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Standard Operating Procedures Standard Operating Procedures Tolman Laboratory Tolman Group Standard Operating Procedures Standard Operating Procedures Tolman Laboratory v.7 updated May 2016 The intent of this manual is to inform you, the chemist, of the potential hazards that exist in the laboratory. This is by no means a manual to memorize or a manual of instruction. These procedures are not intended to be exhaustive or to serve as a single method of training. The procedures outlined here are meant as a refresher for those who have already received training by senior lab members. If in doubt of any procedure, please ask someone before carrying out said procedure. Asking for help when in doubt is the responsibility of every lab member. The first time you use all equipment and perform new experimental procedures, you should have someone work with you to teach you and to inform you of potential hazards, and to help prevent accidents. The purpose of this manual is to supplement personal one-on-one training with safety information that will protect you personally, as well as other lab members. It is important to make sure that you minimize your exposure to chemicals and decrease the chances of any accidents. By reviewing (and later referring to) this manual, you can be aware of the potential hazards in the lab and learn careful techniques. It is your responsibility to learn about safety and proper handling of chemicals from the resources available, including your laboratory members, other persons in the department, and the Chemical Hygiene Plan, which can be accessed via the web, from the Safety link on the Chemistry Webpage www.chem.umn.edu, or http://www.chem.umn.edu/services/safety/. This manual contains helpful links to safety procedures, Material Safety Data Sheets (MSDS), waste disposal, and much more. The general rule in our lab is that most glassware is shared, so please clean up after yourself. Make sure all glassware is clean using the appropriate solvents and procedures to clean it. Also, syringes should be washed after use, using a 5 solvent wash (usually tetrahydrofuran (THF), methanol, acid water, distilled water, and finally acetone). We generally store the syringes in the oven. Sign up for equipment (using the shared group Google Calendar) 1 Tolman Group Standard Operating Procedures TABLE OF CONTENTS I. Guidelines for Good Lab Citizenship in the Tolman Lab ................................................... 3 a. Office Etiquette ...................................................................................................................................... 3 b. Replace what you use ............................................................................................................................ 3 c. Glass and Equipment Repair ................................................................................................................. 4 d. Balance Etiquette .................................................................................................................................. 4 e. Cleaning Procedures: Base/Acid Baths ................................................................................................ 4 f. Glassware Drawers ................................................................................................................................ 5 g. Fume Hoods .......................................................................................................................................... 5 h. Oil Baths ................................................................................................................................................ 5 i. Notebook Page Format .......................................................................................................................... 5 j. Exit Checklist ......................................................................................................................................... 7 II. Tolman Group Responsibilities/Group Member Contact Information ............................. 8 III. Standard Operating Procedures (SOPs) for the Tolman Lab ............................................ 8 IV. Chemical Storage, Use, and Disposal .................................................................................... 8 a. Using the Chemical Inventory ............................................................................................................... 8 b. Storing and Labeling Chemicals ........................................................................................................... 9 c. Purchasing Chemicals ........................................................................................................................... 9 d. Standard Operating Cards (SOCs) ..................................................................................................... 10 e. Diamines .............................................................................................................................................. 11 f. Chemical hazards: Toxicity and peroxide forming chemicals ............................................................. 12 g. Techniques for handling pyrophoric liquids ....................................................................................... 13 h. Techniques for handling fuming/concentrated acids .......................................................................... 16 i. Techniques for handling elemental halides ......................................................................................... 17 j. Solvent health hazards ......................................................................................................................... 22 i. Choosing gloves ................................................................................................................................... 23 k. Scaling-up Reactions ........................................................................................................................... 24 l. Manifesting Chemical Waste ................................................................................................................ 30 m. Materials Safety Data Sheets (MSDS) ................................................................................................ 32 V. General Procedures .............................................................................................................. 32 a. Syringes and needles ........................................................................................................................... 32 b. Safety and sharps ................................................................................................................................ 32 c. Proper use of chemical fume hoods ..................................................................................................... 33 d. Gas tanks ............................................................................................................................................. 33 e. Dispensing liquid N2 tank .................................................................................................................... 34 f. Elemental Analysis ............................................................................................................................... 34 VI. Airfree Procedures ................................................................................................................ 34 a. Oil Baths .............................................................................................................................................. 34 b. Safety and high pressure reaction flasks ............................................................................................. 35 c. Vacuum Oven and Vacuum line procedures ....................................................................................... 35 d. Vacuum Pump Maintenance ................................................................................................................ 37 e. General Schlenk line manipulation review .......................................................................................... 38 f. Vacuum transfer of solvents using Schlenk line ................................................................................... 40 g. Solvent purification system (SPS) ....................................................................................................... 41 VII. Equipment ........................................................................................................................... 41 a. Comments that apply to all equipment ................................................................................................ 41 2 Tolman Group Standard Operating Procedures b. Dryboxes .............................................................................................................................................. 42 c. UV-vis and cryostat ............................................................................................................................. 50 d. FT-IR ................................................................................................................................................... 52 e. GC-MS ................................................................................................................................................. 53 f. React-IR ................................................................................................................................................ 53 g. Electrochemistry .................................................................................................................................
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