Failing Iodine test
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Failing Iodine test
Today is the 5th bourbon batch so far. It's the coolest thing I've done in a really long time, and I am having a blast. However, i have not solved the problem of not ending up with enough bourbon at the end of a run. I typically have 13-15 gallons of mash after fermentation (7-14 day period), and the best I usually end up with is about a gallon of product. Isn't that a small amount? I was expecting 2-3 gallons?
On my latest run, i corrected my PH problem for the first time, thinking that PH was contributing to low starch production, which led to low sugar production, etc. My was was PH 5.4 before the start of this run with 15 gallons of water. I put in 18 pounds of corn maize @ 190 degrees. After 45 minutes, I added enzymes. Waited 45 more minutes. Iodine test still failed. added more enzymes, waited 45 more minutes, still failed. Rinse, wring, repeat 2 more times. I have never passed an iodine test in any batch. Is the failing Iodine test a contributor to low production of alcohol? Or something else? And when I say "fail" an Iodine test.....it turns black as fast as I can snap my fingers....it's not even borderline.
i put a picture of the iodine test as an attachment.
Any pointers, suggestions, corrective actions I could take would be greatly appreciated. Other than quantity.....everything else is spot on!
JP
On my latest run, i corrected my PH problem for the first time, thinking that PH was contributing to low starch production, which led to low sugar production, etc. My was was PH 5.4 before the start of this run with 15 gallons of water. I put in 18 pounds of corn maize @ 190 degrees. After 45 minutes, I added enzymes. Waited 45 more minutes. Iodine test still failed. added more enzymes, waited 45 more minutes, still failed. Rinse, wring, repeat 2 more times. I have never passed an iodine test in any batch. Is the failing Iodine test a contributor to low production of alcohol? Or something else? And when I say "fail" an Iodine test.....it turns black as fast as I can snap my fingers....it's not even borderline.
i put a picture of the iodine test as an attachment.
Any pointers, suggestions, corrective actions I could take would be greatly appreciated. Other than quantity.....everything else is spot on!
JP
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Re: Failing Iodine test
Bits will almost always turn black, but...
Corn takes either lots of heat or lots of time to gelatinise, and then you need to convert the starch to sugar. In general if you're using the easy corn mashing method (add corn to boiling water, stir, maybe add enzymes to help keep things loose), then you need the fifth step... wait. Folks often mix their corn in at night, wrap the container up in blankets to keep the heat in, and come back to it the following day.
What's your actual recipe? What enzymes are you adding? Are you following one of the T+T recipes, or does this come from somewhere else? Do you have a hydrometer for measuring teh gravity at the start and end of fermentation? How are you deciding that fermentation is over?
My lowest yield bourbon came from a set of batches where I didn't leave the corn long enough (a couple of hours max) and I suspect most of the corn was still ungelatinised some weeks later when I squeezed the grains.
Corn takes either lots of heat or lots of time to gelatinise, and then you need to convert the starch to sugar. In general if you're using the easy corn mashing method (add corn to boiling water, stir, maybe add enzymes to help keep things loose), then you need the fifth step... wait. Folks often mix their corn in at night, wrap the container up in blankets to keep the heat in, and come back to it the following day.
What's your actual recipe? What enzymes are you adding? Are you following one of the T+T recipes, or does this come from somewhere else? Do you have a hydrometer for measuring teh gravity at the start and end of fermentation? How are you deciding that fermentation is over?
My lowest yield bourbon came from a set of batches where I didn't leave the corn long enough (a couple of hours max) and I suspect most of the corn was still ungelatinised some weeks later when I squeezed the grains.
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Re: Failing Iodine test
thank you for the quick response.
I got my water (15 gallons) to PH 5.4, then heated to 190 degrees. added 18 pounds of corn maize, and then let it sit for 60 minutes, while applying occasional heat to maintain 190. I stirred about every 5 minutes.
Took an iodine test (failed). added 1.5 tsp enzymes, stirred occasionally, still at 190 degrees, for another 60 minutes.
took another iodine test, failed again, added another 1.5 tsp enzymes, continued to hold heat at 190 for '60 minutes.
Failed 3rd iodine test after 3 hours.....and moved on.
a total of 3 hours at 190 degrees.
Enzyme is LD Carlson Amylase Enzyme. This is not a T&T recipe. i didn't know about your T&T's until I had already started working with this one. 70%corn, 20%wheat, 10% M-barley. i measure starting gravity, when I can, sometimes the mash is too thick and I can't get an accurate reading,
AFter 2 weeks of fermenting, i check the fermenter and if the grain cake that usually rises to the top early on has fallen to the bottom....and there are no bubbles....i assume fermentation is over.
I got my water (15 gallons) to PH 5.4, then heated to 190 degrees. added 18 pounds of corn maize, and then let it sit for 60 minutes, while applying occasional heat to maintain 190. I stirred about every 5 minutes.
Took an iodine test (failed). added 1.5 tsp enzymes, stirred occasionally, still at 190 degrees, for another 60 minutes.
took another iodine test, failed again, added another 1.5 tsp enzymes, continued to hold heat at 190 for '60 minutes.
Failed 3rd iodine test after 3 hours.....and moved on.
a total of 3 hours at 190 degrees.
Enzyme is LD Carlson Amylase Enzyme. This is not a T&T recipe. i didn't know about your T&T's until I had already started working with this one. 70%corn, 20%wheat, 10% M-barley. i measure starting gravity, when I can, sometimes the mash is too thick and I can't get an accurate reading,
AFter 2 weeks of fermenting, i check the fermenter and if the grain cake that usually rises to the top early on has fallen to the bottom....and there are no bubbles....i assume fermentation is over.
Re: Failing Iodine test
I don't believe you are using the correct enzyme if its the LD Carlson powder enzyme.
I may be wrong but i don't think it works at those temps. You need to get hi temp amylase like Sebstar HTL or something.
Then you still have your low temp enzyme you put in at 150 or below.
I may be wrong but i don't think it works at those temps. You need to get hi temp amylase like Sebstar HTL or something.
Then you still have your low temp enzyme you put in at 150 or below.
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Re: Failing Iodine test
so I literally have the batch that i'm describing in this post, in the pot right now as I am typing this. SO, If I let the gelatinized corn get BELOW 150, i can try putting in the LD Carlson powder that I have now?
i will get the Sebstar for future batches, but if I can save this current batch...i would like to do that. Does it matter if I put the enzyme in ahead of the other 2 grains?
i will get the Sebstar for future batches, but if I can save this current batch...i would like to do that. Does it matter if I put the enzyme in ahead of the other 2 grains?
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Re: Failing Iodine test
Don't worry about the order. If your enzyme is happy at normal (malted barley) mashing temps then you can put it in with the other grains. It's possible that the malted barley will do some conversion as well. If your amylase is just alpha-amylase then it won't be making the short chain sugars that your yeast are looking for so even with decent starch conversion you might get a low yield due to lots of unfermentable sugars. Let the temperature drop as slowly as you dare when you put the barley and wheat in. The longer it sits, at the slightly lower end of mashing temps, the more fermentable sugars you'll get (and so the higher the yield).
AG mashes and fruit pulp musts are the reason that I bought a refractometer. It's far from indispensable, but it's really good to be able to measure gravity with only a drop of liquid.
Best of luck. Keep us posted on how the batch turns out.
AG mashes and fruit pulp musts are the reason that I bought a refractometer. It's far from indispensable, but it's really good to be able to measure gravity with only a drop of liquid.
Best of luck. Keep us posted on how the batch turns out.
"I have a potstill that smears like a fresh plowed coon on the highway" - Jimbo
A little spoon feeding *For New & Novice Distillers
A little spoon feeding *For New & Novice Distillers
Re: Failing Iodine test
You definitely need to use some t&t recipes until you have more experience but as I'm reading your recipe you have:
18 pounds corn maize
7.5 pounds wheat
2.5 pounds M barley
That sounds like a decent recipe (maybe).
That's 1.8 lbs/gallon grain to water.
At 100% conversion you'll end up a little over 1.06 specific gravity. Most people consider 85% pretty good which would mean a little less than 1.055. If everything works right and it ferments dry (1.00 or less sg) you'll be putting 7% ABV in the boiler, with 14 gallons you should get about 3 gallons at 30% on the stripping run.
So yes, your efficiency is very low. Your iodine test indicates the same if that's when it's ready for yeast. Yes pH matters but that's probably not the cause of your problems.
Corn maize - what do you mean by this? Whole kernel corn? Cracked corn? Either one ground (milled) after you got it?
In general the finer it is the easier it is to gelatinize. Most here use about the consistency of corn meal. At 190F it will take at least a couple of hours to gelatinize corn meal. Iodine test at this point is meaningless, it says you have starch which is what you want. At this point you should have mush.
Wheat? Is this malted wheat? Milled?
M barley? Malted barley? Milled?
You want both milled. Any malted grains you want to add BELOW 150F same goes for any enzymes that don't state they are high temperature tolerant. You use malts for their natural enzymes if your wheat isn't malted you definitely need to use enzymes. The iodine test IS relevant now, as the starch gets converted to sugar the iodine test will indicate less starch. When it shows no starch or you just give up you should cool it to 90F or less then pitch yeast.
The sebstar and sebamyl enzymes work well. The sebamyl is pH sensitive, make sure you get the pH right before adding it. I think they're expensive and until I adjusted pH for the sebamyl I didn't get good results. If you use them watch Pinto's YouTube instructions
I'm using ferm-solutions enzymes now but the min quantity is one liter and shipping adds cost. But I'm very happy with them especially the wider pH range.
18 pounds corn maize
7.5 pounds wheat
2.5 pounds M barley
That sounds like a decent recipe (maybe).
That's 1.8 lbs/gallon grain to water.
At 100% conversion you'll end up a little over 1.06 specific gravity. Most people consider 85% pretty good which would mean a little less than 1.055. If everything works right and it ferments dry (1.00 or less sg) you'll be putting 7% ABV in the boiler, with 14 gallons you should get about 3 gallons at 30% on the stripping run.
So yes, your efficiency is very low. Your iodine test indicates the same if that's when it's ready for yeast. Yes pH matters but that's probably not the cause of your problems.
Corn maize - what do you mean by this? Whole kernel corn? Cracked corn? Either one ground (milled) after you got it?
In general the finer it is the easier it is to gelatinize. Most here use about the consistency of corn meal. At 190F it will take at least a couple of hours to gelatinize corn meal. Iodine test at this point is meaningless, it says you have starch which is what you want. At this point you should have mush.
Wheat? Is this malted wheat? Milled?
M barley? Malted barley? Milled?
You want both milled. Any malted grains you want to add BELOW 150F same goes for any enzymes that don't state they are high temperature tolerant. You use malts for their natural enzymes if your wheat isn't malted you definitely need to use enzymes. The iodine test IS relevant now, as the starch gets converted to sugar the iodine test will indicate less starch. When it shows no starch or you just give up you should cool it to 90F or less then pitch yeast.
The sebstar and sebamyl enzymes work well. The sebamyl is pH sensitive, make sure you get the pH right before adding it. I think they're expensive and until I adjusted pH for the sebamyl I didn't get good results. If you use them watch Pinto's YouTube instructions
I'm using ferm-solutions enzymes now but the min quantity is one liter and shipping adds cost. But I'm very happy with them especially the wider pH range.
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- jonnys_spirit
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Re: Failing Iodine test
I consistently yield about 2.5 - 3 gallons of cut barrel proof @ ~120pf with approximately 100# of grains. I use the large batch mashing method and let it sit overnight after mixing with boiling water or until it drops to 150*F to add malts and glucoamylase. I do use the high temp enzyme too. Starting a mash around Sat morning and I'm pitching yeast Sunday evening or Monday morning.
Time @ temp helps.
It does take a lot of beer to make whiskey
Cheers,
j
Time @ temp helps.
It does take a lot of beer to make whiskey

Cheers,
j
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i prefer my mash shaken, not stirred
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i prefer my mash shaken, not stirred
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Re: Failing Iodine test
LD Carlson website has a PDF showing their alpha amylase is high temp tolerant, up to 230*F (110*C). I'm thinking 70% corn + 20% wheat + 10% malted(?) barley might be a bit light on the malt if not adding extra low temp gluco-amylase. If you have more malted barley on hand, adding more won't hurt. If the mash has already dropped lower than 145*F, you could cook more malted barley separately on a stovetop and add it to the mash. The enzymes will continue to work during ferment, but more slowly.
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Re: Failing Iodine test
+1 to Jonny.jonnys_spirit wrote: ↑Thu Sep 21, 2023 2:27 pm… Time @ temp helps…
It does take a lot of beer to make whiskey.
JP, your protocol needs to be polished.
190*F is for gelatinization of the corn grist. Grind it to a fine cornmeal and heat and hold it at 190*F for a couple of hours. The porridge will get thick, almost like pancake batter.
Then, drop the temperature to 150*F and add your malted barley (or glucoamylase enzymes, if you go that route). Hold temperature at 148-150*F until the iodine test says you’re converted. This may take an hour, two, ore more. Some brewers here let it rest overnight. But, you need to be patient. And hold the temperature correctly.
After full conversion, you can cool the mash down to pitching temperature (80-100*F for an ale or bakers yeast). Be sure to aerate the wort good so the yweast has plenty of O2 to reproduce.
Then, just wait for the ferment to attenuate and the yeast to flocculate (clear).
Good luck.
ss
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Re: Failing Iodine test
I've looked at LD Carlson as the turboyeast of the enzyme world for no good reason. All the liquids I've seen list 190F max. I'll have to look into their products if I ever use up the ferm-solutions stock in my fridge!BoilerMaker wrote: ↑Thu Sep 21, 2023 2:34 pm LD Carlson website has a PDF showing their alpha amylase is high temp tolerant, up to 230*F (110*C).
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Re: Failing Iodine test
Use a different brand of enzymes, such as SEBstar HTL and SEBamylJPolsgrove wrote: ↑Thu Sep 21, 2023 10:14 am
Any pointers, suggestions, corrective actions I could take would be greatly appreciated. Other than quantity.....everything else is spot on!
JP
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Re: Failing Iodine test
Yea I agree, a liter bottle of ferm-solutions goes a long way, though it's good to have other options too.elbono wrote: ↑Thu Sep 21, 2023 2:53 pmI've looked at LD Carlson as the turboyeast of the enzyme world for no good reason. All the liquids I've seen list 190F max. I'll have to look into their products if I ever use up the ferm-solutions stock in my fridge!BoilerMaker wrote: ↑Thu Sep 21, 2023 2:34 pm LD Carlson website has a PDF showing their alpha amylase is high temp tolerant, up to 230*F (110*C).
This is what came up when I searched the LD Carlson website.
https://storefront.ldcarlson.com/storef ... em-id=3580
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Re: Failing Iodine test
I figure your probably right.jessespa wrote: ↑Thu Sep 21, 2023 12:23 pm I don't believe you are using the correct enzyme if its the LD Carlson powder enzyme.
I may be wrong but i don't think it works at those temps. You need to get hi temp amylase like Sebstar HTL or something.
Then you still have your low temp enzyme you put in at 150 or below.

Here's the powdered LD Carlson
Re: Failing Iodine test
I use the LD Carlson enzymes. Both alpha-amylase and gluco-amylase are necessary. Neither are hi temp so both are added after the temp drops below 150 deg. If I begin steeping corn in the afternoon, try to hold that temp as long as possible by wrapping the barrel in a blanket, it’s ready for enzyme/malts by bedtime and will easily convert overnight. In the morning the grain mass will have settled and leaves a clear, sticky sweet liquid on top that I can easily check for OG. After that I ferment on the grain.
A couple of key points I’ve pulled together-
1. Enzyme needs some free calcium to work effectively. Add a few calcium supplement tabs to your corn grind.
2. Ph is also key, you’ve noted that also.
3. Grind corn as fine as you can to get at the starches, coarse corn meal. Some commercial recipes will even use corn starch- same same just without husk, germ, oil (flavor?)
4. If you’re relying upon malt barley for enzyme content you’ll need 6-row as it has a lot more dP than 2-row. 2-row for flavor, 6-row for dP.
5. Holding the corn at the high temps as long as possible is only going to help make starches more available to eventual enzyme activity. Once malt and enzyme has been added (at the proper temp), then keeping it for as long as possible between 125 and 150 is going to help further conversion. As long as you stay out of the vessel it is above critical innoculation temperature and it’ll be fine until reaching pitch temps.
Beyond that we aren’t sure from the description of the volume spoken of represents that obtained after sparge, or if fermentation is on the grain and this volume is racked at full beer strength, or what. Nor at what strength the final product volume is.
From a 70# grain mass with 30 odd gallons of water addition, I’ll get about 1.5 gal @ 72% from the first draw out of the fermenter (enough to fill the still pot and run with a partial reflux).
But since I ferment on the grain I pull it off a little differently for the strip process. All in all I’m probably getting about 2.5 gal or maybe a bit more cut to 65% for aging from the full batch. In fact by adding an extra strip step to get more from the grain mass I’ve gotten about 30% more. It’s been pretty consistent and while I’ve never actually checked for a complete conversion, the taste and the product yield seem to fit my back of napkin estimates.
A couple of key points I’ve pulled together-
1. Enzyme needs some free calcium to work effectively. Add a few calcium supplement tabs to your corn grind.
2. Ph is also key, you’ve noted that also.
3. Grind corn as fine as you can to get at the starches, coarse corn meal. Some commercial recipes will even use corn starch- same same just without husk, germ, oil (flavor?)
4. If you’re relying upon malt barley for enzyme content you’ll need 6-row as it has a lot more dP than 2-row. 2-row for flavor, 6-row for dP.
5. Holding the corn at the high temps as long as possible is only going to help make starches more available to eventual enzyme activity. Once malt and enzyme has been added (at the proper temp), then keeping it for as long as possible between 125 and 150 is going to help further conversion. As long as you stay out of the vessel it is above critical innoculation temperature and it’ll be fine until reaching pitch temps.
Beyond that we aren’t sure from the description of the volume spoken of represents that obtained after sparge, or if fermentation is on the grain and this volume is racked at full beer strength, or what. Nor at what strength the final product volume is.
From a 70# grain mass with 30 odd gallons of water addition, I’ll get about 1.5 gal @ 72% from the first draw out of the fermenter (enough to fill the still pot and run with a partial reflux).
But since I ferment on the grain I pull it off a little differently for the strip process. All in all I’m probably getting about 2.5 gal or maybe a bit more cut to 65% for aging from the full batch. In fact by adding an extra strip step to get more from the grain mass I’ve gotten about 30% more. It’s been pretty consistent and while I’ve never actually checked for a complete conversion, the taste and the product yield seem to fit my back of napkin estimates.
Re: Failing Iodine test
Just a suggestion, if I didn't read wrong, adjust the pH before adding the corn..... I recommend doing the opposite procedure
Re: Failing Iodine test
Personally, I’ve always adjusted the ph of the water a bit during heating. Mostly just because I want to keep the mineral scale at bay during heating but also because I will need to lower the ph for optimal enzyme activity. I’ve never thought about it in terms of starch production.
Is there a direct correlation between ph and available starch? We know that ph will most certainly affect starches and how they denature but how does that affect their conversion to sugars? I’d think keeping starches soluble is key to obtaining optimal conversion and based upon some experiences I’ve had with starch process streams that means avoiding high ph levels, but typically more in the 9.5-10 range before you wind up with a disaster.
This would be a great question for anyone with in-depth knowledge of wet milling processes.
Is there a direct correlation between ph and available starch? We know that ph will most certainly affect starches and how they denature but how does that affect their conversion to sugars? I’d think keeping starches soluble is key to obtaining optimal conversion and based upon some experiences I’ve had with starch process streams that means avoiding high ph levels, but typically more in the 9.5-10 range before you wind up with a disaster.
This would be a great question for anyone with in-depth knowledge of wet milling processes.