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Dilution problem.

PostPosted: Wed Apr 25, 2018 12:55 am
by PhillT
Diluting 95% down to 38% today, and my perfectly clear 98% turned milky, and got warm, indicating some kind of chemical reaction was taking place.
Never had this issue ever before, and the only difference I am aware of is the rainwater I was using today has been buffered to increase the ph to around 8.5ish, whereas in the past the rainwater I have used was in its natural state, which is usually about ph 5.5 to 6.
Can anyone shed some light please?
Cheers.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 5:27 am
by Sam.
Did it stay cloudy or clear after a bit?

When you mix ethanol with water it has an exothermic reaction which generation heats. You also lose a very very small percentage of alcohol.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 9:09 am
by wynnum1
A TDS meter measures the total amount of minerals and impurities in your water. you could get one of these to check the water getting RO water may be a good option for dilution.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 1:00 pm
by PhillT
Sam. wrote:Did it stay cloudy or clear after a bit?

When you mix ethanol with water it has an exothermic reaction which generation heats. You also lose a very very small percentage of alcohol.

The temp rise was 12C in 4.5 litres, which is quite a bit more than I have ever had before. I usually get 4 to 5C.

20 hours, and no sign of clearing yet.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 1:05 pm
by PhillT
wynnum1 wrote:A TDS meter measures the total amount of minerals and impurities in your water. you could get one of these to check the water getting RO water may be a good option for dilution.


TDS is 80.5 ppm. Which I would have thought was very acceptabe?

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 1:51 pm
by Professor Green
Did it eventually clear? How good were your cuts - did you include any tails?

I've had lots of tiny bubbles created when diluting that made the product look cloudy but it eventually cleared.

One trick I've heard of gin makers using to avoid louching on dilution is to use de-mineralised water. I"m not sure of the science behind it though.

Cheers,
Prof. Green.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 2:15 pm
by bluc
Sounds like louching when there is some tails or in case of gin essential oils when the % drops below a certain point the "oils" drop out of suspension and make the spirit cloudy. While high proof the ethanol keeps this from happening. It is nothing to worry about and mainly cosmetic with gin. In the case of tails you may want to adjust your cuts to exclude tails.

Another thing that happens not related to oils is chill haze with whiskey and also happens with beer. The spirit takes on the same appearance of a louche but is actually caused by chilling it and its only cloudy while cold, poured over ice for example. And is caused by proteins from barley. With whiskey it is seen as purists as a good thing. Beer not so much. Filtration is used to clear it :handgestures-thumbupleft:

Not sure about the temp increase I have never done temp measurements while diluting spirit..

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 4:03 pm
by PhillT
This is pure spirit, or as pure as my still will get it (98%) and I dislike the flavour of tails, so none involved in this or any batch I have done.
Similarly pedantic with heads for the same reason, so this is something not related to slack cuts. A mate recons I am wasting product that he would retain, and he has not had this happen.
Chill haze seem unlikely given that the diluted (38%) spirit ended up at 26C, started at around 15C for both the water & spirit before the exothermic reaction.

I could of course use the spirit for coloured product, like Sambuca, but I would really like to get a solution before clouding up any more spirit destined to become whisky.

I'll give it a couple of days to see if it starts to clear, and I'll grab a bottle of demineralised water and see what result that gives.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 4:38 pm
by bluc
Can you post a photo of it..? I doubt your spirit is at 98% maybe 95-96%..

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 7:22 pm
by PhillT
It appears to be clearing from the top down.


Cloudy brew 45% size.jpg

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 7:39 pm
by wynnum1
Could it be a contamination in the bottle ouzo does this when diluted if you used bottle previously for some other brew.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 7:42 pm
by bluc
How long has it taken to clear that much phillt?

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 7:45 pm
by Doubleuj
Looks like jelly fish to me.. louching from to much tails.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 7:53 pm
by db1979
Doubleuj wrote:Looks like jelly fish to me.. louching from to much tails.

:text-+1:
Have you checked your alcometer? Put it in water at 20 degrees and if it doesn't read 0 then it's out of calibration.
98% is not possible unless you add something else to break the azeotrope. Commercially they use substances like benzene (carcinogenic) to break the azeotrope.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 8:04 pm
by bluc
My spirit always clouds up but clears again in 15-20m, this I have never seen or heard of...sorry cant be more help but keep us posted :handgestures-thumbupleft:

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 10:31 pm
by warramungas
Not as pure as you think methinks.
See if it settles out and leaves a thin layer of white sediment on the bottom you can decant the clear stuff off. Or you could filter it but you'll need some seriously fine lab paper.
Either way you've had soluble at high abv proteins or minerals that are insoluble at lower abv come to life. Not harmful but it wouldn't take very much to create cloudy liquor.

Re: Dilution problem.

PostPosted: Wed Apr 25, 2018 11:44 pm
by Dig Brinker
If you’re cuts were good it may be the water. Could try watering down gradually next time instead of all at once. Or use less water & leave abv higher, 45%.
What wash was it? Could any oils have come over??

Re: Dilution problem.

PostPosted: Thu Apr 26, 2018 10:40 am
by YarraRanges
I have found with good reflux stills that there is no point going below 85%ABV as tails com in below that. At 85% there is hardly any ethanol left in the boiler as the ABV drops really fast after that.
If you went below 85% then you have tails.

Re: Dilution problem.

PostPosted: Thu Apr 26, 2018 2:32 pm
by PhillT
""Could it be a contamination in the bottle ouzo does this when diluted if you used bottle previously for some other brew.""

The bottles are used for nothing else, just clean pure alcohol prior to flavouring etc. They are capped when stored also.




""How long has it taken to clear that much phillt?""

24 hours to clear that much. It has been 48 hours now, and has only cleared a little more,....going to be a long wait.



""Looks like jelly fish to me.. louching from to much tails.""

Can't be because the first bottle I diluted is clear as glass, this bottle clouded,....all from the same distillation.



""Have you checked your alcometer? Put it in water at 20 degrees and if it doesn't read 0 then it's out of calibration.
98% is not possible unless you add something else to break the azeotrope. Commercially they use substances like benzene (carcinogenic) to break the azeotrope""

Checked it this morning, spot on. I only get a small part of a distillation at 98%, the rest is usually around 95% give or take a % point. I do a strip run first in pot mode, then run the column with a slow offtake.




""My spirit always clouds up but clears again in 15-20m, this I have never seen or heard of...sorry cant be more help but keep us posted""

That sounds a bit like when I pour really fast & get microscopic air bubbles, but they seem to clear in just a few minutes, 3 or 4.



""Not as pure as you think methinks.
See if it settles out and leaves a thin layer of white sediment on the bottom you can decant the clear stuff off. Or you could filter it but you'll need some seriously fine lab paper.
Either way you've had soluble at high abv proteins or minerals that are insoluble at lower abv come to life. Not harmful but it wouldn't take very much to create cloudy liquor.""

I am going to wait it out & see just how long it takes, and what is in the bottom.
I just can't see how I ended up with proteins or minerals in one bottle, but not the other bottle from the same distillation, using the same water. Mystery to me.\




""If you’re cuts were good it may be the water.
Could try watering down gradually next time instead of all at once. Or use less water & leave abv higher, 45%.
What wash was it? Could any oils have come over??""

I will try adding more slowly. I still need to end up at 37-38% though.
Sugar, tomato paste, epsom salts, citric acid & yeast.
If oils did somehow come over, why would it not have affected both bottles?

Re: Dilution problem.

PostPosted: Thu Apr 26, 2018 2:41 pm
by PhillT
""I have found with good reflux stills that there is no point going below 85%ABV as tails com in below that. At 85% there is hardly any ethanol left in the boiler as the ABV drops really fast after that.
If you went below 85% then you have tails.""

All the end product that I kept from that distillation was 95% or above, so anything less than 95% is in my tails jar.