I had another attack of paper inspired frustration last week. One of the project students had made a product that I was expecting to be an oil, but instead had a rather beautiful looking solid so I went in search of a melting point or confirmation that it was in fact solid. Our standard mode of doing this is running a search in Reaxys as we have limited access to Chem Abs or SciFinder so I was reasonably pleased to find a couple of hits for a series of similar compounds, and then the holy grail: a published account of the compound itself.
Now, if we’d been trying to make new stuff, we’d have been disappointed at this result but it’s a third year project and doing verification characterisation rather than brand-spanking –new product characterisation allows us to focus on the reason we wanted to make the molecule rather than grabbing a full set of data. Efficiencies have to be made in a Dual Honours system for projects. So, initially enthusiastic, I acquired a copy of the paper, noting fairly contentedly that it was in a high impact chemistry journal.
Well it all goes to show that nothing in the lab is ever as it seems, and nothing is ever easy. After 6 weeks of indoctrinating the new first years with ‘keep good records in your laboratory notebook’, and the second years with ‘fully interpret all spectral data otherwise you don’t know what you’ve made’, it was down with a bump to find a paper that offered absolutely no characterisation of the pivotal organic compounds made. Yes, a very nice applications paper, lovely results, but not a shred of verification that they made what they said they made. And no, it isn’t in the experimental section, nor is there a reference for the procedure/synthesis to point us in the right direction. As far as I can tell (and I appreciate that our literature search is incomplete), there is no previous report of this molecule.
I did verify that it should be a solid however, by way of the line “the solid was used directly” in the experimental section.
I’m aware that different disciplines have different standards in the reporting of experimental data. I’m aware that the expectations of different disciplines vary wildly, but to me the heart of the issue will always be that if you cannot prove something was made properly, every single experiment from that point, using that substance, is a waste of time, money and effort. And on that I’m somewhat uncompromising.