This course is intended to give you a semester-long introduction to modern quantitative chemical analysis in both the lecture and the laboratory. The topics to be covered are given in the attached Lecture Schedule, and the labs are briefly described in the attached Laboratory Schedule. Approximately 70% of your grade will be based on your performance in lecture, and approximately 30% will be based on your performance in lab. The two parts of the course will proceed more or less independently. In lab you will be expected to develop and carry out standard quantitative analytical determinations with high precision and accuracy. You will also work in a team of four students to select, design, and carry out a special project of your own choosing. More detailed information about the laboratory portion of this course is given in the laboratory manual.

Textbook: Quantitative Chemical Analysis, 5th edition, by Daniel C. Harris. Published by W.H. Freeman & Co., New York, 1995; plus Chemistry 221 Laboratory Manual (a copied manual written by our faculty and sold in the bookstore at cost).

Since students almost never come to see me during posted office hours, and since my selection of a particular time may not be convenient for all students, I will meet with students during the semester by setting up an appointment when it is convenient for you. A good time to set up such an appointment is immediately after class. You are also free to try to track me down at any other time. A sign on my door indicates where I can likely be found. A good place to look for me is my research labs, directly across from my office (163-166 Brown), and in 023 Lammot DuPont Lab. Please do not be embarrassed to track me down during these times. I will be happy to talk with you. If it is not a good time, I will tell you so and set up a new time. I usually hang around immediately after lecture for any questions. I will also spend time down in the labs, and you can talk with me then too. If at any time you feel like you can't reach me, send me e-mail and we can set up a time, or if it is a short question I will try to answer it by e-mail.

Quantitative Chemical Analysis
CHEMISTRY 220/221 Fall 2002 Semester
Lecture Schedule (approximate)

Week	Date	Subject of lecture	Reading	Homework due Monday
1	R 5 Sept	Course information and logistics; reading material is mainly for the lab	Ch 0, 1, 2
2	T 10 Sep R 12 Sep	Error, statistics and sampling	Ch 3, 4 App A, B, C
3	T 17 Sep R 19 Sep	Calibration and equilibrium Hourly Exam #1	Ch 5, 6
4	T 24 Sep R 26 Sep	Sampling, titrations and activity	Ch 28, 7, 8
5	T 1 Oct R 3 Oct	Systematic equilibrium, acids and bases	Ch 9, 10
6	T 8 Oct R 10 Oct	Hourly Exam #2 Acid-base titrations and methods	Ch 10, 11
7	T 15 Oct R 17 Oct	Acid-base titrations and methods	Ch 11, 12
8	T 22 Oct R 24 Oct	EDTA titrations, analytical separations	Ch 13, 23
9	T 29 Oct R 31 Oct	Analytical separations, gas chromatography	Ch 23, 24
10	T 5 Nov R 7 Nov	No class - Election Day - Go vote! Hourly Exam #3	No homework !
11	T 12 Nov R 14 Nov	High-performance liquid chromatography, capillary electrophoresis	Ch 25, 26
12	T 19 Nov R 21 Nov	Introduction to electrochemistry, potentiometry and redox titrations	Ch 14, 15, 16
13	T 26 Nov R 28 Nov	Hourly Exam #4 No class - Thanksgiving Holiday	No homework !
14	T 3 Dec R 5 Dec	Coulometry, voltammetry	Ch 17, 18
15	T 10 Dec	Analytical spectrophotometry	Ch 19	No homework. Please use the time to study for final exam.
	TBA	Final Exam, 205 Brown Lab

Laboratory Teaching Assistants

The TA assignments are presently being made at the time this document was posted. When they are available (i.e. by the first day of lecture), I will tell you the missing information, and you can write it in below.

Approximate Grading Plan

Lecture Portion (approximately 70%)

Approximately 15 graded homework sets (10 points each set)	150
Hourly examination #1	100
Hourly examination #2	100
Hourly examination #3	100
Hourly examination #4	100
Final examination (cumulative)	150
Lecture subtotal	700

Laboratory Portion (approximately 30%)

Four regular experiments from the five in the Laboratory Manual (50 points each; the lowest of 5 labs will be dropped)	200
Special Research Project Written Pre-proposal	10
Written Proposal	20
Written Report on Special Project	70
Laboratory subtotal	300
Course total	1000

 

1.) Homework sets Each week of lectures has associated with it a set of homework problems. There is space on the Lecture Schedule for you to write in the homework problems for the week. I will determine the problems that are due and inform you of this list by writing the assignment on the board in the lab on Thursday after the lecture. It is your responsibility to make note of these assignments yourself. The final answer to most of these problems is given at the end of the book, but the steps required to get the answer are not shown. You will have to show all of your steps to get any credit on a problem. The homework sets are due (in the envelope attached to my office door) by 4 PM on the Monday of the next week. There will be no exceptions to this rule. Late homework assignments will be penalized at a rate of 3 points per day (the weekend counts as 2 days).

This course will move very briskly, averaging 1.8 chapters per week. These homework problems are therefore an indispensable part of your learning process in this course, and if you don't do them, there is little chance that you will be able to do well in this course. Since there is no way to cover all the material in my lectures, I will use the homework assignments as an additional teaching mechanism. Do not assume that I am giving you a particular homework problem as an example of what will be on the midterm or final, or as an example of something I covered in lecture. Please get help if you have problems doing the homework. If you can do these problems, you will do well on the tests since the test problems will be taken almost directly from the problems at the back of the chapters.

Cheating

2.) Hourly exams You will be allowed to use calculators on all hourly exams, plus one side of a 3-inch by 5-inch index card with formulae and other information. If you think you have a legitimate excuse to not take the exam at its scheduled time, you will have to present your strong case to me in writing, in an e-mail, or in person during the first week of the semester. If successful in your request, you will be given an oral exam at the chalk board, consisting of different questions.

3.) Final examination You will take a standardized ACS multiple-choice exam in Analytical Chemistry. No cheat sheet will be allowed, and no partial credit will be given. The time of the final exam will be arranged by the university and announced during the semester.

4.) Laboratory experiments (Chem 221) All details are given in the newly updated laboratory manual. The labs start on the Thursday of the second week of the semester. You will complete all 5 regular laboratory determinations in the lab manual, and your best 4 scores will be used to compute your grade. This does not mean that you can skip one lab. If you do this, your best 3 lab scores (plus the zero for the lab you skipped) will be used to compute your grade. Of the 50 points available for each lab, 10 points will be given for lab notebook preparation prior to the lab, neatness and completeness under the heading "pre-lab". The lab assistant (TA) will check your lab notebook at the beginning of lab, to see that you have set up any tables which you will need, written down a sample calculation, and are generally knowledgeable about the lab you are starting.

Most lab exercises will require you to work with one or two partners. It is expected that you and your partners will each be present for the entire lab time. You are not allowed to "split up" the chores and work independently while the other partners are off doing something else. Evidence of this will lead us to divide your final grade by 2 or 3 for that lab.

5 points will be given for the quality of the one-paragraph lab abstract, and the remaining 35 points will be given based on the accuracy and precision of your lab results. We are therefore placing great emphasis on your performance in the lab, and we will expect in general that you achieve a 5-parts-per-thousand accuracy (5 ppt) on quantitative determinations. The lab write-up [consisting of (a.) a typed one-paragraph abstract written in clear English, (b.) a typed 3-inch by 5-inch index card with the numerical results of your determination, and (c.) copies of your lab notebook pages] is due to your lab assistant by 4:00 PM one week after you complete the lab, or one week after its last scheduled lab period, whichever comes first. Please see the lab manual for the format of these cards. Do not hand in your lab to anyone other than your lab assistant.

5.) Special project To develop your skills as independent thinkers and experimenters, and to give you exposure to "research" early in your career, you are required team up with 3 other partners (i.e. in a group of four) to propose, design, and carry out a quantitative determination of your own choosing, using the equipment which exists in the lab, or anything else at your disposal (for example at your place of work, your parents' place of work, etc.). To provide feedback in an iterative fashion, there will be two assignments to plan the project and one assignment to report it. The first is a short 1- to 2-paragraph Special Project Preproposal due in class. Next, your Special Project Proposal will be due approximately 2 weeks later, along with lists of chemicals and equipment needed. I will attempt to return your graded Preproposal and Proposal with comments in a few days. The final write-up, or your Special Project Report, is due in class on the last day of lecture. More information about these items and exactly what is required for the format is given in a section of the Laboratory Manual.

6.) General Information At the end of each chapter in your text is a list of "Terms to Understand." You should be able to define each of these without the use of the book if your understanding of the material is good. Since hourly exams will probably consist of one or more essay-type questions, it is to your advantage to be able to do this. You will also notice special sections of the textbook called Boxes and Demonstrations. When these occur in your chapter reading assignments you are expected to read them and learn about the subject (even though I may not cover them completely or even at all in lecture). These are good because they usually contain very recent state-of-the-art examples of the concepts in the regular parts of the text. Hint: I have been known to give extra credit questions having to do with these Boxes and Demonstrations.

Also at the end of each chapter is a set of "Exercises," which are to be distinguished from "Problems." The Exercises have complete step-by-step solutions at the end of the book. I strongly recommend that you work or read through these Exercises before you begin the assigned homework Problems. They will help you see the best method to approach the assigned problems. If you decide to do these exercises they will not be collected; but the assigned homework problems will of course be collected.

7.) Recommended Study Habits We each have our own study habits. For what it is worth, I will tell you how I would recommend studying to do well in the lecture part of this course. There is little doubt that this course will require a considerable amount of your time if you expect to do well. Before (or immediately after) lecture on Tuesday you should read the textbook material that will be (or was) covered. Attend class and take notes directly in your textbook since my lectures are organized more or less directly from the textbook for most subjects. Before (or immediately after) lecture on Thursday you should again read the textbook material that will be (or was) covered. On Thursday, or over the weekend, do the assigned homework Problems after reading through the solution to the Exercises. Be faithful to this schedule every week and get into a routine. Good luck!!

Laboratory Schedule
Tentative
Fall 2002 Semester

Week in Semester	Date of Thursday Lab	Experiment Scheduled
1	Sept 5	No labs scheduled
2	Sept 12	Lab 1: Basic Quantitative Skills Review and Development
3	Sept 19	Finish Lab 1 and then start Lab 2: Determination of Carbonate in Soda Ash
4	Sept 26	Finish Lab 2
5	Oct 3	Start Lab 3: Redox Titration of Iron in Ore
6	Oct 10	Finish Lab 3 and then start Lab 4: Direct Potentiometric Determination of Fluoride Ion
7	Oct 17	Finish Lab 4 and then start Lab 5: Gas Chromatography Analysis of Isomeric Butanols
8	Oct 24	Finish Lab 5
9	Oct 31	Special Projects
10	Nov 7	Special Projects
11	Nov 14	Special Projects
12	Nov 21	Special Projects
13	Nov 28	No Labs - Thanksgiving Break
14	Dec 5	Last day of labs: Special Projects wrap up; Clean up/Check out
15	Nov 30	Finals week

Note 1: The typed Pre-Proposal is due in class on Thursday, September 26.

Note 2: The typed Proposal is due in class on Thursday, October 10.

Note 3: Special Project Form for Chemicals Handling is due in lab Thursday, October 17 (hand in to your TA).

Note 4: The typed Final Report is due in class on the last day (Tuesday, December 10).

Partners for Regular Labs

Lab 1. Check-in, initial clean up, and review of basic skills. You will learn the proper use of volumetric glassware and standardize a solution by acid-base titration. Work alone.

Lab 2. Applied Acid-Base Titration: Determination of Carbonate in Commercial Soda Ash. You will use the reagents you standardized in Lab 1 to analyze an impure commercial chemical. Work alone.

Lab 3. Redox Titration of Iron in Ore. You will use an electrochemical redox titration to determine the amount of iron in an iron ore sample. Work in groups of two or three.

Lab 4. Direct Potentiometric Determination of Fluoride Ion. You will use a solid-state fluoride electrode to determine very low levels of fluoride in water and toothpaste. Work in groups of two or three.

Lab 5. Gas Chromatography Analysis of Isomeric Butanols. You will use a gas chromatograph to separate and analyze an unknown mixture of very similar four-carbon alcohols. Work in groups of two or three.