Is this flooding or normal? (video)

[StillerBoy]

In general, seeing my conduct, I see that I fell into the most classical beginner mistake: watching the temperature.
I was afraid to bring inside the "tails" when the temperature at the elbow suddenly rises, but I was very far from that moment. I see from my notes that heads are generally around 83-85 °C, and the heart is up to around 90°C. Tails have a vapour temperature of around 93-95 °C. I should not worry about collecting tails temperature until my vapour is up to 90°C. I begun worrying too easily and too fast. The theory is firm,( the theory is not firm ) but the practice is weak.

Birrofilo..

You are learning the wrong way, and you will have to un-learn what it is you have learned.. and you are not doing what I stated you should do with the operation of the unit you have.. re-read what I stated on how to operate your unit.. make notes and an outline the steps to follow.. otherwise I can not be of help..

Forget.. Forget... FORGET Temperature in stilling.. at the very least what you are stating in your quote.. at your stage of understand and experience, stilling temp mean nothing, but create issue like you are having.. stop right there and re-read this time taking notes..

Those temp figure mean dick all in real stilling and especially with the unit you have.. company build unit that are meant for them to profit grossly from and induce buyer into error.. and you have fallin trap to it as many have before you..

Stilling is so easy it is laughable.. yet very little get it.. for a pot operate, no temp probe is require, ANYWHERE.. it need power control and a watchful eye.. for refluxing one temp probe at the top the packing is needed.. and that temp has to remain stable once into the mid section of the heads is reached, and throughout the rest of the run until a good portion of the tails, then you are back into pot mode and stripping.. simple really.. the doing, well, as you have experience, not so simple.. WHY.. cause of the garbage learned having of no value..

But you have start un-learning..

Mars

[shadylane]

Don't worry too much about theoretical temps
Your still can't read
Every still is different and run differently
Keep practicing and you will figure it out

[Rrmuf]

Don't worry too much about theoretical temps
Your still can't read
Every still is different and run differently
Keep practicing and you will figure it out

+1 on this and what Mars is suggesting: Go through Mars's method for operating the CM unit. It is exactly what I had to do in order to get through my first reflux run. The last video of the sight glass refluxing looks consistent with my experience as well.

Glad you ditched that filter disk: It is a non-starter according to myself running into the same issue flooding.

Good luck! I can see you are enjoying the fun in learning I do too. I also have temp readings on my still: I don't drive by them but just like to look at them react to whatever I am doing. It is a just a fun observation point. It's like putting my hand on the column from 10m away while I do something else.

[dukethebeagle120]

Do more research.
Learn to crawl before walking.
Imo

[dukethebeagle120]

Do more research.
Learn to crawl before walking.
Keep trying
Imo

[Birrofilo]

OK I have an update.

First, I knew I don't drive by temperature. That I knew. But being obsessed with collecting neutral, I had this idea that, if I let the temperature rise too much in the elbow, then I would be collecting tails. I was misinterpreting (not his fault at all) the advice about keeping an eye on the thermometer to watch for the tails to come, and not let it raise, but I did that "too early". I do presume that if one controls the dephlegmator in keeping a constant temperature one can "squeeze" or "sift" the heart while having the tail components reflow, but that should be just the very end. I am supposed to have a long intermediate run with the vapour temperature basically constant. For me, that vapour temperature was 73°C or so, which makes me suspect the thermometer well is too thick.

Another source of mistake was tasting the product often and always finding it too strong. That was probably a mistake. Had I just collected the product in many numbered jars, while keeping a constant product flow (reducing the cold water in the dephlegmator when the collection slowed or stopped, and going on) and made all analysis later, I would have thought less and made less mistakes.

Yesterday evening I resumed the stilling, but the leakage in the glass window was showing off brutally with a stink of tails which was all around my kitchen. I definitely know, now, why it's described as "wet dog" or "wet cardboard". It's the only thing which I learned for sure, how to detect the smell of tails . Leakage is not good, obviously.

So yesterday at 4 AM I stopped the work and this morning I woke up with the idea of solving the leakage first. I dismounted the contraption, I tried to open the glass element and I saw that it was somehow stuck, too much tension applied, the "prisoners"* were skewed. So when I reassembled it, I just tightened the screws by hand, telling to myself that less is more. Another mistake. When the still was hot again, all the screws were lose. I tightened them again but there was a tiny little leakage nonetheless. That's certainly due to the inner gaskets being covered with Teflon tape, making the surface not perfectly even. Visual inspection of the gaskets doesn't show any irregularity, though.

Next time I will simply tight the screws by tool, and before mounting the glass on the still I will test the leakage by filling it with water.

Today after two hours of "equilibrium building" I reduced the cold water in the dephlegmator very, very slowly. It took another hour before I begun collecting in order not to disturb the equilibrium of the column. At that point, the temperature at the elbow was 92°C. The probe doesn't go inside the vapour flow (it goes inside a closed well), maybe the vapor is a bit hotter. Maybe it is a lot hotter.

I tasted the product and it was very, very, very smooth, no pricking, no nothing... too smooth... really too smooth, so I measured the alcohol content, and it's a whopping 0 %, as in "distilled water".

I collected overall around 4 litres vs theoretical 8 litres in the pot. My supposition now is that the remaining alcohol escaped through the leak during these three days of run. The stink of heads and tails is detectable, and probably the pure ethanol was not, but it was going away with the rest. The "mirror test", which I applied several times, failed miserably: the mirror would not get steamy even when the glass element was leaking in front of me.

Well, learning is this, correcting one's mistakes.

Now I will have some fun in taking all 30-something jars and noting down first the ABV of each jar. Then I'll do some tasting with some more exact dilution. Then I'll decide what to do with this stuff, there might be some good product in it.

Next move is to make one single stripping run and immediately a spirit run, because the stripping is stupid-easy, while the spirit run is where I have to iron out all the wrinkles.

* I don't know how do you call a prigioniero in English. It's a bar which is threaded at both ends and which serves as element of union between two or three objects, as in a sandwich. This is e.g. used in engines to couple the cylinder head and the oil pan with the main engine block.

[Rrmuf]

Yes. That WOULD be too smooth! Thanks for sharing!

[StillerBoy]

Good to read that progress is being made.. and re-learning the proper way of operating a unit.. re-read what I've posted many time, until it fully understood.. those are the basic and need to be well learn..

With time, experience will be gain, and from that point starting the process of experiencing how to find tune the unit on vapor management behavior.. but right now is not the time..

Congratulation for wanting to spend the time to un-learn and re-learn..

Mars

PS.. on the issue encounter with the slight glass.. the issue is cause by not tighten the nuts in their proper sequence and torque.. much like one would torque a car wheel.. one nut and opposite, and gradually increasing the torque as one goes repleting the cycle..

[kimbodious]

Probably the best thing to do for reinforcing your learning is to dilute the spirit you have collected and rerun it right now.

[Birrofilo]

@kimbodius

That's probably what I will do. But I will first train my nose in tasting the differences between the fractions, and I will jot down the ABV of each jar, just to see if I see some anomalies or to gain some familiarity with the process. More than enjoying the spirit I produced, I enjoy the discovery of the process at the moment.

I would also like to pay a tribute to the genious (who is this guy?) who invented the home reflux still. I found 17 litres at 0% ABV in the kettle out of 25 litres at 32% which I initially put into it. I am astonished at the separation which can be obtained, if one is willing to waste a lot of energy and water. I think I obtained around 4,5 litres, and I evaporated in the kitchen 3,5 litres of alcohol.

[StillerBoy]

I found 17 litres at 0% ABV in the kettle out of 25 litres at 32% which I initially put into it. I am astonished at the separation which can be obtained, if one is willing to waste a lot of energy and water. I think I obtained around 4,5 litres, and I evaporated in the kitchen 3,5 litres of alcohol.

I have to question the lost of alcohol or wasted energy on 3.5L and only collecting 4.5L..

I'm of the view that there was not a lost of 3.5L, and even if it was so, there's no way that it was lost by vapor leaks because you would had some serious leaks and you would be able to smell the alcohol..

I'm of the view that you did not have a boiler load of 32% but more in line to 20%.. In theory, 25L at 32% would has 8L of alcohol at 100%.. and 25L at 20 - 21% would has 5L of alcohol at 100%.. and extraction is never 100% but much lower..

The boiler load must not have been tested correctly, and possibly tested at the wrong temp. as there no way of wasting / loosing that much and not having the whole area smelling alcohol and not being aware of it.. and in all your post, never once was it mention of the still smelling up the place..

What temperature was the boiler load at went tested for alcohol content.. also "you think I obtained" what doe that mean..

Mars

[bluedog]

The one temperature reading I do use in how I control the still is the temperature of the liquid boiling in the still. It tells you if there is any alchohol left in it when it reaches the boiling temperature of water. If I had one inside my deph I'd probably use it too, but I don't really need it. Taking 2-3 hours to reach equilibrium also seems excessive. You're gonna get tired of this hobby with painfully slow runs till 4am. In my opinion that time would be better spent running your still, and getting practice in how it runs, making cuts, ect.. Try creeping up on the azetrope later once you have the basics down. Good thing about running nuetral is, once you have ot down, it runs slow, but basically drives itself. Stillerboy has given you plenty to play with. If you have no interest in drinking anything other than nuetral, just keep dumping your "practice" back into the pot until you have it.

[shadylane]

I do presume that if one controls the dephlegmator in keeping a constant temperature one can "squeeze" or "sift" the heart while having the tail components reflow

Here's a suggestion on learning how to run a CM column.
It uses alcohol output flow rate.

With the dephleg cooling water off.
Power the boiler the same as for a potstill stripping run. And don't re-adjust it.
Once it's been distilling for a little while. Measure and record the alcohol flow rate.
This info is needed for a baseline to figure out what the reflux ratio might be on future runs.

Slowly turn the dephleg cooling water on
Until finding the cooling water flow rate needed to put the column in 99% reflux.
Mark and record the valve setting for future reference.

Note
I'm assuming the cooling water temp supplied to the dephleg is constant.

If your interested, I have some more suggestions

[Birrofilo]

I'm of the view that you did not have a boiler load of 32% but more in line to 20%.. In theory, 25L at 32% would has 8L of alcohol at 100%.. and 25L at 20 - 21% would has 5L of alcohol at 100%..

[...]

What temperature was the boiler load at went tested for alcohol content.. also "you think I obtained" what doe that mean..

I am pretty sure because I did test the alcohol content of the 5 L jars after each stripping run by immersing the alcoholmeter in the jar, after all the collection, at ambient temperature. I think I really evaporated all that goodness.

I don't know what volume I obtained exactly because I collected the product in many jars but I did not fill each of them with the exact same quantity. Today I filled a precision cylinder in order to make alcohol content measures, and I see that I filled each jar for 120 ml more or less. There is also 1 jar of more than 200ml and one jar of around 500ml.

So I should have obtained around 120 x 36 + 100 + 400 = 4820 ml, this is a better extimate. Around 3,2 ml should have gone in the air. Let's remember that I did three stripping runs (one completely flooded, but the other two for many hours) and I smelled a lot of stuff for many hours.

[Birrofilo]

@bluedog

My interest in temperature stems from the fact that I like seeing "where I am" and somehow understanding the process better, and foreseeing what is to come during the distillation.

My problem is that being this the first reflux run, I don't know really where to place my markers, how precise are the instruments, and how reliable or telling is their placement. Basically I have to make some runs in order to "know my still".

I think the thermometer in the kettle is quite good. At the end of the run it indicated 99,5°C and I was collecting pure water. I live at 40m above sea level. Water should boil at 99,9 or 99,8 °C so the thermometer is quite spot on. Actually maybe the indicator was a little more toward 100 than 99. Also, at the end of the collection the well was only half submerged.

The thermometer at the elbow, just above the dephlegmator, has two problems: the well is thick, and the entrance was too narrow. I had to drill it to have the sensor enter it, but I did not drill it deep enough I think. Also, I was not using any thermal paste, and the sensor was a bit lose inside the well.

Seeing my notes, I see that the meaningful extraction went from 72,3 at the very beginning of the foreshot and stayed most of the time fixed at 78,1 °C or so, with a very small climb at the end of what I later discovered was the production period to 79,3 or so (the values begun going up and down). Then production stopped, I had to close the water to the dephlegmator until "production" resumed at 90°C at the elbow and even above that. I realized later than all this production was water and fusel oils. Seen in transparence, there was some slight hint of "milk" floating in the water. The alcohol comes when the heat at the elbow is around 78 not when it is 90°!

I see from a calculator that the theoretical vapour temperature during reflux is exactly that, 78,2 °C which is very good news because I now think that my thermometers are quite accurate and that the process was not so faulted.

In another thread I posted the ABV sequence in the jars.

https://homedistiller.org/forum/viewtop ... 5#p7641635

I was getting high ABV very near azeotropic mixture for most of the run. I am pleasantly reassured. I was misguided by my expectation to collect more than 7 litres, I did not understand why production ended so fast. I was also misguided by my expectation that a high-purity ABV would be without "bite". I have to understand that better. I still haven't made the "tasting" of the jars, I only measured the alcohol content.

[Birrofilo]

I do presume that if one controls the dephlegmator in keeping a constant temperature one can "squeeze" or "sift" the heart while having the tail components reflow

Here's a suggestion on learning how to run a CM column.

[...]

If your interested, I have some more suggestions

Yes I read that procedure in Nixon (or a very similar one) but I thought I would have applied it later on, with more experience on my shoulders.
I suppose I should test the "dephlegmator full open" at the same wattage that I will use during production. Initially I wouldn't know at which power the production will occur so I wouldn't know how to perform this measure.

I also don't know if I can use the foreshots to do this kind of test. I suppose I can.

I see that I can produce, slowly but nicely, at 1200W or something like that. As a side note, I have a 2" column, I don't think packing influences the power-production ratio, anyway it was packed with some 70-80 cm of small SPP and a couple copper scrubbers at the bottom. Next time I will perform this test.

Yes I am interested in any suggestion, absolutely!

And I am also grateful to everybody for the great help!

[Jeroendv]

Sorry to hijack this topic, but i have the same problem with the flooding and i have pretty much the same setup, it runs smooth when stripping but when i want to do a reflux run i get massive flooding. Even when i use only 1200W.

Went from the T500 to a bigger still:
I have a 1 meter 2 inch column packed with the same spp as inside the T500 (500grams) and some copper wool, a 20cm sight glass, a dephlegmator and a 3500Watt element for a 38 Litre kettle.
Is it good to fill the column just under the sight glass with spp or is that too much?
I also used a 30 mesh filter to hold the spp in place like picture below, i will use a scrubber instead next time to see if it helped.

[kimbodious]

Sorry to hijack this topic, but i have the same problem with the flooding and i have pretty much the same setup, it runs smooth when stripping but when i want to do a reflux run i get massive flooding. Even when i use only 1200W.

Is it good to fill the column just under the sight glass with spp or is that too much?

My CCVM also has a 2” column but mine is 1.2 metres long and is packed with SS scrubbers. I can operate at 1550W without flooding. Based on that I’d say that the filter disk and possibly the copper wool is restricting the return of the condensate to the boiler.

It is good to have your sightglass below the offtake free of packing. This gives you space to manage flooding or even to maintain a constant level of flooding without the risk of condensate exiting via the offtake.

[Jeroendv]

Woohoo, I cut the mesh filter into a little cross and now I am running the still with 3000 watts and no sign of flooding, nothing to see in the sight glass but reflux!

I am glad I found these answers in the post.

[Rrmuf]

Woohoo, I cut the mesh filter into a little cross and now I am running the still with 3000 watts and no sign of flooding, nothing to see in the sight glass but reflux!

I am glad I found these answers in the post.

That is exactly my experience from above. Removed the disk and all is good.