Hope the nipper feels better soon, miss K.
I've..made a dr appointment, and spent the rest of the time quenching a NaBH4 reduction of a double bond on a molecule I'm tinkering with, killing off unreacted borohydride by placing the vessel in a bath filled with chunks of salted ice, methylated spirits (I.e cheap denatured alcohol, wouldn't use it IN a reaction but it works just fine for ice baths, circulating through condenser lines etc), water and ethylene glycol (antifreeze), keeping it at between 0 and 3-4 'C, with heavy overhead stirring by means of a hand-cranked drill (because it generates a lot of hydrogen gas during decomposition, which is extremely flammable and can form explosive mixtures with air if allowed to concentrate, and subjected to a flame or spark, and unless they are designed from the outset to be sparkless motors, there is quite frequent arcing around the coils of motors, so in this case a hand drill was used for stirring)
and adding the acid as a 50-50 mix with freezer-cold, anhydrous methanol under an inert atmosphere of argon (the way to do this with not too sensitive but air/moisture sensitive reagents is to drill a hole into a suitable stopper, in this case rubber is fine, cork, etc, and slip an T shaped paddle made from two pieces of thin metal sheet with a small hole in one corner of each, twist a bit of metal wire that won't react with the solvents or acid into a figure of 8 shape on its side and have one of the holes on each side of the twist, threaded on, other end pushed up through the stopper and mounted in a drill or connected to a sparkless motor, the centrifugal forces exerted on the paddles forcing them out into a stirrer when rotated, a bit of glass tubing to serve as a bushing can help reduce friction from the stopper, or allow glass stoppers to be used) and the stirrers other end threaded through then mounted in the drill chuck, mounted in a DIY'ed collet made from a piece of thin mild steel tubing, flattened at one end with a hammer then a hole drilled through both sides to accomodate the wire, held in place with a few twists. Worked quite well.
Been doing that, slowly adding the acid (dropwise at first) over several hours, allowing the coolant bath to bring the temperature down before adding more, from a syringe with a long blunt-tipped cannula needle attached and stirring the crap out of it with the drill, now hydrogen evolution has pretty much ceased and its only continuing, still at just above 0 'C (about 3 degrees) to adjust the PH to the desired endpoint, checking after every addition of acid, larger portions, up to several ml at a time towards the end being just fine.
So far so good. It behaved itself quite as it should have. Although I can't say the same for my back, which is aching like crazy still, having had to do the above for about 9-10 hours, cooling, changing coolant when needed, stirring like crazy and drip-feeding in acid/repeatedly checking PH. Its really sore now and so are my knees.
Also, ate. Some rice pudding and chewy giant chocolate chip chocolate cookies.
