Distilling Operation

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Distilling Operation

Postby Candy » Thu Jan 10, 2019 7:16 pm

Firstly thank you to all that have unknowingly helped me with my distilling operation. I got into the distilling hobby for all the wrong reasons, but being a chemist I couldn't resist the challenge of something new and saving a bucketload coin: the CSA relishes in doing their best to have me destitute so every dollar counts. I have lurked long enough so I would like to share my setup and experience in turning out a great clean spirit with the least amount of fuss and cash, plus it's time to put back what I have taken out - thank you all.
Equipment
35L Robobrew gen 2.
Pot still (Kegland:
Column still of the water management type (Kegland)
Digital thermometer (Traceable)
Ozito submersible pump (Bunnings)
Beer 1um filter setup (Kegland)
2 x 30L standard beer fermenter plastic barrels to generate 2 x 25-30 L TPW washes.
Approach
The stills are cooled with pool water using 15m of garden hose, stainless click lock garden fittings and a return 15m length of hosing back to the pool. An extension cord also runs full length along side from the pump to the still to control the pump. I've run the hoses and the power along the house in the shade and cable tied up them together every so often to keep it tidy.
After fermentation, I rack the wash straight into the robobrew. I then clean the fermenter. I pump the wash using the robobrew pump and sparge arm through the beer filter which flows back into the clean fermenter. Takes about 15 -20 mins or so. The crystal clear wash goes back into the robobrew to be stripped. Once stripped I do the same for the second wash, remembering to change the filter to a clean one (these are back flushed with the garden hose and washed later to be reused). Hence on completion I have two stripped washes ready for a single column distillation.
The Strip
Set robobrew to 105 degrees celcius using 1500W element.
Takes 1 hour to boil. Pool water pump turned when approaching 70 degrees on the robobrew.
Discard first 100mL
Collect 6L of distillate
Repeat for the second wash
12L of distillate collected in total
The spirit run
Set robobrew temp to 105 degrees celcius as before
Turn pump on whenever but before 70 degrees on the robobrew.
Critical - allow column to equilibrate before the collection tap is turned on. My thermometer reads a steady 78.82 to 78.87 degrees.
Discard the first 1L.
Collect the next 3.5L
Don't bother collecting any more.
Adjust to 45% using water from a good under sink water filtration setup. Use RO if you have got it.
Other information
I filter all my spirit, not that I really need to, but it really polishes it up. I can taste the the difference, it very subtle but better is better no matter which way you slice it (better is the enemy of good enough). I use the still spirits carbon filter setup, slow gravity feed and additional granulated activation charcoal free in suspension. To refresh the carbon I boil the filter and loose carbon in distilled water first and burn off the filter and the loose carbon in the oven at 250 degrees for 15 mins. No need for new filters, but maybe a new one in a year.
The final volumes for the cuts above have been established by measurement, smell, taste and chromatography. Agreed, they are aggressive but no heads allowed in my gin...period.
Filtering the wash saves time and it makes a difference to the quality of the stripped product which in turn flows on into the final product. By removing the bulk of the yeast in suspension you reduce the % of cells lysed during the boil thereby reducing intracellular components released into solution. It is noticeable and has been proven in my experiments. After backwashing the filters you will see how much this has worked. It also removes small particles of tomatoes (confirmed by microscope) from the TPW. Stripped alcohol with and without tomato paste confirms that tomato adds flavour. Hence keeping with the philosophy better is better - a cleaner strip makes for a cleaner spirit.
Overall I get 7 L of clean vodka ready for drinking as is or vapour infused gin. I use a fine colander suspended in the robobrew with botanicals.
TPW
5kg sugar
250 grams of 100% tomato paste (double concentrate)
2x cenovis multivitamins crushed
1 teaspoon of vitamin C powder
22L or so of filtered water heated to 30 degrees using robobrew.
I use 60g of lowands yeast from woolies, emulsify in some of the water. Fermentation takes about a 10 days and I strip on day 14.
I make two batches of course for the method above.
Sterility achieved for all components including the robobrew using percorbonate.

Thanks again,

Candy
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Re: Distilling Operation

Postby woodduck » Thu Jan 10, 2019 8:59 pm

Hi mate :greetings-waveyellow: welcome.

Sounds like you have it sorted mate. It's great to see you have done some trials to get the best product you can.

I would like to suggest you turn your cooling water on when you turn your still on. It's just that bit safer. Something could distract you at the wrong time or you might forget and having alcohol vapor filling the area would not be good.

All the best with the future runs :handgestures-thumbupleft:
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Re: Distilling Operation

Postby Sam. » Fri Jan 11, 2019 7:49 am

Welcome here mate, I’m sure you are going to be able to contribute some good information to the site :handgestures-thumbupleft:
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Re: Distilling Operation

Postby Candy » Fri Jan 11, 2019 12:54 pm

Cheers - thanks for the advice. I guess from a risk mitigation I am more likely to forget than have the pump stop for whatever reason, or lose water etc so I might have to think of a fail safe.
I forgot to mention that turbos do suck and this is confirmed by GLC - so many contaminates....You may not taste them but they are there and I'm sure they will be toxic over time. I just want my liver to focus on ethanol - its bad enough!
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Re: Distilling Operation

Postby Professor Green » Fri Jan 11, 2019 2:26 pm

Welcome to AD Candy.

Cheers,
Prof. Green.
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Re: Distilling Operation

Postby PeterC » Fri Jan 11, 2019 5:16 pm

Greetings, very interesting post. I have some questions if I may.

In the GC analysis, I would have thought that the unwanted components would reduce gradually so what are you measuring and at what levels, to distinguish between heads and hearts? (I have a HPLC at work but that doesn't lend itself to this kind of analysis)

The filtration step looks interesting as I have always thought that yeast cells in the boiler contribute off notes. In my work, a 1 micron filter is not considered fine enough and they use 0.65 for yeast and 0.2 for bacteria so do you find the 1 micron does the job? Do you have enough pump pressure to push through the filter without flow loss? The small pumps you can get for this have a 3m head pressure (4 psi) so I am wondering if they can do the job if the filter gets a bit loaded up. I am trying to decide if a pump with a bit more pressure is warranted. I can get a peristaltic pump cheap, slow but high pressure.

TPW does have some flavour so I have gone to other types like FFV because of this. So you are saying filtration to 1 micron removes most of this?

For your gin don't you get residues from the botanicals falling back into your Robobrew? What is that like to clean up? I would be interested in your botanicals choice and quantities plus volume of spirits you start with and run strategy, as I am looking at making gin in the future.

Thanks and Regards,
Peter C.
Last edited by PeterC on Fri Jan 11, 2019 5:18 pm, edited 1 time in total.
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Re: Distilling Operation

Postby Rolls912 » Fri Jan 11, 2019 9:59 pm

Candy wrote:Beer 1um filter setup (Kegland)
Candy


At $30 bucks shipped that’s a cheap upgrade worth doing! Just need to figure out what size pump to run it :handgestures-thumbupleft:
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Re: Distilling Operation

Postby Lowie » Sat Jan 12, 2019 3:54 pm

G'day Candy. Good to have a chemist amongst the mad scientists! :handgestures-thumbupleft:
I have often thought of pumping my pool water through the still (my runoff goes into the pool) as I go through a shitload of water each year but concerned the salt water chemicals would eventually chew out my copper. Your thoughts, apart from flushing with fresh water after each run?
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Re: Distilling Operation

Postby Candy » Mon Jan 14, 2019 5:21 pm

Hi Peter C.
Correct, gradual reduction over time. As you know GLC is quantitative and highly suited for this type and other types of toxicology measurement, hence my initial intention was to assess methanol contamination (as the primary safety concern). I am not using any quantituative measuremnt of other volatiles to determine any cuts perse, only confirming the reduction of other volatiles (compared to the main...huge....ethanol peak) over time. I have overlayed the chromatographs 20 mins apart over time and visualised time lapse so to speak....I wish I had it (GLC) on hand. Submitting samples isn't easy.
The 1um works great. Rest assured the claim of 1um on this cheap filter set-up would not stand up to scrutiny. When gravity fed from a day-12 wash it blocks after 10L to a drip. It doesn't need much pressure hence the 1um claim is BS, but it clears it without the time drag. The robobrew pump works well with it. I've considered an RO pump (12V) but just don't think it needs it. Slow is probably better. When you back flush the filter the orange residues seep out are concentrated - turns the whole bucket cloudy. It works, say 50% or more reduction in clarity - I will do a turbidity measurement of the wash before and after for us both (light absorbance over a path length on 10mm).
I will post the gin method soon when I'm chuffed - it's slow going. I've had some epic failures large scale so I am spooked - I'm thinking about a tiny pot still just to speed things up. Wish I had more time. I'm interested in yours if you have knocked one up.

Lowie - interesting question. I don't know to what extent this is going to be a problem. It's been on my mind. Chlorine will corrode, but rapidly when copper subjected to hypochlorite solutions. I have a salt pool, as most of us, and I would say that for the very short length of copper in the still, exposure and the ppm of free chlorine in pool water - jack shite for the life of the still. I think pH is likely to be the main problem - too acidic and copper chloride formation will increase. It is the copper coil at the hottest point that has me worried - just don't want a pin hole leak and pool water is in my wash - that's what has got me worried but it's a baseless concern now but may be a problem 10 years from now. Pressure test - now that' is an idea for periodic maintenance.
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Re: Distilling Operation

Postby Candy » Fri Feb 15, 2019 10:39 am

I can confirm that filtering the wash removes 40% of everything in suspension.
Light transmission for unfiltered was 31.9% and filtered 71.7%.
Both readings were compared a sample of water.
This confirms filtering is a useful time saving method to reduce bioburden in the wash.
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Re: Distilling Operation

Postby RC Al » Fri Feb 15, 2019 1:16 pm

Nice one candy, might have to look into one of those filters for neutral wases :handgestures-thumbupleft: :handgestures-thumbupleft:
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Re: Distilling Operation

Postby Rolls912 » Sat Feb 16, 2019 9:53 pm

Rolls912 wrote:
Candy wrote:Beer 1um filter setup (Kegland)
Candy


What do you do with the filter in between washes? I pulled mine out and tried to rinse it which was a futile exercise. Now its mouldy. I suspect you leave it suspended in the solution?
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Re: Distilling Operation

Postby wynnum1 » Tue Feb 19, 2019 10:48 am

Candy wrote:I can confirm that filtering the wash removes 40% of everything in suspension.
Light transmission for unfiltered was 31.9% and filtered 71.7%.
Both readings were compared a sample of water.
This confirms filtering is a useful time saving method to reduce bioburden in the wash.

Centrifuge Technology Enters Small Brewing Niche seems this may be the answer to filtering but they all seem too big and expensive to use for a hobby brewing seems they do a good job on beer and the reduction in waste makes viable they use on milk to separate out the solids and the small ones are cheap but there does not seem to be anyone who has tried on beer but with beer would have to eliminate the oxygen but if going to distill probably not needed..
Centrifuge Technology would they use this on water filtration if not using chemicals going to save money and time .
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Re: Distilling Operation

Postby bluc » Tue Feb 19, 2019 11:09 am

Wynum you mean milk centrifuges are cheap?
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Re: Distilling Operation

Postby wynnum1 » Tue Feb 19, 2019 12:34 pm

bluc wrote:Wynum you mean milk centrifuges are cheap?

Yes but now all the vacuum cleaners are cyclonic copied from industrial could they make smaller centrifuge one for home brew .
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