weird heads

[kiwistiller]

Ok so I've been a bit interested in heads recently. As part of an experiment in compressing heads, I tried running off some heads using a CM head, with the water flow very high (which effectively drops the temp at the vapour outlet to the condenser, and then slowly and incrementally decreasing it to see what distinct parts (fractions?) there are. I then planned to pot still the body / tails. the boiler was charged with two stripped rum washes and my jug of rum feints / oils. I got some surprising results.

First I got a few drips around 57-58C. I presume this is the acetone or other volitiles. after a while of VERY slow drips, I had collected maybe 10mls of pretty nasty stuff (in maybe 20 minutes), collection stopped so I figured well thats the acetone gone, time to decrease water flow and up the head temp a bit. a few slight adjustments at the temp sprang up to 61-62C. now that I wasn't expecting, I thought that the next thing I'd hit was methanol at 65C. This head normally sticks to the boiling points of various fractions pretty well, so I was very surprised. I was getting slow drips again, so I collected what I could in a small glass vial. got maybe 20mls. after that I found the meths at 65-66C, and then normal heads etc around 76-77C. then I started tasting body and shut down.

Now, this unexpected stuff smells amazing. not sweet and harsh like meths, or chemical smell like ethyl acetate, but really.... good. if I were to characterize it, I'd say buttery rum and bananas. it tastes smooth. so... What the heck have I got here? All I want to do is add it back into some rum, the smell and taste is really good... have I got some rum ester or something? some other rum 'oil'? is it safe to consume? has anyone else found this before?

your thoughts? this is the first thing i'm going to try again when I get myself a LM column. I know its a crappy CM head that I used to do this, but the process was done very slowly (I probably spent maybe 2.5 hours) so I'm fairly sure it IS a distinct chemical. Please advise

KS

[Slow & Steady]

PM "The Chemist" and see if he has any idea what you have collected at 61-62C.

S&S

[Dnderhead]

Acetone--56.5c
Methanol--64.7
Ethyl acetate--77.1
Ethyl--78.3
propel-97.2
As it is almost impossible to remove these in pure form id say it is a combination of two.(or more)

[kiwistiller]

cheers, SS, dunder, I'll PM the chemist, as this stuff smells sooo good all I want to do it add it back to the rum... might not be safe though...

KS

[Dnderhead]

I believe if stored for a period of time these change , to taste/smells that is beneficial, that is part of "aging". the more that is in it
the longer it takes. these can be converted threw chemistry. but is above me and most on hear.(look up artificial flavors/esters)
some of the more flavorful whiskeys are almost undrinkable in the white.(more aging needed) where the lighter ones have less.(less aging needed)
just like wine, unaged it will give you a "hangover" in a hurry.


the magic of the lepricons.

[kiwistiller]

what if it tastes / smells so good straight off the still that you want to drink it straight away I figure it must be something nasty with a whole lot of esters in it.

[seravitae]

isoamyl acetate = banana flavour/smell. bp is well over >100c but it's probably azeotroping with god knows what else in there

[kiwistiller]

ha I'd forgotten about this post. I ended up adding about 5 mls into the blend. made it taste and smell great, but I was sick as a dog for the first time on my own product. so, not trying that again....

[plonker]

Hrrrm.. interesting, I often get bananas in the hearts, no hangovers though.. and trust me I tried...

[kiwistiller]

yes this was definitely not part of the hearts... came out well before, and there was nasty stuff before and after. only managed to find the 20ml or so of this stuff because the of the cm head doing its auto shut down either side. I also find banana notes in hearts, particularly in a lighter rum wash. I suspect seravitae is right and the ester was coming over with something nasty in the heads. Shame about the vomiting, the stuff was amazing. Girlfriend wasn't too impressed

[plonker]

heh he he heh... that made me laugh... no, my bananas come out during the hearts, and last throughout.. they fade after about three weeks...

[plonker]

Mind you I use a VM still, heads are seriuously compressed, but tails seem to run forever...

[seravitae]

kiwi, that said esters arent *too* bad on the body because they are naturally present in fruits and in lots of foods. It may not have been the esters per se, but maybe something carried over with it as well.

Also, due to the presence of other flavour components in washes, methanol does actually form azeotropes and someone posted lab results here showing methanol actually came over proportional to ethanol content for a a schnapps wash. It's possible methanol or other lower boiling point substances came over as well, further highlighting the importance of making good cuts.

Can i ask how big your wash was and how much you drank? I am curious as to the dilution of that 5mL into your batch, as if it was a large batch, given your sickness if you drank a reasonable amount of alcohol the concentration would have been quite low, so whatever it was that made you sick had to be pretty bioactive/toxic.

[kiwistiller]

Can i ask how big your wash was and how much you drank? I am curious as to the dilution of that 5mL into your batch, as if it was a large batch, given your sickness if you drank a reasonable amount of alcohol the concentration would have been quite low, so whatever it was that made you sick had to be pretty bioactive/toxic.

It was from several (2?) 25 l rum washes, stripped, and then some dunder added. some accumulated heads and tails were added as well. Ester (?) was only added back to about 5 litres of product though. I drank about a litre.... I'm fairly confident it was poison... I believe that was the point that I shelved the 'suck it and see' philosophy...

[seravitae]

So at 5g/5L, that's a 1/1000th concentration, of which you drank a liter which corresponds to 1 gram. Although that's pretty high, I wouldn't automatically assume that it was enough to cause toxic effects.

However, since you drank ~995mL of another toxin, i'd be tempted to blame it on that, or blame the saturation metabolic pathways by redirecting metabolism of the mystery fraction into producing other more toxic metabolites than what would be expected.

naturally i don't have any right to tell you what to do, but I will say that a liter of spirits is enough to put a massive toll on the body, even for those used to drinking that much booze.

[kiwistiller]

haha yes it was a big night, I certainly don't do that regularly, but it has been done before on my own spirits with no (serious) adverse effects. nothing like this anyway. but yeah.... I won't try it again. I've got another bottle of the same batch, and it makes me nauseous to smell it now. other batches - fine. other people think the danger bottle smells good.... So they can drink it

[seravitae]

That too, or perhaps if you wanted to be sure, do a blind test - get your mate to give you a small sample, the 'suspect' one and your equivilant normal one, on different days, and take a few sips (trying to ignore the flavour, maybe quickly wash it down with something) and notice how you feel during/after the effects.

[raybren]

kiwi,
I have run a couple of rum batches made with molasses as the only sugar source on an extremely simple pot still. I have nowhere near the knockdown capabilities that you do using the CM, but I always notice an aroma that occurs before distillate is collecting. I always enjoyed the aroma, and could clearly smell it coming out of the output tube even when no liquid was coming out, but the wash was quite warm. I wondered if maybe my condenser wasn't long enough to condense an extremely low boiling point chemical. Your description reminded me of that aroma, for what its worth, even though it sounds like you're not going to be trying to recreate the hangover.

[kiwistiller]

yes I know the aroma, that is exactly what I'm talking about. essence of that. it smelled and tasted really good, but SO not worth the chance of that again. I've gotten soft from all this home made, I don't like hangovers much these days.

[Dnderhead]

1 litre ???? WoW ,,,that makes me feel like a wimp . that is as much I consume in a month.

Was this redistilled? if not how much did you add?

[kiwistiller]

about 10-15mls of the stuff in 4-5l of product.

1 litre ???? WoW ,,,that makes me feel like a wimp . that is as much I consume in a month.

a) it wasn't a good idea
b) I'm a big guy, about 6'4" I guess in your archaic measuring system , and accordingly have quite the alcohol tolerance.
c) I don't do that often! normal consumption would be 1-2L a month . Although NZ has a lot of problems with people 'binge drinking'.

[vinifera]

Mind you I use a VM still, heads are seriuously compressed, but tails seem to run forever...

Amen! Heads are the biggest problem.

/Vini

[kiwistiller]

...and my idiocy rises up the active topics list yet again

[Centimeter]

I have a guess. I always wondered about the possibility of forming a small amount of diethyl ether. I mean, we're refluxing ethanol, I'd be a bit shocked if some ether wasn't formed, particularly if the contents of the boiler are acidic. This would be my primary guess for the non condensed vapor at the beginning of a run.

Your condensed stuff is quite probably ethyl acetate. Considering the order of its collection and the quantity that you collected, it seems like a likely culprit. Ethyl acetate has a rather pleasant fruity smell to it and could very well be what you're collecting. As was also stated, it could also be some random ester that's forming. However, considering that you collected 20ml of it, I tend to suspect that it's ethyl acetate.

None the less, this is one of the cool things I love about column distillation. Beyond the wonderful thermodynamic environment that it represents, there's a tremendous number of electron rich nucleophiles in a reflux environment with the potential for elegant and exotic chemistry. The smells and tastes that come out of the stil are nothing but astounding. Enjoy your hangover!

[blanikdog]

... but I will say that a liter of spirits is enough to put a massive toll on the body, even for those used to drinking that much booze.

Just reading this gave me a dreadful hangover. A litre of spirits!!! Pharque.

blanik

[guerrila distilla]

you guys obviously dont have polish relatives . the first time i met my in laws, by the time it came to carry me to bed (literally, over her fathers shoulder), we'd managed to get through 6 bottles. unfortunately, there were only four of us drinking, and they drink their vodka straight in shots. this taught me several valuable lessons.

a) dont drink vodka with polish guys, you will fail spectacularly.
b) dont drink home made vodka with polish guys, you will fail spectacularly, and be very sick the next day.
c) dont drink your way through six bottles of home made vodka with polish guys, you will fail spectacularly, be very sick the next day, and make an ass of yourself in front of your newly met in laws.

i learnt my lesson from that experience, trust me . now, when i go to poland, i stick to beer (which i can drink safely at my own pace) .

[kiwistiller]

Haha I have some relatives in the Ukraine (by marrige) and they came to visit a couple of xmas's ago. My cousin who'd married their daughter sat me down and said "Now listen. what you have to remember about these people is that a slav, ANY slav, can drink you under the table". I didn't take him very seriously, until they showed up with many bottles of vodka and this awesome silver chalice for dispensing mulitiple shots fast enough to keep up with consumption

best. christmas. ever.

[dellae]

My 2 sheckles worth on the bananas.
A Still Spirits Turbo made to the letter of the pack, 6kg white sugar, in March.
Brewed out to 0.985 in 3 days - the whole house smelled like a sewer.
Left to settle for 2 days.
Run thru my CM unit with outlet water temp ~50 - 53C.
After 60 mLs of very foul head, I took 200 mLs of banana flavour, cut it with water and me and the boys downed it quick as no problem at all.
The rest of it was reasonably clean.

No bad head at all.
Have never produced it since.

[marc83]

This thread is hilarious..

Next still run i think once its at operating temp i am going to have the cooling flow right up for 15min or so at a steady boil,let the contents sort itself out and very very slowly decrease flow,try to better understand each fraction coming out,should teach myself a bit,and further understand my still...I think that tip is in another thread from you Kiwi.I know i read it here somewhere.

[kiwistiller]

Yeah, every few months this one pops up to haunt me

Someone (I think it was airhill) asserted that equilising a CM was a waste of time. I'm not smart enough to argue with him, but I still see the benefit in at least giving it a few minutes to get a good boil going. I could be wrong though.