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35348962462
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Neat DCE was obtained by distilling HPLC grade DCE (Sigma-Aldrich) three times. The nanopipet preparation was described previously.16 Briefly, a Model P-2000 laser puller Sutter Instrument Co, was used to prepare the pipets from quartz capillaries. The aqueous solution was filled from the back using a 10-μL syringe, and then a 0.125-mm-radius Ag/AgCl wire was inserted in the pipet. A 0.25-mm-radius Ag wire was used as a quasi-reference electrode in DCE. Voltammograms were obtained with a BAS-100B potentiostat. To prepare water-saturated DCE, a portion of thrice distillated DCE was equilibrated with an equal amount of pure water in a closed Erlenmeyer flask for 48 h, while the flask was shaken periodically. Water-saturated DCE was diluted by neat DCE to obtain the desired concentration of water. Conductivity measurements were made using a home-built trans-impedance amplifier and a SR-850 lock-in amplifier. For experimental details and data analysis see ref 16
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16 Briefly, a Model P-2000 laser puller (Sutter Instrument Co.) was used to prepare the pipets from quartz capillaries. The aqueous solution was filled from the back using a 10-μL syringe, and then a 0.125-mm-radius Ag/AgCl wire was inserted in the pipet. A 0.25-mm-radius Ag wire was used as a quasi-reference electrode in DCE. Voltammograms were obtained with a BAS-100B potentiostat. To prepare water-saturated DCE, a portion of thrice distillated DCE was equilibrated with an equal amount of pure water in a closed Erlenmeyer flask for 48 h, while the flask was shaken periodically. Water-saturated DCE was diluted by neat DCE to obtain the desired concentration of water. Conductivity measurements were made using a home-built trans-impedance amplifier and a SR-850 lock-in amplifier. For experimental details and data analysis see ref 16b.
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22
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35349006795
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A significant hysteresis and a current peak after the potential sweep reversal were often observed when the applied voltage exceeded ∼1 V (e.g, blue curve in Figure 1A, Videomicroscopic observations showed that these distortions are caused by the motion of DCE in and out of the pipet and not related to IT see ref 20 for details, For better clarity, only forward portions of some voltammograms are shown in Figures 1 and 3
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A significant hysteresis and a current peak after the potential sweep reversal were often observed when the applied voltage exceeded ∼1 V (e.g., blue curve in Figure 1A). Videomicroscopic observations showed that these distortions are caused by the motion of DCE in and out of the pipet and not related to IT (see ref 20 for details). For better clarity, only forward portions of some voltammograms are shown in Figures 1 and 3.
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(b) Moakes, G.; Daemen, L. L.; Gelbaum, L. T.; Leisen, J.; Marecek, V.; Janata, J. J. Phys. Chem. B 2007, 111, 7312.
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