Sciencemadness Discussion Board - Distillation of Cider.

Distillation of Cider.

FGP - 5-8-2004 at 01:48

Do you have Cider in America?
If I distill it what are the likely products and at what temperatures? Will there be both methyl and ethyl fractions?
FGP in UK

gravenewworld - 5-8-2004 at 03:41

Yes we have cider in America. One extremely good brand of cider is Woodchuck. I don't know much about distilling alcohol, but I'm pretty sure there should be no methanol when you are trying to make alcohol, at least you better hope not. Ingesting a tiny dosage of methanol is very poisonous, it can make you go blind easily. I don't know how they distill cider, but one method is by freezing.

vulture - 5-8-2004 at 03:50

Don't forget to remove the carbondioxide first....

Cider

MadHatter - 5-8-2004 at 19:57

I make hard cider and use the freezing method to remove a large
amount of water. As for distillation, it depends on what kind of
still being used. A reflux still(moonshine still) drives off most of the
methanol initially because methanol's boiling point is lower than
ethanol(at 78 C). This is the "foreshot" that comes off at less than
70 C. The drawback is that you won't retain the flavor of the
cider using this method. The pot still retains the flavor however
the methanol remains. There shouldn't too much methanol if the
cider is fermented using only juice and sugar. More methanol is
produced when fermenting from a corn or grain based mash.

Ramiel - 6-8-2004 at 00:17

This is not true. I have operated a reflux still and a 'pot still' (in which the so-called lyne arm acts as the condensation column). The only difference between the two is the level of reflux. Pot stills will have between one and two plates* of reflux due only to the lid. If run slowly enough at the beginning, you will have a finer separation of the product.

Since the reflux still has between 4 and 8 plates* (in general) you will have a more pedestrian distillation and therefore a finer separation of the products.

To bring the discussion back to a more chemistry related vein, use a thermometer to determine what groups of chemicals you are distilling. You will notice - as in most distillations - that there are sharp divides in the temperature indicating different chemicals.

- D

* A heurism used by distillers which reflects rates of reflux.

ps. MadHatter - what you are posting sounds reliable, but it is shot with mistruth. Not for this reason alone am I likening you to AcidTest.

[edit - layout & spelink]

[Edited on 6-8-2004 by Ramiel]

FGP - 6-8-2004 at 01:25

Quote:

Originally posted by MadHatter
I make hard cider and use the freezing method to remove a large
amount of water. As for distillation, it depends on what kind of
still being used. A reflux still(moonshine still) drives off most of the
methanol initially because methanol's boiling point is lower than
ethanol(at 78 C). This is the "foreshot" that comes off at less than
70 C. The drawback is that you won't retain the flavor of the
cider using this method. The pot still retains the flavor however
the methanol remains. There shouldn't too much methanol if the
cider is fermented using only juice and sugar. More methanol is
produced when fermenting from a corn or grain based mash.

Thanks. What are the practical details of your 'freezing method'?

gravenewworld - 6-8-2004 at 06:57

Wow, I am surprised that methanol appears when trying to make cider. That is scary. If you ingest methanol you liver breaks it down into formaldehyde which is very bad. Funny enough the cure for methanol ingestion is by flushing the body with ethanol. So if you ever ingest methanol, cure yourself by getting hammered off something like grain alcohol.

Cider

MadHatter - 6-8-2004 at 08:19

I freeze my cider to remove some of the water. I freeze it plastic bottles
and pour off the liquid portion. Some of the alcohol will be lost in the ice
portion but most will remain in the liquid portion. It takes a few freezings
but the remaining liquid will have a higher proof as a result.

"plates"

Magpie - 6-8-2004 at 18:49

This is to elaborate on Ramiel's use of the term "plates." Industrial distillation columns have traditionally used plates, either perforated or bubble-cap type. These will be in columns at least a few inches in diameter and up to several feet in diameter. These plates provide for intimate mixing of rising vapor and falling liquid (reflux), thereby resulting in a changing liquid and vapor composition through exchange of components all the way up the column. This provides a more efficient separation. These plates are actual circular metal sheets resting on supports built into the column wall.

Many of these plate columns have been replaced by packed columns which are cheaper and more efficient yet. The packings can run all the way from tiny glass beads in a lab column to large rings, "saddles," or other confiurations designed to minimize pressure drop and maximize liquid-vapor equilibrium.

In a pot still or reflux still there are no actual plates but the still can still be rated by equivalency to a still with a certain number of plates.

Reflux

MadHatter - 6-8-2004 at 19:10

Magpie, I packed my reflux still with 5mm glass beads. The reflux column is 3 inches
wide and 2 feet high. It does a fantastic job although for whatever reason the
flavor of the mash is lost. I don't like using a pot still because repeat distillations
are a pain.

Magpie - 6-8-2004 at 19:23

MadHatter, it sounds like your column is too efficient, taking out the congener flavor enhancers. But this is just speculation, I've never actually done any mash distillations - yet.

But it seems that Jack Daniel's has it both ways - he uses bubble-cap columns followed by charcoal adsorption. He's got it finely tuned, taking out the bad stuff and putting in the good ones. Yes, quite tasty....ahhh. :cool:

[Edited on 7-8-2004 by Magpie]

Jack Daniels

MadHatter - 6-8-2004 at 19:40

Perhaps I'm using too many beads ! I must admit that I never lost
the flavor with a pot still. Here's to JD ! Delicious !

Pot Stills

MadHatter - 10-8-2004 at 07:04

Ramiel, sorry for shooting off my mouth about pot stills. I guess I've never
had any luck with them. When you use a pot still do you just throw away
the 1st fraction that comes off or is your temperature control that good ?
With my reflux still it's not a problem. The smell of the methanol and acetone
is quite noticeable at 65 C. Then the temperature rises and drives out
the ethanol. I shut down the still when the temperature exceeds 79 C.
Those tailshots are nasty too ! Doesn't pay to be greedy ! Your experience
is obviously greater than mine. I'd appreciate any tips you have for using a pot
still. My reflux still strips the flavor out so Magpie may be onto something
here. Pictured here is my reflux still with 2 other items for a sense of scale.
At the far left is the centrifuge I sent to Blind Angel. In the middle is 1 of my
Graham condensers. It's over 3 feet long.

[img]D:\CCS-SMALL.jpg[/img]

[Edited on 10-8-2004 by MadHatter]

Marvin - 10-8-2004 at 09:08

In distillation its normal to talk about plates, this isnt meant literally though. A theoretical plate is the situation where a mixture is boiled, a small amount of vapour is produced and this is condenced. Thats one theoretical plate.

A bubble plate at first glance looks like a theoretical plate because it equilibriates the vapour coming off with the the condensate, however the condensate does not have the same composition of the rising gas, because it only consists of what the rising gas loses plus a little flowback from higher stages. One bubble plate gives you less than one theoretical plate, but they are good for very high volume applications.

Packed columns are only good for much lower volume applications, but a meter high reflux column can achieve over 200 theoretical plates at very low take off.

Theoretical plates are useful for quickly predicting the success of a seperation because they each corrispond to a single zigzag on a vapour liquid equilibrium diagram. From the definition, a horizontal line goes from the liquid phase to the gas phase becuase the temperature does not change, producing a vapour with a different composition (and therefore lower boiling point), this cools with a vertical line (same composition) until it hits the liquid curve and then you repeat the process for the next theoretical plate.

Ramiel - 10-8-2004 at 16:24

IMVHO, The important thing with pot stills is heating it at just the right rate. Since you can't vary the amount of reflux, you must vary the heating applied to find that happy equilibrium between blasting off all sorts of things at once and alternatively: stewing off all sorts of things at once (these aren’t technical terms! I’m just trying to put into words my experience). I’ve found that at a strong simmer, the temperature peaks are very distinct (I put a thermometer above the liquid even though I’m pot stilling). About minute or two either side of the 79*C area is about right for getting all the flavor you want. (for bitter spirits eg sake: perhaps not so many oils at the high end, and vice versa for whiskey, whisky, bourbon etc.).

Yes, I take the foreshots off entirely. And I collect the heads and tails separately – so I can re-process them and mix them according to taste… think of them as salt and pepper on a dish.

I remember more than three years back the aftermath of my ‘greedy’ distillations. Much sickness from the fusel oils. Much pain. A good trick I use now is once the 79*C mark suddenly passes, I switch receivers, turn off the heat, turn off the water coolant, and then wait it out – sometimes the tails need re-distilling in a pot still.

I don't think I've any greater experience - certainly not more than the older members (you alcos...

). But in true madscience fashion, I learned everything by trial and error, and a great deal by tasting everything with my mouth. Try a drop or two (or 500 if it’s clean!) of the distillate at every point once(spitting of course), I learned a lot about my pot stilling that way alone.

Good luck and a sturdy liver,
- D

"plates"

Magpie - 10-8-2004 at 19:03

Marvin,

In consulting my physical chemistry text I find that chemists do indeed refer to theoretical plates for distillation columns. And since this is fundamentally a forum about chemistry I accept that term.

But I also must stick up for my brethren chemical engineers. We look at distillation as just one of several mass transfer unit operations, which include gas absorption, liquid-liquid extraction, solid-liquid extraction, etc. All can be analyzed mathematically with surprisingly similar equations. We only use the term plate when refering to an actual piece of hardware. Instead we use the term "stage," "theoretical stage," or "equilibrium stage." For equipment design we convert theoretical stages to actual hardware stages (or length of packed column) by dividing the number of theoretical stages by the stage efficienicy. These efficiencies vary anywhere from a few % to nearly 100%, depending on the case at hand.

Booze huh!

Democritus of Abdera - 10-8-2004 at 21:55

Quote:

Originally posted by Magpie
MadHatter, it sounds like your column is too efficient, taking out the congener flavor enhancers. But this is just speculation, I've never actually done any mash distillations - yet.

The taste of Jack D. has very little to do with the distillation process and more to do with the "aging" process, to simulate, just toast oak chips(sold for use in BBQ's and Meat Smokers) in your oven to a dark brown and then add them to your distillate for a few days/weeks (warning! with this much surface area some home distillers have gotten WAY too much smokey "character" in their final product so be sure to keep some clear spirit back for tempering (dilution) and to check your product often.

NOTE: this is nothing original on my part but just standard procedure for many quikie homebrewers, however the procedure does put the flavor in quick, at real distilleries they flame the inside of the barrel to char it (saw it in a 70's national geographic that showcased Jack Daniels distillery) This small surface area of burnt oak to large quantity of liquor makes the flavor take a great deal longer to leach into the booze.

For "true" scotch, you smoke the hops with peat smoke on a "smoking floor", at least I think it was the hops.....anyway, the quickie way is to get a smoldering pile of peat going and then to stick a clean metal drum with holes poked into the top, over the pile of smoking peat, then collect the condensed tar off of the metal drum, or to suspend a metal bucket filled with water in the chimney of a peat burning fireplace for a little while, supposably only a few tablespoons of the resulting tar will flavor several gallons of raw white spirit so strongly, even a native scotchman will swear that it's single malt.

It turns out that all of the "mysterious art" of distilling the worlds finest whisky's is mostly hocus pocus. Chemically, you cannot really tell a 20 year old single malt made in a 450 year old distillery from a vintage tuesday made in Uncle Bob's back shed, if you make certain to add the same stuff into it.

The "aura" of great liquor probably has a lot to do with the placebo effect. (people taste what they want to taste)

I'd like to say I've tried these recipes myself but I totally abstain from alchohol myself, but good luck to you all.

If you want to, you can also get bottled additives off the net from someplace in sweden to make all sorts of other flavors of liquor from raw white spirits.....

Jack Daniels

Magpie - 10-8-2004 at 22:31

Democritus,

I agree with you in general. I think where JD has the edge is in taking out the fusel oils that are reputed to cause hangovers. My personal, but limited, drinking experience supports this theory. Good distillation procedure followed with charcoal adsorption is likely the key to that. But putting the flavor back in is likely done in the aging in oak barrels, as you say.

vulture - 11-8-2004 at 03:49

In my chemical engineering course, the number of plates is determined by finding the reflux ratio and/or top destillate flow rate etc.

This is then plotted in a graph alongside with the equilibrium line. You can then draw and count the necessary number of plates.

Ramiel

MadHatter - 11-8-2004 at 14:10

Ramiel, thanks for replying. Looks like I have to get re-acquainted with my
old pot still !