Chemistry Laboratory Techniques

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Chemistry Laboratory Techniques

Massachusetts Institute of Technology Department of Chemistry
Chemistry Laboratory Techniques
Laboratory Manual

Prepared by Katherine J. Franz and Kevin M. Shea with the assistance of Professors Rick L. Danheiser and Timothy M. Swager Revised by J. Haseltine, Kevin M. Shea, and Sarah A. Tabacco

Link: http://ocw.mit.edu/NR/rdonlyres/Chemistry/5-301January--IAP-2004/C563B6CA-261A-4BA6-894D-24EA9A1C65A8/0/complete_manual_2004_ac.pdf

Table of Contents
1. Introduction
1.1. Overview 3
1.2. The Texts 4
1.3. Introductory Reading 5
1.4. Grading 6
1.5. Calendar 7
1.6. How to Use This Manual 8
1.7. Introduction to the Laboratory 9

2. Transfer and Extraction Techniques
2.1. CC: Ethyl Ester's Excellent Adventure 14
2.2. EE: Acid, Base, and in Between 17

3. Purification of Solids by Recrystallization
3.1. CC: How do you Recrystallize a Mothball? 19
3.2. EE: The Single-Crystal Shakedown 21

4. Purification of Liquids by Distillation
4.1. CC: How Did the Peach Get in the Banana? 24
4.2. EE: What’s With Those High-Altitude Recipes? 26

5. Purification by Flash Column Chromatography
5.1. CC: Looks Can Be Deceiving 28
5.2. EE: Setting the Pace 30

6. Protein Assays and Error Analysis
6.1. CC: What’s in a Cow’s Heart Anyway? 32
6.2. EE: A Heart as Strong as Iron 35

7. Introduction to Original Research
7.1. Olefin Epoxidation with Mn(salen) Complexes 37

8. Technique Guides
8.1. FT-NMR Sample Preparation 44
8.2. GC Sample Preparation 46
8.3. Thin Layer Chromatography (TLC) 47
8.4. Extraction and Washing 50
8.5. No-Air Techniques 53
8.6. Two-Solvent Recrystallization 55
8.7. Growing a Single Crystal 57
8.8. Distillation 59
8.9. Flash Column Chromatography 63

9. Instrument Operation Guides
9.1. NMR 68
9.2. IR 73
9.3. GC 74
9.4. UV-Vis 75