Help- No alcohol in my corn wash

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skow69
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Re: Help- No alcohol in my corn wash

Post by skow69 »

I have 5 gallons of bourbon ready to run. I tested with a refractometer before fermentation: 13.5 bx (SG 1.056).
I drew a 4 oz. sample and tested: 4.75 bx (SG 0.997).
I boiled off 2 1/2 oz. (Oops.)
I added 2 1/2 oz. water and tested: 2.5 bx (SG 0.984).

Now, if someone will give me the formula to easily calculate the alcohol in my mash from those two numbers, 0.997 and 0.984, I will apologize for calling the OP a troll.
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Re: Help- No alcohol in my corn wash

Post by Mikey-moo »

skow69 wrote:I have 5 gallons of bourbon ready to run. I tested with a refractometer before fermentation: 13.5 bx (SG 1.056).
I drew a 4 oz. sample and tested: 4.75 bx (SG 0.997).
I boiled off 2 1/2 oz. (Oops.)
I added 2 1/2 oz. water and tested: 2.5 bx (SG 0.984).

Now, if someone will give me the formula to easily calculate the alcohol in my mash from those two numbers, 0.997 and 0.984, I will apologize for calling the OP a troll.
Regardless of a formula, your results show that it wasn't just water you were boiling off. Either that or the boiling caused thermal decomposition of other elements of the mash.

I'd quite like to know a formula though if there is one.
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Re: Help- No alcohol in my corn wash

Post by stevefzr »

Boy! I sure got some discussion happening. I can't take credit for inventing this, but makes perfect sense to me, which is why I was happy to follow it. Here's the process, including the formula at the last step. As I said, when I did this with my rum wash I calculated around 10%, cf a theoretical result of 11%.

•Procedure -

1. - Measure the specific gravity of your cleared wine sample and record the measurement along side the temperature the measurement was taken at.

2. - Correct for the temperature difference between the recorded temperature and the temperature the hydrometer was calibrated at, using the chart values for hydrometers calibrated at 20oC, and record the true specific gravity of the wine sample as SG1.

3. - Measure out exactly 250ml of the wine sample in a 250 ml volumetric flask - (see method)

4. - Empty the wine out of the volumetric flask into the distillation flask and employ a couple of distilled water rinses to remove wine residues from the volumetric flask into the distillation flask.

5. - Add some boiling chips to the distillation flask to prevent bumping when boiling the contents.

Caution: do not add the boiling chips once heating has commenced.

6. - Set up apparatus as per diagram using only the boiling flask. A vertical splash head may be fitted if desired.

6. - Apply heat to the bottom of the boiling flask and boil the wine down to approximately 125ml.

If the heat from the burner is to local or intense, position a tripod and heat diffuser (gauze), to disperse the applied heat, between the heat source and boiling flask.

7. - Allow the wine to cool down and using a funnel, carefully pour the remaining wine into the same 250ml volumetric flask used to measure the wine volume at the start.

8. - Rinse out the remaining wine residues with a few rinses of distilled water, into the same volumetric flask.

9. - Top up the contents of the volumetric flask with distilled water close to 250 ml, bring to 20oC in a hot water bath, then top up to the 250ml graduation mark. Stopper and mix (see method).

10. - Use a small amount the collected, diluted distillate to rinse a clean 250ml measuring cylinder. Then fill a 250ml measuring cylinder with the distillate.

11. - Using an specific gravity hydrometer, measure the specific gravity of the alcohol depleted wine solution and record your reading.

12. - Using a thermometer measure the temperature of the solution and record your reading.

13. - Correct for the temperature difference between the recorded temperature and the temperature the hydrometer was calibrated at, using the chart values for hydrometers calibrated at 20oC, and record the true specific gravity of the alcohol depleted wine solution as SG2.

13. - Using the equation below to calculate the alcohol concentration of you wine sample and record the result.

Alcohol (% v/v EtOH) = (SG2-SG1) / 2.11 * 1000
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Re: Help- No alcohol in my corn wash

Post by stevefzr »

To answer a few other points, all paraphrased:
"We normally start small". I did. I only tried 400l. My only previous ferment was 800l, but that was for rum. One day when I have time I'll post some pix of the automatic cut maker I made using ping pong balls to shut off cuts as they hit specific volumes. It means I just load my still, turn it on, and come back next morning to find all the cuts made. $15 temp sensors from ebay automatically control the boiler temp and switch the cooling pump on for the condenser. A timer switches it all off when it's finished. I got it down to 15 minutes work to empty the still, drain off the cuts, reload the still and hit the restart button.

"start small to refine the process and improve as you go" My brain doesn't work like that. I figure that I do the research up front and it should work, so don't waste time on small projects. Of course that didn't happen this time, but I'm hoping to recover it. I researched the yields for strip and collection runs used in France for cognac and applied the same rules to my distillation of 400l or champagne. It tastes quite good, first go. I did the same for my rum production and tasted that last week after 3 months on oak and a month with spices to simulate Captain Morgan's. I think that tastes pretty good too. I really can't afford for either of them to taste any better, or I wouldn't be able to stop drinking them :-) Jokes aside, my real reason for the corn mash is to practice on cheap corn before I start on the expensive peat dried barley for the scotch. I'll spend my time refining the process for the whisky. I will start with 200L and if that works, go back to a "normal" 800l batch. I'm still hoping for a drinkable product out of the bourbon tests though.

"taste it to see if it's sweet". I did that with my rum ferment and it had no sweetness at all, which I took to mean the ferment had finished. Trouble with doing that with the corn mash though is that the absence of sweetness could just mean (as I suspect) that the enzymes never made the sugar in the first place. Which brings me back to my original questions: would the ph of 3.5 cause the enzymes not to work, and will the enzymes still be present after a week sitting at 20C? My brewing buddy says the enzymes denature over time and would be gone by now, so I'll have to add more barley or a liquid enzyme. If the enzymes have gone, then doesn't that mean it's pointless to ferment of the grain so that the enzymes keep converting the starch?
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Re: Help- No alcohol in my corn wash

Post by BayouShine »

stevefzr wrote:One day when I have time I'll post some pix of the automatic cut maker I made using ping pong balls to shut off cuts as they hit specific volumes. It means I just load my still, turn it on, and come back next morning to find all the cuts made.
Damn, and to think I've been training my senses for years to pinpoint where a cut should be and all I needed were a few freakin' ping pong balls.

Sumbitch, what a waste of time that was!

:lol: :lol: :lol: :lol: :clap: :clap: :lol: :lol: :lol: :lol:
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Re: Help- No alcohol in my corn wash

Post by stevefzr »

BayouShine wrote:Damn, and to think I've been training my senses for years to pinpoint where a cut should be and all I needed were a few freakin' ping pong balls.

Sumbitch, what a waste of time that was!

:lol: :lol: :lol: :lol: :clap: :clap: :lol: :lol: :lol: :lol:
But once you have the cuts the way you like, do you sit there while the still runs making the cuts each time? My collection run takes about 4 hours. Once I have my low wines, my process is to run a load through the still to do a cut run, blend those by taste to get a product I like, then set up my auto cut taker to just reproduce that for the next 10 runs. The results are quite consistent. I can't taste the difference between the manually cut and blended batch and the auto cut ones, and I've saved 40+ hours of watching the still. On a good day I can get 3 runs done.
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Re: Help- No alcohol in my corn wash

Post by skow69 »

stevefzr wrote:Alcohol (% v/v EtOH) = (SG2-SG1) / 2.11 * 1000
For my trial SG1 = 0.997, SG2 = 0.984.
Alcohol yield = negative 27% (I'm pretty sure it's more like positive 7-8%)

To summarize:
* The OP has a fully automated still, presumably his first and home built, which operates totally unattended through the entire run.
* The still is controlled by the temperature of the boiler.
* He makes cuts (automatically) by volume, programmed to imitate the schedule of traditional Cognac production.
* He makes top shelf spirits on his first try with this method.
* He has done all the research necessary, but can't tell if pH level is responsible for his mash failure.
* pH level is the only option he has proposed for the mash failure.

You guys play with the troll. I'm out.
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Re: Help- No alcohol in my corn wash

Post by Mikey-moo »

He's got balls though...

Ping-pong balls.
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Re: Help- No alcohol in my corn wash

Post by stevefzr »

Oh well. last try. I've researched the distillation, but not mashing. I didn't say my results were top shelf, but those who've tried them enjoy them.

skow69, your SG readings seem wrong. You boiled off alcohol and replaced it with water, yet your SG went down. Doesn't make sense does it? As I mentioned, I didn't create that method, I just found it and used it.

Anyway, in the absence of any advice on how to fix my corn mash, here's my plan:
I tasted the wash and it's quite sour, with no sign of sugar. I'll do an iodine test, which I'm pretty confident will show starch. Assuming it does, I'll boil the mash seeing as it's been sitting for over a week now and might have a bit of bacteria, then cool, balance PH back to around 5 with a bit of caustic soda, add some enzymes, then take the mash to 45, 62 then 73 °C, pausing for a few hours at each temp. Does that sound like it'll work? After that, I'll do an iodine test again and if conversion has worked this time I'll cool and pitch my yeast.

I'll check the responses to see if anyone's interested in hearing the results
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Re: Help- No alcohol in my corn wash

Post by rad14701 »

This topic doesn't smell good to me at all... Questionable calculations... Extremely large ferments and distillations for a hobby scale forum... Unattended still operation... Ping pong balls in high proof alcohol... Need I continue...???
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Re: Help- No alcohol in my corn wash

Post by HDNB »

i still don't get it. :cry:

let's go ride bikes.
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Re: Help- No alcohol in my corn wash

Post by MichiganCornhusker »

stevefzr wrote:Alcohol (% v/v EtOH) = (SG2-SG1) / 2.11 * 1000
Never mind the ping pong balls, the ton of rum, and going on holiday with the still running, I am curious about this method of determining alcohol content.
If you suspected that your fermentation had turned to vinegar, would this help determine if any alcohol was remaining?

Just not sure about that math.
I found a chart online that showed an SG for ethanol in water.
10% = SG 0.987

If I have 10% ethanol in water, SG 0.987, and boil out half, refill with water, I should get 1.000 assuming, for simplicity, all alcohol is removed. (I know it's not)
So 0.013 difference. 0.013/2.11 * 1000 = 6.16%, not 10%
Why not just have a multiplier, like 770? 0.013 x 770 = 10% (the chart seemed to be fairly linear)

Suppose there is other stuff in the water, so SG = 1.00 with a 10% wash.
If I boil the alcohol out, SG would increase to 1.013 assuming all alcohol is out and the "stuff" isn't volatile and didn't boil out at all.

I don't see the point in refilling the sample to the original volume. And maybe that's where the formula is horked.
Why not just take the SG for the remaining 1/2 and divide by half?
In my example above, you would end up with the 1/2 volume sample measuring SG .026, so 0.026/2 * 770 = 10%
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Re: Help- No alcohol in my corn wash

Post by Kegg_jam »

Holy balls this is overly complicated.

Was there ever any signs of fermentation? You know, little bubbles of CO2 or perhaps a massive Krausen that explodes all over the floor...
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Re: Help- No alcohol in my corn wash

Post by MichiganCornhusker »

Kegg_jam wrote: or perhaps a massive Krausen that explodes all over the floor...
Always a good sign! :lol: :thumbup:
Yeah, I sure can't see where this method would ever replace simple OG-FG.
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Re: Help- No alcohol in my corn wash

Post by MichiganCornhusker »

stevefzr wrote:skow69, your SG readings seem wrong. You boiled off alcohol and replaced it with water, yet your SG went down. Doesn't make sense does it? As I mentioned, I didn't create that method, I just found it and used it.s
Steve, could you provide an example, with figures, from when you have used this method?
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Re: Help- No alcohol in my corn wash

Post by NZChris »

skow69 wrote:
stevefzr wrote:Alcohol (% v/v EtOH) = (SG2-SG1) / 2.11 * 1000
For my trial SG1 = 0.997, SG2 = 0.984.
Alcohol yield = negative 27% (I'm pretty sure it's more like positive 7-8%)
Using your numbers, I get negative 6.16, not negative 27%, so I don't know how you arrived at the 27%. However, the minus figure is because you transposed SG1 & SG2, so using Steve's method correctly, your result would have been 6.16%, much closer to your estimate.
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Re: Help- No alcohol in my corn wash

Post by NZChris »

When stripping the same wash, subsequent strips will repeat the results of the first, making predicting a foreshot cut and a shut down point easy. The foreshot I do on volume and that would be easy to automate, it could also be done on weight. It could also be safely done with a ping pong ball, because the foreshots are not for human consumption.

The shutdown can be done on boiler temperature, so that is even easier to automate.

For spirit running the same low wines each time, temperatures, weights, abvs, light refraction and volumes can all be used to replicate your initial cut, whether it is automated, or you are swapping jars manually.
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Re: Help- No alcohol in my corn wash

Post by jb-texshine »

Mitch,let me see if I'm understanding correctly....
(Still seems like a bassackwards way to do it but...)
1take a sample 2 take a reading via hydrometer 3 boil away half of the sample 4add water to reach original volume 5 take hydrometer reading 6....? and then I'm lost.
Example...
1&2 reading 0.998
3&4 boil away half and replace with water
5 reading 1.000
Is there a mathematical formula missing?
As is all it does is show that there was some alcohol in the wash. Reading the hydrometer at 0.998 tells the same without the boil. So will dipping a finger and tasting it.
Just don't see how it will tell you HOW MUCH alcohol is in the mash.

To me it seems like a combined effort using a hydrometer in place of a vinometer.

And just confused as to why,if you have a hydrometer,you wouldn't just get an Og and Fg and do the math.no boiling required.
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Re: Help- No alcohol in my corn wash

Post by shadylane »

stevefzr wrote:..... my original questions: would the ph of 3.5 cause the enzymes not to work, and will the enzymes still be present after a week sitting at 20C? My brewing buddy says the enzymes denature over time and would be gone by now, so I'll have to add more barley or a liquid enzyme. If the enzymes have gone, then doesn't that mean it's pointless to ferment of the grain so that the enzymes keep converting the starch?

Low pH will denature enzymes.
Since the pH had dropped to 3.5, that probably means the mash had fermented.
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Re: Help- No alcohol in my corn wash

Post by jb-texshine »

shadylane wrote:
stevefzr wrote:..... my original questions: would the ph of 3.5 cause the enzymes not to work, and will the enzymes still be present after a week sitting at 20C? My brewing buddy says the enzymes denature over time and would be gone by now, so I'll have to add more barley or a liquid enzyme. If the enzymes have gone, then doesn't that mean it's pointless to ferment of the grain so that the enzymes keep converting the starch?

Low pH will denature enzymes.
Since the pH had dropped to 3.5, that probably means the mash had fermented.
I say taste it... if it's sweet it ain't done. If it is sour(dry wine) it's done.
Unconverted grain with water will sour(catfish bait) In a day or two. If it smells that kinda sour you'll know!
Simplest solution to the op is just taste it and see if it's sweet or sour(dry wine). If it's dry sour ,charge it and run.

Then read up on how to properly use a hydrometer.
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Re: Help- No alcohol in my corn wash

Post by shadylane »

On a side note.
If you want success, watch Pintoshines video on using alpha and gluco to convert a corn mash.
And buy some of the enzymes.
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Re: Help- No alcohol in my corn wash

Post by Tater »

This post is just a repeat post of op from another forum. Where he got pretty much the same response.Stop feeding the troll
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Re: Help- No alcohol in my corn wash

Post by jb-texshine »

Ih.
Just my guess
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Re: Help- No alcohol in my corn wash

Post by NZChris »

I would have thought that someone who brings to the forum a solution to a problem, has some value. I could have done with his method for evaluating the abv of a failed corn mash I had only a couple of weeks ago. Using this method, I would have known to chuck it in the compost instead of playing the eternal optimist and putting it in the boiler.
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Re: Help- No alcohol in my corn wash

Post by stevefzr »

Tater wrote:This post is just a repeat post of op from another forum. Where he got pretty much the same response.Stop feeding the troll
I don't recall posting this in another forum. Which one?

I did taste it and it was sour, but I don't know what it would taste like if the enzymes had never converted the starch. I guess I'll do a small batch and measure the ph and SG before I mash it. I'll taste it as well. That'll tell me if I've had any enzyme reaction. There were a few little bubbles, but nothing like the rum which had a big head form in the fermenter which left a ring up the top. No evidence of a ring with the corn wash. To be honest, I didn't think I'd get a sensible SG with all the grain still in fermenter. Now I think about it, the addition of solids shouldn't make any difference. A boat won't higher or lower because of the amount of solids in a lake. Only the soluble components will make a difference.

I'm a bit confused why some people seem upset that that I went straight to distilling 400l of champagne for cognac and moved on to 800l of sugar and molasses wash to do rum. Why do you care? Even if it had failed, what's the problem? Maybe it's because I don't see distilling as a hobby? For me it's a means to a large supply of spirits. Once I have what I need, I'll stop distilling. My objective is to get a worthwhile product as economically (time and money) as possible, not to spend years refining my craft. I expect the majority of you fall into the latter category, but surely I'm not the only one of the former?
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Re: Help- No alcohol in my corn wash

Post by stevefzr »

shadylane wrote:On a side note.
If you want success, watch Pintoshines video on using alpha and gluco to convert a corn mash.
And buy some of the enzymes.
That was my plan. Rather than adding my barley, I was going to buy liquid enzyme. I tried Grain and Grape here in Melbourne but they said they didn't sell the gluco-Amylase and α-Amylase I need. Can anyone tell me where to buy these in Aus and what they're called? I need enough to convert 400l of wash with 50kg of cracked corn and about 10kg each of cracked wheat and malted barley. Anyway, thanks for the tip. I found the video on youtube. If I can just find a source for the enzymes I should be set to go.
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Re: Help- No alcohol in my corn wash

Post by shadylane »

If you can't find the enzymes locally, Enzymash ships overseas.
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Re: Help- No alcohol in my corn wash

Post by Mikey-moo »

stevefzr wrote:I'm a bit confused why some people seem upset that that I went straight to distilling 400l of champagne for cognac and moved on to 800l of sugar and molasses wash to do rum. Why do you care? Even if it had failed, what's the problem? Maybe it's because I don't see distilling as a hobby? For me it's a means to a large supply of spirits. Once I have what I need, I'll stop distilling. My objective is to get a worthwhile product as economically (time and money) as possible, not to spend years refining my craft. I expect the majority of you fall into the latter category, but surely I'm not the only one of the former?
Typically those in the former category are doing this for profit. And they also do it on the scale you are doing it. That makes us suspicious. Also you run your still unattended which is a safety issue.

Where did you get 400L of champagne from? Must have cost a lot to ship to Australia from France...
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Re: Help- No alcohol in my corn wash

Post by stevefzr »

Typically those in the former category are doing this for profit. .......Also you run your still unattended which is a safety issue.
Hmmm. So I'm presumed guilty until proven innocent? The law turns a blind eye to distilling here until you sell some. I have no intention of selling a single drop.

As for safety, my still is electric, and has controllers to make sure it can't boil dry and runs off a timer to make sure it doesn't continue to idle if something happened to me while I was out. The boiler temp controller will also stop it overheating if the condensor pump should fail. It's in a separate concrete outbuilding with a door but no windows and well away from trees and shubbery. It wasn't built as a bushfire shelter, but could serve that purpose. If the still did manage to explode, then no one would probably even know. There's more chance of an accident leaving a slow cooker unattended in the kitchen. The important thing though is that I feel it's safe. So while some here are concerned about the unattended aspect, I personally wouldn't dream of using a reflux still to produce a couple of litres of 90+% ABV alcohol in my kitchen over a gas cooker, even if it was attended. How many people remain in attendance the whole time anyway? Friends' fathers who made grappa always set a timer or watched a clock and went and checked the still every 20 minutes or so, and invariably forgot at some stage. Do all of you sit next to your still and watch it the whole time it's running?


Where did you get 400L of champagne from? Must have cost a lot to ship to Australia from France...
Technically, it's sparkling wine as it's made locally, not in the champagne district of france. By the same rules, I'm making brandy, not cognac as it was not aged at least two years in French oak barrels from Limousin or Tronçais. Tastes like cognac though. The champagne came from a winery that was closing down. It had been sitting in storage too long, like 15 years, and considered unfit for sale as it could impact their brand. It still tasted ok and had lots of fizz. 50c a bottle. I bought 400 bottles but wish I'd bought more. I thought I'd never need that much cognac, but I used some as a base for grand marnier and limoncello and it's so popular that it is disappearing way too fast. When I first made the cognac, it was ok, but not great, although I got no complaints. I thought the liqueurs would be a good way to use it up. Then I tried the cognac again after 6 months on oak and it's so good I'm keeping the rest as straight cognac. There was also the great cognac disaster of 2016, where I felt under a barrel with 20l of 65% ABV cognac in it to check it wasn't leaking. It had been there for 3 months, but I noticed a coin sized wet spot under it. I felt a drop on the bottom of the barrel, but was on my way out and resolved to fix it in a few hours when I got back. I came back to find the equivalent of 30 bottles of cognac on the floor. I'd pre-soaked the barrel with water of course, but I suspect I'd wiped off a drop of water over a tiny leak, and the surface tension of the water had been all that was holding the cognac in. The alcohol in the barrel would have less surface tension, so once the water drop was gone, it was free to run out. I now have catch trays under my rum barrels and check them weekly.

The only reason I went so big on the rum quantity was to use up the molasses. I used it as an opportunity to test fermenting at scale for when I do my whisky production. I don't drink rum so I had to buy a bottle to find out what mine should taste like. The spiced rums tasting pretty good, so I think I'll have no problems finding friends to take a few bottles. If the whisky is successful, then that'll be a different matter. I figure 20 bottles a year should suffice for myself and friends, so 30 years of retirement is going to require 600 bottles! On that basis, I'm going to have to increase my production size! I haven't done the sums, but I guess I'd need about 5 batches at 800l a time to get 600 bottles, provided I can get my wash above 10%
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Mikey-moo
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Re: Help- No alcohol in my corn wash

Post by Mikey-moo »

stevefzr wrote: Hmmm. So I'm presumed guilty until proven innocent?
If we presumed you were guilty your account would be blocked. Stop playing the victim. You're acting suspiciously and breaking forum rules. What kind of treatment were you expecting?
stevefzr wrote: Do all of you sit next to your still and watch it the whole time it's running?
I can only speak for myself here. But yes. Yes I do.

Good luck with the whisky.
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