Physical Chemistry Laboratory Practice

Introductory lecture: students are introduced with the basics of experimental procedures in determination of physicochemical properties of materials, types of experimental errors, calculation and characterization of errors and presentation of experimental results. Mathematical statistics (probability, deviation) will be discussed shortly.
The practical part of the subject consists of 8-10 practices in small groups (6 students in one group) which will be chosen from the following practices at the beginning of each semester. Each practice aims to improve the skills of students in individual work, arranging of experimental setups and critical evaluation of results. The knowledge covers various fields in thermodynamic and kinetics as it follows.
1.    Determination of apparent heat of evaporation in a one-component system. Various organic solvents will be characterized by using the Clausius-Clapeyron-equation and several possible experimental errors will be considered during the measurement. The method of linear least squares regression is used for evaluation.
2.    Phase equilibrium in liquid-liquid two-component systems. Two-component systems displaying either LCST or UCST will be investigated and the composition-temperature phase diagram will be constructed. Component balance equation will be discussed and used to determine the volume ratio of phases.
3.    Adsorption. Two different experiments will be introduced: nitrogen gas adsorption and adsorption of diluted solutions on the carbon surfaces. Theoretical background and limits of the methods will be discussed and results of the methods will be compared with a critical viewpoint.
4.     Determination of the molecular weight of a linear macromolecule using viscosimetry. The terms dynamic, relative, specific and intrinsic viscosity will be introduced and discussed. The molecular weight of a chosen neutral polymer will be determined by the measurement of its relative viscosity by a capillary viscosimeter. Experimental error and its effect on the molecular weight will be characterized.
5.        Rheology.  Flow and viscosity curves will be discussed and classified. Newtonian and thixotropic fluids will be investigated by using an Ostwald and a rotational viscosimeter.
6.    Calorimetry. Various calorimetric methods will be introduced. Heat of an acid-base reaction will be determined by an adiabatic calorimeter while specific heat capacity of an organic liquid will be determined by a heat transfer calorimeter. Experimental results will be compared with literature data.
7.    Conductivity of electrolyte solutions. The basics of conductometry will be introduced and the terms conductivity, specific and molar conductivity will be discussed. The degree of dissociation of a chosen electrolyte will be determined by the measurement of conductivity and thermodynamic functions for the dissociation (enthalpy, Gibbs free energy and entropy) will be calculated.
8.        Rate constant of iodination of acetone. Basics of reaction kinetics (order, rate constants) will be discussed and the reaction rate constant of a simple chemical reaction will be determined by concentration measurements as a function of time with titration. The rate-limiting reaction step will be determined by linear plot.
9.        Order of a component in kinetics of decomposition of hydrogen peroxide.  Reaction rate of the peroxide will be calculated from the flow rate of the product (oxygen gas) in a continuous reactor. Order of the kinetics will be determined.   
10.    Kinetics of reaction between ions. Basic of reaction kinetics and the effect of inert ions on reaction rate will be discussed. A simple ion reaction will be investigated and reaction time will be determined by using a colour indicator of reaction end. Reaction rate constant will be determined and the effect of experimental errors will be analysed.
11.    Electrochemistry. Both electrochemical equilibrium and kinetics of an electrochemical reaction will be investigated. A simple galvanic cell will be constructed and the validity of the Nernst-equation will be analysed in a wide concentration range of components. Polarization of an other cell will be characterized by recording the polarization curve and the Tafel plot of an electrochemically active organic compound.