthaloyl chloride, see the attached figure 1 , the spectrog...
Embodiment 2
[0041] Weigh 2.0g sample of isophthaloyl dichloride finished product 1, add 15mL of methanol, add 15mL of pyridine, heat slowly at 200°C until no bubbles are generated, cool to room temperature, measure the pH of the sample to 4.5, and use it as a sample to be tested.
[0042] Set the detection conditions of gas chromatography: gasification temperature: gasification temperature: 240°C, detection temperature: 260°C, split ratio: 20:1, injection volume: 1.5μL, carrier gas flow rate: 25mL / min, H2 flow rate: 50mL / min, air flow rate: 400mL / min;
[0043] Put the sample on the sample tray of the gas chromatograph, call out the saved sample operation and data processing method, and inject the sample according to the set conditions and procedures.
[0044] Perform data analysis, call out the spectrum, and integrate with the area percentage method.
[0045] The detection spectrogram of finished product 1 isophthaloyl chloride sees attached figure 2 , show in the spectrogram of finish...
Embodiment 3
[0050] Weigh 2.5g of the finished product 2 of isophthaloyl dichloride, add 1.8g of acyl imidazole, add 8mL of dimethylaminopyridine, heat slowly at 280°C for 30min, cool to room temperature, measure the pH of the sample to 6, and use it as a sample to be tested .
[0051] Set the detection conditions of gas chromatography: gasification temperature: gasification temperature: 240°C, detection temperature: 260°C, split ratio: 20:1, injection volume: 1.5μL, carrier gas flow rate: 25mL / min, H2 flow rate: 50mL / min, air flow rate: 400mL / min;
[0052] Put the sample on the sample tray of the gas chromatograph, call out the saved sample operation and data processing method, and inject the sample according to the set conditions and procedures.
[0053] Perform data analysis, call out the spectrum, and integrate with the area percentage method.
[0054] The detection spectrogram of finished product 2 isophthaloyl chlorides sees attached image 3 , show in the spectrogram of finished ...
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