double distilling a TPW

Sugar wash info and questions

Re: double distilling a TPW

Postby Kal » Sat Apr 09, 2016 8:24 pm

you can get ethanol to 100%, beyond azeotrope, but it will absorb water from the air back to 95.5%

*not saying you can do it in a normal still, might need a vacuum or chemical processes to get it to that 100% ;)
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Re: double distilling a TPW

Postby Kal » Sat Apr 09, 2016 8:49 pm

Actually, looking at this wiki page shows my understanding of azeotrope is flawed. You can have an azeotrope mixture of all sorts of compounds, not just water and ethanol. Ethanol has azeotrope mixtures with a whole host of other things, and if you look down the page you will see they even list some 3 way azeotropes. Seems like it is a primordial soup of different boiling points for different mixtures :scared-eek:

Also, I was interetsed to see ethanol boils at 78.4, water 100, but the aeotrope for ethanol/water is 78.1, below both of it's constituents :think:
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Re: double distilling a TPW

Postby bluc » Sat Apr 09, 2016 8:53 pm

Way I read it azeotrope ethanol is as high proof purification as can be done by distilling. Meaning anything heavier than ethanol has been removed. Not sure what the other 5% is though..
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Re: double distilling a TPW

Postby J-boy » Sat Apr 09, 2016 9:26 pm

valkorum wrote:My neighbour (unna) and I did a double distil TPW run yesterday. Here are our findings.

75 Litres TPW
Strip run through a pot still (5 Star 2" on 50L keg) 150ml foreshots each run
Used 20L at 50%, mixed with 5L of water for the spirit run (to make 40%). There was 3L of low abv leftover which we threw in to a keg to use with a future feints run
Spirit run through a Pure Distilling reflux still
400ml foreshot (I am overcautious)
2900m head
3600ml hearts before hitting tails

We have kept the heads and leftover low abv strip run for a future feints run.

Notes:
* The spirit run came off at 98% - *Not temp corrected*
* We cut some down to 40% and drank as a vodka there and then - wow. Both of us have never tasted a neutral vodka like that before.
* This was our first double distil TPW so we were unsure as to where the cuts would be. Our cuts were made by taste and smell only.
* We actually ran a parot and found that the ABV was pretty much 100% the whole run. Once it started to drop (and the temperature started to rise), we found we were in tails. Heads and hearts were at the same temperature and same abv.
* For those that are interested the temperature was 78.7 for the heads/hearts run. Once the temperature started to rise, it rose really quickly.
* The spirit run took quite a while. 1 hour to heat up, 4.5 hours to collect foreshots, heads and hearts. We didnt collect all the tails as it was late and we already had 6L of feints collected, so we just shut it down.


Awesome post! Answered quite a few questions I had on what to expect etc. :clap:
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Re: double distilling a TPW

Postby J-boy » Sat Apr 09, 2016 9:48 pm

I have to say, everyday that I spend reading on this site the more I learn & change (for the better)!

Last week I was going to buy an air still and turbo wash for the rest of my life (after my extensive research on google and youtube). Now I have seen the light :pray: and looking to purchase a Pure Distilling Reflux still, TPW and double distill everything ha ha. Can't wait to see where else this takes me!

Keep up the great work & advice guys & gals! :text-thankyoublue:

J-
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Re: double distilling a TPW

Postby valkorum » Sat Apr 09, 2016 11:41 pm

J-boy wrote:Awesome post! Answered quite a few questions I had on what to expect etc. :clap:


You're welcome
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Re: double distilling a TPW

Postby wedwards » Mon Apr 11, 2016 6:11 pm

Just about finished the annual 200L TPW for the dragon's "vodka" - pot still x 4 runs, then run it all through reflux. The stuff drinks like water at 40%. Way better than anything I produced with a single reflux run.
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Re: double distilling a TPW

Postby EziTasting » Mon Apr 11, 2016 6:49 pm

wedwards wrote:Just about finished the annual 200L TPW for the dragon's "vodka" - pot still x 4 runs, then run it all through reflux. The stuff drinks like water at 40%. Way better than anything I produced with a single reflux run.


What's your expected yield in low wines and then spirit run?
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Re: double distilling a TPW

Postby wedwards » Mon Apr 11, 2016 7:12 pm

EziTasting wrote:
wedwards wrote:Just about finished the annual 200L TPW for the dragon's "vodka" - pot still x 4 runs, then run it all through reflux. The stuff drinks like water at 40%. Way better than anything I produced with a single reflux run.


What's your expected yield in low wines and then spirit run?


low wines was approx 60L in round figures, I wasn't counting, and not sure about spirit yield yet as the second reflux batch is going through now and prob won't be finished for a couple hours yet
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Re: double distilling a TPW

Postby wedwards » Mon Apr 11, 2016 8:08 pm

Spirit run currently looks like this. Forgot the dragon had used some of my mason jars for preserving so I'm down to any glass jars i could find. Most of the jars are 2 thirds full or more as Im pretty spot on with this old rig now, and know exactly where everything falls.

Image
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Re: double distilling a TPW

Postby EziTasting » Mon Apr 11, 2016 9:07 pm

Lol
Just thinking we need to do this! As in this qty wise! Only done 60L so far on a single run... Been told to do double distillation and need more volume!!!
This will help me get a good guesstimate... :D
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Re: double distilling a TPW

Postby wedwards » Mon Apr 11, 2016 9:19 pm

yeah stuff like this i just do in bulk then she has all the booze she wants for the foreseeable future, and i can concentrate on the important stuff :)
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Re: double distilling a TPW

Postby JamieC » Mon Apr 25, 2016 5:26 pm

The last few 40L TPW's i have done has been strip run in a 1M reflux still with stainless wool removed. Then spirit run with reflux stainless in, feints in the boiler and harsh cuts. I'm getting nice product with no filtering. Happy days.
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Re: double distilling a TPW

Postby Chocko6969 » Sat Jul 02, 2016 7:26 pm

Hi all, I'm a total noob to this double distillation but I'm also extremely keen.

I've managed a couple of stripping runs and currently have in storage about 18ltrs @ 50%, with an aim to getting to 25ltrs for a spirit run.

Just one question I'm hoping you can give me some advice.

For the spirit run, should the % be 40% or 50% with my humble alcometer, are there any pros or cons to either or is it just personal preference. I'll have enough for a spirit run after my next strip but would obviously get there a little sooner if 40% spirit run is used with a lower yield on the spirit run.

Cheers, thanks in advance!
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Re: double distilling a TPW

Postby rumdidlydum » Sat Jul 02, 2016 7:36 pm

For saftey concerns never go over 40% alc in the boiler :handgestures-thumbupleft:
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Re: double distilling a TPW

Postby Kenster » Sat Jul 02, 2016 9:11 pm

Bluc, if u have a read of the stuff below, you may see that there are a 'lot' of dodgy things in our wash that are VERY hard to remove completely, and as Kal explained, 'azeo' as we know it is merely the best proportion of eth/water mix we can hope to achieve.It does not guarantee purity.
I hope this 'clip' doesent do too many heads in.
We are all on this site to share and learn...

Fusel Oil Composition

Thanks to Brad, heres a bit more detail on what has been found in the fusels, and can be present in your distilled product:

Quotes from the MERCK INDEX 10th Ed. 1983 (entry number given):
4195. Fusel Oil.

A by-product of carbohydrate fermentation to produce ethyl alc. The material varies widely in composition, depending on the fermentation raw material used, but contains chiefly isopentyl alcohol and 2-methyl-1-butanol as well as isobutyl alcohol(20%), n-propyl alcohol(3-5%), and small amounts of other alcohols, esters and aldehydes. Described as an oily liq with a disagreeable odor; 60% boils at 122-138°. Amyl alcohol (commercial) obtained by chemical treatment and refining of fusel oil contains about 85% isopentyl alcohol and 15% 2-methyl-1-butanol. Ref: Industrial Chemicals, W.L. Faith et al.

5816. Methanol.

Methyl alcohol; carbinol; wood spirit; wood alcohol. Flammable, poisonous, mobile liq. Slight alcoholic odor when pure; crude material may have a repulsive, pungent odor. Burns with a non-luminous, bluish flame. bp 64.7°. mp -97.8°. Caution: Poisoning may occur from ingestion, inhalation or percutaneous absorption. Acute Effects: Headache, fatigue, nausea, visual impairment or complete blindness (may be permanent), acidosis, convulsions, mydriasis, circulatory collapse, respiratory failure, death. Death from ingestion of less than 30ml has been reported. Usual fatal dose 100-250ml. Chronic: Visual impairment, cf.Patty's Industrial Hygiene and Toxicology vol. 2C, G.D.Clayton et al. pp 4528-4541.
The alcohols of interest in the same MERCK: (just the boiling points at atmospheric pressure, some basic characteristics and all the alternative names for each alcohol)

212. Alcohol, Anhydrous. Ethanol

; ethyl alcohol. Clear, colorless, very mobile, flammable liquid; pleasant odor; burning taste. Absorbs water rapidly from air. bp 78.5°. mp -114.1°. Solidif below -130°.

4978. Isobutyl Alcohol.

2-methyl-1-propanol; isopropylcarbinol; 1-hydroxymethylpropane; fermentation butyl alcohol. Colorless, refractive liq; flammable; odor like that of amyl alcohol, but weaker. bp 108°. mp -108°.

5042. Isopentyl Alcohol.

3-methyl-1-butanol; isoamyl alcohol; isobutyl carbinol; primary isoamyl alcohol; fermentation amyl alcohol. Liquid; characteristic, disagreeable odor; pungent, repulsive taste. Vapors are poisonous! bp 132.0°. mp -117.2°. Caution: May be moderately irritating to mucous membranes. High concns may cause CNS depression, narcosis; lower concns, headache, dizziness.

5906. 2-Methyl-1-butanol.

Active amyl alcohol; dl-sec-butyl carbinol. One of the major components of fusel oil. Liquid, bp 128°.
5907.3-Methyl-2-butanol.

dl-sec-Isoamyl alcohol; sec-isopentyl alcohol; isopropyl ethyl carbinol. Liquid, bp 113-114°. Fusel oil component.
211.Alcohol, 95%.

Binary azeotrope having a distillate composition of 95.57% ethyl alcohol (by wt) and bp 78.15°C. Also specified as containing 94.9% by vol or 92.3% by wt of ethyl alcohol at 15.56°C. See U.S.P. XVIII, 20, 1067(1970). d 0.816 at 15.56°C (60°F).

6985. 1-Pentanol.

Pentyl alcohol; n-amyl alcohol; n-butyl carbinol. Liquid, mild characteristic odor. bp 137.5°C. mp -79°C. Slightly soluble in water (2.7g/100ml at 22°C); misc with alcohol, ether. LD50 orally in rats: 3030mg/Kg, P.M.Jenner et al., Food Cosmet. Toxicol. 2, 327 (1964). Toxicity: Irritating to eyes, respiratory passages. Narcotic: E.Browning, Toxicity and Metabolism of Industrial Solvents (Elsevier, New York, 1965)pp 356-367.

6986. 2-Pentanol.

dl-sec-Amyl alcohol; methyl propyl carbinol. Liquid, characteristic odor. bp 119.3°C. Slightly soluble in water (16.6g/100ml at 20°C). Miscible with alcohol, ether. Caution: see 1-Pentanol.

6987. 3-Pentanol.

Diethyl carbinol. Liquid, characteristic odor. bp 115.6°C. Slightly soluble in water (5.5g/100g at 30°C); sol in alcohol, ether. LD50 orally in rats: 1870mg/Kg, Smyth et al., Arch. Ind. Hyg. Occup. Med. 10, 61 (1954). Caution: see 1-Pentanol.

Brad also commented :

As you can probably see from these brief descriptions, methanol appears to be one of the most toxic of all. In fact the other alcohols by and large appear to have much the same effct as ethanol when consumed (with much greater activity/toxicity), except methanol which has some toxic metabolite (formaldehyde) which is somehow toxic to the optical nerves of the eye. Ethanol administration is actually used to slow down the metabolism of methanol when it's accidentally consumed!! Note the Merck note about Chronic effect (long-term use) of methanol being visual impairment; does this occur to heavy drinkers?!?
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Re: double distilling a TPW

Postby Sam. » Sun Jul 03, 2016 12:40 pm

That's the reason we do cuts.
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Re: double distilling a TPW

Postby EziTasting » Sun Jul 03, 2016 4:50 pm

rumdidlydum wrote:For saftey concerns never go over 40% alc in the boiler :handgestures-thumbupleft:


Hey Rumy,
Can you, or any one explain the reason for this?
I mean, I heed this advice because I don't know any better and I don't really want to find out the why by trial and error (well, predominantly error!)... I can see the logic when using an open flame ( :-B ) but I have chosen electric heating elements to remove the open flame to alcoholic vapour danger so don't quite beer stand if there's ready other reasons...
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Re: double distilling a TPW

Postby jacobraven » Sun Jul 03, 2016 5:15 pm

pretty sure cause the temp need to ignite ethanol is around 350c and you elements are a lot hotter then that so by diluting it there is too much water to ignite?

edit surface temp of a water heater for homes is 736-1055°C
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Re: double distilling a TPW

Postby scythe » Sun Jul 03, 2016 6:28 pm

Above 40% ABV ethanol is flamable.
Most if not all OP spirits are sold with a metal mesh disc that covers the bottles opening, this is to stop flames getting in the bottle.
Think olden days mining lamps of a candle in a cage.

It is also why absinthe burns as it is usually around 50% ABV (brand depending), when the flame dies out its back to around 40%.
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