Glass Marbles for Reflux Column Structured Packing

[Spriit Tisler]

Stripped low wines diluted to approx 20-30%. Packing height 900mm, diameter 50mm. Was going to increase packing height to 1.4m soon as I get the column welded.

[Klein]

I have now build a 4" x 61" (room for 60" of packing) column
it holds 40 pounds (18.18kg) of 14mm marbles and has a total weight of 55 pounds (25kg).
i made a copper plate for a piece of type L pipe that sits on top of the ferrule, trimmed two sides so it can be removed if i ever want to take it out. I got the idea from Bobbywolf

[Klein]

Well I’m getting prepared to do an experiment with marbles.
I will be testing the effects of: different size marbles, at different to power inputs, to column sizes.
I currently have 14mm marbles from hobby lobby and am looking for places online to buy other sizes (online would be the best as long as they ship to the United States or Canada)
I can’t seem to find anything other than ~14mm at any store I have gone to.
Any links to online stores would be great
thanks

[Klein]

well i have not even had a chance to think about doing test with marbles. i am now home for a day after being gone for 8 days and have a shit ton of birdwatchers to run (150l of wash to strip ~3 stripping runs as well as 70l of low wines). started well, cold column at the start ups the abv to 90% and then quickly drops to normal.

started my spirit run ~52l 40%abv i have my 2" ccvm head on my 4" column, turns out it cant put in into full reflux at full power
after a few failed attempts on fixing it i took a copper disk with random holes in it,that was in my scrap box and used it to block part of my take off in the tee.
i then used my notes from when i ran the 2" to scale my take off rate to the higher power input. this should give me a fairly similar reflux ratio.
my 2" would give me 96.5abv my 4" with the same marbles and 12" longer column gave me 94-95%abv

i think this is because the reaction between the vapour and reflux is not as violent do to the fact i have not scaled my power input to my increased column size.

[Uncle Jesse]

I've always used marbles for packing. Perfectly happy with them.

I have one 6 gallon still which I packed with copper mesh. It actually puts out too high a proof for my taste, since I like to make whiskies.

[casper the Irish]

I've always used marbles for packing. Perfectly happy with them.

I have one 6 gallon still which I packed with copper mesh. It actually puts out too high a proof for my taste, since I like to make whiskies.

Same here,
I ran with 4 sizes of marbles
I ran with scrubbies, with copper mesh and with SS mesh

in a 3" x36" ccvm column
Marbles drop my ABV% by about 7% and will not tweak with adjustments to power nor TO ratios. Sits there at 85% from start to finish.
My marbles are 14mm. Thats optimum. Smaller marbles ABV drops and just floods so power reduced. Larger diameter, ABV drops and the RC needs turned up, and power reduced.

Scrubbies do work better if more tightly packed, or rolled mesh is best if I want to get above 92%

I know Odin claims a great whiskey at 96% but as UJ says anything that pure does indeed taste different, good for vodka and gin but distinctly lighter, too thin for my whiskey or rum.

In fact since I strip run all my beers I get a better whiskey by potstilling the low wines back with each stripping run and keeping the tight hearts. I am increasingly using reflux to blend with the potstill spirits. Mature each of the hearts separately before blending.

[Rod]

I've always used marbles for packing. Perfectly happy with them.

I have one 6 gallon still which I packed with copper mesh. It actually puts out too high a proof for my taste, since I like to make whiskies.

Same here,
I ran with 4 sizes of marbles
I ran with scrubbies, with copper mesh and with SS mesh

in a 3" x36" ccvm column
Marbles drop my ABV% by about 7% and will not tweak with adjustments to power nor TO ratios. Sits there at 85% from start to finish.
My marbles are 14mm. Thats optimum. Smaller marbles ABV drops and just floods so power reduced. Larger diameter, ABV drops and the RC needs turned up, and power reduced.

Scrubbies do work better if more tightly packed, or rolled mesh is best if I want to get above 92%

I know Odin claims a great whiskey at 96% but as UJ says anything that pure does indeed taste different, good for vodka and gin but distinctly lighter, too thin for my whiskey or rum.

In fact since I strip run all my beers I get a better whiskey by potstilling the low wines back with each stripping run and keeping the tight hearts. I am increasingly using reflux to blend with the potstill spirits. Mature each of the hearts separately before blending.

I make a drop of brandy made from red wine and I am happy with what I get

with the marbles my purity is down a little , but when I dilute to 40% which is what I want for my brandy I am not sure if my yield of 40% is that much different

I normally add some caramel to colour , a handful of raisins and some wood chips and let it sit for about 6 months ,

by that time I do not know how much I have got , I find with the marbles my spirit is cleaner

I suppose my question is although you are down 7% on what the amount of distillate you get are you that much down on what you drink

[casper the Irish]

I am down 7% Alcohol By Volume, not a lower yield by volume. I should have written 7%ABV

[Rod]

I am down 7% Alcohol By Volume, not a lower yield by volume. I should have written 7%ABV

I understood that you spirit was down in strenght

my question was are you down in final volume after cutting to 40 %

that is , say , you were getting 10 litres @ 80 %

are you now getting 10 litres @ 73 %

or approx 11 litres @ 73% which will give you the same volume @ 40 % , cut

[Cletus_Spuckler]

Hi guys,

Just thought Id check in here before I order packing for my soon to be completed 4"x60" LM column build.

As with most people on this thread topic, I will be aiming to pull neutral spirit as fast as possible whilst maintaining azeo (or near to it). Do we still reckon marbles are better than copper packing for this purpose? If so, is 14mm still the recommended size for a 4" column?

I have now build a 4" x 61" (room for 60" of packing) column
it holds 40 pounds (18.18kg) of 14mm marbles and has a total weight of 55 pounds (25kg).

Thanks for posting that info Klein. Very useful.

CS

[still_stirrin]

...Do we still reckon marbles are better than copper packing for this purpose? If so, is 14mm still the recommended size for a 4" column?

You’ll spend a lot more for copper mesh/scrubbies to fill your 4” x 60” column, that’s for sure.

And, marbles can be easily cleaned by rinsing in a bucket of water, whereas cleaning copper mesh will be a little more tedious.

I don’t foresee you having any difficulty attaining azeotropic purity with either form of packing...but the marbles will be more “user friendly”.

If your rig was stainless (which I know it’s not), then the copper packing would help scrub sulfur from the vapors. But, your copper tower will do that just fine and you certainly could use the glass packing.

But...YMMV.
ss

[Klein]

The marbles are very easy to clean, the column is awkward to put on/off the boiler. So I kept it on the boiler all summer, I just ran water down the column after each run to clean it out. I kept the still covered with two sheets sewn end to end. That way it would still be able to breath as I did not want to seal the column. When I emptied the column at the end of the summer everything was perfectly clean.

[Cletus_Spuckler]

Thanks again for another good tip Klein.

You’ll spend a lot more for copper mesh/scrubbies to fill your 4” x 60” column, that’s for sure.

That was my second reason for exploring marbles. In saying that, I just received my first quote for 14mm marbles from an Alibaba supplier; $7 (USD) per kilo. Thats $133!
Cheaper than copper mesh (from what Ive seen), but still not what you'd call cheap!
The borosilicate quote from the same supplier was $300 (USD).

Ive been particular to clarify that there is to be no lead is in the glass. The above quote was for soda-lime glass, which I think is ok. I believe lead is only used for crystal.

From my build post:

For you, I believe the 12mm marbles would be better for 2 reasons....1) price, they’re cheaper per pound and you’ll need a bunch. The 2nd reason, 2) the open area between marbles is less, thereby increasing the surface area to open area ratio throughout your larger column. This will increase heat transfer from the vapors to the condensate, improving efficiency. More (smaller) marbles is more efficient than fewer (larger) marbles.

I need to get some quotes for the 12mm also.

Does anyone know a good online supplier?

CS

[still_stirrin]

I need to get some quotes for the 12mm also. Does anyone know a good online supplier?
CS

These are what I use: https://www.hobbylobby.com/Floral-Weddi ... 4mm/p/3504" onclick="window.open(this.href);return false;" rel="nofollow

Cheap enough to throw in the trash when they fracture...which I’ve had happen to a few. Otherwise, you can “pour” them into the column easy enough. And just tip the column into a bucket of warm water to empty them out. My column is 2” x 39” and holds a little less than 6 lb. worth. No flooding and capable of pushing out 96%ABV.
ss

[Cletus_Spuckler]

I need to get some quotes for the 12mm also. Does anyone know a good online supplier?
CS

These are what I use: https://www.hobbylobby.com/Floral-Weddi ... 4mm/p/3504" onclick="window.open(this.href);return false;" rel="nofollow
ss

Thanks SS (again!), I had checked out those guys, as they have been mentioned a few times. Sadly, they dont ship to AU, so Im going to keep looking. Shame as they are really cheap!

CS

[Bagasso]

Sadly, they dont ship to AU, so Im going to keep looking. Shame as they are really cheap!

How about here: Koch & Co

[StillerBoy]

From my build post:
still_stirrin wrote:
For you, I believe the 12mm marbles would be better for 2 reasons....

These are what I use: https://www.hobbylobby.com/Floral-Weddi" onclick="window.open(this.href);return false;" rel="nofollow ... 4mm/p/3504

SS.. You stated that 12mm size marbles would be best for a 2" column.. then you posted where you have bought yours from.. but those are 14mm size..

So the question is what size are you using, 12 or 14mm.. because the site does not have 12mm for sale..

Mars

[Rod]

I got mine from

https://www.koch.com.au/location-trading-hours" onclick="window.open(this.href);return false;" rel="nofollow

13 mm

what's a mm between friends

Rod

[Cletus_Spuckler]

Rod, that's the best price I have come across for AU so far. $115 delivered for 18kg. So thanks! I'm still hoping I can get them cheaper. Know anyone around these parts that makes SPP?

[casper the Irish]

Hi guys,

Just thought Id check in here before I order packing for my soon to be completed 4"x60" LM column build.

As with most people on this thread topic, I will be aiming to pull neutral spirit as fast as possible whilst maintaining azeo (or near to it). Do we still reckon marbles are better than copper packing for this purpose? If so, is 14mm still the recommended size for a 4" column?

I have now build a 4" x 61"

With my limited experience (3xreflux builds so far) I would say READ again what UncleJesse wrote above. He uses marbles to avoid azeo. He wants it a bit dirty, like the bourbon and brandy legal requirement to keep below 80%ABV. Now thats a whole other discussion. 80%ABV leaves 20% beer flavours. Even a good 96% leaves 4% flavoured beer water. The argument for me is if you want that much flavour, say my 87% which is what I get with a 36"marble filled column, then the base just has to be a well made clean and dandy mash.

For a fixed column dia and height, Marbles are not as efficient as mesh. Which is not as efficient as SPP

To get azeo you are therefore better using SPP, SSmesh or SS scrubbies well packed. Do not use copper mesh or scrubbies except for perhaps at the bottom of your column. About 6' is enough to de-sulphur your vapours. But copper mesh rots to powder needing acid washed and frequent replacement. And it raises the danger of a big build up of Ethyl Carbamate in your still if not your distillate. Thats a white salt encrustation, not good for you if it gets in your spirits. Definitely avoid copper on the cooling side (no copper condensers nor parrot).

As above I have tried all sizes of marbles. 14mm are working best on my 3" dia column. Any smaller, you want to be using a smaller dia. So for your 4" you want bigger, not smaller marbles.

Its OK using marbles if you want less than Azeo. If you want to use them just because its cheap, then you are obliged to build a higher column. To get 96%ABV its the height of the column that changes to suit your chosen packing. Marbles, go 60". Tight mesh or scrubbies, 40". SPP you can work at 30"

[zapata]

If azeo is the goal, and cheap packing is a requirement, why in the world not use lava rock?

I haven't actually tested the HETP because that would require me to not make azeo. But I recently replaced most of my copper mesh with lava and saw zero drawbacks.

No trying to poop on marbles in the marble thread, but Casper has a point, even people who like marbles do not find them as effective as other packings.

[Cletus_Spuckler]

I'm glad I checked in here as I was going to order marble packing within the next day or two.

...READ again what UncleJesse wrote above. He uses marbles to avoid azeo...
For a fixed column dia and height, Marbles are not as efficient as mesh. Which is not as efficient as SPP.
To get azeo you are therefore better using SPP, SSmesh or SS scrubbies well packed.

Thank you Casper, Ive read through this topic a few times, but must have skimmed through yours and UJ's posts which stated that.

Do not use copper mesh or scrubbies except for perhaps at the bottom of your column... But copper mesh rots to powder needing acid washed and frequent replacement. And it raises the danger of a big build up of Ethyl Carbamate in your still if not your distillate. Thats a white salt encrustation, not good for you if it gets in your spirits. Definitely avoid copper on the cooling side (no copper condensers nor parrot).

I have had problems with copper mesh in the past (I first used to soak it in back set to 'clean' it; then wondered why it corroded away). I haven't had the white salt encrustation issue yet; but have had issues getting my previous still where I could not get rid of a red oxide layer which could rub off onto a cloth. Im hoping I dont have the same issue with me new still (thats for another thread ). DAD300's thread on why not to use copper was an eye opener; although this community seems to be split on the issue (again, not for this thread!). Partially too late for me anyway, as I have a copper LM head and condenser.

If azeo is the goal, and cheap packing is a requirement, why in the world not use lava rock? ...even people who like marbles do not find them as effective as other packings.

Thanks also Zapata; I cant get comfortable with the idea of porous rock; as Ive read some people get a dirt flavour and surely it is hard to clean? Its just a personal issue I have. Thanks for your input regarding other packing choices; I read a lot of contradictory information on here so it can be really hard to know what info is considered current gospel.

Thank you again; based on your guys advice, it seems marbles are not the correct choice for me. Im going to go with 6" of copper mesh at the bottom and fill the rest with SS scrubbies.

CS

[Spriit Tisler]

I ended up using raschig rings that I was about to utilize in the first place many years ago and I find they perform better than SS wool packing, which was good on it's own. The still has no problem reaching azeotrope in no time and the collection rate is a bit higher than with SS wool. And I managed to clog the wool packing (it starts making whump-whump - sound) even with medium power, but I can hit everything I've got to the raschigs and they never do that.

[Tomb]

In the “all or nothing category”....

I have used “lava” rock and found it “holds” a lot and is a pain to clean. Have switched to marbles and it seems more stable but nit as efficient.

What about a bit of both? Half marbles and half lava.

I am not sure which would be best on the top? (Possibly marbles in the bottom half to deal with all the gunk? And then again maybe marbles up on top to clean up better?)

Am it too full of the bad stuff?

T

[bcgold]

So, how do you hold the marbles in your column? I'm curious.

I used broken glass from canning jars on my first boiler with excellent results and will use glass again in this new boiler column.

Just avoid using colored glass, clear glass with a hint of green showing from the broken edges is from iron in the glass not likely it will leach out.

[Stonecutter]

Resurrecting this beast. 16 pages and not one person tried to use etched marbles up against polished I’m going to use 1/2” marbles to fill my 2” column etched versus polished.
I use a SS column so I will have some copper packing at the bottom. I’m currently waiting for my etching liquid to arrive so as soon as that comes in I’ll make four runs of the same neutral. I’ll use the same amount of marbles (measured by number and/or weight). Four runs, one run of polished, one of etched and then all over again to give a decent evaluation. This is obviously going to take some time but I’m very interested to truly put some real numbers to the polished vs etched question. Any input or suggestions would be greatly appreciated.

-Edit- I will not be measuring takeoff rate as I don’t have a needle valve. But I will try to upload videos of the reflux within the marbles in order to show the action between the two mediums.

[shadylane]

Go for it

[The Baker]

Never heard of etched marbles.
Be interesting to hear how it went.

Geoff

[Saltbush Bill]

I will not be measuring takeoff rate as I don’t have a needle valve.

Maybe Ive missed something here , what still type ? besides packed column ? Boka ? VM ? CCVM ? CM?

[Stonecutter]

CM. My reflux jacket sits on top of my column just below the condenser. The “takeoff port” is nothing more than my Liebig. As there isn’t a needle valve to set my takeoff I can really only measure an average of what I collect in my jars. I’ve never run a boka but from what I’ve read it seems to be easier to set takeoff rate with them. Am I totally off base? I’m new here and I’m sure my ignorance is showing.