Setting reaction 139 infrared spectra

After the reactor had been cleaned, evacuated and purged with N2, 1.29 g of 2,5-di-tert-butyl-l,4-benzoquinone (5.85 mmol) were added, taking care that the benzoquinone did not touch the ATR sensor. After the desired jacket temperature had been reached, a reference background infrared spectrum was recorded. Then, 19.2 mL dioxan, 8 mL EtOH and 8 mL tert-butyl hydroperoxide (70% solution in water, 58.5 mmol) were added, the stirrer was turned on to 400 rpm and the desired reaction temperature was set. After degassing the solution for 3 minutes with N2, Triton B (0.8 mL of a 40% solution in methanol, 1.78 mmol) was added within 24 seconds into the closed reactor to start the reaction. 

The same membranous material as mentioned in 1) having a thickness of 100 jjl was set in a reactor of the design which would allow only one surface of the membrane to contact with reaction reagents. Thereafter, the reactor compartment was filled with vapour of phosphorous pentachloride ( at 170°C for an hour ) to have one surface of the membrane reacted. The reflective infrared spectrum and dyeing test respectively showed that the membrane had sulfonyl chloride groups and that approximately 5 JJL of non-dyed layer was stratified at the membrane surface where phosphorous pentachloride had contacted. The electric resistance of this membrane was about 1500 ft- cm2 in a 1.0 N hydrochloric acid solution at 25°C when measured by 1000 cycle A.C. The electric resistance of the same membrane before the reaction with phosphorous pentachloride was only 0.38ft - cm2 under the same conditions. 

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