What is this stuff?

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brewit2it
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What is this stuff?

Post by brewit2it »

Hello everyone,

Hopefully someone has seen something like this before and can help me out.
What is this black stuff forming on the inside of my still head?

I've done some reading and I know that sulfur compounds(copper sulphate) will form, but this just seems excessive. It even seems to be flaking off and coming out in the distillate. These pics are from after I cleaned the pot still head with a phosphoric acid solution and did a stripping run of an all grain wash. Since my all grain washes have been coming over dirty(tiny brown and black flecks) lately I've been running them pretty slowly. I can wipe most of it off with just a paper towel, but need to scrub to really get it clean.

Thanks.
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NcHooch
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Re: What is this stuff?

Post by NcHooch »

Is there some reason you're using phosphoric acid? ....

I'm no chemist but there are some dissimilar metals in there, copper and solder at least , neither could be called passive or inert.
...possible reaction with the acid?
you're always going to have some discoloration inside, but shouldn't be flaking in in the hooch. :thumbdown:

I'd be inclined to give it a good vinegar & water soak ..., and then maybe a short water run and see where you are after that.
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rad14701
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Re: What is this stuff?

Post by rad14701 »

NcHooch wrote:Is there some reason you're using phosphoric acid? ....
+1 Why...???
brewit2it
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Re: What is this stuff?

Post by brewit2it »

NcHooch wrote:Is there some reason you're using phosphoric acid? ....
rad14701 wrote:+1 Why...???
Because it's just as effective at removing copper oxide as citric and acetic acid without tarnishing and harming copper.
I use it because it's available, in the form of Star-San. I've been using it for years to clean the copper in my brewing equipment and I know that it's used fairly often in the brewing industry as a whole as a cleaner to remove scale and clean stainless and copper pipes. So I didn't really think it would be a problem, but I mentioned it just to give as much info as I could about the situation. I do rinse it with hot water and let it dry before use if that helps.
NcHooch
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Re: What is this stuff?

Post by NcHooch »

Can we safely assume that the inside of the still looks perfectly clean after the starsan and rinse?
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Usge
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Re: What is this stuff?

Post by Usge »

When I use Starsan at the proscribed concentrations....copper comes out shinny like a penny...not like that. I'm not sure what the flaking is...that's odd. But, it will clean the "dark" tempered areas of the copper down to shiny copper.

You used the premeasured amount per 5 gal water? Then soaked the parts in it for a good while? I leave mine over night. The problem with cleaning still innards like that down to shinny copper is...you have to re-temper it in again. Do, throw away runs, etc. Your distillate will tastes like a copper penny on your tongue until you get it seasoned again. So, you need to do a water and/or water-vinegar run...and then a throw away distillate run (old wine, whatever). Then after that...only rinse your still with water. It will turn dark..that's ok. But, you shouldn't see any flakes. Something else going on there. You have any packing? OR was there some thin layer of solder that the acid reacted with (tin) and turned black and flaked up?

You might want to start again...and get it stripped down to metal. Then re-season it. If you are having trouble with starsan....just use citric acid. Make SURE you rinse it with water after using any acid...to neutralize it. Then re-season your still (just like a cast iron pot) before you do any keeper runs.
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Re: What is this stuff?

Post by rubber duck »

What did you do? Yes I've seen that but why did you heat the whole god damn pipe?
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brewit2it
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Re: What is this stuff?

Post by brewit2it »

NcHooch wrote:Can we safely assume that the inside of the still looks perfectly clean after the starsan and rinse?
Usge wrote:When I use Starsan at the proscribed concentrations....copper comes out shinny like a penny...not like that. I'm not sure what the flaking is...that's odd. But, it will clean the "dark" tempered areas of the copper down to shiny copper.

You used the premeasured amount per 5 gal water? Then soaked the parts in it for a good while? I leave mine over night.
You might want to start again...and get it stripped down to metal. Then re-season it. If you are having trouble with starsan....just use citric acid. Make SURE you rinse it with water after using any acid...to neutralize it. Then re-season your still (just like a cast iron pot) before you do any keeper runs.
I knew I couldn't be the only person using phosphoric around here. As for cleaning I usually don't soak it for that long or get it all the way down to shiny new copper. I'll make up a concentration just slightly stronger than the amount recommended for use as a no-rinse sanitizer. I don't go crazy with it but I'm using it for a cleanser in this instance. The amount recommended per 5gal is the FDA allowed amount as a no-rinse sanitizer, so that there is an allowable amount of product left over in what ever application it gets used for, usually beer.
So usually I'll make up a small solution, put it in the still head and use a white scrubbie with light pressure and then let it soak for maybe 20min to get the inside mostly clean. Then I rinse very well with hot water and let it dry, so there is still a little black/dark staining when I'm done. The point there is so that I don't have to(hopefully) re-season it. I'm just trying to remove the majority of the buildup.

I'll clean it per-usual today and take a before and after pic.

I don't use any packing, and this still head has been around for a while now(about a year) and was thoroughly cleaned after being built including the usual vinegar and sacrificial run.


Rubber duck, I have no idea what you're talking about.
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Re: What is this stuff?

Post by rubber duck »

I have seen that stuff when I've overheated a pipe. I think it's some kind of oxidation. If I use inert gas on the inside of the pipe during the heating it doesn't happen.
Ideas are like rabbits. You get a couple and learn how to handle them, and pretty soon you have a dozen. John Steinbeck
brewit2it
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Re: What is this stuff?

Post by brewit2it »

Ahh, well... I also think it's some form of oxidation, copper oxide was my first thought. I didn't heat up the whole pipe though, and I've sweated a fair amount of copper and haven't seen anything like that before. I wanted to do a spirit run this weekend so I decided to not acid clean it after all. I did give it a nice hot rinse and a wipe down. Here are the after pics.
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Dnderhead
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Re: What is this stuff?

Post by Dnderhead »

out of curiosity what kind of water you using for mash...
brewit2it
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Re: What is this stuff?

Post by brewit2it »

I usually get 10gal at a time in two 5gal jugs from the water station at the store. It's one of those stations that uses local tap water and says it has a sediment and carbon filter, reverse osmosis and UV light treatment. It does taste clean, and I can't smell any chlorine in it. I then usually add some calcium sulfate to the mash before I dump in the grain, to help with enzyme conversion and yeast health.
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Re: What is this stuff?

Post by myles »

If you take some of that water and boil it does anything drop out of suspension? Is it full of minerals?
brewit2it
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Re: What is this stuff?

Post by brewit2it »

I would assume most of the mineral content is removed during the RO process, which is part of why I had back in some calcium.
But I can give it a try next time I pick some up.
I can tell you that it does make decent beer though.
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Re: What is this stuff?

Post by myles »

That's OK, I was just wondering if the process had a leak and some untreated water was getting through, or if it was time for a filter change. It has been known to occur. There was a case reported over here some time back of bottled mineral water that actually was being filled out of a tap and was not the real stuff at all.
brewit2it
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Re: What is this stuff?

Post by brewit2it »

Thanks myles, I use that stuff because I have well water and it is very hard and full of iron, so not great for a mash. I don't always trust those water stations either, so I always give the water a good sniff and taste before use.

Usge - I actually didn't know that you had to redo a sacrificial run after completely cleaning the copper. For some reason I just thought the vinegar and first ethanol run were to clean any residual materials/chemicals from the build. There was one time I didn't clean it down to shiny copper but that was about six runs ago, since then I would just give it a light soak and scrub after a run.

I can also say that the flakes come over more in the tails, and that they are tiny almost like soot. There are some black and brown colors, and sometimes it even glints in the light like it is metallic. The last couple stripping runs I've run the distillate through a couple coffee filters to clean it up.
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Re: What is this stuff?

Post by Usge »

Yes..according to Dnderpedia...it's like a cast iron skillet....once you take it down to metal...you got to re-season it or everything is going to taste like a copper penny in your mouth.

But, I never got any flake, etc. That's got to be some gunk/flux, etc..or solder that just never got cleaned out good that the StarSan loosened up. Star san like Oxyclean...if you leave it long enough..it will lift teflon coating off the pan. So, it could have leeched something out of your soldered joints. It should clear up. But, I'd keep doing sacrifical runs till it does. Might take 2 or 3.
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Re: What is this stuff?

Post by brewit2it »

I guess it makes sense. I did do a couple runs right after cleaning it so well but never noticed a copper taste. However, to be fair they were stripping runs so it might have been cleaned up in the spirit run.

I see where you are coming from Usge, but after looking at my notes it's been about 8 runs since I took it down to bare copper. Since then I haven't soaked it for more than 20min(at the very most) with the Star-San. So if it was gunk, wouldn't it have been at it's worst right after I took it back down to bare copper and slowly gotten better after that? If I had just done a thorough cleaning and and done a couple runs I would completely agree with you.

It really seemed to get like that after I started doing all grain washes, could it be that it's puking and burning on the inside?

Cheap solder(it is meant for potable water/lead free)?
It does have some pin hole leaks in it as well and I use flour paste.

Can someone post a pic of what a "normal" still looks like on the inside?
brewit2it
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Re: What is this stuff?

Post by brewit2it »

Alright, so I didn't end up doing that spirit run. But, I did end up getting some food grade citric acid.
I cleaned up the still head and liebig pretty well and now I'm going to run it and see if as much stuff forms this time.
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Re: What is this stuff?

Post by smokindave »

I am having this same thing happen on my first all grain bourbon stripping run. I have not run any chemical through my still since I did the original cleaning and sacrificial run. I only rinse it very well with hot water.

I also think this has something to do with the fact hat this all-grain. No idea why, but I have made many runs on this still with sugar heads of various grain components and never had any debris in any of my distillate.

I will flush and run again with another mash, and see what happens.
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Re: What is this stuff?

Post by Buster »

What was the out come of this I have the same problem.
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Re: What is this stuff?

Post by FL Brewer »

I had the same issue with one of my stripping runs. It was because the boiler was a little overfilled, or I ran too fast and the still puked. It wasn't as bad as what Brewit2it reported, but I don't distill the grains in the mash.

B2it - how much head space (clear space above the surface of the liquid) do you have? I have never experienced puking with the boiler 2/3 full or less.
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Re: What is this stuff?

Post by DeepSouth »

Shiny, metallic looking film that then becomes black and oily when touched is common with all grain distillation, as well as little black oily flecks in the distillate. There's multiple threads on it. Here's another thread discussing it.

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