Course Numbers: CHEM 434 (CN 01377-01378)
                           CHEM 535 (CN 01392-01393)

Professor:       Howard D. Dewald
Office Hours:  by appointment
Office:            Clippinger 392
Phone:            740-517-8455
email:             dewald@ohio.edu
WWW:           http://machine.chem.ohiou.edu/~dewald/chem434.html

Lab schedule:     T   9 a.m.-12 Noon   Clippinger 071A (CN 01377  & 01392)
                         T   2 p.m. - 5 p.m.    Clippinger 071A (CN 01378  & 01393)
                         Th 9 a.m. -12 Noon  Closed
                         Th 2 p.m. - 5 p.m.    Closed

Text: Skoog, D. A.; Holler, F. J.; Nieman, T. A. "Principles of Instrumental Analysis," 5th ed., Saunders, Philadelphia, 1998.

         "Official Laboratory Research Notebook," Jones and Bartlett, Boston, 1997.

Lab Fee: A $8.00 consumable materials fee will be collected the first week during a regular lab period from a breakage card (available from Cashier's Office in Chubb Hall for $20.00).

Prerequisites:     CHEM 434: CHEM 431 or concurrent
                         CHEM 535: CHEM 531 or concurrent

Grading Policy:     Laboratory Reports: 80% (20% each)
                           Laboratory Notebook: 20%
 

1)  Distribution Between Immiscible Liquids
2)  Ion Exchange Chromatography
3)  Gas Chromatography
4)  High Performance Liquid Chromatography
 

Attendance at laboratory is expected. In the event of absence, the following will apply:

1) Written/documented verification of absence will be required;
2) No laboratory make-up will be given outside of the laboratory schedule; instead a set of experimental values will be provided or alternate written literature summary will be assigned.
 

ACADEMIC MISCONDUCT: "Academic Misconduct is a Code A violation of the Ohio University Student Code of Conduct. Academic Misconduct refers to dishonesty in examinations (cheating), presenting the ideas or the writing of someone else as one's own (plagiarism), or knowingly furnishing false information to the University."[1] If you are found to be involved in academic misconduct, you will receive zero credit on the work in question and the case may be referred to the Director of Judiciaries with a possible sanction of suspension or expulsion.

PLAGIARISM: Examples of plagiarism include [2]:

1.  "Reproducing another person's work, whether published or unpublished."
2. "Submitting as your own any academic exercise prepared totally or in part by another."
3. "Allowing another person to substantially alter or revise your work and submitting as your own."
4. "Using another's written ideas or words without properly acknowledging the source. If a student uses the words of someone else, he or she must put quotation marks around the passage and add indication of its origin, such as a footnote. Simply changing a  word or two while leaving the organization and content substantially intact and failing to cite the source is plagiarism"

If you are unsure about what constitutes plagiarism and/or how to properly acknowledge a source, you must see the course professor before submitting your materials.

References

[1]  Student Academic Honesty for Ohio University Faculty & Teaching Associates, Ohio University Office of Judiciaries, 1994
[2]  Student Academic Honesty for Ohio University Students, Ohio University Office of Judiciaries, 1994.
 

Each student will perform and report on four (4) experiments.  Four (4) written reports will be required and each will count 20% of the course grade. Reports will be assigned a numerical grade. Grades will reflect both the quality of the report and the quality of the experimental results.

All laboratory reports are due by 5:00 p.m. fourteen days (including holidays and Saturday and Sunday) after completion of the experiment.

The grade on any report submitted late will be reduced by 5% the first day, and 15% the second day. Reports that are more than two days late will not be accepted and will be given a grade of zero.

The report will be judged overall as to format and quality of each section. Additionally, factors such as grammar, spelling, neatness, design of tables and figures, and legibility will be used in evaluating the report. The accuracy of the results and correctness of calculations will be a further basis for assignment of the grade. Falsified, fictitious, or copied data will result in an automatic grade of zero credit for the experiment.

The laboratory report grade may also reflect conduct and performance during the laboratory. The factors used in assigning the grade will include adherence to laboratory rules and safety awareness, planning/ preparation for experiments, care taken in
handling equipment, use of good and proper analytical technique, and diligence in attendance and effective use of time.

The notebook grade will be based on adherence to standard rules for the use of a laboratory notebook.

Laboratory SAFETY RULE VIOLATIONS will lead to expulsion from the laboratory and a failing laboratory grade.

Finally, failure to check-out of the laboratory at completion of the course (or as a result of withdrawal) will result in a failing grade for the course. Check-out includes returning all borrowed items, cleaning glassware and returning it to the shelves, helping to assist with putting away equipment, etc.
 

A laboratory notebook provides a complete record of your laboratory work that can be understood and repeated by yourself and others.

Rules:

1) Use a permanently bound book with consecutively numbered pages.

2)  Enter all data directly into the book in ink. Do not record data elsewhere for transfer into the book.

3) Never make erasures. Delete an entry by drawing a single line through it so that it is still legible. Corrections, if needed, should be made adjacent to the deleted entry. Numbers should never be written over.

4) Record sufficient information. All procedures, reagents, apparatus, sketches, conditions, references, etc. should be entered into the book as the work is done. The purpose and significance of the experiment as well as observations, results, and conclusions should be made clear.

5) Date each notebook page as it is used and sign your notebook at the end of each laboratory period. The laboratory teaching assistant must also sign the notebook.
 

Format:

1) The "Records of Contents" page should be used for a table of contents, which should be conscientiously kept up to date.

2) Include the title of the experiment.

3) Include one complete example of every calculation made with the data.

4)  Write balanced equations for all important reactions that take place.
 

Written laboratory reports are prepared similar to manuscript requirements for the journal Analytical Chemistry published by the American Chemical Society.

General Instructions

1) Use 22 x 28 cm (8 1/2 x 11 in.) unruled high quality white paper. Type double-spaced on one side only. Number the pages consecutively in the upper-right corner with Arabic numerals. Staple the report pages together in the upper-left corner. Proofread the report carefully. Make certain spelling errors are corrected and that exponents and symbols have not been omitted.

2) TITLE Page. Give the title as it appeared on the handout. Give your name and your lab partner's name (if any). Give the date you completed the experiment in the laboratory and the date you submit the report.

     Example:             Identification of Phenolic Constituents in Beverages by HPLC

                                 Michael Tswett
                                 A. Tiselius (Partner)

                                 Date experiment completed:  January   8, 2002
                                 Date report submitted:   January 22, 2002
 
3) ABSTRACT Page. State the objectives of the experiment. Give a very brief summary of the methods used and the significant results. Evaluate the results as compared to known values, theory, or expectations. Do not give experimental details. The length of the abstract must not exceed 150 words. BE SPECIFIC--NOT GENERAL

4) TEXT. USE YOUR OWN WORDS. Address yourself to the reader. Assume the reader will have a general knowledge of chemistry, but no background to the experiment performed. Do not use first person (i.e., “I” or “we”) tense. Do not use     footnotes; include the information at an appropriate place in the text. The organization of the text should be divided into separate sections for INTRODUCTION, EXPERIMENTAL, RESULTS AND DISCUSSION, CONCLUSIONS and LITERATURE CITED.
 
 

In this section write a discussion of the theory and principles underlying the experiment. If literature references are summarized cite the article used following the guidelines for LITERATURE CITED. Do not derive every equation, but indicate their application and use in the experiment.

Give proper credit and follow correct punctuation and form with regards to direct quotations. Attempts to alter or failure to properly cite a direct quotation will be treated as plagiarism. Copying the introduction word for word from the laboratory handout constitutes plagiarism.

Diagrams may be used if they are given figure numbers (discussed below).

The minimum acceptable introduction is 350 words. Strive to develop the discussion thoroughly and appropriately, but compactly. (A maximum length for the introduction should be 600-700 words.)
 

Use complete sentences. Do NOT use outline form. Use the third person, past tense, passive voice. Include the following sections:

Apparatus.  Describe only devices of specialized nature. This should include which instruments were used (including model numbers). Do not include equipment that is standard in an analytical laboratory (e. g. , glassware and balances).

Reagents.  Describe the preparation of solutions. Include the reagents used (with their supplier).

Procedure.  Describe the pertinent and critical details of the experiment, but avoid excessive description. Copying the procedure word for word from the experimental handout constitutes plagiarism.
 

In this section the data obtained and calculations performed are to be reported. Numerical data are best presented in tabular form. Use precise values for physical constants and formula weights. Observe the rules for significant figures.

Present the data and results in a logical progression from preliminary work-up to final discussion. Use tables and/or figures to present data, show straight-line fitting, or for calibration. Summarize the important observations of the experiment. Be complete and relevant but concise in the discussion of the data and presentation of the results.

For all straight-line plots (e.g., calibration curves), the data points must be analyzed with by the method of linear least squares. The value of the correlation coefficient, r, must be given. Slopes of lines must be determined by this method.
 

Use conclusions only for interpretation and not to summarize. Discuss what the experiment demonstrates and compare results to known values or expected values, but do not repeat the results section. Discuss any statistical significance of the results. Give realistic suggestions for ways to improve the experiment.
 

References to all resource materials used in writing the report are to be numbered in one consecutive series by order of mention in the text. The complete list of references is placed on a separate page at the end of the report before the tables and figures. Reference numbers in the text are to be in parentheses and on line or superscripted. Repetition is avoided by using the number corresponding to the original reference.

Use "Chemical Abstracts Service Source Index" abbreviations for journal names. Please use the format given in the following examples:

Articles:
Roston, D. A.; Kissinger, P. T.  Anal. Chem. 1981, 53, 1695-1699.

Books:
Willard, H. H.; Merritt, L. L., Jr.; Dean, J. A.; Settle, F. A., Jr. "Instrumental Methods of Analysis," 7th ed.; Wadsworth: Belmont, CA, 1988; pp. 713-715.
 

5) FIGURES and TABLES. Figures and tables are numbered separately beginning with Figure 1 and Table 1.

Tables. Tables must be constructed with an appropriate title and column headings. Units of measure must be clearly indicated.

Tables should be intelligible without reference to the text, but must be cited in the text of the report. Type each table on a separate page. Attach at the end of the report after LITERATURE CITED but before any figures.

Figures. Submit only figures (graphs, diagrams, sketches) done in blue or black ink. Each figure must have a descriptive caption/legend.

Figures are cited in the text, but are attached to the end of the report after any tables.

Drawing graphs. Use only good quality professionally printed graph paper having margins on all edges and fine rulings in all directions. Do not use "engineering data pad" paper.

Place the independent variable along the abscissa (x-axis). Place the dependent variable along the ordinate (y-axis).  Clearly label each axis as to the variable and units. The form i (mA), E (V), time (min), etc. is preferred.

The numerical units should be chosen to allow full use of the entire grid system of the paper. Choose numbers of simple multiples for major grid lines. Each or alternate main grid lines should be marked and numbered along the margin. It may not be necessary to include the origin on the graph.

Data points should be clearly visible without eyestrain. Use standard symbols (e. g., open circles, open squares, or open triangles) to enclose the data points. Experimental error limits should be shown with an 'error bar' on each point when appropriate. Calculated data points are not given symbols, have no error, and are connected by a smooth curve or a straight line.
 

6) NOMENCLATURE. "The Merck Index" and "The ACS Style Guide" and other references provide help on nomenclature. Well-known symbols, acronyms, and formulas may be used (write out in title and abstract) if no ambiguity is likely. Define trade names and abbreviations/acronyms at the point of first use. The first letter of trade names is capitalized.

Use SI units of measurement (with acceptable exceptions) and give the dimensions for all terms. For numbers less than one, a zero precedes the decimal point (e.g., 0.5).
 

7) ORGANIZATION and GRADING. Submit the report in order shown below. Laboratory reports will be graded on the basis of 100 points.
 
a) Title Page (2 points)
b) Abstract Page (10 points)
c) Text
    1) Introduction (10 points)
    2)  Experimental (15 points)
         a)  Apparatus
         b)  Reagents
         c)  Procedure
    3)  Results and Discussions (35 points)
    4)  Conclusions (3 points)
    5)  Literature Cited (5 points)
    6)  Tables/Figures (20 points)
d) Answers to questions (Counted as Results and Discussion)
e) Carbon copies from laboratory notebook
 
Proofread the report carefully. One-half point will be deducted for every occurrence of a spelling error, missing exponent or symbol. Five points will be deducted for failure to number the pages consecutively in the upper-right corner or to staple the report pages together in the upper-left corner.
 

NO FOODS or BEVERAGES are permitted in the laboratory.

NO SMOKING or use of TOBACCO PRODUCTS permitted in the building.

NO CHEMICALS, SUPPLIES, or EQUIPMENT are to be removed from the laboratory.

SAFETY GOGGLES are required to be worn over the eyes while inside the laboratory.

SHOES which completely cover each foot are required (unless medically excused).

NO VISITORS (or pets) are allowed in the laboratory except by permission of an instructor. Visitation may be done in the hallway or outside the building.

NO UNAUTHORIZED experiments, including variations of those in the laboratory handouts, are allowed.

NO HORSEPLAY, TEASING, or HARRASSMENT of coworkers (or instructors) will be tolerated.

NO RADIOS or HEADSET DEVICES are allowed. Loud or boisterous behavior will not be tolerated.

Each worker is responsible for maintaining an orderly, clean laboratory. Immediately clean up all chemical spills, paper scraps, and glassware. Keep drawers or cabinets closed while working and the aisles free of any obstruction. Do not place book bags, athletic equipment, etc. on the floor near the lab bench.

Malfunctioning equipment is to be reported to an instructor.

Items broken or damaged and supplies depleted are to be written on the list by the door.

ABUSE of balances and equipment will not be tolerated.

RULE VIOLATIONS will lead to expulsion from the laboratory and a failing laboratory grade.
 

IT IS YOUR RESPONSIBILITY, NOT THE INSTRUCTOR'S, TO PLAY IT SAFE!

As in any laboratory work, certain precautions must be taken to avoid the potential for accidents to occur. The following section gives minimum guidelines for making the laboratory a safe place to work.

Safety goggles are required to be worn over the eyes at all times while inside the laboratory. Do not wear sunglasses to laboratory. Contact lenses are not advised.

Laboratory aprons or coats are encouraged to be worn to protect clothing.

Shoes which completely cover each foot are required. Shoes that shed liquids are best.

Always wash your hands before leaving the building. Toxic chemicals may be transferred to the mouth.

In case of accident or injury, even if it is minor, notify the instructor at once.

Chemical spills require immediate action. Whenever your skin comes into contact with chemicals wash it quickly and thoroughly with soap and warm water. Avoid rubbing the affected area before washing. In the event of spills over a large part of the body,
use the safety shower to flood the affected area. Remove all contaminated clothing if necessary.

It will be the duty and responsibility of each student to learn the location and operation of the laboratory safety equipment. This includes a fire extinguisher, safety shower, eyewash bottles, telephone, and emergency numbers.

Proper handling of chemicals and glassware will be expected. Instructors will be happy to demonstrate or describe acceptable technique when asked. Students are encouraged to alert fellow students and instructors of situations and/or instruments that appear to create a safety hazard.

Your cooperation in correcting unsafe practice is expected. Repeated violation of laboratory rules and safe practices (including proper technique) will lead to expulsion from the laboratory and a failing laboratory grade.