Chem 347 Fall 2010

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Chem 347 Fall 2010Prof. Rob Ronald. Texts for the course:. Required text: Pavia, Lampman, and Kris, Introduction to Spectroscopy, 4th Ed., Brooks/Cole, 2008. The 3rd Ed. would be acceptable to use.Optional recommended text: Shriner, Hermann, Morrill, Curtin, and Fuson, The Systematic Identifi

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Chem 347 Fall 2010

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1. Chem 347 Fall 2010 Prof. Rob Ronald Chem 347 Fall 2010 The course is an introduction to organic spectroscopy, and includes both lectures and laboratory experience. The course is structured to give you both theoretical and practical experience in the isolation, purification, and identification of organic compounds. This will be accomplished through lectures on spectroscopic techniques, followed by practical laboratory experience involving: purification techniques; reactions and their workup; and the separation and identification of unknowns.

2. Chem 347 Fall 2010 Prof. Rob Ronald Texts for the course: Required text: Pavia, Lampman, and Kris, Introduction to Spectroscopy, 4th Ed., Brooks/Cole, 2008. The 3rd Ed. would be acceptable to use. Optional recommended text: Shriner, Hermann, Morrill, Curtin, and Fuson, The Systematic Identification of Organic Compounds, 8th Ed., Wiley, 2004 (An older edition such as the 6th or 7th would do as well). Optional reference text for the serious chemistry student: Silverstein and Webster (Formerly Silverstein and Basler and Morrill), Spectrometric Identification of Organic Compounds, 6th Ed. Wiley, 1998 (the 5th edition would do just as well, even better because it still has a chapter on UV spectroscopy). Other reference text for the serious chemistry student: Williams and Fleming, Spectroscopic Methods in Organic Chemistry, 5th Ed. McGraw-Hill, 1995

3. Chem 347 Fall 2010 Prof. Rob Ronald Course Format for Chem 347 Fall 2010 The course will consist of lectures on spectroscopy and separations methodology interspersed with some laboratory work until we begin work on the unknown mixture, which should occur about the week of Oct 11, 2010. There will be a mid-term examination and a final examination. There will be graded homework assignments. The laboratory will consist of experiments to give you experience with some basic organic techniques, and it will also include of a multi-component unknown for you to separate, purify, and identify. Written reports on your laboratory work will be required. You will be given instructions as to the size and format for each report.

4. Chem 347 Fall 2010 Prof. Rob Ronald Grading Mid-term examination (in class) 10% Final examination (in class) 15% Graded homework 15% Laboratory reports 50% Performance evaluation 10% Total 100% The laboratory reports grade will be a composite of: your experimental work on the distillation (5%); your preparation of 9-fluorenone (10%); and your unknowns (35%). The grade for the unknowns requires that you separate, purify, and correctly identify the components of the unknown mixture, and if needed prepare appropriate derivatives. Your laboratory reports will consist of describing only the positive results of your experimental work (at this level we are not interested in your creative error analysis). You can use this write-up as part of the writing requirement for graduation. The performance evaluation will be based upon your laboratory performance and will be made by me and the TA’s.

5. Chem 347 Fall 2010 Prof. Rob Ronald Grades in this course will be earned based upon your performance on examinations, homework, and laboratory work – i.e. positive results in the laboratory. Grading scale: A, 90% and above; B, 89-75%; C, 74-65%; below 64% not a passing grade. This is a serious upper level course for chemistry and biochemistry majors, and it is assumed that you will put forth a significant effort to excel in the course.

6. Chem 347 Fall 2010 Prof. Rob Ronald Teaching Staff for Chem 347 Rob Ronald, Professor, phone: 335-3364, email: [email protected] Teaching Assistants: Tyler Biggs: [email protected] Jia Pan: [email protected] Jackie Zhu: [email protected]

7. Chem 347 Fall 2010 Prof. Rob Ronald Students with Disabilities: Reasonable accommodations are available for students with a documented disability. If you have a disability and may need accommodations to fully participate in this class, please visit the Disability Resource Center (DRC). All accommodations MUST be approved through the DRC (Admin Annex Bldg, Room 205). Please stop by or call 509-335-3417 to make an appointment with a disability specialist. If you have questions, please contact Rosie Pavlov at [email protected] or 335-3417.

8. Chem 347 Fall 2010 Prof. Rob Ronald NOTEBOOKS AND RECORD KEEPING You must keep all of your laboratory records in a hardbound notebook, or in a laptop computer. You must keep all the paper copies of your spectra in a three-ring binder. Do not keep your data on loose pieces of paper. You will be given one warning if you are using any means other than a hardbound book or laptop to record data: if you persist you can be penalized 10% of your grade for each infraction! Make copies of your spectra for your structural analysis work, and preserve one clean copy (original) to turn in with your final report – these spectra should be annotated with spectral assignments.

9. Chem 347 Fall 2010 Prof. Rob Ronald The writing style you should employ for your laboratory notebook is the accepted scientific style: third person past tense, passive voice (the compound was treated with… – not I treated the compound with…). You should date each page of your notebook, or each day of work in the laboratory. You should take copious notes marking down all of your observations. Try to develop the sense of watching yourself do the experiments. Write your notebook in a manner such that another person could repeat exactly what you did by following what you wrote.

10. Chem 347 Fall 2010 Prof. Rob Ronald You should develop a code system for keeping track of every experiment you do, and every sample you produce. For an electronic notebook this code system should include: (1) Your name, initials, or some identifying symbol unique to you; i.e. RR (2) The computer folder/file where you have the record for the sample; i.e. RR2dRi1e (in this case the 2dRi refers to a folder in my electronic notebook, and 1e refers to a particular experiment) (3) A number or letter that will clearly identify which of the compounds on the page refers to a particular sample number; i.e. RR2dRi1e-1, RR2dRi1e-2, RR2dRi1e-3, etc (the numbers refer to the first, second, and third samples produced in experiment 2dRi1e. Avoid using characters like commas that are not compatible with computer filenames – this avoids confusion later.

11. Chem 347 Fall 2010 Prof. Rob Ronald If you are using a hardbound notebook the codenames might take the following form: RRI-23-a (date). 1) RRI refers to the notebook number (in this case the I refers to the first notebook, the second notebook would be RRII) 2) 23 is the page number in RRI 3) a is the sample, the next sample produced on page 23 would be b (RRI-23-b), etc. 4) (date) this is good to include the date the work was done – work on page 23 might occur over more than one day.

12. Chem 347 Fall 2010 Prof. Rob Ronald Bring a magic marker to the laboratory with you so that you can label each flask and/or test tube with this code number so that later you can identify the contents. Have your samples clearly labeled with your codes before you attempt to obtain spectra or other data. Spectra obtained should be labeled with the identifying code number of the sample for which the spectrum was obtained.

13. Chem 347 Fall 2010 Prof. Rob Ronald Some suggestions for keeping your notebook Before you come to the lab write a short paragraph describing the purpose and/or rationale for what you are planning to do. If you are going to be doing a series of tests prepare a table in advance. If you are going to be doing a synthetic reaction prepare a ChemDraw reaction scheme, and an Excel spreadsheet with all of the pertinent calculations. Remember: No loose pieces of paper; no spiral binders, no ring binders, except for your spectra.

14. Chem 347 Fall 2010 Prof. Rob Ronald LAB ETIQUETTE and SAFETY Safety Glasses. You must wear safety glasses or goggles at all times when you are in the laboratory. I suggest that you invest in some comfortable safety glasses that you won’t feel like taking off every five minutes. It is not a good idea to wear contact lenses in a chemical laboratory even though your vanity makes you want to. If you insist on not using safety glasses we may have to dis-enroll you from the course. Gloves. “Chemically Resistant” disposable gloves are provided to all students. Be aware that the protection offered by gloves is only temporary. If you have a serious spill you should wash the gloves, and then remove and dispose of them properly. Be sure to wash your hands with copious amounts of water before putting on a fresh pair of gloves. GLOVES CAN AND DO LEAK! Health Problems. Please let me know (privately) if you have health issues that might affect you in the lab so that if a problem arises we will have a plan in place.

15. Chem 347 Fall 2010 Prof. Rob Ronald Spills and accidents If you spill chemicals on yourself immediately rinse the affected area with copious amounts of water. Call for help if it is a large spill, or if you are unsure of what to do. If you get chemicals in your eyes immediately wash with water in the eyewash fountains for at least 15 minutes. Clean up after yourself if you spill, especially when using the balances. You know what you spilled; the next person has to assume that it is a very hazardous material to be on the safe side. Do not contaminate the community solvent and reagent bottles; if you make a mistake don’t pour it back – put it in the waste. If you accidentally contaminate a solvent or reagent bottle, be responsible: take the contaminated bottle to the stockroom for disposal and get a fresh one. Consider that you might be the victim of a mix-up and it could ruin your work, so be considerate of others.

16. Chem 347 Fall 2010 Prof. Rob Ronald Clothing. Many students wear lab coats; these are available for purchase through the chemistry club. Long pants and long sleeved shirts are recommended for working in the laboratory; please do not come to lab wearing shorts. Even if you are using a lab coat you need to have long pants. Be advised that many synthetic fibers are soluble in organic solvents. Wear natural fibers or at least natural fiber blends. Cotton reacts with acid spills and you might find that holes develop after you wash your cotton lab clothing. Wool is the most resistant. Shoes. Open toed shoes and sandals (flip-flops) are not suitable for laboratory use. You will be asked to change into appropriate footware should you show up for lab wearing inappropriate foot protection.

17. Chem 347 Fall 2010 Prof. Rob Ronald Radios, Cell Phones. There will be no radios or recorded music in the lab. Leave your Walkmen, iPods, Gameplayers, etc. in your bag or at home. Some cell phones have been known to set off explosions when they ring in the presence of flammable vapors so keep your cell phones turned off in the lab. If you need to make or receive a call step out of the lab to use them. Also turn off your cell phones during lectures, and especially during examinations – failure to do so may result in a failing grade.

18. Chem 347 Fall 2010 Prof. Rob Ronald Rotary Evaporators. We have only two rotary evaporators available for Chem 347. Rinse the distilling traps with acetone after you are finished and empty the collecting flask into the solvent waste disposal. If you are distilling aqueous solutions, then distill a little acetone to remove the water from the condenser after you finish. Do not grease the ground glass joints unless you are prepared to clean them off with ether (Et2O)or dichloromethane (CH2Cl2) when you are finished. Use plastic Keck clamps to secure the flask. Use only round-bottomed flasks on the rotary evaporators; flat-bottomed flasks can implode due to the pressure differential with disastrous results for you and those around you. When using the rotary evaporators it is a good idea to tare your clean and dry round-bottomed flask before you put your sample solution in to be concentrated. That way a simple weighing will let you know how much stuff is in your flask.

19. Chem 347 Fall 2010 Prof. Rob Ronald General Use your time in the laboratory efficiently. Do lots of preparatory work at home before you come to lab so that you know what it is you are going to try to accomplish each lab period. Plan ahead by cleaning the glassware you will need for the next lab period to have it ready when you come in to work. If you do you will accomplish more and have more fun. Do discuss your experimental work with others in the class to get ideas of how to proceed. Talk to me and to the TA’s about what you are doing. Don’t be afraid to ask for help and advice. You are always welcome to come by my office, but bring all of your data when you come so we can discuss the all the aspects of your problem. Remember always that we are trying to teach you a process: if you learn the process it will generate the correct answers, but always keep focusing on the process.

20. Chem 347 Fall 2010 Prof. Rob Ronald We will start our studies of various spectroscopic methods with Mass Spectrometry (MS) Read and Study Chapter 1 in Pavia, Lampman, and Kris. The material in this chapter will be very useful for you when you get your unknowns. Work the problems at the end of Chapter 1 Begin reading Chapter 8 in Pavia, Lampmann and Kris.

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