I was the one that coined the phrase "nanoscale" ( a spin on a legit marine science accomplishment of mine).
there was never any one way to do it- all depended on what was onhand at the moment. 50 ml boiling flask sitting in hot water with a balloon on it for all day worked (I let the reagents start cold and slowly react. Used a microwave granite thingy that held heat as a heat source. Used IR heating lamps. Used lightbulbs. Used a rubber stoppered and taped coke bottle on a lightbulb. worked great once. another time it disintegrated into high velocity glass shards and droplets while I was still holding it. not even a scratch, but luck was on my side. my bedroom wall was henceforth painted a nice HI color (faded over time).
on a slightly larger synth, I used the hotplate from a coffee maker as the heat source, and a length of braided hose taped along the side of my frozen windows in the dead of winter.
there's no need for this p/p vs reflux pissing match- the long reflux is a historical fact passed down. the p/p has some theoretical merit (high conc under pressure). Of course a controlled p/p (not the incendiary fun) is acting as (a relatively inefficient) condensor to a ccertain extent..
I used to place flasks with fitted condensors pumping icewater through them in the presto kitchen kettle with a rheostat and an oil or sand "bath". I'd run a braided hose off my condensor, up a wall, and sometimes in some h2o for backpressure. worked great. put the street rp/i to shame- probably because of a little xtra time to react.
if I find time and privacy to post it. I'll detail my "final" method that was the last one I used for a couple cooks before I gave it up. It's another kinda hybrid reflux-p/p.
method alone accts for a relatively s mall variable- you put rp/i together in proper proportions, and it's gonna spin the pfed 'round regardless of what you do. I believe there are plenty of other variables, denaturants in pills, contaminants hiding in your glassware. then there are the steps that are ONLY honed by practice. you learn to trust your eyes, your nose, your tactile senses- the stuff that comes into play after the rxn and it's time to separate shit and tweak pH, and dick with emulsions, then properly form a salt, wash it, and xtylize in ways that make your friends green with envy. you cannot learn much of the truly important skills- lab techniques, without performing them many times, fucking up, refining, etc. Yeah, I fucked up a lot of shit for a long time- but one day it was kinda like it all clicked. my failures had forced me into good techniques that seem to be the cornerstone of a rxn.
anyone else just kind of have it happen this way? like finally learning to ride a bike? and after that, you had to try pretty fucking hard to screw it up.
