A Calorimetric System Based on the LKB 10700-1 Flow Microcalorimeter

Abstract

An electrically calibrated and computer-controlled apparatus based on the LKB 10700-1 flow microcalorimeter was set up and tested by determining the enthalpies of dilution of aqueous solutions of sucrose and HCl at 298.15 K. The obtained results are in good agreement with the corresponding reference values recommended in the literature. The quality of the calorimetric signal in terms of noise, linearity and baseline drift, and the instrument time constant were analyzed. Also investigated were the influences of the flow rate and of the viscosity of the calorimetric liquid on the position of the baseline. The new calibration system enables powers ~25 times smaller than those possible with the original one to be released inside the calorimetric cells. Electrical calibrations carried out with water as the sole calorimetric liquid indicated that the precision of the calibration constant, ε, quickly improved from ~9% to ~0.4% with the increase of the input power, P, from ~2 µW to ~50 µW, and stabilized at ~0.1% for P ≥ 100 µW. The calibration constant was also found to linearly increase with the flow rate of the calorimetric liquid and to vary by less than 1% over a period of eight months under similar experimental conditions. Finally a new experimental procedure for heat of dilution measurements, which combines calibration and experiment in a single run, was evaluated. This method allows a significant economy in experiment time with apparently no accuracy loss relative to the conventional procedure recommended in the literature.

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