Chem 253: Introduction to Quantitative Analysis
Fall Semester 2007
Instructor: Professor Peter R. Griffiths (pgriff@uidaho.edu)
Office: Renfrew Hall (REN) Room 001
Phone: 885-5807
Office Hours: 2:20 – 4:30 p.m., Mondays and Fridays
Textbooks: Exploring Chemical Analysis, 3rd Edition, Daniel C. Harris
[Three copies of a more advanced textbook by Harris (Quantitative
Chemical Analysis, 7th Edition, by Daniel C. Harris) will be on reserve in
the library:]
Calculator: An inexpensive calculator is required. You will need the calculator during
labs and exams. It should have the capability for logarithms,
exponentiation (antilogarithms), yx and scientific notation operations.
TEXT ENTRY CALCULATORS WILL NOT BE PERMITTED TO
BE USED DURING EXAMS OR QUIZZES.
Padlock: Two key or combination padlocks with up to 3/8 inch diameter shank
Goggles: Please bring the safety goggles that were given to you upon completion of
your general chemistry classes. If you have lost these goggles, you should
purchase another pair from ChemStores (Basement, Renfrew Hall). If you
transferred her, you will be issued with a new pair of goggles free of
charge. Only departmentally approved safety goggles will be permitted to
be worn in the laboratory. It is Chemistry Department policy that
safety goggles MUST be worn at all times in the laboratory or
handling chemicals.
Sandals: In light of the fact that strong acids are frequently used in this course,
neither sandals nor shorts may be worn in the laboratory.
Introduction: This course serves two primary purposes. The first is to reinforce much of
what you already know about aqueous equilibria and to apply it to the determination of
selected components in several types of samples. (Note that all students who are required
to take Chem 253 must have a solid understanding of aqueous equilibria for their majors.)
The second is to introduce you to ways of obtaining really accurate determinations of
materials by three different approaches: volumetric analysis, gravimetric analysis and
spectrophotometry. The theory behind each experiment will be covered in some detail in
class.
The Labs: You will often be given a sample the concentration of which is accurately
known by your TA. It will be your task to show that you can obtain a concentration to
within one part per thousand (ppt) of the correct answer. Your sample is different from
everyone else’s in the lab. (We purchase these samples from a company that has made
very accurately prepared mixtures for over 50 years. I have never known one of these
samples to be in error by as much as 1 ppt.) The only way to come close to the correct
answer is to follow the lab procedures very carefully. Often the techniques that you have
been taught in high school or in general chemistry are inadequate, so be sure to listen to
your TA and read up about lab techniques in the textbook. If you don’t keep your
glassware and the analytical balances scrupulously clean, your results will suffer.
The balances you will use are accurate to 0.1 mg, provided that they are level and
not abused. See your TA if you have any reason to believe that there is anything wrong
with the balance you are using. If there is and you don’t do anything about it, your lab
grade will suffer as a result. Remember that your task is to determine the exact
concentration of one of the components of your sample to an accuracy of 1 ppt; if your
balance is inaccurate, your results will be in error.
A secondary goal of this course is to teach you to keep a good lab notebook. The
lab book should be hard-bound, not spiral bound, with all pages numbered by you. All
entries in your notebook must be in pen. Your lab grade will suffer any time your TA
sees you either entering data in your notebook in pencil or writing something down on a
scrap of paper to enter in your book later. Your notebook doesn’t have to be a work of
art. It does have to be used to record everything that you did in the lab in a way that can
be understood by you and by others (your TA and me, for example). Draw a simple line
through the results of any experiment that you decide to reject and give the reason why
you chose to reject this result.
There will be a prelab question that is associated with each lab that is designed to
ensure that you know how to calculate your results. Please hand in your answer to this
question as you arrive in the lab. Anyone arriving more than 15 minutes late for the lab
will receive a grade of zero for that question.
Each measurement is done in triplicate and you should calculate the result
immediately you have finished each run. If one result is obviously out of line with the
other two (e.g., by the Q test), there is often time to carry out a fourth or even fifth run, so
that you can discard the outlying result.
Classes and Homework: I will spend most of each class period introducing you to a
given topic. I will then assign a few pages out of Harris’s book for you to read, together
with a few problems from the relevant chapter. At the start of the following class, I will
spend a few minutes answering questions about my previous lecture or about the assigned
reading material before introducing a new topic. Don’t be bashful about asking me to
discuss any topic that you don’t understand. The answers to the questions will be posted
on my web site. Every Friday, I will assign two problems (one easy and one difficult)
that you should do; please give your answers to your TA on the following Tuesday lab.
Your Teaching Assistant: Each section has a different TA. If you have any questions on
any material that you would prefer to ask your TA, please see him during his office hours
in REN 049. Their office hours are as follows:
Section 1 (T, Th morning lab lab): REN 337, TA: TBA
Section 2 (T, Th afternoon lab): REN 337, TA: TBA
Section 3 (T, Th evening lab) REN 337, TA: TBA.
Section 4 (T, Th morning lab) REN 334, TA: TBA
If you can’t make it to your TA’s office hours, try to see one of the other Chem 253 TAs
during his/her office hours. (They will know much more about the course material than
any of the other TAs who are staffing REN 049 at other times.)
Grading Policy: There will be three mid-term examinations and a comprehensive final.
Your final grade will calculated in the following way:
Mid-Terms 45% (15% each)
Lab 25%
Homework 10%
Final 20%
The grades will be as follows: A,100-80%; B, 79-65%;C, 64-55%; D, 54-45%; F, less
than 45%. I don’t grade on a curve. If you can’t work out how well you are doing in the
course at any point in the semester, you can work out your score by dividing your current
score for a given category by the possible score and multiplying it by the percentage
given above. Most people do about as well on the final as they do on the mid-term
exams, and I make this assumption. Simply add the scores for each category to find your
current score. Let us say that at a certain point in the semester, you have scored 387 out
of a possible 500 in the lab, 58 out of a possible 70 points on the homework assignments
and 72 and 68% on the first two mid-terms. Your current score would be:
Lab: (387/500) x 25 = 19.35;
Homework: (58/70) x 10 = 8.29;
Exams: (140/200) x 65 = 45.50
Current projected score: 19.35 + 8.29 + 45.50 = 73.14, i.e., you currently have a B.
Approximate Schedule
August 20 Introduction to the class
August 22 Introduction to chemical analysis, units of concentration (to include “p
functions”), accuracy and precision (Chapters 0, 1 and 2 and Appendix
IA)
August 24 The significance of data, introductory statistics (Ch. 3 and Appendix IIA)
August 27 Statistics, rejection of data (Chapter 4)
August 29 Chemical equilibria, introduction to acids and bases (Sections 6-1 and 6-2,
Sections 8-1 through 8-4)
August 31 Activity; activity coefficients (Chapter 12)
Sept. 3 No class (Labor Day)
Sept. 5 Introduction to volumetric analysis, titration of strong acids and bases
(Section 6-1 and 6-2, Section 10-1)
Sept. 7 Titration of Weak Acids and Bases (Sections, 8-5 through 8-7, 9-2, 10-2
through 10-6.
Sept. 10 Polyprotic acid-base equilibria and titrations (Chapter 11)
Sept. 12 Buffer solutions (Section 9-3 through 9-5)
Sept. 14 Acid-Base Indicators (Section 9-6)
Sept. 17 Review of statistics, acid and bases and neutralization titrations
Sept. 19 First Mid-Term Exam
Sept. 21 Introduction to Spectrophotometry (Chapter 18)
Sept. 24 Beer’s law and spectrophotometric analysis (Chapter 18)
Sept. 26 Applications of spectrophotometry (Chapters 19 and 20)
Sept. 28 Introduction to Precipitation (Section 6-4)
Oct. 1 The formation of precipitates (Not covered well in the textbook)
Oct. 3 Precipitation titrations (Sections 6-5 and 6-6
Oct. 5 Gravimetric analysis (Chapter 7)
Oct. 8 Gravimetric analysis (Chapter 7)
Oct. 10 Effect of Ionic Strength and pH on Solubility
Oct. 12 Separation by precipitation (Section 9E)
Oct. 15 Review of specrophotometry, precipitation equilibria, precipitation
titrations and gravimetric analysis
Oct. 17 Second Mid-Term Examination
Oct. 19 Complex formation (Sections 13-1 through 13-3)
Oct. 22 Complexometric titrations (Sections 13-4 through 13-6)
Oct. 24 Indicators for EDTA titrations (Section 13-3)
Oct. 26 Fundamentals of electrochemistry (Sections 14-1 and 14-2)
Oct. 29 The Nernst equation and standard electrode potentials (Sections 13-3
through 13-5)
Oct. 31 Redox titrations (Chapter 16)
Nov. 2 Redox titrations (Chapter 16)
Nov. 5 Potentiometry (Chapter 15)
Nov. 7 Reference electrodes (Chapter 14-6)
Nov. 9 pH and other Ion-Selective Electrodes (Sections 15-3 and 15-4)
Nov. 12 Review of potentiometry, redox titrations
Nov. 14 Third Mid-Term Examination on complexometric titrations and
electrochemical methods
Nov. 16 Coulometric analysis (Section 17-1)
Nov. 19 No class (Thanksgiving break)
Nov. 21 No class (Thanksgiving break)
Nov. 23 No class (Thanksgiving break)
Nov. 26 Principles of Chromatography (Chapter 21)
Nov. 28 Gas chromatography (Section 22-1)
Nov. 30 Liquid chromatography (Sections 22-2 and 22-3)
Dec. 3 Other forms of chromatography (Chapter 23)
Dec. 5 Modern spectroscopy (Chapter 20)
Dec. 7 Review for final examination
Dec. 10, 10:00 a.m. Final Examination
IMPORTANT NOTICE: The final examination is scheduled at 10:00 a.m. on
Moday, December 10. This is the first day of finals week. Everyone in the class is
expected to take the exam at this time. No accommodation will be made for students
who have made arrangements to have left Moscow by this time.
Laboratory Schedule
First Lab No lab
Second Lab Check in; clean glassware; instruction on balance
First Lab No class (Labor Day)
Second Lab: Experiment 1: Use of analytical balance; dry KHP
First Lab: Experiment 2: Preparation of standard solutions of NaOH and HCl
Second Lab: Experiment 2: Determination of purity of impure KHP sample
First Lab Experiment 3: Volumetric analysis of a drain cleaner
Second Lab Experiment 3: Volumetric analysis of a drain cleaner
First Lab Experiment 4: Spectrophotometric determination of manganese in steel
Second Lab Experiment 4: Spectrophotometric determination of manganese in steel
First Lab Experiment 5: Spectrophotometric determination of copper in an alloy
Second Lab Experiment 5: Spectrophotometric determination of copper in an alloy
First Lab Experiment 6: Volumetric determination of chloride by Fajan’s method
Second Lab Experiment 6: Volumetric determination of chloride by Fajan’s method
First Lab Experiment 7: Gravimetric determination of chloride
Second Lab Experiment 7: Gravimetric determination of chloride
First Lab Experiment 8: Gravimetric determination of iron
Second Lab Experiment 8: Gravimetric determination of iron
First Lab Experiment 9: Complexometric determination of Ca and Mg in water
Second Lab Experiment 9: Complexometric determination of Ca and Mg in water
First Lab Experiment 10: Determination of Vitamin C by redox titration
Second Lab Experiment 10: Determination of Vitamin C by redox titration
First Lab Experiment 11: Potentiometric analysis of acid in soft drinks
Second Lab Experiment 11: Potentiometric analysis of acid in soft drinks
First Lab No class (Thanksgiving break)
Second Lab No class (Thanksgiving break)
First Lab Experiment 13: Coulometric acid-base titraton
Second Lab Free lab to catch up if you are behind
First Lab Small Group Project
Second Lab Small Group Project
First Lab Small Group Project
Second Lab Check out