I have read the entire thread and realise isopropyl was mentioned earlier on. But, having some other possible candidates immediately to hand on the shelf, thought I'd try it with isopropyl anyway to check it again. You can click these photos to make them bigger.

Before commenting, please remember I have read this entire thing. I was trying these because they were in front of me.

Given the gigantic length of this thread (a lot of it arguing for no sake), I thought it might be nice to centre align this to make it easily visible as an actual test, as opposed to more arguing.

The paraffin


Checking the EEC code, it appears this is actually kerosene turbine fuel


10ml's of it


Weighs that much


The BP is 180C


To give this the best chances possible, I'm using a German pencil sharpener, and drilling it into a piece of Swiss cheese with a German drill


These are the biggest chips I used. Most of them were a lot smaller.


I'm using an excess of magnesium, as I suspect my KOH is rather damp. I have been using it to do the washing up for years, so it'll have picked up moisture


1ml of IPA. An excess again, due to my solvent's BP being a few tens of degrees lower than the D70 I expected it would take significantly longer using the proscribed quantity


KOH. I can see the reading going up as it's picking up moisture


20ml of the kerosene, the Mg chips and the KOH


Blowing dry argon through the glass. The entire thing is sealed. The top of the condenser is going out through an oil bubbler


Ready to go


The alcohol mixed with 5ml of solvent


Warming it up to around 100C. I immediately note the solids at the bottom have clumped into a more homogeneous layer, the cement nurd spoke of


There is a large amount of gas evolving around this temperature and for a period of around 15-30 minutes. The solvent is not boiling, it's hydrogen evolution. After 30 minutes, I raise the temperature and the solvent begins to reflux 10 minutes later


It is now boiling. As I can still see a slow evolution of bubbles, I leave it to do so for an hour and twenty minutes. When I return, the bubbles are now leaving at a rate of one every 20 seconds. I suspect this could go on for a long time at this rate, so decide to add the alcohol. Before doing so, I note what looks like it could be moisture on the upper half of the condenser. Woelen mentioned this on his page. I doubt it is moisture in this case, but blow more argon through. The solvent pushes up the condenser and is miscible with the material on it. So it's simply solvent that's evaporated before I switched the condenser on


The IPA drips in over 25 - 30 minutes. As it goes in, the solution boils more vigorously with the low BP IPA present. However, my condenser is at 10C, well below the BP of either, and neither is making it past the first turn of the coil. The solution has now turned a light grey


An annoying problem of using a high BP solvent and an angled port is that the solvent is condensing in the equalising arm, and blocking it. The slight vacuum the column of solvent creates in the top of the funnel is enough to stop it dripping correctly. Be nice if the funnel was on the other side. I reflux this for 9 and half hours


Some of the spare magnesium burning, after it fell into the sink. I couldn't get the camera in time to show the typical white glow


The result


I can see some unreacted magnesium in there, but no signs of any potassium. I (carefully) empty the flask out and rinse it. Nothing. Thankfully, also no signs that the long reflux with the KOH in there has damaged the glass.

- Although this wasn't done under ideal conditions (the KOH was probably damper than it should be, and the BP is slightly lower than it should be), this appears to confirm that IPA won't work.

Given the very long reflux time, and slight excess of magnesium, I would have expected to see at least a tiny sparkle from it. The only thing I can conclude, other than isopropyl not working, is that too much of the magnesium has been passivated. Again though, no sign of life.

I posted the pictures of the poppers above, as it would seem to be an easy source of the longer chain alcohols. It is worth noting, amyl and butyl nitrite have largely been removed from the shelves, and there are exactly seven trillion different bottle labels that are all the propyl nitrite. You will need to check the bottles before buying them, and may need to do some searching around for the two of interest. I am not sure why these two in particular where removed, perhaps due to them being sources of naughtiness. However, poppers are potentially good everyday sources as they are simply bottles full of the nitrites with nothing else purposefully added; and you can find them in off licenses, alternatives stores and sex shops (although you may feel the urge to try and explain that you're buying them for 'an experiment' ). Reducing them back to the alcohol requires only base, which is already part of this process.

- Something worth nothing for anyone wishing to repeat this. IPA forms azeotropes with water. And it is often sold at less than 99% purities (70% for instance). The azeotrope is at 87.9%, and it can be broken by distillation with cyclohexane. I haven't redistilled mine, but I believe it was 99%+ when I bought it, and it hasn't been opened since.

--------------------------------------------------------------------------------

Method. Open KOH tub, empty some out onto dish in balance. Wait. Empty, wash and dry dish. Empty some more KOH out, crush it, add to dish. Wait.

Result. The pile of powder picks it up quicker, at first, but they both end up the same provided they're left alone. Likely as a result of the bulk of the crushed material not being in direct contact with the atmosphere.

The line for the crushed KOH appears to be decelerating, whereas the flakes are close to a straight line. It doesn't look like it makes much difference. The important thing would be not to get it out and then go for a 2 hour lunch break before using it, which Len will undoubtedly already know. Powdering is also not necessary, as Pok pointed out and some have discovered first hand. But here's a graph that shows it's perhaps not such a lethal mistake as was suggested towards the beginning of the thread.

{edit}Oh... I left all the doors open on the balance doing this, so the samples had the same amount of access to the atmosphere as they would normally. The balance wasn't particularly happy about that, but you can still see the trend clearly enough.

Flakes straight out the tub



Crushed





There is still some muck stuck to the glass, after a 12h soak, but it's slowly coming back off. A wash with some acid got most of the rest off after this photo. No signs of a chewed up surface after 9 1/2h reflux at 180C.