As most people who have undertaken a PhD in organic chemistry know, synthesis can take a long time, even when the objective is not primarily synthesis, so to get a sense of proportion in this account, this seems to be time for an interlude, wherein some various tales of, well, you can choose your word, can be told. So, here are some things that should not have happened.
The prequel, and warning that not all is as it should be, happened in the summer when I had been hired for my first taste of research. I came back from lunch and saw water on the floor from the bench behind me. A hose had come off a small condenser, and a small "river" of water was snaking across the bench. By itself, a nuisance, but in two dry bits, enveloped almost by the winding "river", were two sizable lumps of sodium sitting there! Fortunately, I knew where some tongs were, so tongs, then tap, then when the perpetrator returned, some language not befitting an output of the RSC!
I started the PhD in a small “temporary” building called “The Armoury”, a sort of overflow lab because the main chemistry building was “full”. One advantage was it was near the Students’ Union cafeteria, so coffee was at hand. Soon after starting, my supervisor announced he was to do some lab work, a statement not greeted with unqualified enthusiasm by the senior PhD students. His first move was to purify a very large amount of acetic anhydride by distillation, but after a short period into this exercise, there was a yell, an emergency wash, and a very strong smell of acetic anhydride. No boiling chip or stirring, and not a lot of work for the rest of the afternoon. There was no repeat of this enthusiasm for lab work! It was also suggestive that good advice for lab work might not be forthcoming.
One morning I came in and saw a remarkable sight. There was a small room at one end directly facing the path to the Student’s Union, and on a bench on the far side from the window, someone had carried out a sealed tube pressure reaction. The top had blown, there was a 2 mm hole drilled through the safety shield, and in a direct straight line from the tube, hole in shield, there was a further 2 mm hole in the window about 3 meters away. That did not put me off pressure reactions (I have done quite a number through my career) but I always used steel.
After a year I was moved to the top floor of the chemistry building, and old stone building with basically one entrance. At some point, a Colombo Plan student was brought in and put at the bench behind me. Since nobody knew what his skill level was, I was asked to offer assistance. His first synthesis involved reacting a ketone with a Grignard reagent, so I discussed what would happen and set him off. I had to help him get it started, but soon the magnesium was reacting well. About two hours later, I heard the bleat, "I've got two layers." I pointed out that was expected when he poured his ether into the acidified ice-water. "But I haven't done that yet." Somewhat annoyed, I had to go around the other side of the island to see what he had done, and there were two layers! Had I tried, I could not have done that in a hundred years! He had managed to add the ketone as an ethereal layer on top of the Grignard! His hand shuddered, and as I dived for the floor there was a roar like a rocket motor (OK- slight exaggeration). Fortunately, there was no gas lit in the room. So, I gave him a lecture about the need for stirring or refluxing, and he was at it next day. About three in the afternoon, another bleat, "I've still got two layers!" I succeeded in getting him removed from the lab. More next week.