Spring 1997 Dr. Zellmer
Office: Science Building, Room 244
Telephone and Voice Mail: (209) 278-2113
Chemistry Dept. Office: (209) 278:2103
E-mail: david_zellmer@csufresno.edu
Text: Skoog, West, and Holler, Fundamentals of Analytical
Chemistry, 7th Edition (required)
There will also be a packet of handouts for sale at the Kennel Bookstore.
Other required materials: Safety glasses, bound laboratory notebook, and scientific calculator. There is a lot of computer work in this course. Although computers are available in the Science Building and elsewhere on campus, owning your own machine is a very good idea for this course. The type of computer is unimportant, but it must be capable of running a fairly recent version of an advanced spreadsheet such as Microsoft Excel. E-mail and internet access will also be useful.
Grading:
| Lecture: | 3 Hour exams, at 100 points each | 300 points |
| Final Exam | 200 points | |
| Total Lecture (60% of grade) | 500 points | |
| Laboratory: | Experimental Results | 550 points (appx) |
| Reports and Lab Book | 205 points (appx) | |
| Total Laboratory (40% of grade) | 755 points (appx) |
Homework and InClass participation help decide borderline cases.
How your grade is calculated: You must have a passing grade (40% in lecture, and about 60% in lab) both in lecture and in lab, in order to pass the course. Past experience shows that lecture grades of A generally fall in the 85% and above category, B at 70% and above, and C at 50% and above. Grades below 50% but above 40% have been D in lecture. Lecture and lab grades are combined by adding 3/5 of your % lecture score to 2/5 of your % lab score. Assuming you have a passing grade both in lecture and in lab, the combined score will be used to compute your letter grade for the course. 85% will be an A for sure; 70% will be a B for sure; 50% or more is required to get at least a C. If you are below 40% in lecture, you will have failed. (Grades under 60% in lab will fail you also, but these are almost unheard of for students completing all of the experiments.) Borderline grades just below the stated A and B cut lines will be decided from diligence in the homework plus an evaluation of the pattern of overall performance in the course. The most common helpful pattern is evidence of improvement and ultimate competence.
Reports are generally formal write-ups of experimental procedures and results for those lab experiments where a reliable comparison of your results with a standard are not possible. Reports are due no later than 10 minutes from the beginning of lab one week from the Monday or Tuesday following the last scheduled day for the experiment. (The last IE/GLC/HPLC/ISE report is due by noon Tuesday of the final exam period.) Late penalties of 5 points per lab day will be assessed for late reports and must be turned in within 10 minutes of the beginning of lab to avoid an additional late day penalty . We may also experiment with student-generated hypertext documents written in HTML and attached to the World Wide Web on the Internet.
The following lecture schedule is somewhat tentative, due to the need to cover laboratory topics before the experiments begin. In many cases it will be necessary to interrupt the detailed lecture discussion of a topic in order to provide introductory information on an impending experiment. Some lecture periods, usually on Fridays, will be devoted to in-class problems.
The problem assignments given below are due when announced in class, generally at the conclusion of the material covered by them. Most of these have the answers in the back of the book. To get full credit for your homework, you must turn in complete solutions. on the day specified. Answers simply copied from the back of the book will not be accepted. Late homework can be turned in for reduced credit up to the day of the exam that covers that homework; after that it will not be counted. Some homework assignments will require the use of a computer spreadsheet (ss). If you have been considering buying a computer, now would be a good time, although computer labs are available on campus. Microsoft Excel or a similar spreadsheet will be needed. Some older integrated packages (e.g. versions of Microsoft Works 3.0 or older) do not produce true XY scatterplots, making them unsuitable for this course. The Macintosh and PC versions of most spreadsheets are almost identical, so computer type is not a factor.
The chapters assigned for reading will often contain much more material than is covered in the class. Concentrate on the topics emphasized by your instructor, or on material needed to solve assigned problems. In most cases it is not necessary to master all of the material in your text.
Week 1 MWF 1/27-1/31. Introduction to the course. Introduce gravimetric chloride experiment. Review mass, volume, concentration units and calculations. Begin particle size & purity. Read Ch. 1 (Introduction); Ch. 35 (Chemicals, Apparatus, and Unit Operations of Analytical Chemistry); Ch. 5 (Gravimetric Methods); Ch. 6 (Volumetric Calculations)
Problem Set: Basic1: Ch. 5, p. 98: 12, 14, 18, 20; Ch. 6, p. 119: 6, 10, 13, 17, 19.
Lab Check in/bal instr/Grav. Cl.
Week 2 MWF 2/3-2/7. (Mon) Conclude stoichiometry, particle size and purity of precipitates, gravimetric calculations. (Wed) Begin Statistics. Read Ch. 2 (Errors in Chemical Analyses); Ch. 3 (Random Errors in Analyses).
Problem Sets: Grav1 Ch. 5, p. 98: 21, 29, 31, 35, 37. Stat1 Ch. 2, p. 20: 6, 7; Ch. 3, p. 44: 5, 13; Ch. 4, p. 68: 1, 8 (Stat1 covers mean, median, range, CV, pooled s and 95%CL)
Lab Grav. Chloride/Glassware Calibration.
Week 3 MWF 2/10-2/14. Intro Vol Cl Exp. Statistical methods and computer calculations with spreadsheets. Read Ch. 4 (Statistics), Statistics Handouts, Excel spreadsheet handouts.
Problem Set: Stat2: Ch. 4, p. 69: 13, 17, 19 (Stat2 covers CL of two means, Q-test, and LLS analysis -- problem 19 must be done by spreadsheet.)
Lab (M/Tu) End Grav Cl. (W/Th) Begin Vol. Chloride
Week 4 M 2/17 Holiday, WF 2/19-2/21. Solubility product equilibrium calculations. Read Ch. 7 (Chemical Equilibrium), pp. 126-137 (Ksp), Ch. 8 (ionic strength and activity); Ch. 9 (Equilibrium calcs in complex systems--charge and mass balance); Ch. 13 (Precipitation Titrations).
Problem Set: (Do each set as the topic is covered.) Ksp1 Ch. 7, p. 146: 9, 10, 11, 12, 14, 16; Ionic 1 Ch. 8, p. 158: 7, 8, 11. Ksp2 Ch. 9, p. 187: 5, 6, 12 (see spreadsheet solutions in class for Ksp2). KspTitr Ch. 13, p. 277: 29.
Lab Volumetric Chloride
Week 5 MWF 2/24-2/28. Introduce Acid/Base Experiment. Begin formal treatment of acid/base equilibria. Read Ch. 7 pp. 122-133, 137-146 (Strong acids and bases, mostly monoprotic weak acids and bases.); Ch. 10 (Monoprotic Acid/Base Equilibria).
Problem Sets (do each set as topic is covered): AB1 Ch. 7, p. 146 (SA, SB, WA, WB): 4, 6, 8, 16, 21, 22. AB2 Ch. 10, p. 222 (buffers): 34, 37, 42, 43. AB3 (monoprotic titr curves & alphas) Ch. 10, p. 222: 47. 50. 51, 53.
Lab (M/Tu) end Vol Cl; (W/Th) begin Acid-Base.
Week 6 MWF 3/3-3/7. Hour Exam I. (Monday) Covers all topics through Ksp. Lecture continues with acid-base equilibrium on Wednesday. Read Ch. 11 (Polyprotic A/B Equilibria); Ch. 12 (Acid/Base Titrations)
Problem Sets (do each set as topic is covered): AB4 Ch. 11, p. 245 (polyprotic): 6, 9, 10, 11, 12, 20, 28. AB5 Ch. 12, p. 262 (real AB analyses): 29, 44.
Lab Acid-Base.
Week 7 MWF 3/10-3/14. Introduce EDTA Experiment. Complete discussion of acid-base equilibrium. Begin discussion of Complex Formation Equilibria. Read Ch. 14 (EDTA Titrations)
Problem Sets: CF1 Ch. 14, p. 302 (messy vol calcs): 16, 18, 20. CF2 Ch. 14, p. 302 (equilibrium and titr curves): 25, 27.
Lab (M/Tu) End Acid-Base; (W/Th) Begin EDTA.
Week 8 MWF 3/17-3/21. (Mon) Complete complex formation discussion. See week 7 for readings and problems. (W) Intro Spectrophotometry & Spectro Experiment. Read Ch. 22 (An Introduction to Spectrochemical Methods), Ch. 23 (Instruments for Optical Spectrometry)
Lab EDTA ends on W/Th.
*** Spring Break 3/24-3/28 ***
Week 9 MWF 3/31-4/4. Spectrophotometry continues. Read Ch. 24 (Molecular Absorption Spectroscopy), Ch. 25 (Molecular Fluorescence Spectroscopy, Ch. 26 (Atomic Spectroscopy). Friday is Hour Exam II. Covers Acid-Base and Complex Formation.
Problem Set: Spec1 (%T and Beer's Law) Ch. 22, p. 525: 11, 16; Ch. 23, p. 555: 10; Ch. 24, p. 598: 8. Spec2 (Working Curves--do with spreadsheet) Ch. 24, p. 600: 27, 28; Ch. 26, p. 636: 11.
Lab (M/Tu) Begin Spectrophotometry.
Week 10 MWF 4/7-4/11. (Mon) Introduction to Electrochemistry. Half-reactions, electrochemical cells, use of the Nernst equation. (Wed) Intro Redox experiment. Read Ch. 15 (An Introduction to Electrochemistry)
Problem Set: EC1 (redox eqns--balance the half reactions first) Ch. 15, p. 328: 9, 10, 11. EC2 (Nernst) Ch. 15, p. 328: 13, 16, 18.
Lab Spectrophotometry ends on W/Th.
Week 11 MWF 4/14-4/18. Complete Cells & Nernst; Oxidation-Reduction Titrations. Read Ch. 16 (Potentials and Redox Titrations), Ch. 17 (Applications of Redox Titrations)
Problem Set: Redox1 Ch. 16, p. 359 (cells and titration curves): 3, 30, 33. Redox2 Ch. 17, p. 383 (messy redox vol calcs): 28, 30, 32, 43, 49.
Lab (M/Tu) Begin Redox.
Week 12 MWF 4/21-4/25. (Mon) Redox Titrations; Potentiometric methods and Ion Selective Electrodes. (Wed) Intro ISE Experimental Method(all students are responsible for the method and calculations, not just those selecting this experiment). Read Ch. 18 (Theory of Potentiometry), Ch. 19 (Applications of Potentiometry)
Problem Set: ISE Ch. 19, p. 429: 7, 11 (also problems on F- handout).
Lab Redox ends on W/Th.
Week 13 MWF 4/28-5/2. Hour Exam III (Monday) Covers Spectrophotometry, Redox, and Ion Selective Electrodes. (Wed) Separations (liquid-liquid, ion exchange). Chromatography, especially HPLC. Read Ch. 28 (Introduction to Chromatography), Ch. 29 (Gas Chromatography), Ch. 30 (High Performance Liquid Chromatography).
Problem Set: Sep Ch. 29, p. 700: 17.
Lab (M/Tu) Begin IE/HPLC/GLC/ISE
Week 14 MWF 5/5-5/9. Conclude chromatography.
Problem Set: None.
Lab IE/HPLC/GLC/ISE
Week 15 MW 5/12-5/14 Review for final
Lab (M/Tu) Complete IE/HPLC/GLC/ISE and check out; (W) Check out only--no lab work on the last day.
Finals The Final Exam is scheduled for Wednesday, May 21, 1997 from 1100-1300. Students may turn in their IE/HPLC/GLC/HPLC report by 12 noon on Tuesday; after that time, no credit will be given for this last report.