Sciencemadness Discussion Board

Moonshiners' 'Thumpers': Myth or Reality?

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aga - 20-2-2015 at 12:14

That was the earlier Bam Bam design.

Crowfjord - 20-2-2015 at 12:42


Anybody ever see/read this little book? It's a pretty entertaining read, copyrighted 1966. I think that it was from this that I initially thought that a slobber box and thumper were the same thing. It seems to operate on that assumption. Also, it doesn't specify whether or not the tube should reach to the bottom, or whether to start with some liquid inside.

A favorite quote:

"Some old moonshiners never add yeast, depending on yeast which remains in the fermentation barrels or vats or on natural yeasts of the air. Some operators maintain, even vehemently, that no yeast is involved in their fermentation, and in certain circles one sometimes hears, 'I don't like yeast whisky!' But add yeast; it's fast and sure and one cannot often afford to waste time."

Pardon the crappy images, my camera kind of sucks.

IMG_0409.jpg - 2.5MBIMG_0410.jpg - 2.6MB

aga - 20-2-2015 at 13:15

Quote: Originally posted by Zombie  
The heat from the water vapor in the Alch. depleted boiler is now coming over at or near 210 - 212 * f, and the BP in the thump is at or near 185 - 190 *f.
No need to move anything

I don't understand how the Boiling Point in the Thump can be static - as i see it it will be very much a dynamic, first going lower as it takes up the EtOH from the boiling pot, then going higher as it loses EtOH, and takes in Water (steam) at the same time.

Sealing the intake from the first boiling pot after it gives up it's Shine, and moving the heat will surely give more % in the distillate.

By adding Steam (i.e. water) from the first pot, the Thumper pot gets Diluted as well as heated.

With out setup, we can unhook the first pot easily, plug the open neck and move the flame, so that might be worth trying After the initial runs to get the Thump data.

We'll know for sure when the last two glass jigsaw pieces arrive.

Oh. Question @ Zombie: what are you guys actually measuring during runs ?

[Edited on 20-2-2015 by aga]

Zombie - 20-2-2015 at 13:17

Quote: Originally posted by Magpie  
I've been looking at the ethanol-water VLE chart in my textbook (Foust) in regard to the enthalpy. It is presented as BTU/lb-mole. What's amazing is that the enthalpies for both the liquid and the vapor stay almost the same as the streams (liquid and vapor) increase in ethanol content. I interpret this to mean that once the thumper reaches maximum ethanol concentration it's not only going to put out a richer vapor but it's going to come over like gangbusters. My conclusion is based on the fact that a lb-mole of water weights 18 lbs whereas a lb-mole of ethanol weighs 46 lbs.

Zombie: Does your experience support this?

Edit: This is likely due to the fact that on a per mole basis water and ethanol heats of vaporization are very close, ie, for water it is 40.65 kJ/mol and for ethanol it is 42.3 kJ/mole. So 14 g of condensing water should evaporate 44 g of ethanol.

[Edited on 20-2-2015 by Magpie]



Everything you said here is absolutely correct. This is why I keep repeating the heat to the boiler must be throttled or reduced to control the product output.

If left alone, once the boiler is depleted of EtOH, it will quickly over power the thumper due to the drastically lower boiling point of the thumper liquid.

You will begin spewing water in the vapor out of the thumper, and negate the effect of the thumper.

[Edited on 20-2-2015 by Zombie]

[Edited on 20-2-2015 by Zombie]

Zombie - 20-2-2015 at 13:23

Quote: Originally posted by deltaH  
Quote: Originally posted by Zombie  
Quote: Originally posted by blogfast25  
Quote: Originally posted by deltaH  
[...] if you're willing to make an improved design then I'd rather build a refluxed tray.



Completely second that. A controlled refluxer/tray would be far more efficient and demonstrably effective.

Even simpler: a decent fractionating column. Easy peasy and highly effective.

[Edited on 20-2-2015 by blogfast25]



That's where all this comes full circle back to the nature of the builders, and operators of thumpers.

For the most part they were back woods Tennessee hill folk.
The most they understood was basic trading math, and how to fit a lid on a bucket.
If you think about the origin, it's actually quite a leap in evolution for them.


I included some old looking rum still setups a while back in this thread that appeared to be using thumpers, so I'm not so sure these 'billies invented them. I think it's much more likely that this knowledge was imported from rum making methodology and that in itself might be very old, who knows?



Chicken or the egg?

Most claim the Irish invented distilling, but there are documents going back to ancient Persia, and Egypt showing distillation apparatus.

Rum was generally an English distillation in later eras so Scotland / Ireland would have the same technologies, and most of the early hill folk were Celts.

Chicken or the egg...

Zombie - 20-2-2015 at 13:26

Quote: Originally posted by blogfast25  
I saw a thumper on The Flintstones once! ;)



That was Wilma's I believe. She needed it to put up w/ Fred's hi-jinx.

Zombie - 20-2-2015 at 13:32

Quote: Originally posted by Crowfjord  

Anybody ever see/read this little book? It's a pretty entertaining read, copyrighted 1966. I think that it was from this that I initially thought that a slobber box and thumper were the same thing. It seems to operate on that assumption. Also, it doesn't specify whether or not the tube should reach to the bottom, or whether to start with some liquid inside.

A favorite quote:

"Some old moonshiners never add yeast, depending on yeast which remains in the fermentation barrels or vats or on natural yeasts of the air. Some operators maintain, even vehemently, that no yeast is involved in their fermentation, and in certain circles one sometimes hears, 'I don't like yeast whisky!' But add yeast; it's fast and sure and one cannot often afford to waste time."

Pardon the crappy images, my camera kind of sucks.



That is also partly true. Depending on where you are, and the vegetation around you.
If you are near apples or grapes there is no need to add yeast. It abounds at certain times of the year.
Also long time distillers WILL have enough yeast on / in their equipment that adding yeast is never needed ie: wooden mash barrels.
My Grandfather was a minimalist, and added 1/2 a teaspoon sprinkled over the top of a 55 gallon mash. Normally that is less than you need for a loaf of bread but he had enough in the wood to really do the job anyway.


Zombie - 20-2-2015 at 13:38

Quote: Originally posted by aga  
Quote: Originally posted by Zombie  
The heat from the water vapor in the Alch. depleted boiler is now coming over at or near 210 - 212 * f, and the BP in the thump is at or near 185 - 190 *f.
No need to move anything

I don't understand how the Boiling Point in the Thump can be static - as i see it it will be very much a dynamic, first going lower as it takes up the EtOH from the boiling pot, then going higher as it loses EtOH, and takes in Water (steam) at the same time.

Sealing the intake from the first boiling pot after it gives up it's Shine, and moving the heat will surely give more % in the distillate.

By adding Steam (i.e. water) from the first pot, the Thumper pot gets Diluted as well as heated.

With out setup, we can unhook the first pot easily, plug the open neck and move the flame, so that might be worth trying After the initial runs to get the Thump data.

We'll know for sure when the last two glass jigsaw pieces arrive.

Oh. Question @ Zombie: what are you guys actually measuring during runs ?

[Edited on 20-2-2015 by aga]



You missed the point.

The run is very much dynamic. At the END of the run is where my statement applies.

The fact is the boiler is now 2-3% ABV. The thump is near 18% abv. The steam coming over does NOT dilute as the EtOH is vaporizing at a faster rate than the water. That is the sole purpose of heat control. It is the EXACT same thing as moving pots around, and you end up with the exact same abv, and amount as if you had moved pots.

You will understand completely once you see it in action. I promise.;)

aga - 20-2-2015 at 14:15

So you expect the ethanol to evaporate off faster than the steam coming in.

OK.

From what you say, you imply that you're measuring the EtOH % in the boiling pot liquid, and the Thumper liquid.

If that's true, then how do you obtain samples without disrupting the temperature/pressure conditions, or is that part of it as well ?

Zombie - 20-2-2015 at 14:20

Quote: Originally posted by aga  
So you expect the ethanol to evaporate off faster than the steam coming in.

OK.

From what you say, you imply that you're measuring the EtOH % in the boiling pot liquid, and the Thumper liquid.

If that's true, then how do you obtain samples without disrupting the temperature/pressure conditions, or is that part of it as well ?



There is no need to sample the pots. Physics dictates that EtOH will be the primary vapor untill it becomes to low in percentage to apply.

If you wished you could shut down at 50% abv product out of the thumper, and verify this. The boiler will be dramatically lower abv than the thumper.

[Edited on 20-2-2015 by Zombie]

blogfast25 - 20-2-2015 at 14:23

Quote: Originally posted by aga  
So you expect the ethanol to evaporate off faster than the steam coming in.



You're using the term 'steam' wrongly here. Steam is water vapour. What comes of the pot is water/EtOH vapour.

Zombie - 20-2-2015 at 14:31

Oh... To verify the former... You are collecting an average of 50% abv for the entire run, so in the end the thumper proves out to displace 50% water, and 50% EtOH average,

The single pot still will wind up around 80% abv. translating to 60% water, and 40% EtOH. That alone points to the thumper being more efficient than a pot by itself.

In the beginning , Yes the pot will displace more EToH. After 50ABV the pot will produce more water. BUT the thump now takes over, and the pot is simply a heat source..
So in reality it does not matter hat the pot is putting out It is only there for heat, and the thump is displacing more EtOH than water. You stop at 40% because that shift has now transferred to the pot,and we don't want / need the water.

aga - 20-2-2015 at 14:37

Your point is clear, yet i still feel that moving the flame will give a slightly higher yield.

Well, we'll see once the data is collected.

It is a real pain waiting for deliveries of small bits of glassware.

aga - 20-2-2015 at 14:50

DRY STATES ?

Sorry, i only just realised that it wasn't a Joke.

Prohibition is still alive and well across entire States in the US ?!?!

Zombie - 20-2-2015 at 14:54

Quote: Originally posted by aga  
Your point is clear, yet i still feel that moving the flame will give a slightly higher yield.

Well, we'll see once the data is collected.

It is a real pain waiting for deliveries of small bits of glassware.


I love you guys, and really appreciate all the time/ money you are investing.
This has been very enlightening because I am learning that I should be paying more attention to the technical side of chemistry.
I tend to learn the mechanics, and ignore the math, formulas, and lingo.

Perhaps it is because I never enjoyed discussing methods in a common language. I'm more of a do'er, than a talker.

If I did pay attention, and apply what I know to formulas, Perhaps I could have conveyed the formulas in a manner much more precise than my hitting the keyboard with a hammer, and you all would have understood more clearly what I am trying to express.

Many thanks. You are making a monster you know... :D

Super Brain 2016!!!

careysub - 20-2-2015 at 14:57

Quote: Originally posted by aga  
DRY STATES ?


No, there are no "dry" states in the US.

There are "dry" counties however, but what "dry" means varies from county to county. Usually it means no alcohol sales, sometimes just no distilled spirits sales, and often a ban on possessing in public.

Even where dry counties no longer exist, their legacy can often be seen by liquor stores still sited just over one side of the county line.

Until 2013 there were states that prohibited home brewing, but Mississippi and Alabama climbed aboard the home brewing bandwagon mid-year.

Home distilling for the purposes of consumption is right out by Federal law.

[Edited on 20-2-2015 by careysub]

aga - 20-2-2015 at 15:11

So you can Brew, but not Shine.

Drink, but not publicly.

Next they'll want to ban Drugs and stop all those Sober people carrying guns ...

[Edited on 20-2-2015 by aga]

Zombie - 20-2-2015 at 15:22

Quote: Originally posted by aga  
So you can Brew, but not Shine.

Drink, but not publicly.

Next they'll want to ban Drugs and stop all those Sober people carrying guns ...

[Edited on 20-2-2015 by aga]


GOD FORBID! I Like gettin' doped up, and shootin' at sh^t. Especially at drunks!

Dry county map...

http://www.washingtonpost.com/blogs/govbeat/wp/2014/09/02/wh...

careysub - 20-2-2015 at 15:30

Quote: Originally posted by Zombie  
Quote: Originally posted by aga  
So you can Brew, but not Shine.

Drink, but not publicly.

Next they'll want to ban Drugs and stop all those Sober people carrying guns ...

[Edited on 20-2-2015 by aga]


GOD FORBID! I Like gettin' doped up, and shootin' at sh^t. Especially at drunks!

Dry county map...

http://www.washingtonpost.com/blogs/govbeat/wp/2014/09/02/wh...


You will observe that the upper part of the "dry county belt" correspond closely to Appalachia, which one might regard as also being the "moonshine belt".

http://en.wikipedia.org/wiki/Appalachia

aga - 20-2-2015 at 15:30

So to be Safe, and not being familiar with US State geography, i need to head for Miami or Arizona (Avoiding California on grounds of it being too strange to matter) ?

Holiday with Jail Time for drinking beer = no holiday.

Zombie - 20-2-2015 at 15:47

Quote: Originally posted by aga  
So to be Safe, and not being familiar with US State geography, i need to head for Miami or Arizona (Avoiding California on grounds of it being too strange to matter) ?

Holiday with Jail Time for drinking beer = no holiday.



We have a saying, and a song to back it up.

Arrive on vacation, Leave on probation!

[Edited on 20-2-2015 by Zombie]

aga - 20-2-2015 at 15:52

I googled "hot dicketty dang holidays"

Currently regretting.

Zombie - 20-2-2015 at 16:17

This is the one you want...

https://www.youtube.com/watch?v=0nRC8VNlu-A

aga - 26-2-2015 at 13:35

Apologies for the delay in posting any results of a definitive experiment.

Ebay. Gah !

Currently waiting for delivery of a 19 male/24 female adapter and (embarassingly) a 500 ml RBF.

I broke my only 500ml quickfit RBF testing the idea that 'whacking heat into sodium benzoate + NaOH will break your glassware when it cools'

It does. Use metal.

blogfast25 - 26-2-2015 at 14:04

Quote: Originally posted by aga  
[...] + NaOH will break your glassware when it cools'

It does. Use metal.


It didn't mine. ;)

aga - 26-2-2015 at 14:18

Quote: Originally posted by blogfast25  
It didn't mine. ;)

300g versus 5g maybe ?

Bottom got a thick coating.

Cracked all over the coated area.

This was Chinese glass, and not thick-walled.

Zombie - 26-2-2015 at 14:22

I heard somewhere that hammers, and rocks do the same thing to glass.

It's one of the few things I do believe on face value, and therefore never felt the need to prove.

It's all good fellas. Just be careful sampling the product... :D

aga - 26-2-2015 at 14:26

Hammers and Rocks do Not break glass per se.

Place a Rock or a Hammer on a Glass sheet, and the glass will happily support the weight of the hammer.

A metal hammer moving at sufficient Speed will break glass.

This particular Theory is well known, and there should be be data supporting it.

Zombie - 26-2-2015 at 14:49

Quote: Originally posted by aga  
Hammers and Rocks do Not break glass per se.

Place a Rock or a Hammer on a Glass sheet, and the glass will happily support the weight of the hammer.

A metal hammer moving at sufficient Speed will break glass.

This particular Theory is well known, and there should be be data supporting it.



You, and Blogfast have a LOT in common. :D

gsd - 5-3-2015 at 15:56


Sorry for barging in late into this thread. I was not following it, but after some discussion with Magpie, I browsed thru'. Here is my take on it for whatever it is worth.

1) This "thumper" is a contraption for Steam Distillation with an added twist that the heat source i.e. motive steam contains the feed stream as well.

2) The thumper pot is equivalent to one distillation stage wherein the intimate vapour liquid contact is achieved by bubbling the steam into residual liquid. This is a batch operation in which bottom product (largely water) accumulates in the pot and the top product (enriched ethanol) is distilled-off.

3) As stated above the heating and feeding is thru' the steam from boiling pot. The un-insulated walls of the thumper act as "reflux condenser ".

4) If the thumper is made tall (like column) and filled with marbles (as packing material) and if only the bottom portion - which holds water - is insulated then it will significantly improve its efficacy.

That is all I can make out of this rather longish thread.

Gsd

Zombie - 5-3-2015 at 16:40

You summed it up, and added a twist.

Everything you said is correct to a degree.

The pot or elongated container can not create enough reflux by itself to achieve any discernible gain in ABV simply by adding packing. It's the liquid vapor interaction that strips EtOH from the falling liquid (reflux).

Without creating a way to drop liquid down the column full of packing all you create a a partially blocked column, and the vapor will rise but have Very little to strip on it's way up.

The thumpers capacity to act as a "Partial Reflux condenser" is minimal. It stays hot enough that EtOH will not re condense yet the water fraction will. Too cold, and everything condenses.

Too hot, and everything passes thru.

Lets suppose the thumper WERE 100% efficient, and insulated. Then it would have NO effect. It would simply be a bulge in the pipe.


gsd - 5-3-2015 at 18:45

Quote:

The pot or elongated container can not create enough reflux by itself to achieve any discernible gain in ABV simply by adding packing. It's the liquid vapor interaction that strips EtOH from the falling liquid (reflux).


The packing is not added to increase reflux. It is added to increase contact area between upcoming vapour and downcoming condensed liquid.
Quote: Originally posted by Zombie  

Without creating a way to drop liquid down the column full of packing all you create a a partially blocked column, and the vapor will rise but have Very little to strip on it's way up.


The exposed walls which are acting as condenser are partially converting vapour into "drop down "(reflux)
Quote: Originally posted by Zombie  

The thumpers capacity to act as a "Partial Reflux condenser" is minimal.

Of course. It is a crude devise presumably designed by trial and error without any theoretical consideration. A little external cooling of the top wall (even by using a small fan) will increase reflux and the product purity.
Quote: Originally posted by Zombie  

Lets suppose the thumper WERE 100% efficient, and insulated. Then it would have NO effect. It would simply be in the pipe.



Here I assume you are talking of "Thermal Efficiency" of thumper. It is not made to make the system thermally efficient. It is made to extract as much "juice" from the pot as possible.

gsd

Zombie - 5-3-2015 at 19:47

You are correct on the packing. It is there to create surface ares for the vapor liquid interaction.

The "drop down" reflux is actually a bad condition in any column. It is called wicking or column weep.
The reason it is bad is it cools the volatile compound (EtOH), and wicks it back to the pot or boiler or re boiler. It stagnates the run making collection difficult, and in severe cases impossible.

Quote:
"Of course. It is a crude devise presumably designed by trial and error without any theoretical consideration. A little external cooling of the top wall (even by using a small fan) will increase reflux and the product purity."

Again wicking
In a properly designed column reflux control is CRITICAL!
Media packed columns use centering rings to minimize reflux / column wall contact. I have designed several different systems for this purpose.
some ar simple funnel type devices, while others are staggered, downward facing"teeth" welded into the column wall at specific stages, and still others are complex computer designed "vein plates" that direct relux while allowing maximum vapor / liquid interaction thru the device.

Then you get into Plated columns similar to "cracking towers where plate flow dynamics are precisely controlled. Flow rates, bath depth, and vapor / liquid interaction are paramount to a properly engineered column.

You HAVE to know exactly what the mole fraction will be at every plate, and reflux control is the only way to determine this. Wier, and dams are engineered. Not guessed at

Otherwise you have spent a lot of money on scrap.

It took me a year of number crunching to design ONE column.
I don't copy other peoples ideas or designs. I started with a column that has failed for 100 years, and made it work. A concentric, mixed media (plates, and packing's) fuel ethanol column that runs at reduced pressure. (vacuum)

The numbers are all in the plates, weirs, dams, structured packings that did not exist until I designed them.

Same thing for the columns them selves. They rely on the temperature gradient created at each stage to efficiently power each other.
Things like thermal mass transfer , and material selection... Insulating properties of different compounds, and metals.

Some of my work was based on this article... http://repository.tudelft.nl/assets/uuid:2517a2e2-7376-485c-...

Most of it was done on the computer I am posting from.

Thumpers are fucking easy!

Hillbillies did not know the math, but they did know what they were after, and knew how to get it.
You'll never know how much credence I put in that method. Set a goal, and make it happen.

Edit:
Yes we are discussing a "thumper here but all the dynamics that I listed, and many more I did not make them work.
All the same numbers apply, and wrong is wrong.

[Edited on 3-6-2015 by Zombie]

Luke - 8-3-2015 at 03:48

any word on the experiment yet?

Zombie - 8-3-2015 at 21:01

Drank the samples, and have to re run the experiment.

37 bottles of beer on the wall, 31 bottt... shoot.:mad:

99 bottles of beer on the wall

blogfast25 - 9-3-2015 at 07:10

Quote: Originally posted by gsd  

Sorry for barging in late into this thread. I was not following it, but after some discussion with Magpie, I browsed thru'. Here is my take on it for whatever it is worth.

1) This "thumper" is a contraption for Steam Distillation with an added twist that the heat source i.e. motive steam contains the feed stream as well.
[big snip]


With all due respect but much of the arguments you make have already been addressed by 'thumper skeptics' like me and Fulmen.

In particular the belief that the thumper represents a steam distillation is simplictic at best.

Imagine a pot of pure EtOH at BP. Now we lead pure water vapour (steam) through it. Do you really believe the vapour leaving the thumper would be 100 % EtOH?

That would only be true if the steam and EtOH were kept rigorously separated, for instance by using the steam in a heating coil placed in the EtOH bath (or in a heating coil heating the EtOH pot from the outside with a mantle or such like).

DJF90 - 9-3-2015 at 08:37

Quote: Originally posted by blogfast25  

Imagine a pot of pure EtOH at BP. Now we lead pure water vapour (steam) through it. Do you really believe the vapour leaving the thumper would be 100 % EtOH?


This is the fallacy that prevents you from making sense of the thumper. It is not claimed to work under these conditions, nor those using 50% EtOH as you have referred to previously. Its clear from the VLE diagram that if a thumper is capable of working, it has to start towards the lower end of the scale.

Zombie - 9-3-2015 at 09:07

Quote: Originally posted by DJF90  
Quote: Originally posted by blogfast25  

Imagine a pot of pure EtOH at BP. Now we lead pure water vapour (steam) through it. Do you really believe the vapour leaving the thumper would be 100 % EtOH?


This is the fallacy that prevents you from making sense of the thumper. It is not claimed to work under these conditions, nor those using 50% EtOH as you have referred to previously. Its clear from the VLE diagram that if a thumper is capable of working, it has to start towards the lower end of the scale.



Exactly.

The ABV in the thumper is continually enriched from a LOW beginning point.
At some point during the process there is an equilibrium where the boiler can no longer enrich the thumper, and the output from the thumper will begin reducing in ABV, but by that point it (thump) has done it's job.

It's just a fun thing, like baseball cards in the spokes of your bicycle.
Some might argue that they don't make the bike faster but I always got home by dark with them installed.

gsd - 9-3-2015 at 21:48

Quote: Originally posted by blogfast25  


Imagine a pot of pure EtOH at BP. Now we lead pure water vapour (steam) through it. Do you really believe the vapour leaving the thumper would be 100 % EtOH?

That would only be true if the steam and EtOH were kept rigorously separated, for instance by using the steam in a heating coil placed in the EtOH bath (or in a heating coil heating the EtOH pot from the outside with a mantle or such like).


By definition in steam distillation you inject live steam as a heat source. It would be very funny to distill pure alcohol by injecting live steam into it (as zombie would say even hillbillies won't do it.)

If you use steam in heating coil (as you should for distilling pure alcohol) then it is no more a steam distillation. It is distillation by using steam in the coil (or jacket) as an indirect heating medium.

gsd

blogfast25 - 10-3-2015 at 06:59

Quote: Originally posted by DJF90  
It is not claimed to work under these conditions, nor those using 50% EtOH as you have referred to previously.


I didn't claim it worked like that. Learn to read, instead of setting up straw men. Re. the latter you've got previouses and I expect this latest one won't be the last either.

Quote: Originally posted by gsd  

If you use steam in heating coil (as you should for distilling pure alcohol) then it is no more a steam distillation. It is distillation by using steam in the coil (or jacket) as an indirect heating medium.

gsd


Yawn.


[Edited on 10-3-2015 by blogfast25]

gsd - 10-3-2015 at 08:06

Quote: Originally posted by blogfast25  
Quote: Originally posted by DJF90  
It is not claimed to work under these conditions, nor those using 50% EtOH as you have referred to previously.


I didn't claim it worked like that. Learn to read, instead of setting up straw men. Re. the latter you've got previouses and I expect this latest one won't be the last either.

Quote: Originally posted by gsd  

If you use steam in heating coil (as you should for distilling pure alcohol) then it is no more a steam distillation. It is distillation by using steam in the coil (or jacket) as an indirect heating medium.

gsd


Yawn.


[Edited on 10-3-2015 by blogfast25]


Zzzzzzzzzzzzzzzzzzzzzzzzzz.........
OK. You have your last word.
Zzzzzzzzzzzzzzzzzzzzzzzzzz........

Gsd

DJF90 - 10-3-2015 at 10:38

Quote: Originally posted by blogfast25  
Quote: Originally posted by DJF90  
It is not claimed to work under these conditions, nor those using 50% EtOH as you have referred to previously.


I didn't claim it worked like that. Learn to read, instead of setting up straw men. Re. the latter you've got previouses and I expect this latest one won't be the last either.


It was Magpie and Fulmen that were discussing starting with 50 %. Its easier to remember "who said what" when the thread isn't 22 pages long and filled with multiple posts in succession by the same author. The only person worse at that than you is zombie, who somehow managed nearly two pages of posts without a reply.

My point still stands. This is the second (or is it third?) time you've suggested that little thought experiment of yours. It bears no relevance to the content of this thread; you're considering something that is far removed from the operating conditions of a thumper yet somehow you believe it provides some proof that your stance on the matter is correct.

I'll say once more that I do not know if a thumper provides a higher EtOH content than simple distillation, but it is not an unreasonable claim. It may or may not work, and to be honest I do not care either way.

Zombie - 10-3-2015 at 14:03

Quote:
" The only person worse at that than you is zombie, who somehow managed nearly two pages of posts without a reply."

To keep it in context, as is the crux of your post...

Those nearly 2 pages were all replies to statements or questions. I was replying to others. Not making random posts.

It's all good. :cool:

DJF90 - 11-3-2015 at 00:12

I appreciate that zombie. Theres an edit button and you can quote multiple statements in a single post; It would help keep the page count down as each page displays x number of posts. Some threads are a serious burden to read and this is partly why. Just don't turn into a serial offender like Blogfast...

See http://www.sciencemadness.org/talk/viewthread.php?tid=19143 for the forum guidelines. I'm discussing section 9 point 3.

[Edited on 11-3-2015 by DJF90]

Zombie - 11-3-2015 at 01:54

That multiple quoting is something I don't know how to use.

Now that you explained the "edit" button is part of that I will give it a try.

I do understand your point. Thanks...

DJF90 - 11-3-2015 at 03:11

When I find myself in need of quoting multiple posts, I click the "quote" button in the top right corner. That brings you to the reply box/text editor, where I copy the text including BBcode.and paste it into notepad or other word processor. Rinse and repeat as necessary. After compiling all the posts I wish to comment on/reply to, I write my reply and then copy/past back into the "quick reply" box at the bottom of the thread. In the FAQ you will find the BBcode to make text appear in a quote box (as well as various other formatting tools) but to quote a specific post by a member you need to use the quote button as I mentioned.

Sure, it may not be an elegant approach, but its the best I've come up with so far. It also helps avoid twenty-page threads that are of little use to any new or existing members not willing to trudge through the swamp in order to find a little quality content.

Magpie - 11-3-2015 at 08:46

To add to an existing post all you need to do is use the "edit" button. But edits must be done within 24hrs, except in the "prepublication forum" where there's a 30 day window, IIRC.

Zombie - 11-3-2015 at 09:09

Quote: Originally posted by Magpie  
To add to an existing post all you need to do is use the "edit" button. But edits must be done within 24hrs, except in the "prepublication forum" where there's a 30 day window, IIRC.



Lets see...


When I find myself in need of quoting multiple posts, I click the "quote" button in the top right corner. That brings you to the reply box/text editor, where I copy the text including BBcode.and paste it into notepad or other word processor. Rinse and repeat as necessary. After compiling all the posts I wish to comment on/reply to, I write my reply and then copy/past back into the "quick reply" box at the bottom of the thread. In the FAQ you will find the BBcode to make text appear in a quote box (as well as various other formatting tools) but to quote a specific post by a member you need to use the quote button as I mentioned.

Sure, it may not be an elegant approach, but its the best I've come up with so far. It also helps avoid twenty-page threads that are of little use to any new or existing members not willing to trudge through the swamp in order to find a little quality content.
Code:
When I find myself in need of quoting multiple posts, I click the "quote" button in the top right corner. That brings you to the reply box/text editor, where I copy the text including BBcode.and paste it into notepad or other word processor. Rinse and repeat as necessary. After compiling all the posts I wish to comment on/reply to, I write my reply and then copy/past back into the "quick reply" box at the bottom of the thread. In the FAQ you will find the BBcode to make text appear in a quote box (as well as various other formatting tools) but to quote a specific post by a member you need to use the quote button as I mentioned. Sure, it may not be an elegant approach, but its the best I've come up with so far. It also helps avoid twenty-page threads that are of little use to any new or existing members not willing to trudge through the swamp in order to find a little quality content.


[Edited on 3-11-2015 by Zombie]


I'll try on another forum to get this down.. :D

[Edited on 3-11-2015 by Zombie]

DJF90 - 11-3-2015 at 09:43

When you press the quote button, you're provided with the entire post between two bits of BB code, e.g.

[rquote=396532&tid=61566&author=Magpie]To add to an existing post all you need to do is use the "edit" button. But edits must be done within 24hrs, except in the "prepublication forum" where there's a 30 day window, IIRC.[/rquote]

Notice how it starts with [rquote...thread id...author]... that provides the hyperlink back to the original post that you're quoting. Then you have the content of the post (delete the bits you aren't interested in) and finally, it ends with [/rquote]. Then you can write your reply underneath. If you want to address each paragraph of the post in separate quotes, just make sure the BBcode is in place: [rquote...thread id...author] at the start, and [/rquote] at the end.

NB: Notice how you can see the BB code (square brackets) in this post? Thats because I've ticked the "Turn BB code off?" box so you can see whats happening "behind the scenes".

Zombie - 11-3-2015 at 12:47

Ok, That part I understand,

I am able to reduce to a few sentences or the "meat" of the quote.
I also understand the edit...

I Don't understand how to do Multiple quotes, and add the "quote box".

Even when I try to use the "quick reply", and go back one page to pull a quote, my response disappears.

Forget about shifting numbers up or down. It's all voodoo to me.

I can build an awesome computer, but know rats all about using them.

aga - 11-3-2015 at 13:07

It's more fun to just type a reply with no quote.

The delay allows others to reply before you do, thus causing all sorts of mayhem.

Magpie - 11-3-2015 at 13:26

For multiple quotes I open a 2nd window. Then just block and copy to the first window. You have to remember to enclose each quote with the proper BB codes. This may be crude, but it's effective.

[Edited on 11-3-2015 by Magpie]

Fulmen - 11-3-2015 at 14:08

Quote: Originally posted by Zombie  
Even when I try to use the "quick reply", and go back one page to pull a quote, my response disappears.

Yes, that will happen. Other software allows you to see the thread below when composing, sadly this doesn't. The trick is to pull up the thread in a new tab.
Some browsers have shortcuts for this, don't know what they are except on Firefox. But there you simply press [AltGr] while clicking a link or the back-button.

Zombie - 11-3-2015 at 15:26

Quote: Originally posted by Magpie  
For multiple quotes I open a 2nd window. Then just block and copy to the first window. You have to remember to enclose each quote with the proper BB codes. This may be crude, but it's effective.

[Edited on 11-3-2015 by Magpie]


Maybe...

Quote: Originally posted by Fulmen  
Quote: Originally posted by Zombie  
Even when I try to use the "quick reply", and go back one page to pull a quote, my response disappears.

Yes, that will happen. Other software allows you to see the thread below when composing, sadly this doesn't. The trick is to pull up the thread in a new tab.
Some browsers have shortcuts for this, don't know what they are except on Firefox. But there you simply press [AltGr] while clicking a link or the back-button.



Maybe more...


Quote: Originally posted by aga  
It's more fun to just type a reply with no quote.

The delay allows others to reply before you do, thus causing all sorts of mayhem.



By George I think he's got it.

That second tab was the trick.

Thank you guys. I owe ya' one! :D

aga - 11-3-2015 at 15:30

Quote: Originally posted by Zombie  
Thank you guys. I owe ya' one! :D

Oh good.

When can we expect repayment ?

Zombie - 11-3-2015 at 15:33

What do you need my friend?

I'll not share my sample red head but all else is open for discussion.

aga - 11-3-2015 at 15:39

Perhaps a little Science ?

It is called Science Madness after all.

Zombie - 11-3-2015 at 15:43

Hmmmm.

Now to wrap my head around that one. Constant challenges here.

Sure you don't want a puppy or something? ;)

aga - 11-3-2015 at 15:52

Nope.

Some Science would be good.

Chat shows we already have.

aga - 18-3-2015 at 14:25

... and as for Science, an Experiment has happened.

The initial results are a bit confusing, but then, this was a test of the apparatus, sensors etc.

First off, is the 'Thumper' so-called because it causes the first distillate (from the boiling pot) bash up and down in the thumper feeder pipe ?

Second, is fairly violent suck-back from the Thumper to the boiling pot normal ?

If so, that would explain why some people say that an empty Thumper pot is best, although suck-back would probably occur after it fills up.

Crowfjord - 18-3-2015 at 14:36

Hooray for experiment! I will begin my own attempts this Friday and/or Saturday.

I would expect suck-back at the end, when the pot cools down. Was this the case?

aga - 18-3-2015 at 14:49

What i saw was the distillate from the boiling pot crashing up and down in the feeder pipe to the Thumper pot, suggesting (to me) the reason for the name.

Semi-violent suck-back occurred after about 15 mins, dumping almost all of the Thumper load back into the boiling pot.

It may be bad design, so don't take anything as 'fact' just yet - this was just a preliminary experiment to try to establish some parameters, now that the required glassware has arrived.

[Edited on 18-3-2015 by aga]

Loptr - 18-3-2015 at 15:03

So the thumper does provide reflux by returning the distillate to the pot? ;)

aga - 18-3-2015 at 15:07

No idea yet.

Suck-back occurred in the experiment is all.

Might just be an error in the design.

It would be nice if Zombie would describe the functioning of a Thumper in more detail, so the experiment can be more accurately designed.

Zombie - 18-3-2015 at 16:08

There should be no suckback. Perhaps it will occur on cooling but not when running.

I am guessing the "thumper" pot was too high in relation to the boiler, or there is an air/vapor leak on the boiler fitting.

The other "maybe is you were heating too hard.

The object is to simmer That is the most efficient way to extract drinking EtOH, and that is what you are trying to replicate.
The term "thumper" is because of the noise. The thump intake will make a pounding sound that slows down as the thump heats up

I would try to make the bottom of both containers as level as can be.
I would also try to control the heat to keep it to a minimum. Just above simmering, and try to keep it there for the entire run.

If you have a thermometer in there the vapor temp should be above 170*f, and below 212*f

That will rise as the EtOH boils out but it is a fair guide.

aga - 18-3-2015 at 16:12

Thanks for the info.

Just a guess : the word Thumper must mean that it makes a noise.

Any clues ?

Zombie - 18-3-2015 at 16:49

That is exactly right.

It starts off with slow steady "thumps" as the pipe bounces off the bottom.

It will get crazy loud until the pots equalize in temperature, and then quite back down.


Just another thought... "suckback" might be the wrong term. Perhaps the "thumper" is not allowing vapor out fast enough, and pressurizing.

Be careful.:cool:


aga - 19-3-2015 at 02:47

Suck-back is occurring from the thumper back to the boiling pot.

I just tried it again with 200ml, and violent suck-back occurred 6 mins after distillate started entering the thumper.

It appears that a very steady/constant heat is required to ensure a continuous positive pressure from the boiling pot.

I can't help feeling that suck-back is the 'thump' and that in copper pipes you just can't see it happening.

Perhaps with a few more practice runs it can be made to run as expected.

Zombie - 19-3-2015 at 06:51

Do you see liquid transfering from the boiler to the thump pot?

That could be the issue... Scale.

There should be NO liquid transfer. That is called "Puking" in distilling or "Bumping" in chemistry.

in forty years of distilling I have never once experienced any sort of "suck back".

Quote: Originally posted by aga  


It appears that a very steady/constant heat is required to ensure a continuous positive pressure from the boiling pot.


It is also possible that your hot plate is cyclic, and can not hold a steady enough heat.
We can not use hot plates in distillation boilers because they tend to switch off, and on in cycles rather than maintain a heat setting.

Try to avoid any sort of "puking, maybe boiling chips will help I do use them in even large boilers, and perhaps a water bath might help to maintain a steady temp.

I know you will figure something out, and I really do appreciate your efforts here.

If I were to document any of this from MY end... It would be tantamount to a written confession.
I sort of like having access to daily life. :cool:

aga - 19-3-2015 at 08:25

No liquid transfer ?

As the EtOH vapour leaves the boiling pot, it was condensing on the walls of the short transfer pipe into the thumper = liquid transfer.

Zombie - 19-3-2015 at 09:16

Quote: Originally posted by aga  
No liquid transfer ?

As the EtOH vapour leaves the boiling pot, it was condensing on the walls of the short transfer pipe into the thumper = liquid transfer.


I see your point. This may be a scale issue combined with a materials issue.

Copper being much better at conducting heat will quickly reach the same Temp. as the containers, and greatly reduce or totally eliminate condensation inside the pipe. What little does condense can simply roll / flow out due to the size of the plumbing.
I imagine you are having liquid actually fill the diameter.

The same thing may be happening on the outlet from the "thump" causing pressure to build inside.

Is there any way you could increase the diameters of the plumbing?

Perhaps a pair of mason jars / water bath boiler, and 1/4" copper tubing installed thru grommets...

Something else that might help reduce this would be a burner under the transfer pipe to keep it from condensing. Insulation would never be enough due to the properties of glass. , ie: heat transfer.

Sorry this is getting so complicated.

[Edited on 3-19-2015 by Zombie]

aga - 19-3-2015 at 10:05

I came up with two possible anti-suck-back ideas: replace the thermometer on the stillhead of the boiling pot with a balloon, or turn the heat up under the boiling pot.

The balloon would expand as vapour pressure increased, then would contract sufficiently to relieve the partial vacuum.

Amusing as that would be, i opted to just turn up the heat, which worked.

As i'm not drinking the distillate, the speed of the process is largely irrelevant.

Finishing off a Vigreux distillation, then i'll have the data for Standard, Thumper and Vigreux setups.

Some Experiments Regarding Distillation Techniques

aga - 19-3-2015 at 13:18

A series of experimental distillations were made to Quantitatively compare the effects of using a 'Thumper' and a Vigreux column in the distillation of Ethanol/Water mixtures, specifically targetting the EtOH w% in the product.

The equipment used was all standard quickfit glassware, two thermometers, a kitchen timer and a refractometer (to measure the ethanol w%).

The thermometers were calibrated using boiling water, an ice slurry, and the standard y = mx + c formula along with a bit of algebra (to determine slope multiplier and offset constant)

Ironically an ethanol spirit burner was used as the heat source.

The FeedStock for all experiments was 500ml of cheap 37.5 w% Vodka diluted with DIW to give 1875ml of 10 w% EtOH/Water (as measured by the refractometer).

refract.JPG - 180kB

To determine the behaviour of a Thumper, a preliminary experiment was made with the apparatus seen here :-

thumprig.JPG - 212kB
thumper.JPG - 196kB

250ml of feedstock was loaded into the boiling pot, and 150ml into the thumper.

Less than 1 minute after lighting the spirit burner bubbles (of air) were seen leaving the pipe in the thumper liquid.

@10 mins the liquid in the 500ml flask boiled.
@12 mins condensate was forming in the transfer piping, and entering the thumper.
@14 mins the liquid level in the vertical pipe into the thumper could be seen rapidly rising and falling.
@16 mins violent suck-back dumped the contents of the thumper back into the boiling flask.
@18 mins the thumper felt significantly warm to the touch.
@28 mins the first distillate product left the apparatus.
@38 mins distillate stopped leaving the exit pipe.

7ml of distillate were collected.

A second attempt was made with 150ml in the boiling pot, 50ml in the thumper.

The suck-back problem was worse, with several suck-back events after 16 mins.
These were prevented by removing the thermometer stopper as the suck-back developed, and so it was determined that the suck-back was caused by sudden temperature drop in the boiling flask, which was in turn caused by the experiment being done outside in a light breeze.

A shield made from Al foil was devised to prevent this in subsequent experiments.

Logically, the thumper will heat faster with less mass in there, so a much lower volume was thought to be beneficial, so long as the inlet tube was covered.

A line was noticed in the boiling flask, so this experiment was immediately aborted.

Turned out to be a just a manufacturing defect rather than a hairline crack.


#1 Thumper Distillation

190ml was loaded into the boiling pot, 10ml into the thumper and the flame lit.

After 36 mins 3ml of final distillate was collected.

Testing with the refractometer showed no result at all (off-the-scale).
The distillate was diluted 50:50 with DIW and this solution was measured at 49 w%, meaning that the actual product was 98 w% indicating some error, probably in the dilution, as the azeotrope max is 95.6 w%.

The remaining 175ml of boiling pot liquid was measured at 4 w%.
The remaining 22ml thumper pot liquid measured 37 w%


#2 Standard Distillation (no column etc)

straight.JPG - 218kB

200ml FeedStock was loaded into the 500ml RBF boiling pot, and the flame lit.

After 10 mins 3ml of distillate had been collected.

This measured 76 w%


#3 Eleven-tier Vigreux Column Distillation

vigreux.JPG - 212kB

200ml FeedStock was loaded into the 500ml RBF boiling pot, and the flame lit.

After 16 mins over 3ml of distillate was collected.

This measured off-the-scale, and so was diluted 50:50 with DIW.

The resulting liquor measured 47.5 w% meaning 95 w% in the actual product.
Dilution error could have occurred as only 1ml of distillate was used.

Notes:-

In the Thumper distillations, the final product distillate was seen to stop after a certain time.
The experiment was stopped at that point, and the boiling pot had not yet begun to boil the remaining water.
It is suspected that more distillate would be seen after water began to boil and enter the thumper.

Suck-back is likely due to the similar volumes of boiling pot and thumper pot.
All photos seen of thumpers show them to be significantly smaller than the boiling pot.

Speculation is that the sheer volume of boiling liquid, and EtOH leaving the normal-sized boiling pot keeps up a positive pressure at all times, regardless of the volume of the thumper contents.

More experiments are required to quantitatively determine the full distillation profile for the three techniques, such as total time, yield and w% of product for a full run, and the w% of the product at set intervals into each run.

This set of experiments simply show that Thumpers do actually work in raising the w% of the product, at least in the early distillate product.

Magpie - 19-3-2015 at 13:43

Thanks for buying all this equipment and running this experiment.

I think your suck back is caused by condensation in the tubing between the pot and the thumper. Insulating shoud eliminate most of this. I'm sure your aluminum foil helped a great deal.

Is that Spain or England. Looks very nice!

Fulmen - 19-3-2015 at 13:48

Interesting. I haven't had time to crunch the numbers yet, but this suck-back could explain everything. Since few of it's proponents has had the opportunity to see it (metal construction), is it possible that this is the way they actually behave? If so, this provides the reflux needed to turn it into a complete stage. Mystery solved?
As long as there is a reflux caused by suck-back it behaves in accordance with basic distillation theory. It's a simple single stage reflux stage as far as I can tell. But I'll try to study the numbers a bit.

aga - 19-3-2015 at 13:49

Spain.

I'm sure that a much larger boiling volume of 'mash' would NOT exhibit rapid temperature changes, and so the Real distilleries using Thumpers would see little or no suck-back at all.

Their boiling pot Output would always be more than sufficient to overpower any pressure the Thumper could exert.

[Edited on 19-3-2015 by aga]

[Edited on 19-3-2015 by aga]

Zombie - 19-3-2015 at 13:52

You fought thru a series of hurdles to do all this. Kudos for all your efforts.

Your findings are in line with what I expected, and could not have been achieved if you did not apply such a valiant effort.

I also believe you numbers are correct. I have hit 99% Many times in column distillations, and several more times in "Triple distillations" using nothing but a pot, and thumper. That level never holds due to the hygroscopic nature of EtOH but the numbers can be reached.

The action(s) explained are also to be expected. Distillation will stop as molar fractions change. More heat/power is required as the EtOH is vaporized out. Generally there will be 3% EtOH in a "spent" boiler. Beyond that you are recovering more water than EtOH so distillation is impractical at this level.

At this point I would suggest getting a 10Ml beaker, and some teeny/tiny ice cubes... nEnjoy!

aga - 19-3-2015 at 13:53

Quote: Originally posted by Zombie  
At this point I would suggest getting a 10Ml beaker, and some teeny/tiny ice cubes... nEnjoy!

Ah Crap.

What now ?

Edit:

99% would be an error.

Break the aeotrope with say CaCl2 and maybe.

[Edited on 19-3-2015 by aga]

Magpie - 19-3-2015 at 14:07

I agree that both the pot and the thumper are acting as distillation stages. I don't think, however, that condensation is a necessary part of this. I would insulate all the way from the top of the pot, over to the thumper, and the thumper itself. The vapor coming off the pot is just at saturation temperature and carries no superheat. It's on the verge of condensing from the git-go. So it needs a lot of insulation so that the heat can be carried into the thumper instead of being lost to the environment.

Zombie - 19-3-2015 at 14:10

Unless you run thousands of distillations you would never believe 99% is real.

Fact is when a 100 gallon boiler is running for 7-8 hours, and has 9) 4" bubble plates, the combination of the heat in the system, and the purity at the top can break the azeotrope.

Like I said... Iv'e done it with a simple pot / thumper. For fuel use we use Benzene to break the azeotrope. It's cheap, and readily available here.

If I were you I'd get the "I Broke Azeo" badge, and wear it proudly!

aga - 19-3-2015 at 14:17

I'll do a potassium iodide/sodium thiosulphate/potassium dichromate back-titration and find out for myself, and for sure.

That's the wonderful thing about Science : there's no need for speculation or argument where a proven experimental procedure is available.

Edit:

Breaking this particular azeotrope isn't simply a matter of how many TEPs there are or what fuel you use.

[Edited on 19-3-2015 by aga]

aga - 19-3-2015 at 14:24

By what measuring device are you claiming 99 w% ?

Edit :

Pardon me.
I forgot that shaking a bottle and looking at the bead size was the most accurate EtOH w% measuring method ever devised.

[Edited on 20-3-2015 by aga]

Zombie - 19-3-2015 at 16:28

Two floating Nova Tech.Alch meters, calibrated at 60*f.
The first is a general test, and the second is exact. I send them both in once a year to be calibrated.

I believe it is a matter of heat at the top of the column, and the near perfect separation at the 7th stage. Taking off product from the 7th stage is azeotrope. Actually with a higher reflux ratio I can pull azeo. off of the 5th stage but I run at a faster rate, and add the extra plates.

At nine plates, and 182*f vapor temp. at the top of the column it is 99% consistently. It will not hold tho unless treated immediately w/ Benzine, and sealed. I store EtOH in 15 gallon Polypropylene drums for fuel use.

http://www.novatech-usa.com/Products/Alcohol-Hydrometers/B61...

http://www.novatech-usa.com/Products/Alcohol-Hydrometers/661...

Left open to air it will return to Azeo usually within two hours in Florida. Depending on how fast you work at the titration you will see the percentage drop on successive tests.

aga - 19-3-2015 at 16:33

7th stage ?

You have 7 Thumpers in your rig ?


[Edited on 20-3-2015 by aga]

Zombie - 19-3-2015 at 16:40

Nooooooo. I'm talking about a plated column in this case. One run beginning at 40% concentration. This is strictly a fuel still.

I have hit 99% on three successive runs thru a thumper tho, and there are several people I know that run 2 or three thumpers in line. Three is the MAX you can run due to heat transfer losses.

blogfast25 - 19-3-2015 at 16:42

I want to thank aga for the tremendous effort and time he's put into running this experiment.

But I cannot say I'm remotely satisfied with the results so far.

The aim was to compare distillate compositions using a thumper and without a thumper, in as near identical conditions as such a comparison allows. Instead technical problems were encountered from the get go: unexpected suckback. To claim the comparison has been carried out is like claiming the LHC found the Higgs Boson but with a seriously limping detector. No, first you repair the detector to how it's supposed to work, then you carry on. Anything else gets you laughed out of court and rightly so.

I had also hoped the experiment would shed light on how the EtOH concentration of the distillate evolves during the run, and not yield a mere single datapoint. This should have been fairly easy to achieve considering how well the refractometer performed and how little sample volume it requires per analysis.

There are in the immediate responses above a number of things I strongly object to (not in the least Zombie's phantasmagorical "I broke the azeotrope") but current poor health and other priorities prevent me from spending much time on them. Maybe later.

aga - 19-3-2015 at 16:43

Sorry, my mistake.

I thought you were referring to the OP's question.

Using a Standard Plate Equivalent distillation model is not thumper-related.

blogfast25 - 19-3-2015 at 16:45

Quote: Originally posted by aga  
Sorry, my mistake.

I thought you were referring to the OP's question.

Using a Standard Plate Equivalent distillation model is not thumper-related.


Sorry, but I really do not know what you mean, or even who you are addressing.

Zombie - 19-3-2015 at 16:47

Quote: Originally posted by aga  
Sorry, my mistake.

I thought you were referring to the OP's question.

Using a Standard Plate Equivalent distillation model is not thumper-related.



Just answering the questions.

aga - 19-3-2015 at 16:53

As to Blogfast25's comments, all i can say is Humbled.

In the light of those comments, it is now Obvious that i've just heated stuff up and written stuff down, then thought i Knew something.

Feck.

More Thinking required before randomly doing stuff and thinking i've somehow done anything significant.

Further experimentation to follow, hopefully with more robust data.

Zombie - 19-3-2015 at 16:54

Quote: Originally posted by blogfast25  


There are in the immediate responses above a number of things I strongly object to (not in the least Zombie's phantasmagorical "I broke the azeotrope") but current poor health and other priorities prevent me from spending much time on them. Maybe later.



With all due respect, I'm not here posting B.S. just for the sake of having something to type.
If you want to debate theory, you win!
If you want to debate what "actually" happens in a distillation run, I have explained it all the best I can. Breaking Azeo is not anti gravity. It happens.

I'm glad you saw the results, and hope you fell better soon.



aga - 19-3-2015 at 16:57

Quote: Originally posted by Zombie  
Just answering the questions.

It'd be helpful if you did answer the more specific ones.

Zombie - 19-3-2015 at 17:07

Like?

aga - 19-3-2015 at 17:14

Quote: Originally posted by Zombie  
Like?

I clicked it endless times, but this doesn't work like facebook.

Ah well, so the Thumper distillation Profile needs Properly comparing to a Standard distillation profile.

A new Project ! WooHoo !

This Learning thing is wonderful. Love it.

blogfast25 - 19-3-2015 at 17:29

aga:

I would be happy, if the suckback problem cannot be overcome, with an experiment with an initially empty thumper, if possible using multiple EtOH measurements over about 50 - 100 ml of distillate.

Zombie:

The claim that you broke the azeotrope is simply anti-scientific misinformation that should have no place on a science forum. I know in your mind there's the 'world of booklearnin' folk and theory' and the 'real world of billies' but in reality, there is only one world: one in which azeotropes cannot be broken the way you claim they can.

[Edited on 20-3-2015 by blogfast25]

Magpie - 19-3-2015 at 17:51

Zombie I'm trying to respect your skills and your extensive experience but telling me you broke the azeotrope with plates and heat is straining my nerves. If you are correct you had better take out a patent quickly. Those industrial fuel manufacturers like Archer Daniels Midland are going to want that technology bad. Then they won't have to waste all that money on running their mole sieve columns. ;)

blogfast25 - 19-3-2015 at 18:01

Quote: Originally posted by aga  
In the light of those comments, it is now Obvious that i've just heated stuff up and written stuff down, then thought i Knew something.



I think you may be a bit too hard on yourself but the difference between Good Science and Faulty Science is only a cigarette paper wide.

You're very close to solving this 'controversy' for once and for all. So lets try and do this.

Good luck: Good Science is seriously hard.

[Edited on 20-3-2015 by blogfast25]

Zombie - 19-3-2015 at 18:51

I won't beat this into the ground but I will say this.

In pressure swing distillation (which it appears Mr Aga, inadvertently achieved) you get different behaviors from azeotrope.
Even tho AT azeotrpe the mixture is basically at one boiling point the mole fraction can be shifted by varring the pressure.

These shifts in mole fractions show that the azeotrope can be broken.

Quote:
Pressure swing distillation[edit]

Azeotrope composition shift due to pressure swing.
A hypothetical azeotrope of constituents X and Y is shown in the diagram to the right. Two plots are shown, one at an arbitrary low pressure and another at an equally arbitrary, but higher, pressure. The composition of the azeotrope is substantially different between the high- and low-pressure plots – higher in X for the high-pressure system. The goal is to separate X in as high a concentration as possible starting from point A. At the low pressure, it is possible by progressive distillation to reach a distillate at the point, B, which is on the same side of the azeotrope as A. Note that successive distillation steps near the azeotropic composition exhibit very little difference in boiling temperature. If this distillate is now exposed to the high pressure, it boils at point C. From C, by progressive distillation it is possible to reach a distillate at the point D, which is on the same side of the high-pressure azeotrope as C. If that distillate is then exposed again to the low pressure, it boils at point E, which is on the opposite side of the low-pressure azeotrope to A. So, by means of the pressure swing, it was possible to cross over the low-pressure azeotrope.

When the solution is boiled at point E, the distillate is poorer in X than point E. This means that the residue is made richer in X than point E. Indeed, progressive distillation can result in a residue that is as rich in X as is required.

http://en.wikipedia.org/wiki/Azeotrope

I know my instruments are accurate I pay for them to be, and I can watch the gauge float back up to azeo.

deltaH - 20-3-2015 at 01:00

Zombie, even if you crossed the azeotropic point, you forget that the phase diagram flips at that stage and that vapour coming off thereafter is, in fact, enriching in water, so it can't happen without a separate column or stage and collecting the bottoms as product.

Pressure swing distillation is conducted using two separate columns. First column brings it near the azeotrope, then the distillate is flashed into a second column operating at very low pressure and the very concentrated ethanol is taken from the bottoms of the second column.

Distilling in the phase diagram region past the azeotropic point is also really difficult, because you will notice on the phase diagram that the curve lies very close to the x=y line. That means a great many EXTRA stages are required to enrich those few extra percent in that region.

I believe that you got false readings because of the presence of contaminants (e.g ketones, other alcohols, whatever) that skew the result, so-called matrix effects in analytical chemistry. You would need to calibrate with those contaminants present in order to get accurate readings, but that is off course not practical, but just saying.

aga - 20-3-2015 at 01:31

Quote: Originally posted by Zombie  
I know my instruments are accurate I pay for them to be, and I can watch the gauge float back up to azeo.

It'd be more convincing if you could show us the test certs from the calibration people.

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