Is see through good? And is it better if it is continuous?

[Sadi]

My observations on how successfull the seperation with this setup is below.

Allow me to shortly go over the process for the sake of some of our friends who may not be familiar with it.

As I am feeding the coil/pot with wash from below, it gradually becomes hotter while going up and at the time it reaches the finger, wash temperature becomes hot enough to vapourize heads and hearts but cold enough for tails and water and they remain liquid.

Keeping that flow/feeding rate for wash that is going in to the coil constant, and as the heat coming from below is constant, the temperature of the wash at the finger will be constant also. At that state I get an equilibrium. And if the constants remain constant, the still will run continuosly at that state, vapourising heads and hearts and keeping tails and water as liquid continuously.

As heads and hearts are vapour now, they go up filling the the top column. As the temperature along the column goes from hot to cold moving to the top, and it is coldest at the top, the heads should stay there on top of hearts and as we are feeding the column continously with heads+hearts as vapour, finaly there should be enough heads accumulation in the globe and will be pushed out from the top exit continuously.

As the column is stacked up this way (heads stacking on top of hearts and hearts accumulate below them), hearts will exit from the arm to the condenser.

This takes a little while to stabilize and work like this continuously.

However some tails may also vapourise. But as there will be less amount of tails as vapour than heads and hearts combined, and as the column is being stacked on top with hearts and heads, the tails trying to join the que will face two problems to stay as vapour. The problem of space and temperature. There will be less space on top and the temperature will not be hot enough for them and they will not be able to go up high. Hopefully they get refluxed and they will join the backset as liquid and go down.

Does this work? and how successfull it is?

The definitive answer could come from having a lab test the samples coming out from each exit. I did not have the opportunity to do so yet. So I don't have any scientific proof.

So, what tools do I have to observe? Taste, smell, and as a plus, sight.

As I was using glass equipment all the time, I was able to see how vapour looks on glass during each phase when using my pot still. You know the sight of water vapour on glass. I see that happening when tails start coming. It starts with a few patches here and there and finally invading everywhere, if I don't end my run before. During heads, the column looks perfectly clean and shiny. During hearts, its all shiny too, but you can see a little phase change from vapour to liquid in the arm/bridge. It happens as little drops at the start of the arm but increases and becomes lines alongside its length up to the condenser.

Using these observations, what I see while operating this still is this.

If I don't see any water vapour anywhere up the column, I think there are no tails coming up. This happens when the thermometer at the top shows 74-75C or less. I also see some little drops alongside the arm. Which is similar to what I see during hearts run with my pot still. If I dont see any drops then I know that the temperature of the wash at the finger is not hot enough to vapourise all the hearts and I am loosing some product.

However, if the temperature at the top approaches 76C then I see little patches of water vapour around the hole where the arm connects to the column. Interestingly enough it is just around the hole, not inside. I also see some at the level of the finger.

If the temperature nears 77C then I see more patches of water vapour here and there and the hight of it around the finger rises. If the temperature keeps rising then there are more.

These are my visual observations. Do they mean something? I am positive.

When I take samples of product during different temperatures at the top, dilute and taste, I can taste tails from the samples taken at 76C or above. below 75-74C it is very clean and nice. I did not run below 72C as I am losing product then. I did not feel heads from these samples.

When I smell the heads jar, it smells like you know how. I don't taste them.

I do another test which I read somewhere. A moonshiners way. I take one or two drops on a spoon and light it with a lighter (away from the still and in a dark corner) and look at the flame. According to what I read, hearts flame is blue, heads are yellow, and if there is lead contamination you see red.

I never saw any red. and haven't seen any yellow from the drops from the condenser. Only a very nice blue flame. However, when I dip my spoon in the heads jar and then light it, I always see yellow sparklings.

All these tell me that there is some success. Howmuch and how accurate? Only lab tests can tell.

I haven't tried running these low wines in a ruflux setup yet. That will tell me more when I do in the future.

I like to experiment and learn. I haven't ran out of experiments yet.

I hope this sums up my observations on seperation with this still. I respect all your judgements.

Next, I will try to share my thoughts on what practical ends we might get from this setup.

Cheers

Sadi

[Sadi]

Hello friends,

Here are some opportunities for flavour, this setup provides and I hope you will find some as interesting/useful enough to try.

I can potstill a small batch of 1 Lt of the given wash, collecting into small glasses, dilute taste&smell to see which one I like, thus having an idea what kind of flavour this wash can produce at certain intervals. Then using this setup, I can try to match that, in the beginning of the run, when I am tuning. That is, I can target a certain flavour.

I already put back into the wash bucket what I get from the condenser, while I am doing the tuning at the beginning to find an equilibrium. This opportunity/possibility gives me ideas.

I can always add/mix low wines, flavourings, anything, when I want, to the wash bucket during the run. And as I am mixing with wash in the bucket, I will end up enhancing flavour.

I can use tools like the pearsons square and phase charts to calculate the proportions and timing and I can put an alcoholmeter in the wash, add the low wines I got so far, stir and read alcoholmeter to see the new abv and decide if I have reached a target. Or I can go by taste and smell.

I can pour back, say every 100 ml I get, or even use the wash bucket as my collection vessel for a while, pumping from it and recieving to it at the same time. While running like this I can read the abv from the alcoholmeter and wait till it reaches to a certain % then I can run the rest without recycling. I can also go by taste and smell and when after some recyling like this, if I am satisfied, I can run recieving that product till the end. That is, I can select a certain flavour. This was not possible as easy as this without this setup.

Can I get better seperation and/or more flavour and/or perhaps some different products? I have yet to experiment and see.

I can use this procedure to do some kind of neutral runs aswell. For example, during recycling (I can dilute also) like this, if at one point I decide that the vodka is good enough, I can go at that state till the end. Moreover, at that point, I can add some apple juice or some other flavouring (Fruit juice, herbs, anything like that) to the remaining wash and can collect something different with the clean enough vodka that I have produced so far.

I will not go any further as I am sure you have the idea.

Even with the current yeild% this setup produces, I think I am having savings in terms of time and cost and I am having some extras.

For example, when I do ouzo/araq/raki with my potstill, First I strip a fruit wash. Second, mix low wines with anise and do a sprit run making cuts. Third I dilute and do a final sprit run to cut a somewhat wider middle portion to get a more balanced product.

With this setup my next run will be a dried figs/sugar wash. I will attach my 2Lt thumper and fill some of it with anise seed. I hope to combine the first two steps of my method by doing this, and afterwards potstill making cuts and may be achieve a more flavourfull product with one less step. I may also end up using less anise seed than my other method needs without loosing quality.

This procedure can be used to make gin or absinthe also.

As I am writing more ideas keep coming to my mind. But I better not try your patience.

So, what is the verdict?

Is see through good? And is it better if it is continuous?

Let me answer first, I think all our potstills strip and as it is a matter of taste, one can choose whatever one likes. For me with the extras and opportunities/possibilities this continuous setup gives, the answer is yes it is better.

Is see through good? Well, although it is nice, as long as we have a stripper, I think it does not matter.

I hope you enjoyed reading this long post.

Next I will add a few ideas that I already have to improve the current setup and I will try to be brief.

Cheers,

Sadi.

[Sadi]

I think making three changes will improve this setup.

At the enterence of the arm if I can make some kind of door which is open from the top. I think heads will find it more difficult to escape from there (if they ever do) and It may be harder for tails to go up to that point and get in either (perhaps as when I run near 76C which may give me a broader flavour profile). I think I have a design and I am thinking about how to implement this design with glass. It would be easier with metal though.

As this setup is dependent on equilibrium, and equilibrium is dependent on keeping some variables constant, I want to eliminate preheating and change the way the pot/coil is heated.

I will make the finger detachtable from the coil and close its base. I will let the backset to exit/drain near the base.

I will have a different coil/pot perhaps made of copper and try to heat it with gas/hot air or both. This will also reduce the height.

If I am successfull then I think I will have better seperation and can double or triple the wash flow which is about 7.5 Lt per hour at the moment.

Cheers

Sadi.

[Abussive]

Transparency is invaluable when we're not sure what's going on inside, I'd say.
It's of little or no value for the more mundane components (lyne arm, condenser etc.)
But for a fractionator.... invaluable.
It would be wonderful to see a "scrubbie"-packed fractionator and then, side-by-side, photos of an SPP-packed transparent fractionator "doing their stuff".

You're very clearly making huge inroads into quality continuous distillation.
A lot of Members will be watching, and learning!

[Abussive]

Sadi,
I forgot to ask:
Are you having your output distillate analysed using Gas Chromatography by your Chemist / Chemical Engineering contacts?

If you do, and as you understand the taste and smell of "tails", can you post or PM ANY data you have (or discover) regarding the identities of which particular compounds make "tails" versus those which add flavour?

We have a Member in New Zealand (Kiwi) who is trying to get a Chemist friend to do analyses, and it would be really powerful to get a second input. I have suspicions about two compounds which probably make particularly smelly contributions to "tailsiness" (2-Nonenal and Geosmin).

All such data will help us decide on good strategies for targetting tails removal in a continuous single distillation, I think.......


Separate question:
Does your "heads" output smell very pungent - lots of acetaldehyde?

[Sadi]

You're very clearly making huge inroads into quality continuous distillation.
A lot of Members will be watching, and learning!

Thank you for your kind words, I am only trying to apply what I have learned from all of you friends here.

As for having my output to be tested, my time is very limited these days but I will be on it rightaway. It may take some time to happen though.

I hope I can make the changes/improvements I am planning on the setup soon. And I will start a new fresh grapes/reisins/sugar ferment, part of it will be my first try on some brandy. I think that will give me better samples to do the tests. Any ideas on what kind of samples to collect? I mean, should I take a sample with some tails, or should I try to get a very clean output and have that tested along with the heads? or all of it?

As for heads smelling how much acetaldehyde, I am not sure how to answer that. I don't know the names of the smells. I can differentiate some number of different smells, and in the heads, the only one which I know for sure is the smell of acetone which is not very dominant.

[Abussive]

You're very clearly making huge inroads into quality continuous distillation.
A lot of Members will be watching, and learning!

Thank you for your kind words, I am only trying to apply what I have learned from all of you friends here.

As for having my output to be tested, my time is very limited these days but I will be on it rightaway. It may take some time to happen though.

I hope I can make the changes/improvements I am planning on the setup soon. And I will start a new fresh grapes/reisins/sugar ferment, part of it will be my first try on some brandy. I think that will give me better samples to do the tests. Any ideas on what kind of samples to collect? I mean, should I take a sample with some tails, or should I try to get a very clean output and have that tested along with the heads? or all of it?

As for heads smelling how much acetaldehyde, I am not sure how to answer that. I don't know the names of the smells. I can differentiate some number of different smells, and in the heads, the only one which I know for sure is the smell of acetone which is not very dominant.

Any sensible approach will work.
An analysis of the heads should be very straightforward for a first analysis.
Acetaldehyde gives a stinging, acrid (makes you push the sample away) smell.
You can remove any acetaldehyde (and it's smell) from the mixture using sodium bisulphite.
http://en.wikipedia.org/wiki/Sodium_bisulfite
That reaction may also prove useful in removing undesirable higher aldehydes chemically, later (2 nonenal for example....).

Acetone is often described as either " green apples" or, these days, "nail varnish remover" (which it is!)

Ethyl acetate is a fruity smell when pure, but easily overpowered by other contaminants.
It can be removed by saponification (add a little dilute caustic soda and it will convert to ethanol and sodium acetate).
http://en.wikipedia.org/wiki/Saponification
A GLC trace will easily pick them out.


If you found that tuning to a certain temperature causes "tailsiness" to spoil your output, that would be a great place to take samples either side of...... it should hugely assist in identifying which compounds (or at least which peaks on the GLC trace if no MS is connected!) causes that particular type of "tailsiness", for your particular type of wash input.

It's highly likely that many compounds are capable of causing bad taste and smell, so what may be a problem for you (and your chosen wash) might be no problem at all for others using a different wash.......

I believe that whatever they are, once identified, we can develop strategies for keeping them out of our distillate. All sorts of options exist for targetting them. Physical and chemical.
But first we need to "get them in our crosshairs" so to speak!!!!

The same theory also applies to flavoursome traces.... we might easily discover that too much of a particular tasty compound begins to spoil the effect. So we learn what the maximum limit is.

I'm sure you get the idea.

I suspect that we can at least derive a fractionation regime where we can say with considerable confidence that "removing x" keeps tails taste out of our liquor.
Even if in doing that we remove some flavour as well, we can take separate action with the removed fraction, extract what we want and remove what we don't, then blend it back in.

("Hydro-separation" is one form of this technique, and can be very effective.)


By now it may be dawning on some readers that there can be little hope of detailed, precision flavour fractionation in a varying composition (batch still) system. So it's probably fair to believe that further and significant improvements in the removal of undesired flavour compounds can only be reliably and reproducibly achieved in a stable, steady-state continuous system.

[punkin]

("Hydro-separation" is one form of this technique, and can be very effective.)

Shutup will ya. you'll summon mike.

[Abussive]

Everytime I throw those old bones into the air, they come down saying "Mike!"

[Sadi]

I finally got my new pot/boiler today.

new_pot1.jpg (37.72 KiB) Viewed 844 times

new_pot2.jpg (24.67 KiB) Viewed 844 times

The coil is around 10mt long and internal diameter is 6mm. The drain is wider to allow easier exit of the backset. The middle part is 6.1cm wide and 10cm long. the tube inside which is connected to the coil at the bottom is 1.8cm dia and 13 cm long. There is a cap fitted on top of it to act as a stop if the wash overboils and wants to go up in the column during tuning. And finally there is a glass fitting to which the upper column will be fitted.

With this boiler/pot, I eliminated preheating. And I can drain directly to the basin with a hose. Which is a big help from the previous design. I also reduced the height a lot. The height of the coil with the glass fitting is 29cm long.

I did a cleaning run without the top column. While cleaning I checked if the pump can deliver more flow than the boiler can handle. Yes it is a lot more which means I can run it with adjusting flow.

After running/boiling some diluted vinegar I adjusted flow and set the temperature around 75C which is around my normal operating temperature. At that temperature I collected from the drain some hot water/vinegar. It was 50ml at 5 seconds. Which means 600ml a minute and 36Lt an hour. It is a BIG improvement. I was able to do around 7.5Lt an hour previously. I am very excited.

I was able to touch the outside at the 5th row from the top. What I did not expect was, because the outer coil is colder there is condensation of air on the coil. And finally drops of water/condensation occurs. Not a big problem but may be I can eliminate that with insulation.

Tomorrow I will run a figs/sugar wash. I plan to use a 2Lt thumper with some anise seed in it. I will post results with some pics.

All in all, I am very happy.

Cheers.

[Sadi]

Here is how the setup looks, I took this picture before running it.

setup1.jpg (49.71 KiB) Viewed 797 times

After setting it up and firing it, I started collecting low wines almost immediately. I made the mistake of starting at full power, and the product flow was more than the condencer can handle. I reduced heat and increased flow and was able to stabilize around 75C. At that point, looking at the product output, I saw that it was a little bit slow, then I realized it was due to the thumper and also realized I should run at a higher temperature (around 77-78C). Which meant some tails coming out, but as I had the thumper some of it should be trapped in it.

Putting a thumper with some anise seed in it was a mistake for this first try of the new coil/boiler. I should have tested it on its own for this try.

I put a little water in a little cup and got some product in it. It immediately louched. The idea of both stripping and making a product was working. I took a sip and it was somewhat smelling and tasting raw. Maybe it was not a very good idea. I will see that when I pot distill it, as I was intending. At least I was able to extract enough anise oil in the low wines.

There was 150gr of anise seed in the 2lt thumper and no liquid. Although some of the anise wetted a bit after a while, I stopped and put around 750 ml water in it, hoping the rawness might go away. It turned out that I should have put less water and there was not much difference in taste. The level rose and here is how it looked like after running like that for some time.

thumper1.jpg (43.73 KiB) Viewed 792 times

I liked being able to stop and startback almost immediately whenever I want.

I collected around 3Lt product. The flow of wash was around 18-19Lt per hour.

This is the product.

product1.jpg (45.65 KiB) Viewed 798 times

I think there can be some improvements for the boiler.

I will think of finding a new way of making the coil. It is coiled to work from cooler to hotter when going towards the middle. This creates condensation on it.

Also the diameter (6mm) of the coil might be a little small. After a while some CO2 accumulates and this becomes a variable affecting stability. Previously this was not a problem, maybe because the diameter was 10mm and the speed of the flow was taking care of this problem. Thinking about it now, it may be due to the pump. I changed the way the hoses are connected and used reducers before coil entry and did not use the automatic flow control thingy. I think I will be better off using it.

In the column after the coil, the drain should be going down like a bent finger keeping its enterence always in backset that is accumulating in it. As I was using a thumper there was more pressure inside and some vapour might have found its way out of the drain. I might also have a valve on the drain before the hose to be able to adjust the level of the backset in the column.

There was some heads collection but it was somewhat less. I will think about seperation after I make the necessary changes to the boiler.

Although this run was not a complete success, eliminating preheating and increasing flow is a big plus for me. I think I have a good alternative stripper to the pot I have. My biggest pot is 17Lt and now I can run more than it can hold in less time than it takes it to heat up.

Cheers.

[Sadi]

Thank you for your kind words, and yes I am trying to be careful.

I have pot distilled the low wines and made cuts. The product was great. I think the idea of using a thumper to extract anise oil in the low wines when stripping and then pot distilling for a sprit run making cuts is good.

I was doing a strip run then a sprit run and then a product run and then running the product to get out the undercooked and overcooked parts of anise by making a somewhat wider middle cut. Now I combined the first and third step and then the second and fourth getting the same product in two distillations instead of four. This time, I also diluted with some wash and therefore less water before pot distilling and I think the flavour is improved.

So far, I am happy with the progress I made.

It was my first try making araq/raki from a dried figs/sugar wash. I am very pleased with it.

I hope I can have the changes to the coil/boiler made soon. I have a melons/sugar and a raisins/sugar wash bubbling which will be ready to run in a couple of days.

Cheers.

[Sadi]

At last I could strip melons/sugar wash. I also had the changes made to the coil/boiler. Everything worked fine. I used the AFC, tried to run without it after a while but then turned back to it. I could not measure the flow rate but can roughly estimate it to be around 9-10 Lt per hour. I was trying a few new things but measured the product output which was around 1.5Lt per hour at 50-55 Abv. Which is ok.

As this new boiler can be heated at higher temperatures I decided to run at a lower abv this time, without considering seperation like a pot stripper. It was easy to adjust but I stopped after 28Lt because I felt somehow I was not getting enough product. I will pot distill the remaining 12Lt and see how much I can strip out of it and then I will know if I really lost some product.

Everything seemed fine and I can't think of any reason as to why all the alcohol may not be stripped. I am sure none escaped from the drain as vapour. Any ideas?

Given that there is not any product loss, I think the coil/boiler is a worthwhile idea as I am trying to strip around 100Lt of wash in one go without using a big pot. As the product flow is increasing seperation/fractionation is not as successfull as the previous boiler setup. I will think about it after successfully stripping the wash at a rate of at least 15Lt per hour.

Cheers.

[Sadi]

I am relieved, I was not losing any product. After stripping 10Lt with my small pot I got 1.5Lt of 50%abv.

I was adding melons during fermentation to have more flavour. It seems I lowered the abv of the wash by doing so.

However, thinking about solutions in case I was losing product, I think I have an idea that may be of use. I will replace the cap and add a piece to spray/splash the hot wash/vapour going in to the column. I hope to try it next time I run the still.

So far I think I am on the right track with this boiler/coil. With a higher abv wash, I will surely strip to get more than 1.5Lt low wines per hour.

I made some wine from fresh grapes and ofcourse after racking added sugar on the skins and fermented for grappa. I even racked that and added more sugar for another round. I plan to add 5kg sugar each time and see how many rounds I can go like that.

Cheers.

[Sadi]

I stripped 100 Lt raisins/sugar wash at around 7.5 hours yesterday. If I can keep it below 6.5 hours then I think it will be ok.

I collected ~12Lt of low wines at ~57% abv. Considering some of the tails going out from the drain I think that is reasonable.

I tried to run at ~78°C but it was not set and go always. I had to move the AFC up or down a couple of times to keep it there. I think I have to work on controlling wash flow better. I hope the peristaltic pump will be an answer when I get one.

The boiling looks like this.

boiling.jpg (14.84 KiB) Viewed 743 times

This run I used a glass tube instead of the cap to splash the vapour/liquid coming out of the boiler. I think it is successfull. Here is how it looks like.

splasher.jpg (28.98 KiB) Viewed 744 times

So far I see that the idea is working. Now I can think about improvements. My primary goal is to have a stripper that I can use instead of a big boiler.

Cheers.