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Chemistry Laboratory Techniques >> Content Detail



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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.

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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)

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

The Laboratory Introduction (PDF) document reviews safety guidelines as well as check in and check out procedures for the course.

Introductory Reading Assignment
Technique Modules
Original Research Project
Technique Guides
Handouts


Introductory Reading Assignment

Before we get started in the lab, 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. This text was selected because it's 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. A copy of this text will be available in the Reserve Book Room of the Science library. 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. Tabacco and your TAs will facilitate a discussion of the assigned reading and the actual lab experiment. You will also view relevant portions of The Digital Lab Techniques Manual to give you a visual representation of the important techniques. 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. 6th ed.
(
Chapters 1- Safety; 2- Notebooks; 4- Jointware; 6- Interesting Equipment; 9- Clean and Dry; 10- Drying Agents; 11- On Products; 15- Extraction and Washing; 18- Heat; 19- Clamps; 31- Instrumentation in the Lab)

Leonard, Lygo, and Procter. Advanced Practical Organic Chemistry. 2nd ed.
(Chapters 1- Introduction; 2- Safety; 3- Keeping Records; 4- Equipping the Lab; 8- Vacuum Pumps)


Technique Modules

Sections 2–6 cover technique modules that make up the bulk of the class. The five topics included here are "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 sections 2-6 is the techniques checklist. Each section 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.

These files are also available for download from iTunes®.

 

LAB MANUAL SECTION #TOPICSREADINGSVIDEOS
2Transfer and Extraction Techniques
  • CC: Ethyl Ester's Excellent Adventure (PDF)
  • EE: Into Thin Air (PDF)

Extraction: Zubrick Ch. 15, LLP Ch. 10

Theory of Extraction: Zubrick Ch. 37

Melting Point Determination: Zubrick pp. 87-92

NMR Theory and Operation: Zubrick Ch. 35, LLP Ch. 15.2

Additional EE Module Reading:
  • Air Sensitive Techniques: LLP Ch. 9
Digital Lab Techniques Manual:
3Purification of Solids by Recrystallization
  • CC: How do you Recrystallize a Mothball? (PDF)
  • EE: The Single-Crystal Shakedown (PDF)

Theory of Recrystallization: Zubrick Ch. 13, LLP Ch. 11.2

Digital Lab Techniques Manual:
4Purification of Liquids by Distillation
  • CC: How did the Peach Get in the Banana? (PDF)
  • EE: What’s with Those High-Altitude Recipes? (PDF)

Theory of Distillation: Zubrick Ch. 36, LLP Ch. 11.3

Distillation Glassware and How to Set it Up: Zubrick Ch. 20

Use of the GC: Zubrick Ch. 32

5Purification by Flash Column Chromatography
  • CC: Looks can be Deceiving (PDF)
  • EE: Setting the Pace (PDF)

Theory of Column Chromatography: Zubrick Ch. 27

TLC - Polarity/Solvent Systems: Zubrick Ch. 28, LLP Ch. 9.3.1

Setting up a Silica Gel Column: Zubrick Ch. 29, LLP Ch. 11.6

Applying Crude Mixtures to the Column

Running a Flash Column

Digital Lab Techniques Manual
6Protein Assays and Error Analysis
  • CC: What's in a Cow's Heart Anyway? (PDF)
  • EE: A Heart as Strong as Iron (PDF)


Original Research Project (PDF)

Found in section seven of the Lab Manual, this brief set of experiments will introduce you to some of the realities and excitement of performing original research.


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.

LAB MANUAL SECTION #TOPICS
8.1FT-NMR Sample Preparation Guide (PDF)
8.2GC Sample Preparation Guide (PDF)
8.3Thin Layer Chromatography (TLC) Guide (PDF)
8.4Extraction and Washing Guide (PDF)
8.5No-Air Techniques Guide (PDF)
8.6Two-Solvent Recrystallization Guide (PDF)
8.7Guide to Growing a Single Crystal (PDF)
8.8Distillation Guide (PDF)
8.9Flash Column Chromatography Guide (PDF)


Handouts

Introduction to Spectroscopic Techniques (PDF)

The Digital Lab Techniques Manual (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, and Sarah A. Tabacco.


 








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