Chemistry 106 -- Fall 2004

 

Instructor in Charge:   Dr. David L. Zellmer, S-244, 278-2113
Other lectures by:        Dr. Kin C. Ng and Dr. Barry Gump

 

Course Texts:
Laboratory: Sawyer, Heineman & Beebe (SHB), Chemistry Experiments for Instrumental Methods, Wiley, 1984
Lecture: Skoog, Holler and Nieman (SHN), Principles of Instrumental Analysis, 5th Edition, Saunders, 1998

 

Week

 

Date

Topic

Speaker

Lab Group
Experiment

1

T

Th

8/24

8/26

Introduction to the Course, Assignment of experiments and instruments.
Discussion of Experiments

Zellmer

"

1 2 3 4
A B C D

2

T
Th

8/31
9/2

The Instrumental Approach to Analysis; sensitivity, selectivity, S/N, detection limit, interferences, treatment of data, treatment of samples, and calibration.

Zellmer
"

1 2 3 4
A B C D

3

T

Th

9/7

9/9

Dealing with interferences -- chemical steps prior to analysis & methods for post processing of data.
Chromatographic Techniques
Also--Student Show & Tell Day

Gump

"

1 2 3 4
A B C D

4

T
Th

9/14
9/16

Chromatographic Techniques

Gump
"

1 2 3 4
D A B C

5

T
Th

9/21
9/23

Chromatographic Techniques
                  "

Gump
"

1 2 3 4
D A B C

6

T
Th

9/28
9/30

Separations and Mass Spectroscopy (GCMS, LC-MS and other variants)

Gump
Ò

1 2 3 4
D A B C

7

T
Th

10/5
10/7

Hour Exam I
Atomic Spectroscopic Techniques


Ng

1 2 3 4
C D A B

8

T
Th

10/12
10/14

            "
Plasma Spectrometric Techniques

"
"

1 2 3 4
C D A B

9

T
Th

10/19
10/21

            "
Spectroscopic Lasers

"

1 2 3 4
C D A B

10

T
Th

10/26
10/28

Hour Exam II
Computer Automation


Zellmer

1 2 3 4
B C D A

11

T

Th

11/2

11/4

Special Project Prelim Proposal Due
Molecular Spectroscopy - UV, Vis, IR
Molecular Spectroscopy instruments and techniques.

"
"

1 2 3 4
B C D A

12

T
Th

11/9
11/11

X-Ray Fluorescence Spectrosopy
Electrochemical Methods

"
"

1 2 3 4
B C D A

13

T
Th

11/16
11/18

"
Oral Reports

"
Students

1 2 3 4
Special

14

T
Th

11/23
11/25

Oral Reports
Thanksgiving

"
Holiday

1 2 3 4
Special

15

T
Th

11/30
12/2

Oral Reports
Oral Reports

Students
"

1 2 3 4
Special

16

T
Th

12/7
12/9

Special Project Reports Due
No Class -- Faculty Consultation Day

 

1 2 3 4
Clean Up

Final

Th

12/14

Final Examination 0845-1045 (Lab time used.)

 

 

 

 

Grading:

Lecture:

Two hour exams and one final exam, each worth 100 points.

 

Lab:

Five Lab reports (4 written and 1 oral), each worth 100 points.

 

 

One Special Project Preliminary Proposal, worth 20 points.

 

Lecture and Lab each count 50% of the course grade. You must pass both lecture and lab to pass the course. 40% of possible points is considered passing; a score of 85% or better is considered "A" work. B and C cut points may vary with point distributions in the course, but are commonly 55% for a C and 70% for a B.

 

Statement on Cheating and Plagiarism.

 

Please see the statement on Cheating and Plagiarism in the current schedule of courses for University regulations and penalties. In Chemistry 106, any work that you copy from another student or copy from the literature, that you represent as your own, will be considered plagiarism. Penalties can range from loss of all points on an hour exam or lab report, to dismissal from the course with an F, to expulsion from the University. At least half of 106 deals with the production of lab reports that follow the same standards used for professional papers, so violations will be treated very seriously.

 

Examples: The following list of examples and penalties is not all-inclusive, but does illustrate situations that have arisen in the past. The instructor reserves the right to apply penalties he/she deems appropriate for other examples of cheating and plagiarism that fall under the University regulations.

 

(1)   A student turns in a lab report on Gas Chromatography. Several paragraphs in the theory section are copied from a textbook or downloaded from the Internet. No references to the origin of this information are given. A few minor rewordings are attempted to make it look like it wasn't copied. Penalty: The student is given an F for the entire course.

 

(2)   A student turns in a lab report on Gas Chromatography. The theory section is copied directly from a textbook, but referenced. Penalty: Loss of all points for the Theory section. The reference prevented this from being called plagiarism, but since the student is being graded on the quality of his or her own explanation of the relevant theory, no credit is possible. (Remember, quoted references should be very brief and should be used very sparingly. The report must be your own work.)

 

(3)   The instructor agrees that two students working on an instrument may share the data from one of the standard calibrations, but reminds them that all lab reports are to be solely the work of the author and that workup of the data collected must be done individually by each student. Student "A" works up the data on a spreadsheet, complete with statistical analyses and graphs. Student "B" asks to borrow a copy of this spreadsheet so that he/she can "study it." Except for minor label changes or shifting of positions, report A and B have virtually identical data workups. It is obvious that student B just used the work of student A. Penalty: BOTH Student A and Student B get zero points on the entire report, since it cannot be determined who copied from whom. "We just worked together" is not a defense for this kind of duplication.

 

(4)   A student turns in a lab report that looks suspiciously familiar. Checking with a previous semester, it is discovered that the student had taken the computer file from a previous student, made a few minor changes, then printed out the report and turned it in. Penalty: The student is given an F for the entire course.

 

(5)   A student turns in a lab report that seems suspicious. A search of the Internet uncovers that it was downloaded from a Lab Reports web site. Penalty: The student is given an F for the entire course.

 

Remember: Do all your own writing and data workups and all will be well. If situations arise where lack of time or instruments requires sharing of certain data, get approval from your instructor first, then reference the exact source of the data used. Shared data workups or shared written material may never be used on Chemistry 106 lab reports.

 

Experiments: Core Experiments (4) plus Special Project (1). At any given time there will be four groups of students working on the four Core experiments. Each group will consist of two students, with additional students added if the class enrollment exceeds eight. Within a group, each student will have a distinct variation on the basic experiment. Please Note: The students within a group are not considered to be "lab partners" who share all the experimental work and co-author the resulting lab report. A group may work together on learning how to use the instrumentation, but all data and reports must be the work of a single student. Scheduling of time on the instruments must be worked out within the group. Duplication of data or of any portion of a lab report or other presentation would be considered plagiarism, and would bring a minimum penalty of loss of all points for that experiment. The four Core experiments are found in SHB. A formal written report is required for three of the Core Experiments. The fourth report will be either an oral presentation to the class (20 minutes) or given as a poster session. Both of these styles are modeled after those given at professional meetings.

 

Note the Student Show & Tell Day scheduled above near the conclusion of the first round of experiments. Lecture will be shortened to allow time for each group to demonstrate to all assembled how to use the equipment they have been working on and share the triumphs and frustrations. This will also be an opportunity for your instructor to catch any egregious procedure errors before they spread to the rest of the class! There are no points for this, so relax and help out your fellow students. Try for about 15 minutes per demo.

 

After planning your experiment, please provide the storeroom a list of the chemicals you will need one period in advance of the lab. Once the basic chemicals for core experiments have been checked out in this manner, they can be left on the shelves in S-251 for use by the next group. Certain stock solutions for calibration purposes may be used by successive groups also. Check with your instructor on which solutions can or should be shared.

 

You must have a bound laboratory notebook. All setups, procedures and data must go into your notebook. Copies of computer printouts should be taped in place. Computer disks must be available for review. You may be asked to show your lab book at any time. Lab reports that cannot be supported by your laboratory notebook may be rejected. Verification of data is part of standard industry practice and is a part of Chem 106 also.

 

Report Deadlines: Reports are due at 8:00 a.m. on the Tuesday following the Tuesday following the last day scheduled for the experiment. This gives you about 10 days to write your report in most cases. The very last (special project) report is due when scheduled above near the end of the semester. Late reports WILL be assessed 5 points per lab period late. Reports turned in at 8:01 a.m. on the specified Tuesday are docked 5 points. At 8:01 a.m. the following Thursday late reports are docked 5 more points, and so on. Final reports not turned in on time for final grading are given zero points. A grade of Incomplete is not usually given because of missing report(s) that simply were not finished on time. If other circumstances prevent you from completing Chemistry 106, then the grade of I is appropriate if University specified conditions are met.

 

Core Experiments:

 

á      General Lab Procedures: Do not forget what you learned in Chemistry 102. Use "Class A" methods for making up standard solutions. Many 106 experiments have been turned into trash by students who try to weigh out 1.0 mg of standard on a balance with ±0.2 mg precision, then wonder why they have a 20% error. Also, follow all standard safety precautions (WEAR YOUR SAFETY GLASSES!), and check all chemicals used for toxicity using the Material Safety Data Sheets (MSDS) that are available either in Joyce Weber's Office, or in the Safety Section of the Departmental Web Site at www.csufresno.edu/Chemistry.

 

á      A. Molecular Spectroscopy, SHB Experiment 6-1. After completing the basic exercises, choose one of the Supplementary Experiments on p. 180 as well. Each group member should choose a different Supplementary Experiment. Each student should use the following instruments in the course of doing this experiment: (1) A Spectronic 20 must be used for Part I unless you have relative response values for the phototube in another instrument. (2) The Hewlett-Packard 8452A Diode Array Spectrophotometer with computer data station (in room S-262) is be used for parts II, III, IV, and the Supplementary Experiment. The procedures in SHB will need to be modified to do things The Computer Way. Each student is expected to store the spectra obtained on a DOS formatted floppy compatible (720K or 1.44MB) with the student's own computer (if you have one). Students with older Macintoshes that cannot read PC disks should see Dr. Zellmer, who can resave your DOS files into Mac format . The Macintosh computers in S-232 can read either Mac or PC disks and files and can do this conversion also. Office 98 on these machines can read all previous Microsoft Word or Microsoft Excel files, (until Microsoft releases Office 2000 for the PC.) See Dr. Zellmer for a demonstration/discussion of the data processing features on the data station itself and on how the data stored on floppy can be worked up on your own computer.

 

á      B. Atomic Spectroscopy, SHB Experiments 9-1 (Atomic Absorption) and 9-4 (Atomic Emission). Each student will do a different unknown where called for. Use both Direct Calibration and the Internal Standard Method. Instruments include the GBC atomic absorption spectrometer in S-251 as well as the hydrogen/oxygen flame photometer. Also the Inductively Coupled Plasma instrument in S-266 if available.

In addition to the experiments in SHB, each student shall hook up an old analog chart recorder to the Heath Flame Photometer, place a Hollow Cathode Lamp in the proper compartment, and record the emission spectrum of this lamp. (Possible alternative: Use the Ocean Optics fiber optics probe and spectrometer if available.) The portion of the spectrum recorded must contain the lines used in the atomic absorption part of the experiment. Identify these lines, and comment on the wavelength and slit width required to isolate the appropriate Atomic Absorption line. Also comment on the combination of slit width, photomultiplier voltage, sensitivity, and amplification needed to produce this spectrum, and how these choices affected the Signal to Noise ratio.

 

á      C. Gas Chromatography (GLC/GCMS) - Advanced applications using megabore capillary columns, the Mass Selective Detector, and the HP Chemstation software. Details to be announced.

 

á      D. High Performance Liquid Chromatography (HPLC), Details to be announced Instrument: ISCO HPLC with variable wavelength (254 nm) in S-251. If available, the students may also be able to gain experience on a heavily automated HP Series 1050 HPLC with data station. Use both Direct Calibration and Internal Standard Methods.

 

Special Project.

 

The Special Project should be based on your own research interests and may come from anywhere in the literature or from projects of interest to you. Some originality is expected on the Special Project. Start early in the semester, and discuss possible special projects with any of the analytical staff or other faculty members in chemistry or related areas. A Preliminary Written Proposal for your special project must be turned in on the date in the schedule above. A formal written report is required at the conclusion of the Special Project.

 

Instruments not previously mentioned that may be used include (if available--see faculty member in charge for availability): HPLC's with advanced data stations, DOS and Macintosh computers with data acquisition boards for interfacing experiments, advanced electrochemical instrumentation for amperometric and other methods, Inductively Coupled Plasma Spectroscopy (ICP, see Dr. Ng), Fluorescence Spectroscopy in the biochemistry labs, Mass Spectroscopy (GCMS), FT NMR and IR, or other instruments in the department or where you work. Discuss possible choices with your instructor before investing a lot of time in planning your project.

 

The Chem 106 Lab Report:

 

The lab reports are modeled after those found in professional journals such as Analytical Chemistry. Your goal is to be clear and concise, so that the reader knows what you did, the theory underlying the method, how you did it, what you found, and how good the results were. Common errors include very basic things like failure to identify the make and model of the instrument you used, and the sources and purity grade of the reagents. The only major differences between a 106 lab report and a professional paper will be in the level of the theory and the amount of the data presented.

 

á      Title and Abstract (5 points): Your cover sheet should include a clear title for the project, your name and the date. The abstract should be on a separate sheet, and should be a concise summary of what you did and what you found. See professional papers for examples of good abstracts. Remember, this abstract is not an "Introduction" where you say something inane like "All good chemists should understand Atomic Absorption because it is a neat method."

 

á      Theory (15 points): Professional papers assume all readers understand basic concepts, and limit their discussion to new material only, with many references to previous work. Your report should contain references also, but should go into more detail on the basic theory underlying your method. Be sure you direct your theory section toward the specific analysis you are doing; don't include unrelated material just because your sources did so. Be careful not to copy sections of texts or other literature. Read them, and once you understand what is going on, write the theory section in your own words, with specific reference to the analysis you have done.

 

á      Description of Procedure (15 points): Describe what you used to do your experiment. Include make and model of all instrumentation and/or significant pieces of apparatus. Describe the features of the instruments used. A diagram is often a good idea. Cite the grade and manufacturer of all chemicals used. Finally, describe your procedure in enough detail that others could replicate your work. Reference to standard methods in your text may be cited for detailed procedures if they were followed unchanged, but at least an outline should be provided.

 

á      Data and Results (25 points): Professional papers tend to present only a few graphs of the most important results. Your 106 lab report will include all relevant data in clear tables, charts and integrator outputs, and computer printouts, as well as computer processed data, graphed results, and statistical analysis. Organize your data such that the most important results are put together in the center of your report such that the critical evaluation follows right after them. Supporting raw data, charts, and other output can be put in an appendix for reference and checking of your processed data. Error estimates or computed statistics are expected on all measurements made. Working curves and other plotted data should use either linear least squares with the error about regression computed (see the Chemistry 102 Websites under Zellmer in Spring of '96 and '97 for a review of these methods), or make an estimate of the error about the least squares line by visual estimation. Replicated data should have 95% Confidence Limits computed. Be sure to calculate the real error between a standard or known value and your value when this is available. Compare this to the computed uncertainty of the measurement. (These numbers will be used to support your Critical Evaluation in the following section.) There will be deductions if you fail to do these statistical analyses.

 

á      Critical Evaluation (30 points): This is the most important part of your report. Having presented your data in an appropriate form, supported by statistical analyses in the Data and Results section, here you explain all these results, telling what you found, how reliable the results were, what worked well, and what could have been done better. No method is perfect, and some are just plain awful choices for the samples you had. You must tell your readers just how good or bad this method was, giving numerical statistics to back up your discussion.

 

á      Quality of Result (10 points): Some of the experiments will have an actual unknown, or a reference standard against which your work is measured. Back in Chem 102 your final number was 100% of your grade on many experiments. In Chem 106 we place 90% of the emphasis on what you did and how well you explained it, and only 10% on how close you came to the "right" answer. Of course, if you were far removed from the "right" answer, chances are you will lose points in other parts of your report because you did not have adequate control of your method.

 

The Special Project Preliminary Proposal is to be a submission patterned loosely after a grant proposal. In this proposal you

 

(1)  Describe the planned work, with references to the literature or other sources,

(2)  Describe the feasibility of doing the work in the time allotted and with the equipment and materials available (check on the availability of needed equipment, chemicals and supplies first), and

(3)  list the equipment and materials required to do the project for submission to the chemical or equipment storerooms. This report is worth 20 points.

 

The Oral Report is designed to duplicate a paper given at a professional meeting. You must prepare overhead transparencies that give the essentials of how your instrument and method work, followed by data tables and graphs that show what happened. You will have twenty minutes to make your presentation. Grading will be on the same basis as is used for written reports, with due regard for certain details that may have to be sacrificed for brevity. If you prefer, you may use a poster in place of the overhead transparencies, but you still must make an oral presentation of the material there to the class.