DESCRIPTION

           

            CHEM 321 is designed to provide the student with the theoretical background and practical problem solving skills needed for quantitative chemical analyses.  The primary emphasis is on practical problem solving.  A major emphasis is also placed on the statistical treatment of experimental uncertainty.  Methods for assessing the quality of data are covered in detail and students will learn to critically analyze data. 

 

            Good problem solving skills are essential for success in this course.  Detailed examples for the most common types of chemical analyses are covered.  Many other analyses can be performed by similar but modified approaches, so a student should be able to adapt the methods that have been learned to solve related problems. 

 

TEXT 

 

            Daniel C. Harris, "Quantitative Chemical Analysis", Seventh Edition, W.H. Freeman and Company (2006).  textbook web page: http://bcs.whfreeman.com/qca7e/

 

CLASS HOURS

 

MWF   2:10 –3 :00

 

OFFICE HOURS

 

            MWF   10-11, 3-4        T 1-2                             or by appointment       

            Byrd Center 315                       304-876-5430                ddilella@shepherd.edu

            web page: http://WEBPAGES.SHEPHERD.EDU/DDILELLA/

 

PREREQUISITES

 

            Chem 207, 207L, 209, 209L.  Computer skills are not a prerequisite but students who do not know how to use a computer spreadsheet program should see the instructor as soon as possible to get special tutoring.  With the aid of a computer spreadsheet program, the time required to do many problems will be significantly reduced.  The textbook gives many examples of problems that can be solved using spreadsheets.

 

Homework

           

            Exercises and problems from the text are assigned but will not be collected or graded.  Detailed solutions to all of the exercises are given in the text.  Answers, without details, are given for most of the problems.  The assigned problems and exercises represent a minimum that should be attempted.  You should work as many problems as necessary until you feel comfortable with the material.  The assigned problems and exercises are excellent practice for tests. 

            Students are encouraged to work together in solving these problems. 

            Students should use computer spreadsheets and other calculation aids whenever possible.  Many problems require considerably less work if you use a computer spreadsheet.  An answer guide for the problems in the text is available.

 

ATTENDANCE POLICY

 

            Students are expected to attend all classes.  Makeup exams will not be administered without a valid written excuse.  Term exams that are missed with a valid excuse may be made up during finals week.

 

ACADEMIC HONESTY

 

            Cheating in all its forms, including plagiarism and cheating on visual work, is considered an academic matter and will result in automatic dismissal from the course and will be recorded on the official transcript.

 

Tests

 

            There will be three term tests and a comprehensive final.  There will be several graded take-home assignments and/or in-class quizzes.  Copies of previous tests are available. 

 

Grading

                        Term tests                                                                    60%

                        Take Home Assignments and in class quizzes    20%                

                        Comprehensive Final                                                    20%

 

FINAL GRADE          

 

            The final grade will be based on the following scale

 

                        A         89 %  to 100 %             C          65 %  to 76+ %

                        B          77 %  to 88+ %                         D         50 %  to 64+ %

                       

TOPICS

 

Chapter 3 (3.1-3.5) Experimental Error – 3.1 Significant Figures, 3.2 Significant Figures in Arithmetic, 3.3 Significant Figures and Graphs, 3.4 Types of Error, systematic error, random error, accuracy, precision, absolute and relative uncertainty, per cent relative uncertainty propagation of error, 3.5 Propagation Of Uncertainty, Note: Table 3-1 is an excellent summary for propagation of error, Exercises: A, B Problems:  1, 2, 5, 7, 10, 12, 14, 15, 20

 

Chapter 4 (4.1 - 4.9)  Statistics – 4.1 Gaussian Distribution, mean, standard deviation, 4.2 Confidence Intervals, Student’s t, 4.3 Comparison Of Means,4.4 – F-test, 4.5 t-test with spreadsheets,  4.6 Q-test, 4.7 Method of Least Squares, 4.8 -Calibration Curves, 4.9 Spreadsheet for Least Squares -  Exercises: A,B,E,F,G  Problems: 1,2,8,15,16,18, 23

 

Chapter 5 (5.1 - 5.4) Quality assurance and Calibration Methods -  5.1 Basics of Quality Assurance, 5.2 Method Validation, 5.3 Standard Addition, matrix effect,  5.4 Internal Standards,  response factor,   Exercises: A, B, C Problems: 6, 7,19, 22, 28, 30

 

Chapter 18 (18.1 - 18.4) Spectrophotometry – 18.1 Properties of Light, frequency, wavelength, photon, 18.2 Absorption of Light,  excited state, ground state,  transmittance, absorbance, molar absorptivity, Beer’s Law, 18.3 Measuring Absorbance, 18.4 Beer’s Law in Chemical Analysis, Exercises: A, B Problems:  1,3,6,7,8,1012,16,17,18

 

Chapter 6 (6.1-6.9) Chemical Equilibrium – 6.1 The Equilibrium Constant, manipulating equilibrium constants, 6.2 Equilibrium And Thermodynamics, enthalpy, entropy, free energy, le Chatelier’s Principle, 6.3 Solubility Product, 6.4 Complex Formation, 6.5 Protic Acids and Bases, Bronsted-Lowry Acid, conjugate acids and bases, 6.6 pH, 6.7 Strengths of Acids and Bases, weak acids and bases, polyprotic acids, Ka, Kb. Exercises: A, C, E, F, H   Problems: 1,2,6,7,8,10,14,29,30,31,34,37,49

 

Chapter 8 (8.1- 8.4) Activity and Systematic Treatment of Equilibria -  8.1 The Effect of Ionic Strength on Solubility of Salts, ionic strength, 8.2 Activity Coefficient, activity, mean activity coefficients, extended Debye-Huckel equation, 8.3 pH Revisited, 8.4 Systematic Treatment of Equilibria, charge balance, mass balance, 8.5 Applying Systematic Treatment of Equilibria,    Exercises: A,B,C,F,H Problems: 2,3,4,9,11,15,20

 

Chapter 27 (27.1 - 27.4) Gravimetric and Combustion Analysis  - 27.1 An Example of Gravimetric Analysis, 27.2 Precipitation, crystal growth, precipitation, nucleation, colloid, adsorption, coprecipitation, digestion, gathering, ignition, 27.3 Examples Of Gravimetric Calculations, 27.4 Combustion Analysis, Exercises: A,B,C Problems: 1,2,3,4,5,7,10,12

 

TEST 1

 

Chapter 7 (7.1- 7.7) Let the Titrations Begin – 7.1 Titrations, equivalence point, end point, titration error, indicator, standardization, primary standard, standard solution, direct titration, back titration, 7.2 Titration Calculations, Kjeldahl analysis, 7.3 Spectrophotometric Titrations, 7.4 Precipitation Titration Curve, 7-5 Titration of a Mixture, 7.6 Calculating Titration Curves with a Spreadsheet, 7.7 End Point Detection, Volhard titration, Fajans titration. Exercises: A, B, E, G  Problems: 1,2,3,16,18

 

Chapter 9 (9.1-9.5) Monoprotic Acid Base Equilibria – 9-1 Strong Acids and Bases, 9.2 Weak Acids and Bases, 9.3 Weak Acid Equilibria, fractional dissociation, 9.4 Weak Base Equilibria, fraction of association, 9.5 Buffers, Henderson-Hasselbalck equation, buffer capacity, Exercises: A,E,G,I  Problems: 1,2,4,5,6,8,9,11,18,19,21,26,28,31,34,36

 

Chapter 10 (10.1-10.6) Polyprotic Acid-base Equilibria – 10.1 Diprotic Acids And Bases, acidic, basic and intermediate forms, 10.2 Diprotic Buffers, 10.3 Polyprotic Acids And Bases, 10.4 Which Is The Principal Species , 10.5 Fractional Composition Diagrams, 10-6 Isoelectronic pH, Isoionic pH, zwitterion. Exercises: A,D  Problems: 2, 4, 11, 15, 20, 23, 27, 36, 38

 

Chapter 11 (11.1-11.8) Acid-Base Titrations – 11.1 Titration Of Strong Acid with Strong Base titration, 11.2 Titration Of A Weak Acid With Strong Base, 11.3 Titration Of A Weak Base With Strong Acid, 11.4 Titrations in Diprotic Systems,  11.5 Finding The End Point with a pH Electrode, derivative plots, Gran plots, 11.6 Finding the End Point with indicators, indicator error,11.7 Practical Notes, 11.8 The Leveling Effect, titrations in nonaqueous solvents,   Exercises: A, B, C, F Problems: 1,3, 5, 8,19, 25,33,36,37,41,42,43,45,54

 

Chapter 12 (12.1-12.3, 12-6-12.7) EDTA Titrations - 12.1 Metal-Chelate Complexes, ligands, chelate effect, 12.2 EDTA, acid-base properties of EDTA, EDTA complexes, formation constant, conditional formation constant, 12-3 EDTA Titration Curves,  12.6 Metal Ion Indicators, 12.7 EDTA Titration Techniques, direct titration, back titration, displacement titration, indirect titration, masking.  Exercises: B, C, D, E  Problems: 1,2,3,7,26,27,28    

 

TEST 2

 

Chapter 14 (14.1-14.6) Fundamentals of Electrochemistry – 14.1 Basic Concepts, oxidation, reduction, oxidizing agents, reducing agents, charge, current, voltage, electrical work, Ohm’s Law, power, 14.2 Galvanic Cells, half reaction, salt bridge, 14.3 Standard Potentials, 14-4 Nernst Equation, calculations with the Nernst equation, Lattimer Diagrams, 14.5 E° and Ksp, 14.6 Cells As Chemical Probes.  Exercises: A,B, D, E  Problems: 1,2,12,13,14,19,24,25,28

 

Chapter 15 (15.1-15.7) Electrodes and Potentiometry – 15.1 Reference Electrodes, silver-silver chloride electrode, calomel electrode, 15.2 -Indicator Electrodes. 15-3 Junction Potential, 15.4 Ion Selective Electrodes, 15-5 pH Measurement with a Glass Electrode, 15.6 – How Ion-Selective Electrodes Work, 15.7 – Using Ion-Selective Electrodes, Exercises: C  Problems: 1,2,3,20,21,23,24,29,30,35

 

Chapter 16 (16.1-16.7) Redox Titrations – 16.1 Redox Titration Curves,  16.2 Redox End points, 16.3 Adjustment of Analyte Oxidation State, pre-oxidation, pre-reduction, 16.4 Oxidation With Potassium Permanganate, 16.5 Oxidation With Cerium(IV), 16.6 Oxidation With Potassium Dichromate, 16.7 Methods Involving Iodine, iodimetry, iodometry, sodium thiosulfate  Exercises: B, D Problems: 6,8,13,15,16,19,21,24,27

 

Chapter 17 (17.1-17.3) Electroanalytical Techniques – 17.1 Fundamentals of Electrolysis: ohmic potential, concentration polarization17-2 Electrogravimetric Analysis, current-voltage behavior during electrolysis, constant-voltage electrolysis, constant current electrolysis, controlled potential electrolysis with a three electrode cell,  17-3 Coulometry,  coulometric titration,  Exercises: B Problems: 1, 2,

 

Chapter 23 (23.1-23.5) Introduction to Analytical Separations  - 23-1 Solvent Extraction, partition coefficient, extraction with a metal chelator,  23-2 What is Chromatography , types of chromatography, 23-3 A Plumbers View of Chromatography , retention time, 23.4 Efficiency of Separation, resolution, diffusion, plate height, 23.5 Why Bands Spread, van Deemter Equation, longitudinal diffusion, packed and open tubular columns, asymmetric band shapes,  Exercises:  B   Problems: 1,2,7,8,15,1627,29,30

 

Chapter 24 (24.1) Gas Chromatography- 24-1 The separation Process in Gas Chromatography, gas chromatograph, packed and open tubular columns, retention index, temperature and pressure programming, Exercises: A, Problems: 1, 2

 

Chapter 25 (25.1) High Performance Liquid Chromatography 25-1 The Chromatographic Process, HPLC columns, the stationary phase, elution, isocratic and gradient elution, solvents, Exercises:  A  

 

Chapter 26 (26.1) Chromatographic Methods and Capillary Electrophoresis- 26-1 – Ion Exchange Chromatography

 

TEST 3 – May 1, 2009

 

COMPREHENSIVE FINAL – 9:00AM, May 8, 2009