black/brown film ?

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mrfineshine
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black/brown film ?

Post by mrfineshine »

ok first off . big big big thank you , this is a grate resource and ive been reading it like crazy.

so my issue; today i completed my second ever distillation , the wash was a simple sugar about 8% made from tomato paste, multi vits and bakers yeast.

as it began to run i noticed a little brown/Gray film begin to appear, just a tiny bit on the surface.

i separated it out to look closer it appear to be shiny or metallic.

so i wiped it off with a cloth and it appear black.

i have a simple pot still with copper condenser is this copper oxide ?

i know its normaly blue but the inside of the condenser pipe appears a little dark.

i guess the real question is is it safe to drink ? :?:
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Re: black/brown film ?

Post by LWTCS »

Did you do a cleaning run on your rig? Or was that your cleaning run?
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Re: black/brown film ?

Post by mrfineshine »

yes i did a cleaning run after i built it , 2 weeks ago. i used vinegar. then did my first distillation.....

oh ...... you going to tell me i need to do this every time ? :oops:
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Re: black/brown film ?

Post by rubber duck »

How fast are you running your rig? How much are you collecting it say 15 minutes?
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Re: black/brown film ?

Post by mrfineshine »

about 2 or 3 drops a second
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Re: black/brown film ?

Post by Dnderhead »

did you flood the column when it started?
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Re: black/brown film ?

Post by Kifi »

Acid left on copper can result in blue distillate. Clean your column with by filling it with warm/hot water mixed with citric acid and salt, and leave it for 30 mins. Then fill it with an alkaline solution of water and baking soda. That will neutralize the acid deposits and you won't have a blue distillate problem anymore.
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Re: black/brown film ?

Post by MichiganCornhusker »

I'm reviving this thread because it describes exactly what I saw on my last few runs.

i noticed a little brown/Gray film begin to appear, just a tiny bit on the surface.
i separated it out to look closer it appear to be shiny or metallic.
so i wiped it off with a cloth and it appear black.


I have noticed this mostly since i began stripping with steam, especially when stripping with grains included.

I get strange black/brown sort of film, more like specks actually, floating on top of the distillate.
The sort of float around and if i disturb them the float back together and sort of reconnect into a floating debris field.

I leaves a blackish oily film at the level of the distillate when it comes over, which seems to be when the abv gets down to around 30% or 40%.

I thought this was just garbage coming over from the steamed grains, but on my last run I noticed a film inside my thumper plumbing that looked like liquid chrome.
When I gathered some on my finger it did look very shine and metallic and reflective. If I rubbed my fingers together it just turned to a black filmy smudge.

Has anyone ever run into this sort of thing? I've run the still many many times after cleaning runs, so I don't believe it's from any solder or flux.
My concern is that it could be something metallic getting into the works, either from my Corona mill, or my mash stirrer, which I believe is stainless, or even a brew pot.
I suppose it could even be from one of the kegs but they are both regular stainless kegs.

I only seem to get it when I steam distill on the grain, or less so when I steam distill filtered trub.

Sorry I didn't get any photos, next time I will post what I'm seeing.
For now I'm setting the likker aside, not drinking until I can get to the bottom of this.
Just wondering if anyone else has seen this specific effect.
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Re: black/brown film ?

Post by StillerBoy »

What grain mash were you stripping, for it seem that oily film you are getting comes in near the end..

When I strip an Odin's rye bread, it gets very oil at the end at that level but is somewhat clear in colour.. I just filter it and talle it to the shorting in the bread and maybe a little bit from the grain in the bread.. but there is also lots of oil residue in the boiler about the backset level..

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Re: black/brown film ?

Post by der wo »

Because it's floating on the top, it can't be a metal.
I know this from grain stripping runs. Especially corn. Looks like a metal, but between the fingers it's oily and black. I have this after the first half of stripping. At the end of the run the distillate often is more clean again.
After the run, when I clean everything, I see much of it in the riser and lyne arm.
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Re: black/brown film ?

Post by MichiganCornhusker »

der wo wrote:Looks like a metal, but between the fingers it's oily and black.
Thanks for the quick responses guys, it has settled my mind just a little.

Just like that, der wo, seeing it on my copper pipe it looked silvery, even on my fingers, but as soon as i wipe it or rub it, it just goes to an oily greasy blackish smear.
I've seen it before, but this time seeing it so much like chrome or silver it really threw me.

I've had it happen before with corn heavy recipes, but I think even more so with barley recipes. This one was about 65% barley, 30% rye. And 5% smoked grain.
I didn't get it at all when I stripped the racked clear ferment, but then I did that with my copper pot.
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Re: black/brown film ?

Post by contrahead »

I got here because I was looking for more information about cleaning, a topic that I myself have too long neglected. I was thinking about starting a thread called “Anethole Andy & his Ouzo effect”.
What is the use of having a glossary if a word like anethole isn't in there? Anyway, the Ouzo effect occurs in anise-flavored liqueurs (like Ouzo and Absinthe) after water is added. You get this opaque, milky looking liquor or imagine that you see little green fairies after droplets of water fall through a sugar cube and hit the surface of the liquor.

I have a very small still, with small copper column, stainless steel pot scrubber packing and a 20ft coil of copper tubing used as a worm. 168 proof is as high a concentration as it can achieve. Have only cleaned the still once (after making it) but use it frequently. Up until now the still has produced crystal clear products. For a couple of years now my regime has been to triple distill everything and to bottle at 50% ABV.

Last week though my heads and tails came out murky. Since the heart was clear I figured to bottle it and re-cook the other. That's when something unusual happened. I added water (well water which is usually adequate) to about half of it and the clear hooch turned milky. Confused, I added distilled water to the other half - and it turned milky too.
Looking down the throat of the column I saw black ooze and encrustation. I then plugged up one end of both column and worm, soaked the insides of both with strong vinegar overnight and flushed both out with warm water and then a cola (like Starstan – this contains a little phosphoric acid) the next day. The vinegar came out blue as might be predicted and more crud was removed by the rinse.

I put the milky mistake along with the heads and tails back into the boiler and cooked them for a forth time. This time the heads and heart came out crystal clear but the tails were very slightly murky. I add some distilled water to cut down the proof for bottling and BOOM. Anethole Andy gets his ouzo effect back...
ouzo595c.jpg
Guess I'll try next to add soda to the spirit and blast some vinegar steam through the column.
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Re: black/brown film ?

Post by olecajun »

I want to follow this thread to see posts about all this.
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Re: black/brown film ?

Post by skow69 »

Can you take the packing out and run without it? You could replace it later if you like but it probably won't run any different since there is no forced reflux. I would pitch the packing for a test run, at least. I would take a big bottle brush or something similar to it as well.
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Re: black/brown film ?

Post by contrahead »

Unfortunately I took the expedient route when constructing my column. I'd have to break out the Bernzomatic and MAP gas to sweat both end caps off, just to get to the packing.

Yesterday I ran vinegar steam through the works for 15 to 20 minutes. Damn, vinegar vapor sure stinks when you do that. It smells toxic. Good thing I didn't do it inside.

Did a stripping run on some new mash this morning. This came out murky and blue at first but finished up clear at the end. These results are encouraging. Will do another couple of stripping runs before attempting to clear up the milkshake, ouzo effect liquor. That's still being treated with soda and is only slightly less opaque than before.
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Re: black/brown film ?

Post by HDNB »

i think the ouzo effect is oils. lipids to be specific. I was having the same issue with dilution. 46% crystal clear, 45% cloudy...more it proofed down cloudier it got.
Swedish Pride hooked me up to a link that described lipids and the magic 46% number. the little buggers have a hydrophillic end and a hydrophobic end and they all get together and clump up at 46% and lower. higher ABV there is not enough water for the hydrophobic ones to try to get away from...it was just a couple weeks ago, i'll go find the link.

found it: http://homedistiller.org/forum/viewtopi ... 3#p7467963

look for swedish's post down a ways.

so long story short i tested everything i could think of and cleaned the snackers out of every goddamn thing...it still came through...in the HEADS

MCH what you describe sounds more like tail oil to me. shiny mica looking stuff floating on top. I always get it on strippers. The spirit run always cleans it up for me, except for a little comes through in deep tails on the second run.

multiple distillations cleaned it, (the ouzo effect) but that's a pain in the arse. strip/spirit should be enough. I was more careful on the ferment temps on the last few mashes and the lipids problem seems to be gone now (contra heads problem)...but i still get tons of tail oil through.(MCH's Problem)

what i get... that i have not quite figgered yet, is black dust in the bottom of the procap downcomers. It's pretty much like graphite, just dry dust but so fine it is slick. I think it's just really cooked grain from where the mash cooks down the steam jacket and cooks on the boiler wall. it gets quite a bit over 4 strippers, when i rip everything down and clean it for a spirit run.
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Re: black/brown film ?

Post by contrahead »

HDNB wrote:
found it: http://homedistiller.org/forum/viewtopi ... 3#p7467963

look for swedish's post down a ways.
Good information in that '.pdf''. Read it twice. It did not explain to my satisfaction however how the surface of an adsorption (not absorption) filter can cling to lipids under pressure. Searched for “chill filtration” and discovered many whisky links and conflicting opinions about the practice. Found a YouTube video showing some -chill filtration in progress in a small distillery and another where this German guy (some science PHD) built a little chill filtration unit using diatomatious earth as the filter. He just called it kieselguhr.

I figure my column was dark and slimy inside. Enough oils were getting through that water turned my spirit milky before the proof was lowered to 46%.

The still has been cleaned. After several days now the soda does seem to be slowly clarifying the milky looking spirit. At this point though it would make the most sense for me to simply 'chill filtrate' it some myself before one final cooking. I'll put it in a freezer overnight and later let it drip through a coffee filter while it is cold.
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Re: black/brown film ?

Post by der wo »

Kieselgur is funny stuff. In my early days I had some postilled neutral alcohol I wanted to clean further with active carbon for wineries. It worked, but the alcohol had a grey color now and it didn't settle out. So I tried to funnel filter it. But the grey color wasn't filtered out completely. Then I tried it with Kieselgur and it worked. It's a siica powder you mix into the spirit and then you filter it as usual. The alcohol came out colorless and the filtering was even faster.
It was an experiment. It got redistilled anyway. I never used it again.
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Re: black/brown film ?

Post by contrahead »

ouzo_3botc.jpg
For the sake of currosity, the same 1.75 Liter bottle was photographed on 3 separate days - after a tablespoon of soda was mixed with the 50% spirit.

(a Tablespoon = 14.79 cc, 6.2003968E-05 hogshead of wine or 7.2337963E-05 hogshead of beer).
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Re: black/brown film ?

Post by tzzler44 »

I just did my first run with an all grain (2-row) and I think I'm getting the same film. You can see in this picture a few spots where I've wiped my finger on it and cleared the film. Yes I know my coil looks like hell, it was my first one :roll:

Anyway, I'm worried the inside of my column has the same oily coating. Anyone have any input on how to clean this crud off short of scrubbing the inside of the column? Getting at the inside of a 4 1/2 foot column is a bit of a trick for me.

This was on a detuned boka still with a 2" column.
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Re: black/brown film ?

Post by still_stirrin »

tzzler44 wrote:...Anyone have any input on how to clean this crud off short of scrubbing the inside of the column?...
Many have asked this and it's been answered repeatedly. But for your benefit: soak it in a vinegar solution. The acid will reduce the build up. But make sure you rinse thoroughly afterwards.
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Re: black/brown film ?

Post by Danespirit »

+1 Ss

And if it's really bad pitted, fine steel wool is the solution (use water and dishwasher soap, too).
If you are lazy, cook it in vinegar for a few minutes and let it stay in there the night over.
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Re: black/brown film ?

Post by rgreen2002 »

MichiganCornhusker wrote:I'm reviving this thread because it describes exactly what I saw on my last few runs.

i noticed a little brown/Gray film begin to appear, just a tiny bit on the surface.
i separated it out to look closer it appear to be shiny or metallic.
so i wiped it off with a cloth and it appear black.



... When I gathered some on my finger it did look very shine and metallic and reflective. If I rubbed my fingers together it just turned to a black filmy smudge.

Has anyone ever run into this sort of thing?
Look anything like this MCH?
Metallic looking...
Metallic looking...
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Re: black/brown film ?

Post by DeepSouth »

Vinegar or other mild acids work to remove mineral and other com pounds that bind to the copper, but won't dissolve the oils beijng discussed here. You need either a solvent or detergent to remove these. What is commonly done to clean commercial stills is a warm water rinse, followed by a rinse or soak with caustic, followed by a rinse with water, then mild acid rinse or soak, and finally rinsed again with water.

Go to the hardware store and buy some lye crystals and mix them with water and make a mild caustic solution to fill your column and soak the packing. The oils and organic compounds will dissolve and can be flushed out with warm water. You'll need to neutralize it so a citric acid or vinegar soak is the next step.

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Re: black/brown film ?

Post by Danespirit »

+1 Deep South..

Very bad contaminated stuff can be cleaned with Sodium hydroxide.
Btw...it also works with stainless or glassware coffee cans (Thermos flask).
Let it be in there with hot water the night over, and you'll have it like brand new.
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Re: black/brown film ?

Post by contrahead »

Vinegar steam alone was insufficient to thoroughly clean the still. Although soda will clarify a murky spirit, it is a waste of time. The soda taste horrible and needs to be cooked out, but if the still isn't clean then your're put back to square one, and reproduce a new murky spirit. One beneficial side effect of cooking spirit off the soda water however, was that I was left with a cleaned stainless steel cooker. A very tough yellow/brown film which was bonded to the sides of my pot, and couldn't be scoured off – was removed by this soda. Sorta like soda is used in toothpaste to remove plaque – but faster.

As DeepSouth & Danespirit mentioned, sodium hydroxide is mean stuff. It dissolves animal tissue and should easily deal with the oils trapped in the packing of a riser. I used all the lye I had though, while cleaning a sewer line this last winter. Rather than rush off to the nearest Home Depot which is 45 miles away, I used some sodium hypochlorite instead. Laundry bleach is a disinfectant that is only slightly lower in pH factor than lye.

Pouring a generous mixture of bleach with boiling hot water into the riser and letting it soak for a couple hours resulted in a bunch of nasty gunk finally being washed out.
z24d.jpg
In the interim of dealing with cleaning maintenance, I was left with a quantity of spirit that I can't use (since it turns cloudy when cut with water). I experimented with a couple bottles of opaque liquor; adding about 3 times more than normal charcoal to one bottle, and a big tablespoon of dry onion skin flakes to the other.
z637b.jpg
Clarification is occurring quickly, with pronounced changes in just 3 days. The lipids in suspension are being bound up by the charcoal or flakes (homemade / ground up in a coffee mill). The refinement, maturation, aging or whatever you want to call it is occurring faster in the onion bottle, probably because of the increased surface area of the particulate. Even at this early date the two bottles that started as the same spirit have distinctively different taste. At first the intention of the experiment was to see how they clarified and then recook them. From past experience I know that the smokey flavor of my homemade charcoal-ed twigs will begin to overpower and over darken the liquor in that bottle. The same thing may happen with the onion flakes bottle too.

For now though it taste very good for a spirit that is only 4 or 5 days old! The sharp jagged taste edges of the new white dog have been partially rounded off (quickly too). The taste improvement is subtle and not particularly reminiscent of onion. The ouzo effect liquor (50% ABV) in this bottle should become crystal clear in another week – at which point it would need to be filtered to remove the sediment.

I don't know if I should be freely giving these new revelations away just yet. I perceive that oaking and this onion flake infusion might work well together, also. Many questions about taste and color control remain. I'm no herbalist or organic food nut, but the crisp, flaky outer scales of onion and garlic skins are supposed to be very healthy. Both are full of powerful antioxidants. Onion skins are especially full of flavonoids like quercetin which “is under study as an agent for lowering LDL cholesterol and blood pressure, fighting allergies, reducing inflammation, enhancing muscle growth and function, treating depression, some forms of cancer, and other conditions”. Quercetin may work fine upon free radicals in a test tube but, researchers haven't decided yet if or not, it has the same effect inside the body.
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Re: black/brown film ?

Post by MichiganCornhusker »

Not sure how I lost track of this thread.
Yes, rgreen2002, just like that, like liquid chrome, terminator juice.
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Re: black/brown film ?

Post by Pikey »

I'm not sure whether the OP got his question answered or not :?

But I'm feeling a little validated - when I first realised that people made stills which couldn't be cleaned, I was confused - but assured that "the next run will sort it out"

Now I'm glad I made one that comes to bits so I can access every part mechanically.

My next will be constructed in similar vain :)

It's not hard to make one that can be broken down, even if it does mean a few more minutes with the "Pastry" as it warms up :thumbup:
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Re: black/brown film ?

Post by rgreen2002 »

MichiganCornhusker wrote:Not sure how I lost track of this thread.
Yes, rgreen2002, just like that, like liquid chrome, terminator juice.
I don't think it is a polymimetic alloy or anything....

I've noticed it mainly after doing multiple runs of all grains. It looks silvery when it is dense on my finger but just oily when I spread it on a white paper. I assume it is related to the oily byproducts of grain distillation but I cannot be fully certain. I also steam mash as well which could possibly be related...but I don't know how....

The short of it.... just started noticing it.... not sure where it is from or what it is. :mrgreen:
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Re: black/brown film ?

Post by bentstick »

All plants soak up zinc,and other heavy metals out of dirt is it enough to worry about? we eat the same all yr long its just concentrated in the still maybe :silent:
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