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CHM314 COURSE COMPACT Course Course code: CHM 314 Course title: Experimental Physical Chemistry Credit unit: 1 Course status: Compulsory Course Duration Three hours per week for 15 weeks (45 hours) Time of Lecture: Monday (2pm – 5pm) Lecture Location: Chemistry Laboratory Time of Lecture: Monday (2 – 5pm) Lecturer’s Data: 1. Name of the Lecturer: DADA, Oluwasogo Adewumi Qualifications obtained: B.Sc (Hons), M.Sc (Chemistry), MCSN, MSAN College: College of Science and Engineering Department: Physical Sciences Unit: Industrial Chemistry E-mail: [email protected] Office Location: 1st College Building, 1st Floor, A132. Consultation Hours: Monday – Wednesday: 2 – 4pm Thursday – Friday: 12 – 2pm Course Content: CHM 314: Experimental Physical Chemistry II (1 Unit) Determination of rate, rate constant and activation energy of a reaction. Determination of standard thermodynamic quantities of a reaction, phase rule. Application of electrochemical principles in titration reactions. Conductance measurements. Viscosity measurements. 1|P a ge Course Justification: This course will provide strong foundation in Experimental Physical Chemistry that can be built upon later and it will also prepare students for relevant approaches to some aspects of production in the industries through the knowledge of thermodynamics. Therefore, the course becomes highly imperatives for students who will finds relevance in Production arm of the Industry. Course objectives The course objectives and goals are: i. It is to provide strong practical foundation in Physical Chemistry that would be a basic tool for their relevance in the industries. ii. It will give students opportunity to learn the techniques involved in physical chemistry, and make them develop a careful, painstaking and a critical analytical attitude to practical work. iii. Also, it will prepare students for relevant approaches to some aspects of data analyses and some laboratory techniques which will later be useful in their final year research and career in future. Course Requirement: You are strongly advised to read the manual carefully before you come to the laboratory. An attempt has been made to explain the theory of basic principle behind each experiment to enable you understand what is going on. To be able to perform an experiment successfully and enjoyably it is imperative that you should read the script for the experiment thoroughly before doing the experiment. It should be borne in mind that in general it is of little value to carry out a set of instruction without understanding what the experiment is really about. One way of ensuring that you have read thoroughly the script of an experiment is to prepare a table of reading to be taken before you proceed to do the experiment. The table of results should be such that you can record directly the results of your measurements. 2|P a ge 1. Students should work in pairs, but laying out the table of results, calculations and writing up should be done individually. However, laying - out of table of results and calculations may be crossed – checked with the partners. Each experiment must be written up in the laboratory and submitted for marking at the end of the period. Remember that the experiments in this manual are designed to be finished and reported in one 6 hour laboratory period. However, in order to be able to finish you must organize your time and plan your work carefully. 2. Marks will be awarded for good lay – out of results, precision, accuracy and understanding. A precise result is one in which successive values are close to each other and an accurate result is one in which the experiment value is very close to the true value. If there are no systematic or instrumental errors then precision and accuracy are equivalent but an incorrectly calibrated instrument for example could be read to high level of precision and still give inaccurate results. THE LABORATORY NOTEBOOK AND FORMAT OF LABORATORY REPORT An essential part of any laboratory experience is the keeping of full and accurate records. The laboratory report book is one of the most valuable pieces of equipment the chemist uses. A properly prepared notebook can be examined at any time to determine what actions were performed, what transpired during the experiment, what results and conclusions were obtained, and even what was done incorrectly or improperly. Another chemist should be able to use a laboratory notebook to repeat an experiment to obtain results identical to those of the original investigator. When scientists perform experiments, they make observations, collect and analyze data, and formulate generalizations about the data. When you work in the laboratory, you should record all your data in a laboratory report. An analysis of data is easier if all data are recorded in an organized, logical manner. Tables and graphs are often used for this purpose. 3|P a ge The format of your laboratory exercise is given below: i. Title: The title should clearly describe the topic of the report. ii. Objectives: Write a statement to express your expectations of the results and as an answer to the problem statement. iii. Materials: List all laboratory equipment and other materials needed to perform the experiment. iv. Procedure: Describe each step of the procedure so that someone else could perform the experiment following your directions. v. Results: Include in your report all data, tables, graphs, and sketches used to arrive at your conclusions. vi. Conclusions: Record your conclusions in a paragraph at the end of your report. Your conclusions should be an analysis of your collected data. Essential conclusions of calculations and results in a clear and systematic manner and where possible, these should include accepted literature values. All symbols must be defined and units indicated. For instance an account which concludes with the statement “X = 20” where X has not been defined and its unit has not been stated is meaningless. The conclusion should include brief discussion on major sources of errors and how to improve the experiments. Note: No information should be written on scraps of paper, however temporary in plan. According to good laboratory practice (GLP), all entries should be recorded directly into the laboratory report. All entries should be documented in terms of name of material, units, etc., in blue or black ink, never in pencil. No entry should be erased or heavily marked over; one neat line should be drawn through and initialed for each incorrect or undesired entry to signify that 4|P a ge it is discarded. Each page should be numbered in the upper right corner, the numbers running consecutively throughout the laboratory report. The first two pages should be reserved for a Table of Contents. Pages should never be torn out of the laboratory report, and pages should not be skipped or left blank. Alignment with Goals and Vision of Landmark University: To build a total man and intelligent student who will break a new ground in the field of Science and Engineering. Contemporary Issues/ Industry Relevance: Most of the topics covered under the course would provide strong foundation for the students in areas of Science and Engineering. It will provide knowledge on the Chemistry of clay and the technology behind Composite Materials. STRUCTURE OF PROGRAMME/METHOD OF GRADING: This course has been structured such that the student will compulsorily visit the laboratory for his/her practical laboratory per week. Pre-laboratory test will be attempted before coming to the laboratory. Students will be divided into groups for presentation before Alpha semester examination will be done. The weekly practical exercises together with the presentation will be graded 50% while the Alpha semester examination will also be graded 50% following the NUC standard. Course Delivery Strategies: Provision of detailed explanation on different experiments that will be carried out for proper understanding of the subject matter. Solving of pre-laboratory exercises. Practical Manual will be provided for proper guidelines Recommended Readings: 1. Findlay, Practical Physical Chemistry 5|P a ge 2. Glasstone, Textbook of Physical Chemistry, p. 745 – 9 3. Moore, Physical Chemistry p.145 – 147 4. Vogel, Quantitative Inorganic Chemistry Brief Overview of Course These experiments are practical aspects of what will be done in CHM 311. It will cut across Determination of rate, rate constants and activation energy of a reaction. Determination of standard thermodynamic quantities of a reaction , Phase Rule. Application of electrochemical principles in titration reactions. Conductance measurements. Viscosity measurement. Note: The experimental work will be done for three hours within which students are required carry out the practical by following the procedures in the practical manual provided and gather their data after which they will attempt questions base on the practical. Course Outline: Week 1: Experiment 1: Phase Rule Objectives: - To determine the phase rule: two component solid-liquid system - To draw phase diagram of naphthalene and naphthol Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Questions: i. Define Phase Rule ii. State the Phase Rule equation and define the meaning of each parameter in the equation. iii. From the data collected, draw a labeled Phase diagram Week 2: Experiment 2: Distribution Co-efficient of Iodine Between Carbon Tetra Chloride and Water 6|P a ge Objective: - To determine the distribution coefficient of the Iodine Between Carbon Tetra Chloride and Water Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Question : Give a vivid report of the experiment Week 3: Experiment 3: pH – Its Measure and Applications Objective: - To carry out Measurement of The pH of Typically Salt Solution - To Determine The Dissociation Constant of Weak Acid Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions 1. 2. 3. 4. 5. Study Questions: Simple define a buffer solution and explain how to prepare both acidic and alkaline buffer solutions From the experimental data, determine the dissociation constant of the weak acid Calculate the pH of a 0.25moldm-3 solution of phenylamine Kb for phenylamineis 4.8x10-4 moldm-3 Find the pH of a solution of 0.06M ethanoic acid if Ka = 1.8x10-5moldm-3 Find the degree of dissociation of a 0.2moldm-3 solution ethanoic acid if the pH is 5 Week 4: Experiment 4: Spectrophotometer Determination of the Acid Dissociation Constant 7|P a ge Objectives: 1. To determine the absorption spectrum of each from of methyl red. 2. To Verify the Beer-Lambert’s law 3. To Determine the values of pK from the experimental data obtained Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Question 1. Determine the pH value of each solution and measure the absorbance of each solution at two wavelengths chosen to enable you to calculate the concentration of both the acid and basic form of the indictor in the solution. Week 5: Experiment 5: Thermodynamics: Determination of Heat of Neutralization Objective: To determine the heat of neutralization for the acid-base reaction Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Questions: 1. Define the Heat of Neutralization 2. Plot the graph of time against temperature and explain what can be deduced from the graph. Week 6: Experiment 6: Thermodynamics: Determination of Heat of Solution Objective: To Determination of Heat of Solution 8|P a ge Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions 1. 2. Study Question Define the Heat of Solution, Lattice Energy and Hydration energy From the experimental data, plot the graph time against the temperature. Week 7: Experiment 7: Thermodynamics: Simultaneous Determination of Several Thermodynamics Quantities (K, ∆Go, ∆Ho, ∆So) Objectives: 1. To standardize hydrochloric acid solution 2. To determine the solubility product of Borax as a function of temperature 3. To determine the standard free energy, standard enthalpy and standard entropy change for the dissolution of borax in an aqueous solution (∆Go, ∆Ho, ∆So) Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Questions: 1. Calculate values for the solubility product constant (Ksp) for borax at the various temperatures. 2. Plot ln Ksp vs. 1/T for all ten samples. Determine ∆H (kJ/mol) and ∆S (J/mol K) from this graph. 3. Calculate the values for ∆G for each sample from the experimental data collected: 9|P a ge Week 8: Experiment 8: Using Beer Lambert’s Principle for the Determination of Manganese in a Steel Sample Objective: Determination of Manganese in a Steel Sample using Beer Lambert’s Principle Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Question: 1. Measure the optical density of the solution. Using the calibration curve obtained, 2. Calculate the concentration of potassium permanganate from the steel and hence calculate the percentage of manganese in the steel sample. Week 9: Experiment 9: Chemical Kinetics I: Investigation of Effect of Temperature on the Reaction between Oxalic Acid and Potassium Permanganate System Objective: To investigate the effect of Temperature on the reaction betewwen H2C2O4(aq) and KMnO4(aq) Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Questions: 1. State the effect of temperature on the kinetics of the reaction between H2C2O4(aq) and KMnO4(aq) 2. From the experimental data collected, plot an appropriate graph. 10 | P a g e Week 10: Experiment 10: Chemical Kinetics II: Determination of the Reaction Time, Order of Reaction and the Specific Rate Constant Objectives: 1. To determine the rate law for a chemical reaction 2. To utilize a graphical analysis of experimental data to determine the order of each reactant in the reaction. Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Question: 1. Calculate the rate of reaction using: (mol I 3 ) rate and compute the logarithm of the reaction rate. t 2. Calculate the initial molar concentration of [I-]o and logarithm of initial molar concentration of the iodide ion, log [I-]o for each kinetic trial. 3. Calculate the initial molar concentration of [H2O2]o and the logarithm of initial molar concentration , Log [H2O2]o for each kinetic trial 4. Plot the graph of rate (mol I 3 ) versus Log [I-]o at constant hydrogen t peroxide concentration and determine the order of reaction p 11 | P a g e (mol I 3 ) 5. Plot the graph of rate versus Log [H2O2]o at constant Iodide ion t concentration and determine the order of reaction q using the kinetic trial 1, 5, 6,and 7 6. Determine the specific rate constant k’ for the seven solutions using the rate law: rate (mol I 2 ) k ' [ I ] P [ H 2 O2 ] q . Calculate the average value of k’ with proper units. Also t determine the standard deviation and the relative standard deviation (%RSD) of k’ from your data. Week 11: Experiment 11: Chemical Kinetics III: Determination of Energy of Activation Objective: To determine the activation energy of reaction. Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Question 1. Plot the graph of lnk’ versus 1/T(K) for at least three trials at which the experiment was performed. Take R= 8.314J/mol/K. From the appropriate plot, determine the Activation energy Week: Experiment 12: Chemical Kinetics II: Determination of the Order of Reaction and the Specific Rate Constant of a Reaction without using a Buffer Solution Objective: To determination of the order of reaction and the specific rate constant of a reaction without using a buffer solution 12 | P a g e Description: First Hour: General Class briefing and demonstration of the practical. Second and Third hours: Data Collections; Treatment of data and Solving of other practical questions Study Question: From your data: 1. Calculation the rate and logarithm of the rate which each relation occurs by taking the reciprocal of the time (seconds) required for the blue colour to appear for each of solutions. 2. Calculate initial normality of the hydrogen peroxide for each solution and its logarithm. Remember the total volume of the solution is 250cm3 Week 13 and 14: Thorough Revision and Tutorial Objectives: 1. To fully equip the students for the examination 2. To get the student familiar with the experiment 3. To examine different technical questions. 4. To build more confidence in the mind of the students Week 15 Topic: Examination Objectives: To examine the students on some selected practical that have been covered during the semester. NOTE: Download your practical Manual on the Intranet Site (Landmark University base) The Practical Manual has been uploaded on the E-learning platform on the intranet site of the University. Recommended Readings: - Quantitative Chemical Analytical Chemistry by Vogel Physical Chemistry by K.K. Sharma Sharma Physical Chemistry by Thomas Engel 13 | P a g e 14 | P a g e