Doing Good Research
It's much more than following a recipe!!
[By the way, I know you've heard this warning in organic teaching labs you've already been through. The big difference here is that, this time, WE REALLY MEAN IT!!! You're doing chemistry that has never been done before, sometimes via reactions whose outcome is questionable, and you cannot make decisions on what to do if the reaction misbehaves if you're just playing cook-for-a-day.]
The top section of your laboratory notebook (reaction, reference, reagents) must be filled out prior to beginning any lab work. This is not optional, not a matter of style, and not a negotiating point. Do not let me catch you running a reaction without the lab book entry already filled out, as described on the next page.
2. Set up your reaction equipment with great care, ensuring (when appropriate) tight connections, safety-wired rubber hoses, stability, dryness, etc.
3. Accurately measure all reagents, including solvents and catalysts. Discrepancies which may seem unimportant at the time can drastically alter the course of a reaction. When you're discovering new chemistry, it's impossible to tell beforehand what's important and what isn't!
the (hardbound) notebook format illustrated on the following page.
Before beginning experimentation, fill in the reaction you intend to
run (either use a template or draw very neatly), the literature
precedent, and all reagent quantities. Reagents should be listed by name,
followed by the density (if it's a liquid), mass (g or
mg), and mmoles.
5. Record the progress of your reaction meticulously, beginning with a description of your reaction setup. Note all observations - you can not assume any change (i.e., temperature, viscosity, color, gas evolution, stirring rate, etc., etc.) to be unimportant! If any environmental variables are unusual (cold or hot in the lab, extra-high humidity, etc.), note that too.
6. Describe workup/purification conditions in detail - they are important!
7. When you isolate a compound in crude (impure) form, record its physical characteristics, weight, and usually at least one spectral or chromatographic measurement. How complete your analysis should be depends on the compound's purity (this just makes sense - why do lots of analysis on impure stuff?). The following table outlines some of these differences:
8. Assign each compound a unique number, which has four parts, each separated by a dash: your (two-letter) initials, which # lab book you're on (Roman numeral), the page no., and a letter (assigned sequentially: A..B..etc.). So, a compound of mine might have the number HB-II-123-B. This unambiguously states that I made it, in my second lab book, on page 123, and it it the second compound isolated on that page. Often, a crude product will be A, and, after purification, will be designated as B. The idea is that if a sample vial of yours is discovered years after you leave, it can be quickly matched with your notebook, and its identity discovered without trouble.
9. End your notebook entry with a sentence or two describing your conclusion(s) concerning the experiment's outcome. Was it a success? If not, what do you think went wrong? What should be tried next? On what notebook page is the next trial in the experimental series?
10. Overall - BE COMPLETE! Someone should be able to reproduce your experiments exactly using only your notebook as a guide.
11. When you are finished with an experiment, including its notebook entry, please ask another group member to look over the notes to be sure that they conform to the guidelines and then to sign and date the page in the spaces provided at the bottom. It is especially important that the notebook contain all appropriate yield and analytical data, as well as a clear, brief conclusion.
When you are asked to sign someone's book, please take the responsibility seriously! If I find a page which is not complete, it's the signer that I'll look for first!
By the way, if you don't understand how important this is, you just haven't been around long enough to be intensely frustrated by trying to follow someone's book who left the group years ago, and find poor record keeping, no yield, no physical or spectral data, a failed reaction with no conclusion, etc.
12. Finally - keep a positive attitude and have fun!
It is very tempting to skip some of the steps outlined above, in the desire to keep things moving. However, in the end, skipping or glossing over any of these steps will come back to haunt you, especially when it's time to write a semesterly report. Incredibly, however, during any year, every single group member has usually violated most of the guidelines provided above. The following are the most egregious examples, in approximate order of importance and thus ability to annoy me when I find out (going from worst to least):
Before you run a reaction, the top part of your lab notebook must be filled out completely, with the information outlined previously. It should be legible, and include all data specified. If you are repeating a previous, successful reaction, it's fine to outline the reaction, as usual, and then, for the reference, write "Page XX, this book (or book X, if you've already filled one). You can also write "Reagents/solvents exactly as before", or "Reagents/solvents 3x scaled up", etc.