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Lab Packet for Chem 457 Experimental Physical Chemistry PDF

160 Pages·2017·28.021 MB·English
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Preview Lab Packet for Chem 457 Experimental Physical Chemistry

Lab Packet FOR CHEM 457 Experimental Physical Chemistry Spring, 2017 Instructor: Dr. Bratoljub H. Milosavljevic Revised: January, 2017 Foreword Experimental Physical Chemistry, CHEM 457 course is designed to reinforce the theoretical Physical Chemistry courses with the introduction of physical chemistry applications in a laboratory environment. Placing abstract concepts in an experimental framework, physical chemistry may become more self-explanatory and more enjoyable. This laboratory course mainly utilizes fast kinetics, thermodynamics, electrochemistry, surface chemistry, and spectroscopy experiments. The topics for this course are chosen to improve the science and engineering students theoretical and experimental physical chemistry backgrounds and skills. In addition, each student will work on a special project to demonstrate her/his independent ability in performing literature searches, planning and designing the experiment, interpreting the data, communicating in written scientific language, by writing a paper in the format of a Physical Chemistry Journal, and in verbal scientific language, by presenting a poster. The synopsis of the eleven experiments performed in this course is given below. 1) Dissociation of a Propionic Acid Vapor The equilibrium constant for the dissociation of propionic acid dimer in the vapor phase will be determined as a function of temperature. From this data, thermodynamic constants and enthalpy and entropy changes will be calculated. The change in enthalpy is a measure of the strength of the hydrogen bonds in the dimer. 2) Adsorption from Solution An adsorption isotherm will be constructed for the adsorption of acetic acid onto charcoal. Using this isotherm, the surface area of the charcoal will be determined. The relation between adsorption and surface chemistry will be introduced. 11 3) The determination of thermodynamic functions of the reactions in commercial alkaline-manganese dioxide galvanic cell (Duracell®) Temperature resolved measurement of the electromotive force of AA Duracell® galvanic cell will be performed in order to determine the thermodynamic parameters such as ~rG0, ~rS0 and ~rH0• 4) Real Gas Behavior: Determination of the Second Virial Coefficient of C02 The pressure vs. amount of COi relation under isochoric condition will be studied in order to determine departure from ideal behavior in the pressure range 0 to 10 bar. The data obtained will also be used to determine the second virial coefficient of C02. 5) Nanosecond Laser Photolysis Study of Pyrene Fluorescence Quenching by r Anion Pyrene in its singlet excited state oxidizes iodide anion. The pyrene fluorescence decays in the presence of various iodide concentrations will be measured using pulse laser photolysis technique in order to determine the second order reaction constant. 6) Modeling Stretching Modes of Common Organic Molecules with the Quantum Mechanical Harmonic Oscillator The use of the harmonic oscillator model to interpret a vibrational spectroscopy will be introduced. Using a refined value for the effective single-bond force constant, stretching mode frequencies will be estimated to within about ±10% with a simple calculation. 7) Resonance Energy of Naphthalene by Oxygen Bomb Calorimetry The resonance energy of naphthalene will be determined by calculating its standard enthalpy of combustion both experimentally using bomb calorimeter and by using bond energies. lll 8) Pyrene Excimer Formation Kinetics Combined steady state fluorimetry and time resolved laser photolysis measurements will be performed in order to explore a complex kinetic system comprising two parallel and two consecutive reactions, that is, to determine the kinetic rate constants associated with pyrene excimer formation and decay using laser photolysis. 9) Polypropylene Phase Transitions Studied by Differential Scanning Calorimetry The enthalpy of melting and T g of two different polypropylene samples will be measured using a first class research grade instrument as an illustration of a typical industrial problem solved in material chemistry labs. 10) Fluorometric Determination of the Rate Constant and Reaction Mechanism for Ru(bpy)32+ Phosphorescence Quenching by 02 A Stem-Volmer plot will be constructed to find an experimental kq for the quenching of Ru(bpy)32+ by oxygen The fundamental principles of fluorescence measurements as well as quenching mechanisms will be covered. 11) Determining the Spin-Lattice Relaxation (Tt) of 1-Hexanol using 13C-NMR The spin-lattice times (T1) of each C atom of n-hexanol will be determined by using NMR spectroscopy. The inversion recovery method will be utilized to obtain T1 times of C atoms of n-hexanol. The observed times will be related to atomic motion of C J lV Table of Contents I. Preliminaries 1. Forward ................................................................................ . 2. Table of Contents..................................................................... 1v 3. General Information.................................... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . v111 II. The Experiments 1. Dissociation of a Propionic Acid Vapor Objectives.............................................................................. 1-1 Introduction... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1 Laboratory Procedure................................................................ 1-5 In Lab Questions..................................................................... 1-12 Data Analysis......................................................................... 1-13 Report Questions..................................................................... 1-15 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-15 2. Adsorption from Solution Objectives.............................................................................. 2-1 Introduction............................................................................ 2-1 Laboratory Procedure................................................................. 2-4 In Lab Questions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6 Data Analysis.......................................................................... 2-6 Report Questions...................................................................... 2-9 References.............................................................................. 2-9 v 3. The determination of thermodynamic functions of the reactions in commercial alkaline-manganese dioxide galvanic cell (Duracell®) Objectives.............................................................................. 3-1 Introduction............................................................................ 3-1 Laboratory Procedure................................................................. 3-2 Data Analysis......................................................................... 3-4 References............................................................................. 3-5 4. Real Gas Behavior: Determination of the Second Virial Coefficient of C02 Objectives.............................................................................. 4-1 Introduction ............................................... :............................ 4-1 Laboratory Procedure................................................................. 4-4 Data Analysis.......................................................................... 4-6 Report Questions...................................................................... 4-7 References.............................................................................. 4-7 5. Nanosecond Laser Photolysis Study of Pyrene Fluorescence Quenching by 1- Anion Objectives.............................................................................. 5-1 Introduction............................................................................ 5-1 Laboratory Procedure................................................................. 5-5 Data Analysis.......................................................................... 5-7 Vl 6. Modeling Stretching Modes of Common Organic Molecules with the Quantum Mechanical Harmonic Oscillator (QMHO) Objectives........................................................................... 6-1 Introduction............................. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 6-1 Laboratory Procedure............................................................... 6-10 In Lab Questions.................................................................... 6-13 Data Analysis.................. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . 6-14 Report Questions.................................................................... 6-15 References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-16 7. Resonance Energy of Naphthalene by Bomb Calorimetry Objectives.............................................................................. 7-1 Introduction........................................................................... 7-1 Laboratory Procedure................................................................ 7-11 In Lab Questions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 -1 7 Data Analysis......................................................................... 7-18 Report Questions..................................................................... 7-22 References ............................................................................ 7-22 8. Pyrene Excimer Formation Kinetics Objectives.............................................................................. 8-1 Introduction............. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1 Laboratory Procedure................................................................. 8-3 Data Analysis.......................................................................... 8-5 References.............................................................................. 8-8 vu 9. Polypropylene Phase Transitions Studied by Differential Scanning Calorimetry Objectives.............................................................................. 9-1 Introduction........................................................................... 9-2 Laboratory Procedure................................................................ 9-3 Data Analysis......................................................................... 9-5 References............................................................................. 9-5 10. Fluorimetric Determination of the Rate Constant and Reaction Mechanism for Ru(bpy)32+ Phosphorescence Quenching by 02 Objectives.............................................................................. 10-1 Introduction............................................................................ 10-1 Laboratory Procedure................................................................. 10-8 In Lab Questions...................................................................... 10-9 Data Analysis.......................................................................... 10-10 Report Questions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-10 References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . 10-10 11. Determining the Spin-Lattice Relaxation (Ti) of 1-Hexanol using 13C-NMR Objectives.............................................................................. 11-1 Introduction............................................................................ 11-1 Laboratory Procedure................................................................. 11-8 In Lab Questions... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-18 Data Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 11-19 Report Questions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-19 References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . 9-19 Vlll 3. General Information Instructor: Dr. Bratoljub H. Milosavljevic 331C Whitmore, 865-7481, bhml [email protected] Office Hours: As announced in class and by appointment Prerequisite: CHEM450 Materials Needed 1) CHEM 457 Lab Packet. 2) Lab notebook with alternate tear-out carbonless copy pages. 3) A flash drive. 4) Approved safety gogg]es. Eye Protection There are three types of eye protection acceptable for use in the Penn State Undergraduate Chemistry Labs. You MUST wear one of these models in the laboratory AT ALL TIMES! 1) Safety Glasses: Comfortable and offer better peripheral vision compared to gogg]es. However, they offer less protection than goggles. The bookstore has Panaspec Plus (Bouton). 2) Visor goggles: Reasonably comfortable, good splash protection, better peripheral vision than goggles. The Penn State Bookstore carries, Visorgogs (Jones and Company). 3) Goggles: The highest level of splash protection. However, fog may build up and limit peripheral vision. There are four different kinds of goggles available at the Penn State Bookstore. Course Requirements You need to complete eight experiments, and a special project to fulfill the requirements of this laboratory course. A student should submit the following for each

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