The new time domain measurement system for dielectric measurements is described. The current model is comprised of an IBM PC-AT/486, ‘‘TDM-2,’’ a new time domain measurement system, a set of thermostabilized sample holders, and operation and analysis software. This system is designed for use in the measurement of dielectric parameters of liquid and solid materials over the frequency range 100 kHz–10 GHz. Software consists of programs of registration, accumulation and data collection, Fourier analysis, time domain treatment, analysis software: fast and reliable nonlinear curve fitting programs to determine spectroscopic parameters and correlation analysis in time domain. The system utilizes the difference method of measurement with the registration of primary signals with multiwindow nonuniform sampling. Such a system permits the overlap of a frequency range of five orders in a single measurement.
Three methods of electrode polarization correction developed for time
domain dielectric spectroscopy are reviewed in the paper. Two of them are based
on the representation of the parasitic double electrical layer by an additional
capacitor connected in series with the working electrodes of the sample holder.
The third one takes into account the fractal nature of electrode polarization.
The advantages and limitations of each method are discussed in the review.
Dielectric relaxation spectroscopy was used to investigate the properties of residual water in lyophilized formulations of a proprietary tri-phosphate drug containing a sugar (trehalose, lactose or sucrose) or dextran. The dielectric properties of each formulation were determined in the frequency range (0.1 Hz-0.1 MHz) and temperature range (30˚C-T g ). The temperature dependence of the relaxation times for all samples showed Arrhenuis behaviour, from which the activation energy was derived. Proton hopping through the hydrogen-bonded network (clusters) of water molecules was suggested as the principle mode of charge transport. Significant differences in dielectric relaxation kinetics and activation energy were observed for the different formulations, which were found to correlate with the amount of monophosphate degradation product.
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