Chemistry 303

Fall, 2008

Dr. Jay Hanna Dr. Aaron Hartel

Email: hannaj@winthrop.edu hartela@winthrop.edu

Phone: 323-4933 323-4942

Office: 301B Sims 314B Sims

Office Hours: R 12:00 – 2:00 TWR 1:00 – 2:00

Text: Anne B. Padías, Making the Connections: A How-To Guide for Organic Chemistry Lab Techniques.

Notebook: The Jones and Bartlett laboratory notebook.

You will need the following for lab this semester:

· Laboratory text

· Laboratory notebook

· Approved Safety Glasses

Objectives:

The major objectives of this course are to:

1) Introduce you to more advanced laboratory techniques and instrumentation

2) Develop your skills in proper scientific record keeping and technical writing

3) Help you to better understand some of the topics covered in CHEM 301

Laboratory Text and Handouts:

The lab text is a valuable source of information on the techniques used in organic chemistry. The experimental procedures used are in the form of handouts and are posted on the course webpage (accessible from chem.winthrop.edu.)

Laboratory Notebook:

The lab notebook is where you record your procedures and observations. Proper experimental record keeping is very important in any research field.

Approved Safety Glasses:

Each student must purchase an approved pair of safety glasses, available at the bookstore. Only approved safety glasses are acceptable. You will not be permitted to check-in to lab if you do not have an approved pair of safety glasses.

Experiments:

Each week you should report to the assigned pre-lab room for a briefing on that week’s experiment. Experiments should be performed individually unless instructed otherwise.

Pre-lab Quizzes:

Each week there will be a brief quiz before the lab briefing. The quizzes will be based on information used to prepare the Prelab section of your report.

Lab Station:

Each student will be assigned a lab station to be used during the semester. It is your responsibility to leave your area clean and organized for the next lab section. Failure to do so will result in a 5-point penalty on your subsequent lab report.

Lab Reports:

Complete lab reports (Pre-lab, In-lab and Post-lab) for CHEM 303 are due at the beginning of the following week's lab meeting and will be returned to you the week after they are submitted. A 5 point per day penalty will be assessed on reports turned in late. A guideline for writing lab reports is attached to this syllabus. Each report MUST be submitted with a cover sheet which is available from the CHEM 303 web page (accessible from chem.winthrop.edu). Each student must submit an individual report.

Absences:

In order for an absence to be excused appropriate documentation must be presented to your instructor. Any missed experiments will be counted as a zero unless made up. Experiments may only be made up with permission from your instructor. Any report due on the day of absence must be turned before your next scheduled lab period.

Withdrawing from lab:

In order to drop CHEM 303, you must also drop CHEM 301.

Grading: Each Laboratory Report is worth 100 pts. Your final course grade is based on your average score on the Laboratory Reports according to the scale below. The +/- system will be used for “A”, “B” and “C” grades. Roughly, a “+” will be awarded to scores in the top third of each grade range and a “-“ to those in the lower third. Typically, the grading scale has been the following:

A = 90 – 100%

B = 80 – 89.99%

C = 70 – 79.99%

D = 60 – 69.99%

F= < 60%.

General Lab Order:

- Only dispose of waste in containers labeled for waste collection Do not put any chemical waste in the trash, down the drain or in any container not labeled as waste.

- Replace lids on all containers immediately after use. Open containers increase everyone's exposure to the substances within them. Spills are also more likely when a container is open. Some reagents can also be ruined by excessive exposure to air.

- Clean your glassware after each experiment.

- Clean up any spills you create. If you don’t know how a spill should be cleaned up, ask.

- Put things back where you found them (equipment and anything non-disposable).

- Dispose of broken glass, used pipets and capillaries in the white broken glass containers.

- Make sure you lock your lab drawer at the end of each experiment

Lab Safety:

- SAFETY GLASSES ARE MANDATORY ANY TIME YOU ARE IN THE LAB. Even if you are simply recording data, safety glasses must be worn. If you are found not wearing safety glasses, you will be asked to leave and will receive a zero for the experiment.

- Wear sensible clothing. Shoes and shirts are required. Long hair needs to be pulled back. Sandals, open-toed shoes, and high heels, as well as shorts, short skirts, bare midriffs and backs are prohibited. It is best not to wear your good clothes into the lab, since spills are common.

- Eating, drinking and smoking are prohibited in the labs.

- Report any spills, cuts, burns or breakage of glassware immediately. Accidents happen and they will not affect your grade.

- Report any malfunctioning equipment (Mel Temps, hot plates, etc.).

- Particularly noxious substances should be handled in a fume hood. The constant draft of air prevents exposure to harmful fumes and vapors. Make certain the sash is lowered to a safe level, as shown on the side of the hood.

- A safety shower located in each laboratory. These are to be used in the event of a major spill of a hazardous chemical on yourself.

- Each laboratory has an eyewash station to be used if a chemical has come in contact with your eyes. Just place your face between the two fountains and press the lever to activate the water. Try to keep your eyes open as best you can, as this flushes them much more effectively.

- Disposable gloves can be found on the shelves of each laboratory. Wear gloves when dealing with any hazardous chemical. You may even want to wear gloves at all times in the laboratory. If you get a hazardous chemical on your gloves, take them off within a few minutes, wash your hands and put on a fresh pair. Gloves are not impervious; they simply prevent immediate exposure.

Guidelines for Writing Lab Reports for CHEM 303/304

Each lab report for this course must include a cover sheet (on the CHEM 303 webpage accessible from chem.winthrop.edu) and three sections: Prelab, Inlab, and Postlab. Each source used for information in the lab report must be appropriately cited. All structures (including those included in chemical equations) must be drawn by hand. Example reports are posted on the CHEM 303 webpage (accessible from chem.winthrop.edu). In addition, there are useful links posted on the CHEM 303 web page to assist in finding the information needed to complete the lab reports.

Prelab (40 points)

The Prelab section of the report must be completed before coming to lab, and will be checked by the instructor during the pre-lab briefing (the quiz will be given at the beginning of the lab meeting). The Prelab must include the cover sheet, if a cover sheet is not included with the pre-lab, you will not get credit for having the pre-lab. The pre-lab must contain:

Experiment Title and Introduction (15 points)

Provide a short title that clearly describes exactly what the experiment involves. Example:“The Synthesis of Ethoxybenzene by Williamson Ether Synthesis from Phenol and Iodoethane and its Analysis by ¹³C-NMR Spectroscopy” Write an explanation of the purpose, principles, and methods the experiment. Reaction and synthetic experiments should include balanced equations and mechanisms. Technique experiments should include diagrams of any newly introduced equipment and apparatus. Refer to the sample reports for guidance.

Table of Chemical Substances (10 points)

Create a table listing all chemical substances used with the role of the substance in the experiment and the appropriate chemical data. “Appropriate chemical data” depends on the role of the substance in the experiment and the type of experiment. The “appropriate chemical data” is summarized below:

Role	Information required for Technique Experiments	Information required for Synthesis Experiments
Reactant	Name, structure, formula, mol. wt., mp, bp, density	Name, structure, formula, mol. wt., mp, bp, density, amount used, moles used, mole ratio
Catalyst	Name, structure, formula, mol. wt., mp, bp, density	Name, structure, formula, mol. wt., mp, bp, density, amount used, moles used, mole ratio
Product	Name, structure, formula, mol. wt., mp, bp, density	Name, structure, formula, mol. wt., mp, bp, density
Solvent	Name, structure, formula, mp, bp, density	Name, structure, formula, mp, bp, density
Aqueous auxiliary (i. e. 10% NaOH, saturated NaHCO3)	Name, formula, concentration	Name, formula, concentration
Drying agents (i.e. sodium sulfate, calcium chloride)	Name, formula	Name, formula
Adsorbent (i.e. alumina, silica gel)	Name, formula	Name, formula
Other	Name, formula (if available)	Name, formula (if available)

Safety Information (5 points)

Create a table of the chemical substances used and indicate (by Yes or No) whether the substance is toxic, corrosive, flammable, or carcinogenic. If you are unsure, assume yes. For substances which are toxic, list the LC50 or LD50, if available. For substances which are flammable, list the flash point. List any precautions for potentially dangerous techniques.

Prelab Quiz (10 points)

To be given during the pre-lab briefing

Inlab (15 points)

The Inlab section is to be done in the laboratory and should be written directly into your lab notebook. If you do not write the Inlab portion directly into the required notebook, you will not get credit for this section. The Inlab should contain:

Procedure (10 points)

Write a step-by-step account of what you did in the experiment. It should be detailed enough so that the experiment could be repeated exactly as you did it, using only your procedure.

Data and Observations (5 points)

Record any data (masses, mp, bp, etc.) you measured, including units. Record any significant observations (color change, evolution of gas, precipitation, etc.).

Postlab (45 points)

The Postlab section should be done after the experiment itself is completed. The Postlab should contain:

Experimental (10 points)

Formally write up your procedure, data, and observations in a manner similar to that in an article from the Journal of Organic Chemistry – one that can be understood and repeated by someone in the field of organic chemistry. Include product mass and analytical data at the end of this section. Refer to the example reports for guidance.

Results and Discussion (15 points)

Thoroughly interpret your data and observations. Provide calculations (percent yields, etc.). Explain the significance and meaning of your data and observations. State what you can determine from them. Discuss any problems or sources of error and how they could be avoided or minimized. Refer to the example reports for guidance.

Conclusions (5 points)

Provide a brief summary of your findings. Was the experiment a success, especially relative to the statement of purpose?

Answers to Questions (15 points)

Answer any assigned questions.