Great Apple brandy: Toasted or charred barrel?

Treatment and handling of your distillate.

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Slow & Steady
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Slow & Steady »

[quote="The Chemist"]"Age" is a small word with a pile of meanings...

"Once the wood components are in the distillate, aging will proceed whether in barrel, glass, or stainless steel."
************************************
Hmmm... I don't get any aging after I move my distillate to glass. My wine continues to age due to the nature of the many esters created during fermentation. That is the reason that I age my hard cider for such a long time. The clear spirit is delicious and aging in a used barrel creates a very fine spirit in 3 years time. The aging process stops for 40% ABV and above distillates, at least that is my experience.

Currently, new 5 gallon White Oak Char barrels cost about $140 each from The Barrel Mill and about $170 from 1000 Barrels. I don't think that a bad price considering the improvement it makes on my Brandy.

You do need to plan ahead. I start a batch of Bourbon equal to the amount of Brandy I will produce. The bourbon barrel ages while the hard cider ages as a wine in those 59 Gallon Plastic barrels that apple juice concentrate is imported in from Argentina. When the Bourbon is done the barrel is perfect for aging Brandy.

It is my experience that the 5 Gallon Barrel shortens the time needed to achive the desired amount of Oak Flavor so the used barrel becomes a valuable item for long term slow aged Brandies and Single Malts Whiskeys.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by The Chemist »

HookLine wrote:Not clear in my mind. Does 3) type ageing still occur if fresh white spirit is stored in an inert airtight container?
Some reaction in type 3 will proceed in an inert, airtight container, but some require oxygen. If the oxygen is there, they will 'go', if not, they won't.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Slow & Steady »

I should have written:
The aging process stops for 40% ABV and above distillates after I put it in glass containers, at least that is my experience.
"If it worthwhile then it is worth a little extra time and effort... all impatiens ever got me was burned fingers and charred eyebrows"
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Slow & Steady »

punkin wrote:I appreciate you input slowandsteady, you sound like you have an indepth knowledge of this subject.
Does your work bear on this?
No... not as a job... but I have enjoyed twenty six years as a hobbist "wine maker/distiller".
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Re: Great Apple brandy: Toasted or charred barrel?

Post by theholymackerel »

Slow & Steady wrote:I should have written:
The aging process stops for 40% ABV and above distillates after I put it in glass containers, at least that is my experience.
In my experience, a bottle that sat on the back of a shelf for a year is way better than it was as a fresh spirit. Maybe yer sniffer and taster has been dented by tobacco?
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Slow & Steady »

theholymackerel wrote:In my experience, a bottle that sat on the back of a shelf for a year is way better than it was as a fresh spirit. Maybe yer sniffer and taster has been dented by tobacco?
No... I'm not a smoker, but this I know for sure, whisky aging refers to the time spent in a wooden barrel.

The US federal law for Bourbon is quite specific concerning claims of Age or Aging. The product can only claim the amount of time it was in a Oak Barrel.

Scottish law regulates the aging claim to the same criteria for all Single Malt Whiskey.

I'm not an expert, so my claim means nothing, but if I tell you it is 3 years old, I'm referring to the time it spent in a cask not in a bottle on the shelf.

Concerning your claim as to the difference between fresh spirit and some stored in glass for a year... I suspect the improvement you have detected is the break down of Ethyl Acetate. Light, oxygen and time work on Ethyl Acetate to break it down to something else... I forget what becomes of it but it tastes bad and time helps change it. I get rid of my Ethyl Acetate with air bubbles and light while in the low wines stage. Kind of a resting period to get rid of some of the nasty wet cardboard flavor that some mashes produce.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by The Chemist »

While you are correct, S&S, as to the legal hoops regarding "age", chemistry is no respecter of the law...

Ethyl acetate is one of the most important compounds (especially in regard to aroma) in Bourbon and most other spirits, and increases during aging. I routinely test for it and can assure you that it increases "in the bottle"...

(BTW, welcome!! Please be assured that I don't mean to "slam" a new member, just trying to correct misconceptions.)
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Re: Great Apple brandy: Toasted or charred barrel?

Post by minime »

The Chemist wrote:Ethyl acetate is one of the most important compounds (especially in regard to aroma) in Bourbon and most other spirits, and increases during aging. I routinely test for it and can assure you that it increases "in the bottle"...
Does that apply to neutral in the 95+ range also?
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Re: Great Apple brandy: Toasted or charred barrel?

Post by goose eye »

yup brandy will age in glass or ss round here



so im tole
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Re: Great Apple brandy: Toasted or charred barrel?

Post by The Chemist »

minime wrote:
The Chemist wrote:Ethyl acetate is one of the most important compounds (especially in regard to aroma) in Bourbon and most other spirits, and increases during aging. I routinely test for it and can assure you that it increases "in the bottle"...
Does that apply to neutral in the 95+ range also?
Not so much. The whole idea of that "range" is higher purity. Higher purity, less of anything else. It's also not going to do much good to "age" pure ethanol.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Dnderhead »

Finely confirmed! Thank you. I had some (xxx white) that was many years old, and from memory was just as bad when opened as when put in.
glass. doing some research found X acid works with Y alcohol = Z ester. (if you look up esters you will see a big list) if part of this formula is
missing then it will not change much if any.( it is not the wood it is the acids in the wood?) ( also look up artafishel flavors)
I believe oak is used because of high acid content?. much of this "conversion" takes place in the first year or two. catalyst can be added
to speed this up but I'm not about to play with chemicals that I know little/nothing about.(nor any way of testing)


(I'm just an old hillbilly so what the hell do I know)
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Slow & Steady »

The Chemist wrote:Ethyl acetate is one of the most important compounds (especially in regard to aroma) in Bourbon and most other spirits, and increases during aging. I routinely test for it and can assure you that it increases "in the bottle"...
That's interesting... can you refer me to some reading to clarify my misconception concerning the increases of Ethyl Acetate (EA) in the bottle. I have been lead to believe that EA comes across at (77.1 degrees C) just before Ethanol (78 degrees C) and that it can increase in the column during the distillation process and that is why some folks put baking soda in their low wines to reduce the EA altogether during the distillation process. I have never read that EA is a key flavor in bourbon and would be most interested in reading more about it.

Now concerning your low respect for the law... that is your business... but as most of the reading I have done on the subject over the years supports the barrel aging claims, and due to the shifting nature of information made by posting hobbyists. I think I will stick with my current beliefs concerning aging.

We will have to agree to disagree.
"If it worthwhile then it is worth a little extra time and effort... all impatiens ever got me was burned fingers and charred eyebrows"
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Re: Great Apple brandy: Toasted or charred barrel?

Post by goose eye »

dunder you been readin books again
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Re: Great Apple brandy: Toasted or charred barrel?

Post by HookLine »

He he
Be safe.
Be discreet.
And have fun.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by The Chemist »

Slow & Steady wrote: That's interesting... can you refer me to some reading to clarify my misconception concerning the increases of Ethyl Acetate (EA) in the bottle. I have been lead to believe that EA comes across at (77.1 degrees C) just before Ethanol (78 degrees C) and that it can increase in the column during the distillation process and that is why some folks put baking soda in their low wines to reduce the EA altogether during the distillation process. I have never read that EA is a key flavor in bourbon and would be most interested in reading more about it.
I don't know that there are any published studies on increases of EtOAc in the bottle, and you certainly can't have my proprietary data. As to the role of EtOAc in Bourbon (and other spirits) there are many sources of information. You may want to start with Chapter 17 of the Handbook of Food and Beverage Stability (Acedemic Press, Inc.) entitled "Maturation of Potable Spirits" by James Swan; or "Changes in Whisky While Maturing" by Liebmann and Rosenblatt, Industrial and Engineering Chemistry, v. 35 No. 9, pp 994-1002. They are both foundational to the study of aging.
Slow & Steady wrote: Now concerning your low respect for the law... that is your business... but as most of the reading I have done on the subject over the years supports the barrel aging claims, and due to the shifting nature of information made by posting hobbyists. I think I will stick with my current beliefs concerning aging.
If you'll read a bit more carefully, I said that chemistry is no respecter of the law. I am. I do not illegally distilled spirits, either as a hobbyist or otherwise. If you are a "hobbyist-distiller" in the US, YOU may be the one with a "low respect for the law"...

I also haven't said that barrel-aging doesn't work...
Slow & Steady wrote: We will have to agree to disagree.
Indeed...
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Re: Great Apple brandy: Toasted or charred barrel?

Post by rad14701 »

Unless I'm mistaken, the reference to legalities above was in regard to the legal definition of government standards for distilled spirits around the world and not the legality of the activity itself... I don't think anyone was questioning or accusing anyone about their personal respect for the law in general, or their lack thereof...

I've been hunting around for a site that I visited some weeks ago which had the best legal standards for distilled spirits in various countries that I've ever come across which, unfortunately, I never bookmarked... It had a great breakdown of percentages, storage, aging, and a whole lot more... It was an obscure site so I haven't been able to locate it with a Google search yet...
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Re: Great Apple brandy: Toasted or charred barrel?

Post by The Chemist »

Yes, rad, the first reference was to legal barrel-aging standards. Then I mentioned that the chemistry responsible for aging didn't give a whit about "the law". Somehow, this got turned into ME having a low respect for the law...

If you find that site, please be sure to post it. It's often quite difficult to find that information.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Slow & Steady »

rad14701 wrote:Unless I'm mistaken, the reference to legalities above was in regard to the legal definition of government standards for distilled spirits around the world and not the legality of the activity itself... I don't think anyone was questioning or accusing anyone about their personal respect for the law in general, or their lack thereof...
You are correct I was referencing "standards" not the "legality of the activity". I just don't have any information available to change my perception without reading resources... "The Chemist" was very helpful concerning resource material by others.

I
rad14701 wrote:I've been hunting around for a site that I visited some weeks ago which had the best legal standards for distilled spirits in various countries that I've ever come across which, unfortunately, I never bookmarked... It had a great breakdown of percentages, storage, aging, and a whole lot more... It was an obscure site so I haven't been able to locate it with a Google search yet...
If you find the site please post it... maybe on a new thread as we have digressed a bit from the original "Toasted or Charred Barrel Question...
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Re: Great Apple brandy: Toasted or charred barrel?

Post by The Chemist »

Another thread may be interesting. I've worked on aging for the last 15 years, some I can talk about, some I can't...but it sho' is interesting...

There was one paper using radioactive tracer ethanol to determine "where it went", but I don't have that one at my fingertips.

And, if I seem uncharacteristically cantankerous, it's because I've got a weiner dog 'in hospital'...I'm not in the best of sorts...my apologies.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Slow & Steady »

No, no, no... no offence taken. I just finished searching the two references you offered. My-o-my what a huge amount of scientific research papers were offered a $10 a pop. A man could go bust trying to read all the research as to what goes on during "aging" of whisky, brandy and scotch.
I'm going to have to take this slow or my head will explode... thanks again for pointing me in the right direction
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Re: Great Apple brandy: Toasted or charred barrel?

Post by The Chemist »

Slow & Steady wrote: A man could go bust trying to read all the research as to what goes on during "aging" of whisky, brandy and scotch.

:D That's what university libraries and copy machines are for...
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Re: Great Apple brandy: Toasted or charred barrel?

Post by The Chemist »

The Chemist wrote:There was one paper using radioactive tracer ethanol to determine "where it went", but I don't have that one at my fingertips.
Found it. "Determination of the Congeners Produced from Ethanol During Whisky Maturation", Reazin et. al., Journal of the AOAC, v. 59, no. 4, pp. 770-776.

"As shown in Table 2, the ester fraction was radioactive. Only ethyl acetate was detected. Therefore, the data indicate that ethanol is transformed into ethyl acetate during the maturation process."

"Table 1" shows that "esters" increase from 6.87 g/100PL at 0 months to 57.2 g/100PL at 56 months. "Table 2" show radioactivity in the "esters" fraction (which as quoted above is said to be "only" ethyl acetate) increasing from 0 nCi/PL to 57.52 nCi/PL.

Now, as I said, this IS barrel-aging. I don't know of any "bottle-aging" studies, other than my own. And we don't publish...
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Re: Great Apple brandy: Toasted or charred barrel?

Post by schnell »

simple oxidation of the alcohol itself will lead to EtOAc. first ethanol is oxidized up to either the aldehyde or carboxylic oxidation state, which further reacts with more alcohol to form the ester. air oxidation can accomplish this.

the big question in my mind is not what happens to the alcohol. the real question is what happens to the congeners!

is suspect that one of the dominant reactions in "aging" is transesterification. Esters hydrolize and reform readily and always exist in equilibrium with their components, even though we seldom draw the reaction arrows in both directions anymore. One of the most important factors is availability of reactants. When we add wood or a barrel placed in intimate contact we add a heaping horde of reactive alcohols => the polyalcoholic carbohydrate cellulose!!!!

What happens when ethyl acetate transesterifys with ethanol? Nothing you could measure! You get another molecule of EtOAc another ethanol.
Now think about this: What happens when you transesterify ethyl acetate with cellulose? Something interesting! You get the ethanol molecule freed up AND you lose a molecule of acetic acid from solution. It's now effectively a mono acetyl cellulose, which isn't in solution.

Use this model to consider what happens to all the organic acids that can so react. Aren't "aged spirits" less sharp? Maybe it's that the organic acids have been removed, which also then reduces the ester burden, by dragging the equilibrium back toward hydrolysis.

This doesn't work in glass, because the reactant isn't there.

I don't believe this has been tested. To test this hypothesis would require labelled congeners and some fancy instrumentation, such as a pyrolysis inlet for a GC/MS. At various points I've had all but the inlet. Alas, no longer and this project is on hold until some gracious benefactor showers me with resources.

I once worked as a chemist on a project that allowed me to look at some internal documents for a famous rum distillery. Wow! They had a lot of ethyl acetate.

Someone in this thread mentioned the different B.P. of EtOAc vs ethanol. I should mention the binary azeotrope. No, Not That One. The ethanol/ethyl acetate azeotrope, the one we call "heads". It boils, before the ethanol/water azeotrope.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by schnell »

I should note that simple pH measurements won't be fully informative.

Remember that many of these carboxylic acids are sequestered as nonpolar esters. This reservoir is very important to the changing flavor profiles over time.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by snuffy »

The heads azeotrope has a bp of about 71C, but it's never in high enough concentration to go that low. It's presence will depress the bp as low as 75C. I haven't been able to get it lower than that. It is most sharply present during very low power equalization - 150W - 450W in a 2" column. If you boil too hard, it doesn't show strongly.

I've been doing some stress aging of apple eau de vie with American and French toasted oak chips. It goes in the freezer for 12 hours, pop the cap on the quart jar, put the cap back on, shake it up. Let sit 12 hours at room temp. Pop the cap, air it out, shake it up and back in the freezer.

The difference is remarkable in a very short time. I speculate that the temperature cycle and expansion/contraction works the liquid into the wood chips faster. In a few days, they all sink
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Re: Great Apple brandy: Toasted or charred barrel?

Post by goose eye »

schnell you sayin apple brandy wont age in glass . have you tryed it or is this all book learnin.
you put apple brandy in 6 gal glass pickle jugs an let it sit in a bulk barns for a year an let me
here you say that it aint changed.
truth be tole they aint got a clue why but they no it do.

so im tole
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Hack »

goose eye wrote:schnell you sayin apple brandy wont age in glass . have you tryed it or is this all book learnin.
you put apple brandy in 6 gal glass pickle jugs an let it sit in a bulk barns for a year an let me
here you say that it aint changed.
truth be tole they aint got a clue why but they no it do.

so im tole
And the apple brandy I've had in a glass jar since the second of December with a lone 3/4" cube of toasted oak tastes damn good tonight. When I put the jar in the cupboard in December I was debating whether I should toss it out because it tasted so bad.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by Slow & Steady »

This subject thread is suddenly turned exciting.

I'm not sure I understand it all. Lets see if I have grasped this much:

1) If toasted wood, oxygen, temperature change, and pressure change are present in the glass container then some aspects of barrel aging are taking place. At least that is what some of the posted responses are experiencing with their "Bottle Aging"

2) If the change will take place in a barrel due to the reactant being present then why not in the Bottle with toasted wood inside. Allowing that Item 1) is a correct supposition.

3) EtOAc continues to increase in the bottle after toasted wood has been removed (go back to "The Chemist" post of his research).

4) EtOAc is an important congener in the flavor profile we call Bourbon (go back to "The Chemist" post of his research).

Then my question is; When if ever does the bottled spirit become a stable product that can be saved for future consumption?
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Re: Great Apple brandy: Toasted or charred barrel?

Post by The Chemist »

Slow & Steady wrote:Then my question is; When if ever does the bottled spirit become a stable product that can be saved for future consumption?
Well, that's kinda like asking if you go half the distance to a goal, then half the distance again, then half the distance again, etc., etc.,...will you ever get there?

I expect everything is drunk up before each and every one of the many, many and complex equilibria settle down.

As to schnell's observations: an interesting hypothesis, and, as you say, very difficult experimentally, to nail down. I've long suspected the lurking of some surface chemistry, but can't say anything concrete. However, esters and acids both in fact increase during aging, so THAT aspect, at least (removal/sequestration of acids), isn't accurate.
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Re: Great Apple brandy: Toasted or charred barrel?

Post by blind drunk »

Then my question is; When if ever does the bottled spirit become a stable product that can be saved for future consumption?
... when we tighten our lids. :lol:
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