Gas chromatograph analysis method for tetrafluoroethane-beta-sultone
A gas chromatographic analysis, tetrafluoroethane technology, applied in the field of gas chromatographic analysis of tetrafluoroethane-β-sultone, can solve the uncertainty of measurement relationship that is not suitable for tetrafluoroethane, strong activity, direct or Indirect analysis is difficult to achieve and other issues
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Embodiment 1
[0022] Column stationary phase preparation:
[0023] Weigh 2.5g of fluorochloro oil and 0.5g of perfluorooctanoic acid ethyl ester fixative into a 50mL beaker, add 10mL of trifluorotrichloroethane (F-113) solvent to dissolve the fixative in the solvent, add 10g of 80-100 mesh poly Ethylene / tetrafluoroethylene (PE / TFE) white microbead carrier, stir gently to make the fixative solution evenly coated on the carrier, and install the column after the solvent evaporates (can be baked with infrared light).
[0024] Column stationary phase packing:
[0025] The packing operation adopts the vacuum packing method. A polytetrafluoroethylene column is used as the chromatographic column, the column length is 2.1m, and the inner diameter is 3mm. The inlet end of the chromatographic column is directly connected to the inlet end of the chromatograph, and 90mm is reserved as a sample vaporization chamber. The outlet end (connected to the thermal conductivity detection The end of the detector...
Embodiment 2
[0032] Column stationary phase preparation:
[0033] The preparation method is the same as in Example 1, except that 1.5 g of chlorofluorocarbon oil and 1.0 g of ethyl perfluorooctanoate are weighed.
[0034] Column stationary phase packing:
[0035] Packing method is the same as embodiment 1, and difference is that chromatographic column connects sample inlet end and reserves 70mm as sample steam.
[0036] Chemical chamber, column aging:
[0037] The aging method is the same as in Example 1, except that the aging time is 5 hours.
[0038] Sample preparation: Take 2mL tetrafluoroethane-β-sultone reaction solution, add 8mL ether, cover and shake well.
[0039] Sample determination:
[0040] Using Shimadzu 14B gas chromatograph, high-purity nitrogen dehydrated with 5A molecular sieve and color-changing silica gel as carrier gas, the column temperature is 60°C; the gasification chamber temperature is 120°C; the thermal conductivity detector temperature is 120°C ; thermal con...
Embodiment
[0042] Column stationary phase preparation:
[0043] The preparation method is the same as in Example 1, except that 1.0 g of chlorofluorocarbon oil and 1.0 g of perfluorooctanoic acid ethyl ester are weighed; chromatographic grade 80-100 mesh polystyrene / divinylbenzene (PS / DVB) white porous microbeads For the carrier.
[0044] Column stationary phase packing:
[0045] The packing method is the same as in Example 1, except that the length of the tetrafluoroethylene chromatographic column is 3.1 m, the inner diameter is 3 mm, and 60 mm of the end of the chromatographic column connected to the injection port is reserved as a sample vaporization chamber.
[0046] Column Aging:
[0047] The aging method is the same as in Example 1, except that the aging time is 6 hours.
[0048] Sample preparation: Take 2 mL of tetrafluoroethane-β-sultone reaction solution, add 8 mL of ethyl propyl ether, cover and shake well.
[0049] Sample determination:
[0050] Using Japan Shimadzu 14B g...
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