CHEMISTRY 457/557

PHYSICAL CHEMISTRY LABORATORY I

WINTER 2012

INSTRUCTOR: David A Grossie, 202D Oelman, 775-2210, david.grossie@wright.edu OFFICE HOURS: I will be in the P-Chem laboratory (074 BL) during most of the lab section meeting times or next door in 072 BL. In addition to these hours, I also will be available during posted office hours. I encourage you to use these times, but I will meet with students at other times by appointment. TEXT: "Experiments in Physical Chemistry" by Shoemaker, Garland, & Nibler (McGraw-Hill). OBJECTIVES: The purpose of this course is to provide students opportunities to observe, in practice, some of the principles treated in the physical chemistry lecture course. Students will gain "hands on" experience with experimental equipment and learn methods of data analysis and reporting. They will be expected to learn to use the software available in the P-Chem computer lab for data analysis and presentation. Recitations are scheduled to provide regular opportunities for RECITATIONS: quizzes and for discussion of specific experiments or other general topics of experimental physical chemistry. EXPERIMENTS: Each student must complete four of the experiments that are set up in the laboratory and a series of five computer-based exercises. Successful completion of this course requires the preparation, performance, and reporting of all five of these experiments. The scheduled list of experiments will be provided as a separate handout. In order to use the four-hour laboratory periods efficiently you should visit the laboratory before your scheduled meeting to acquaint yourself with the apparatus. Students may be requested by the instructor to demonstrate sufficient preparation for and knowledge of the intended experiment before being allowed to work in the lab. Consequently, it is the student's responsibility to prepare adequately before the lab meeting and to ask questions when necessary. Lost time in the lab and poor data because of insufficient preparation will be reflected in the course grade. Be advised that for some experiments it may be helpful to make up solutions in advance; however, you must obtain permission to work outside of scheduled meeting times. The laboratory experiments will be carried out in 074 BL as scheduled. Students may not do experimental work in the laboratory without the supervision of the course instructor or a teaching assistant. We have only limited apparatus for each experiment, requiring students will work in groups of two to perform the experiments. Data analysis and the writing the laboratory reports are to be individual efforts by each student. Expect to spend the full four hours in the lab collecting data and doing a sufficient amount of analysis, before leaving the lab, to be sure that your results are meaningful. Many students who try to breeze through in order to leave lab early do so with worthless data. Students are required to present preliminary data analysis to the teaching assistant and to obtain his or her initials or stamp on the lab notebook pages.

LABORATORY NOTES: Laboratory notes have been prepared for each experiment. These help to emphasize particular points and to modify the experimental description in the text for our operation at WSU. The laboratory notes are frequently updated, and some mistakes may have been made in this process. If you discover some probable mistakes as you prepare for a laboratory experiment, please notify the instructor or your graduate teaching assistant so that the mistake can be verified and the class be made aware of any corrections. Watch for such announcements on the doors of and bulletin boards near 074 BL. When in doubt, ASK! COMPUTERS: Personal computers will be used in the physical chemistry laboratory to acquire and analyze data in one or more experiments. Additional personal computers will be available in the computer room adjacent to the laboratory for data analysis. They also may be used to prepare laboratory reports via word processing software. The computers in 072 BL are available to CHM 457 students at any time, except during other sections of this course. The computers are on the campus network. All students must login to the campus network using their Novell username and password, and on the local computer using Chemistry as the username (leaving the password blank) in order to use these computers. LABORATORY REPORTS: The preparation of a laboratory report is as important as performing the experiment itself. Whether in graduate school or in the "real" world of industrial research and testing, the written report often is your only tool to explain your experimental method, the results, and the data analysis. You will be judged by your colleagues and/or supervisors by your ability to communicate orally and through written reports. It is a real challenge to be complete and yet concise as one writes a report, and it is unlikely that most students have been required to write such a report in undergraduate labs up to this point. It is wise to begin your writing early and to be critical and objective in editing your own report. All reports should contain the following sections: 1. Title Page and Abstract 3. Experimental Method 5. Sample Calculations 2. Introduction 4. Results & Discussion 6. References

There may be rare occasions when an appendix is helpful, but do not include raw data. ALL LABORATORY REPORTS ARE TO BE WORD PROCESSED. THEY ARE DUE TWO WEEKS AFTER THE DATE OF THE EXPERIMENT, BY THE END OF THE LABORATORY PERIOD. Grades for late reports will be discounted by 10% per day (not including weekends), from the date due Reports not submitted by the beginning of the laboratory period two weeks after the experiment report due date will be assigned a grade of zero, and no reports will be accepted after 5 pm Tuesday, March 13. Lab reports will be submitted electronically as described on the last page of the syllabus. Remember that although the experiments may be performed as a team, data analysis and reports are to be the work of the individual student.

LABORATORY NOTEBOOK: A laboratory notebook must be used for recording allimportant information in the laboratory. You must request the TA's acknowledgment of your notebook at the end of each laboratory period as indicated above, and the notebooks may be required at any time for grading. Follow the procedures outlined in the text for using the notebooks. Resist the temptation to write down data on the backs of envelopes, paper towels, etc. Record all your data and observations directly in your notebook. Data should be recorded in ink. GRADING: The course grade, based upon a possible total of 500 points is to be calculated as follows: Quizzes Performance evaluation Other assignments Four laboratory reports (50 pts each) Final exam 75 points 25 points 100 points 200 points 100 points

The final exam will be given per the schedule of classes at the time provided for "common chemistry lab final." It is expected that grades will be assigned according to the following performance levels. >90% = A 80-89% = B 70-79% = C 60-69% = D <60% = F

READ the safety notes of the experimental physical chemistry textbook by SAFETY: Shoemaker, Garland, and Nibler-pages 6, 739-745. These rules are to be followed during your enrollment in CHM 457/557. Consider possible safety hazards and read the "Safety Considerations" section in your text as you prepare for each laboratory experiment. Students who may be pregnant should obtain permission from their physician to enroll in this course. Students are expected to conduct experiments with consideration of all safety precautions for themselves and for their colleagues. Unsafe actions may result in the removal of a student from the laboratory with a grade of zero assigned for that experiment. Extreme cases may result in removal of the student from the course. Safety glasses are required for this course. Safety is everyone's concern! Potential hazards should be reported to the instructor immediately for evaluation. Let's all get through the quarter safely.

Physical Chemistry Laboratory

Computer-based Exercises
Word Assignment This exercise is intended to familiarize the student with the use of Microsoft Word in the writing and formatting of reports in Chemistry Excel Assignment This exercise is intended to familiarize the student with the use of Microsoft Excel for the analysis of chemical data. ChemDraw Assignment This exercise is intended to familiarize the student with the use of ChemDraw, a molecular drawing program. ChemDraw allows one to draw molecules of any size for inclusion into a Word document or Excel spreadsheet. A tutorial is available and recommended. SigmaPlot Assignment This exercise is intended to familiarize the student with the use of SigmaPlot for the analysis of chemical data. A tutorial is available and recommended. Origin Assignment This exercise is intended to familiarize the student with the use of Origin for the analysis of chemical data. A tutorial is available and recommended.

Laboratory Experiments
pKa of a Weak Acid (handout) Inversion of Sucrose (Shoemaker, page 264, with modifications) Solution Calorimetry (Reference: Shoemaker, page 145) Vapor Pressure of a Pure Liquid (Shoemaker, page 199, with modifications) Joule-Thompson Effect (Shoemaker, page 97) X-ray Diffraction (Shoemaker, page 480, with modifications)

Turning in lab reports

1 Convert the document to the Acrobat Reader (pdf) format, naming the file as follows: experiment-LastFirst.pdf Experiment in the file name is specific to the experiment you are reporting. pKa of a weak acid Solution Calorimetry Vapor Pressure of a Pure Liquid Joule-Thomson Effect Inversion of Sucrose X-ray Diffraction PKA SC VP JT IS XRD

2. Browse to the class web page, http://www.chm.wright.edu/grossie/chm457 3. Click on the link, Upload Lab Report. 4. Enter pchem as the username. 5. Enter pchem as the password. 6. Click on the browse button and select the location of your lab report. 7. Click on upload.