The use of TSDC analysis [1][2][3][4] for iced water has only been carried out by a limited number of researches. [5][6][7][8][9][10] Jeneveau et al. 6 found three major depolarizing current J peaks on J-Temperature (-170 --20˚C) curves, obtained at a heating rate (β) of 3.0˚C/min. Three peaks at -154˚C, -113˚C and -94˚C were found to have activation energies (Ea) of 20.2, 27.0 and 57.8 kJ/mol, respectively. Pissis et al. 7 reported three peaks at -148˚C with an activation energy (Ea) of 24.2 kJ/mol and at -111˚C and -48˚C with no Ea data obtained at β = 3.5˚C/min. They also later reported three peaks at -165˚C with Ea = 23.2 kJ/mol, at -154˚C with Ea = 29.9 kJ/mol and at -53˚C with Ea = 40.6 kJ/mol, obtained at β = 3.0˚C/min. 9 The peak temperature might be dependent on β, the polarizing temperature (Tp), the electrode utilized, and very small amounts of ionic contaminants. Herein, we report on results of the iced water structure, analyzed by TSDC, as a function of β and the polarizing voltage, with a consideration of the contaminant upon TSDC application to tap water samples.
Experimental
Water samplesSuper pure water (SPW), ion-exchanged water (IEW) and distilled water (DSW) were utilized. SPW was prepared by the ultra-filtration of DSW using acrylic micro-filter and ultrafilters. IEW was prepared by a Millipore apparatus. DSW was prepared by distilling tap water. The IEW was used as the standard for all experiments discussed in this paper. The main cation concentrations, pH values, electric-conductivities (EC) and dissolved oxygen concentrations (DO) are collected in Table 1. Cations other than Si 2+ (ca. 100 ppb for IEW, DSW) were found to be in negligibly small amounts (less than 2 ppb). Naturally, the electric-conductivity of IEW was smaller than that for DSW. However, that of SPW was slightly larger than that of IEW. The reason is not clear, but it might be related to the fact that the dissolved oxygen level of SPW is high. As can be seen in Table 1, IEW has an EC of 0.35 -0.39 µS/cm (25˚C) and a dissolved-oxygen concentration of 4.12 -5.13 ppm. The IEW was determined to contain Si 2+ , Fe 3+ , K + , Zn 2+ , Na + in concentrations of only 97, 0.51, 0.47, 0.12 and 0.05 ppb, respectively, without any detectable Mg 2+ and Ca 2+ . In order to examine the influence of various cations in the water on the TSDC profiles, the water samples containing 2 -100 ppm levels of K + , Li + , Na + , Mg 2+ and Ca 2+ were prepared by dissolving the corresponding hydroxides in the IEW. Guaranteed-grade deuterated water (HW, NMR use) was also used as a reference. TSDC measurements were also made on tap water for drinking (TWD, Takatsuki city) and two tap water samples for industrial use (TWI) (Takatsuki city, Tonegawa), which have much higher cation contents (see Table 1). Quantitative ion analyses (EC, pH and DO) for all water samples were carried out on an atomic-absorption spectrophotometer (Shimadzu Co., Ltd. AA-6400F, flame emission type), EC meter (Toa-Denpa Co., Ltd.), pH meter and DO meter (Horiba, Ltd.), respectivel...