5.301 | January IAP 2012 | Undergraduate
Chemistry Laboratory Techniques

Labs

WARNING NOTICE

The experiments described in these materials are potentially hazardous and require a high level of safety training, special facilities and equipment, and supervision by appropriate individuals. You bear the sole responsibility, liability, and risk for the implementation of such safety procedures and measures. MIT shall have no responsibility, liability, or risk for the content or implementation of any of the material presented.

Legal Notice

This section includes course modules for mastering a series of chemistry laboratory techniques. Information on the original research project assignment and a listing of techniques guides are also provided. All materials may be found in the complete laboratory manual. (PDF - 2.4MB) (*Please note: for users on Mac machines experiencing problems viewing the images, downloading and saving the document should resolve this issue.) 

Video instruction tutorials from the Digital Lab Techniques Manual (DLTM) are recommended for some of the modules and are noted below.

Introductory Reading Assignment
Technique Modules
Technique Guides
Instrument Operation Guides

Introductory Reading Assignment

Before we get started in the lab on our first class meeting, there are several chapters in the text that you must read first. Our time in the lab will be intense, but of limited duration, so it is important that you complete the readings on time. Not only is the reading essential to your success in 5.301, but it also will help in your development as an experimental chemist.

So, before you begin your experiments, take some time to read over the following chapters in Zubrick & Mohrig. These texts were selected because they’re easy to read and very practical. For more in-depth reading on these and related topics, we recommend the listed selections in the text by Leonard, Lygo, and Procter. It is often difficult to fully grasp a laboratory concept by simply reading about it, but using the strategy of introductory reading, practicing in the lab, and post-lab review reading you will retain most of what we will cover in 5.301.

At the beginning of each lab period, there will be a short overview of that day’s topic, where Dr. Dolhun and your TA will facilitate a discussion of the assigned reading and the actual lab experiment. Much of this time will be set aside to answer questions that you have from the readings.

The following list is the bulk of the reading for the course. There will also be additional reading during IAP, but this introductory reading is meant to familiarize you with the typical chemistry laboratory.

Zubrick, James. The Organic Chem Lab Survival Manual: A Student’s Guide to Techniques. 8th ed. Wiley, 2010. ISBN: 9780470494370.
(Chapters 1 - Safety, 2 - Notebooks, 4 - Jointware, 6 - Interesting Equipment, 9 - Clean and Dry, 10 - Drying Agents, 11 - On Products, 15 - Extraction and Washing, 17 - Heat, 18 - Clamps, 27 – TLC, 28 - Column Chromatography, 30 - Gas Chromatography, 32 - Infrared Spectroscopy, 33 – Nuclear Magnetic Resonance 34 - Distillation)

Leonard, J., B. Lygo, and G. Procter. Advanced Practical Organic Chemistry. 2nd ed. CRC Press, 1994. ISBN: 9780748740710.
(1 - Introduction, 2 - Safety, 3 - Keeping Records, 4 - Equipping the Lab, 8 - Vacuum Pumps)

Mohrig, J.R., C. Noring Hammond, and Paul F. Schatz. Techniques in Organic Chemistry: Miniscale, Standard Taper Microscale, and Williamson Microscale. 3rd ed. W.H. Freeman, 2010. ISBN: 9781429219563.

(Part 1: Basic Techniques: Chapters 1 thru 16 pages 1-197 Part 3: Spectroscopic Methods: Chapters 20-24 pages 275-438.)

Technique Modules

The technique modules make up the bulk of the class. The modules fall under the topics of “Transfer and Extraction,” “Purification by Crystallization,” “Purification by Distillation,” “Purification by Flash Column Chromatography,” and “Protein Assays and Error Analysis.” It is important to note that the manual does not contain all of the information that you will need to complete these experiments. Some important information will be found in your pre-lab reading, while the rest will be covered during the pre-lab discussion. This three-pronged approach (the texts, the manual, and the discussions) will prepare you to tackle the experiments outlined in the technique modules.

An important part of the modules is the techniques checklist. Each module begins with a list of techniques that you will encounter during the experiment. When you have completed a technique module, you should return to the techniques checklist and check off all of the techniques that you have mastered. If you are still uncomfortable with a specific skill then you should practice it until you feel confident that you could apply it in a different experiment. In addition to various purification and manipulation techniques, this section will also introduce you to spectroscopic techniques like nuclear magnetic resonance (NMR) spectroscopy, infrared (IR) spectroscopy, gas chromatography (GC), and ultraviolet-visible (UV-Vis) spectroscopy.

Note:

“CC” refers to the “Competent Chemist” modules.
“EE” refers to the “Expert Experimentalist” modules.

Transfer and Manipulation (CC)

Acids, Bases & In Between (EE)

Recrystallization—Mothball (CC), and Single Crystal (EE)

Distillation (CC, EE)

Column Chromatography (CC, EE)

Biochemistry (CC, EE)

Original Research Project

Technique Guides

Found in section eight of the Lab Manual, these guides will provide you with step-by-step instructions for some of the more common techniques encountered in a chemistry laboratory.

TOPICS FILES
NMR Sample Preparation (PDF)
GC Sample Preparation (PDF)
Thin Layer Chromatography Guide (PDF)
Extraction and Washing Guide (PDF)
No Air Technique Guide (PDF)
Two-Solvent Recrystallization Guide (PDF)
Guide to Growing a Single Crystal (PDF)
Distillation Guide (PDF)
Flash Column Chromatography (PDF)

Instrument Operation Guides

These guides will provide you with step-by-step instructions for some of the instruments commonly encountered in a chemistry laboratory.

INSTRUMENT FILES
NMR (PDF - 1.3MB)
IR Guide (PDF)
Refractometer (PDF)
UV (PDF)
Mass Spectrometer (PDF)
GC (PDF)

Acknowledgements

The laboratory manual and materials for this course were prepared by Katherine J. Franz and Kevin M. Shea with the assistance of Professors Rick L. Danheiser and, and Timothy M. Swager. Materials have been revised by J. Haseltine, Kevin M.Shea, Dr. Sarah A. Tabacco, Dr. Kimberly L. Berkowski, Anne M. (Gorham) Rachupka, and Dr. John J. Dolhun.

Course Info
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January IAP 2012
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theaters Demonstration Videos
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