The separator was a polypropylene microporous film, and the electrolyte was 1 M LiPF6 dissolved in a mixed solution of dimethyl carbonate, diethyl carbonate, and ethylene carbonate (1 1 1 by volume).
For visualization, the plate was dipped into a modified anisaldehyde (detection reagent solution consisting of diethyl ether-glacial acetic acid-anisaldehyde-sulphuric acid in volume composition (136 : 91 : 1 : 20)) for exactly 2 s and heated at 120°C for 30 min in a drying oven.
For each 1 mL of TFA solution, 10 mL of diethyl ether was used.
Briefly, indole, dissolved in ice-cold diethyl ether, was reacted with a solution containing 2 equiv of oxalyl chloride in diethyl ether followed by a 20 wt %/vol solution of dimethylamine in diethyl ether until the pH reached 9 10, while maintaining the reaction mixture at 0 °C with an ice bath.
The insertion/extraction characteristics of lithium ions for the electrode prepared with composite:poly vinylidene fluoride) = 90:10 mass% were examined in 1 mol L−1 LiClO4 solution of ethylene carbonate:diethyl carbonate = 50 50 vol%.
The polymerization was initiated by the addition of 1.0 M solution of HCl in diethyl ether (1.5 ml, 1.5 mmol); the reaction was maintained at 25°C for 24 h with vigorous stirring under nitrogen atmosphere.
Briefly, samples were lyophilized to remove water, redissolved in a 1 1 solution of acetonitrile and diethyl ether, and analyzed using gas chromatography tandem mass spectrometry using isotope dilution.
Solution of internal standards (Diethyl phthalate-d4 e Bis(2 ethylhexyl) phthalate-d4) in hexane was supplied by Supelco, Milano, and used for all analysis.
to a solution of the corresponding diethyl phosphonate (1 equiv). in CH2Cl2 followed by removing all volatiles in vacuo and characterization of the compounds by P and H NMR spectroscopy.
Treatment of the solution with diethyl ether led to precipitation of a yellow orange solid, which was isolated by filtration and dried under high vacuum.
