Chemistry 407
Integrated Analytical and Physical Chemistry Laboratory
Fall 2002
Instructor:
- Dr. Paul F. Endres
- Office: Overman 152
- Phone: 2-8744
- e-mail: endres@bgnet.bgsu.edu
Textbook:
- There is no formal (commercial) textbook but there is a very complete set of notes. Additions may be made throughout the term. You should put these in a three ring notebook or some other permanent binder. Additional printed copies will not be provided. Most of these notes will also be available on line, often with supplemental material. We also hope to make a CD available with much of the same material, but that project was in progress as these notes were being prepared.
Exams:
- There are no exams or quizzes in this course
Grading:
- Course grades are based mainly on grades you receive for individual lab reports.
- reports of your progress and likely grade based on work to date.
Reports:
- The course notes include a separate section on writing laboratory reports.
Read it!
Meeting Times:
- The course is scheduled Tuesday and Thursday 1:30 - 4:20 p.m. and regular attendance is required.
- Because several students have 3:30 conflict, lab will be available from 12:30 pm.
- The scheduled Friday session (8:30 am) will be used only on a limited basis.
Beyond Scheduled Times:
- You should expect to spend about an hour or two preparing for each experiment. This includes reading background material and the experimental procedures. Several experiments have tutorials you are to complete prior to lab.
- Most experiments will require 1-3 hours for data analysis and calculations; some of this can be accomplished during lab, but you will generally need additional time. You should expect to spend several hours outside of lab writing and revising each lab report.
Laboratory Access:
- We will try to maintain access to the lab 9:30 - 5:00 M-F. This is mainly to provide access to data, computers and your notes. Laboratory work is not permitted outside of the regular lab hours
unless you have made specific arrangements with the instructor. We may allow you to do nonhazardous lab tasks (solution preparation, instrument runs) at other times as needed.
Web site:
- A Web site for the course can be found through
chem.bgsu.edu/~endres . There will also be a course
list serve for questions, sharing data and for last minute instructions. You should check your e-mail daily; Dr. Endres will check twice daily and will try to give fast response to questions.
Experiments:
Preliminary Exercises
(8/28 , 8/30 and 9/4, 9/6) (notes: sections I, II, III)
safety and procedures
experimental: spectrophotometry, chromatography, volumetrics, transient signals
computing: data collection, spreadsheets and MathCAD
background: errors and statistics, report writing
The next six Experiments form the first block of experiments
Spectrophotometry: The Spectrum of Ni: ethylenediamine Complexes and the use of Job's Method
(notes: V-A)
Liquid Vapor Equilibrium: Binary Phase Diagram (GC Analysis) (notes: V-B)
HPLC (High Performance Liquid Chromatography) (notes: V-C)
Electronics and Computer Interfacing (notes: V-D)
Atomic Absorption and Atomic Emission Spectrometry (notes: V-E)
Inorganic Synthesis and Separations: Co(III) complexes
(notes: V-P)
The next three Items form a break between the first and second round of experiments
- Scanning Electron Microscopy (Demonstrations)
(notes: V-M)
Library Exercise (notes: V-O)
Lab View Software (notes: VII-B)
The final round of experiments are these six items
Gas Chromatography Revisited (notes: V-G)
Fluorescence Spectroscopy and Fluorometric Methods of Analysis (notes: V-R)
Kinetics: Stop Flow (millisecond reactions) (notes: V-I)
Inorganic Synthesis and Characterization: Boron Chemistry (notes: V-Q)
Electrochemistry / Computer Interfacing: Voltammetric Analysis (notes: V-L)
Kinetics: The Oxidation of Ascorbic Acid (notes: V-H)
This course will operate differently from the laboratory in your previous courses.
Each experiment will take 2 laboratory sessions (6 hours.)
the first two weeks are different, consisting of a series of many 15-60 minutes exercises.
You will generally work within a small group (usually 2-3 persons.) The experimental work will be much easier if if you organize and divide the tasks.
Should your experimental results be unsatisfactory, your group will be expected to collect additional data. This may occur in the following week, perhaps while one of you makes progress on the next experimental project.
Each group will work on a different experiment and you will rotate through a group of experiments in a 5-6 week period. You will generally change partners with each experiment and will have a chance to work with all of your colleagues during the semester.
We will often have different groups vary the experiment so the class collectively examines a more complex problem or obtains more detailed data.
Note that there is no formal connection between Chem 405 and Chem 407. Some of the topics are common, of course. A topic may appear first in lecture or in lab. With a 5-6 week experimental cycle we couldn't synchronize the two courses if we tried.
The experiments and the instruments have been chosen to meet the objectives of the course. However, our goals are often more complex than the list of experiments might suggest. The primary goal is to help you develop into professional scientists. (That's quite different from being a good science student.)
One goal is for you to learn how to effectively use the tools and instruments of advanced experimental chemistry. This includes major instruments like NMR, but it also applies to the more mundane devices like gas regulators and temperature control.
Some of the experiments demonstrate specific chemical principles. The goal of the experiment may be to illustrate and perhaps clarify ideas developed in lecture.
We also want you to understand the ways of designing an experiment. This involves planning activities to answer specific questions, often by isolating the effect of each parameter that affects the results.
One closely related goal is to for you to develop the ability to critically evaluate experimental procedures and experimental data and to draw correct inferences. This will show up in our emphasis on error analysis, the statistical treatment of data and the methods used to calibrate our measurements.
A major goal is to develop good communications skills. Scientific reports have some special characteristics, but basically what we want is just effective writing and presentation.
Modern chemists rarely work as isolated individuals. One of our goals is to give you experience working effectively within a larger group. You also need to be able to work effectively without detailed supervision and directions.
To be a successful chemist, you need to know a variety of other techniques and tools that we borrow from other fields: statistics, graphics, computer spreadsheets, electronics,...
Professional development brings with it increased independence and responsibility. This means you need to know how to operate safely and efficiently and to find sources for needed information.
Finally, we have included some "orphan topics" into the syllabus. These are topics we feel are important to the education of chemists, but do not logically fit into the formal courses that make up our curriculum. This includes issues of professional ethics, environmental and workplace regulations, the chemical literature and the economic side of laboratory work.
Link to Endres home page
Link to course Web page including on line notes.