Glass Marbles for Reflux Column Structured Packing

Distillation methods and improvements.

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Re: Glass Marbles for Reflux Column Structured Packing

Postby Spriit Tisler » Sat Apr 01, 2017 3:58 am

I don't know about theory but since smooth glass marbles have the smallest possible surface area the effectiveness on distillation must have something to do with thermal buffering which would keep the equilibrium better. If we would go the surface area path scrubbers should do much better job but this appears to be not the case.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby spiff » Sat Apr 01, 2017 6:19 am

I just bought a shit load of marbles to try this too. It'll be curious to see if it'll make enough difference to warrant the extra hassle of dealing with the 50lbs of marbles that it takes to fill my column. 6 plates VS 1800 marbles...

Anybody come up with any cool ideas for this or is everyone just scooping them out a handful at a time? Maybe a SS mesh bag to hold the marbles so you're dealing with bags instead of individual marbles?

I could just remove the whole column, which would be about 70lbs and just let the marbles fall out, but I'm guessing that's a good way to get broken glass all over the place.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby casper the Irish » Sat Apr 01, 2017 11:30 am

thecroweater wrote:Enough with the story's of how much better the still runs flooded and puking, some of us are having a hard enough time just trying to swallow that marbles are equal to packing with hundreds of times the surface area, sheez :roll: .


I agree with your logic, but...
The parent site article on running a reflux still instructs to dial back to 80% off puking.
I have seen some Russian glass columns on video with ethanol bubbling thru liquid.
And, I thought, but must be wrong, Odin stated that his new helical coils run at their most efficient when saturated, allowing him to cut the packing to under 30"

So wrong wrong wrong? Thanks fellas, that's a problem solved for me.

The question on the size of our balls could do with more attention. Whether etched or simply smaller, the increased surface area has to be better.... unless small balls make the column less porous. There must be a mathematical curve for optimum size v column diameter.

Conductivity for efficient heat transfer: surely glass as a good insulator cannot facilitate gas:liquid equilibrium. The state changes that are necessary for fractionating or separating the constituents on glass spheres can therefore only happen on the surface area. Where is the heat transfer happening? NOT to and from the glass marble. Glass will at the start be cold but eventually will stay hot. Thermally inactive. Apart from surface area, the mass itself just sits there, effectively narrowing the column. So the only two active sites for reflux may be the surfaces and the spaces between.
If there is no flooding at all, then the spaces are inactive, too. If the spaces hold gas but no liquid (no flooding), then nothing is happening in the spaces.
So, thermally inactive glass balls, interstitial spaces filled with hot gas, no liquid. That just leaves capillary wetted surface for our thermal exchange within the surface film. Have I missed something here? We need a lot of heat transfer to make reflux efficient (maximise our HETP) but I don't see how big glass balls can do it on surface film alone and especially when that area is exponentially smaller than mesh.

So how does the rising gas condense, where does its heat sink in or give out? Is it possibly given up to falling condensate?
In other words, rising gas pushes through falling liquid. Is it not possible this heat exchange is happening BOTH on the surfaces and in the small interstitial spaces between, where gas meets liquid in confined cells it can be atomised, vaporised, and condensed.

For hot gas to meet cooled liquid in small spaces, there will have to be a degree of flooding there, balanced by an appropriate volume of rising hot gasses. How else is gas and condensate to exchange heat and states unless they meet and mingle
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Re: Glass Marbles for Reflux Column Structured Packing

Postby joeymac » Sat Apr 01, 2017 2:44 pm

This thread is really not about why marbles are so great. But rather can we figure why they are so much better than traditional fractionating column models and theory would predict. Very poor volume to surface area ratio and poor thermal conductivity yet they appear to have great production rates and power handling at 95-96% purity.

I think primarily it has more to do with the volume the glass marbles take up rather than their surface area interactions.

And secondarily, to a lesser degree of importance, I also think that glass being fairly heavy but with low thermal conductivity helps them regulate the packing temperature gradient very well. In contrast, copper scrubbers have a ton of surface area, extremely high thermal conductivity and not very much mass/thickness to those little strands ensuring that scrubbers absorb heat quickly and retain any heat very poorly... I would think all that means a copper scrubber column is more prone to temperature fluctuations.

As for my volume hypothesis, I physically measured that 5/8" (~15mm) marbles occupy 58% of a 3" column's volume. This means that only 42% of the area is available for open vapor flow upwards and it's also highly turbulent due to the way marbles stack onto each other - each layer blocking the gaps open in the layer just below. So this means when your 3" column has 4000-5000w of vapor rushing through it, that the vapor speed through the marbles must be closer to the speeds seen in an open 0.97" column. That has got to be some significant vapor speed considering the power we are putting into 3" columns!! And you've got reflux is falling down onto the marbles and consuming space too. I'm convinced that the excessive vapor speed is enough to suspend and entrain liquid distillate in the column.

This is not the same mode of interaction as traditional column packing theory would predict... where reflux whets the surface of a packing and vapors passing by at reasonable speeds cause further distillations at the surface boundary. In cases of packing that supports fluidized beds, I think we have highly turbulent fast vapor literally having to slosh through raining liquid and in some areas, bubble it's way into pools of suspended fluid zones for reboiling. Several youtube videos of both marbles and SPP in clear columns would appear to show this. That's basically how a plated column works by creating flat layer of liquid distillate where gas is bubble into and reboil, right? Well in a similar fashion to plates, marbles and SSP and scoria might be doing this except with alot more fluid volume distributed all over the column instead of just on a small handful of structured perforated plates.

So, yes... marbles should be poor performers using the traditional theory of whetted surface area supporting gas-liquid interactions. Maybe we need to accept that a different mechanism is at play here. I know personally that the same wash recipe in my marble column produces azeotrope output at nearly twice the rate that my copper scrubbers do and the copper scrubbers can't take the power that marbles do.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby RedwoodHillBilly » Sat Apr 01, 2017 3:25 pm

joeymac wrote: That's basically how a plated column works by creating flat layer of liquid distillate where gas is bubble into and reboil, right? Well in a similar fashion to plates, marbles and SSP and scoria might be doing this except with alot more fluid volume distributed all over the column instead of just on a small handful of structured perforated plates.


When I did a thought experiment about marbles a while ago, that's the conclusion that I came to also. Another analogy that I had was a long string of parallel/series thumpers.The interstitials being individual thumpers. But, logic can be a good way to come to the wrong conclusion with confidence :?

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Re: Glass Marbles for Reflux Column Structured Packing

Postby Badmotivator » Sat Apr 01, 2017 11:29 pm

Another kinetics hypothesis: the refluxing liquid flows over the surface of the marbles and not straight down. It dwells, not like a puddle on a plate, but spread out thinly on round surfaces. Its average vector is considerably sideways. Its path downward is a lot longer than the column, and at every part of that path down it is re-boiling.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby casper the Irish » Sun Apr 02, 2017 1:50 am

RedwoodHillBilly wrote:
joeymac wrote:a liquid distillate where gas is bubbled into liquid and reboiled ...marbles and SSP and scoria might be doing this except with alot more fluid volume distributed all over the column
That sounds like a flooded column to me. And yes, it may indeed be working by direct heat exchange gas to liquid within the distillate in spite of our accepted wisdom on flooded columns. [/color][/size]


When I did a thought experiment about marbles a while ago, that's the conclusion that I came to also. Another analogy that I had was a long string of parallel/series thumpers.The interstitials being individual thumpers. But, logic can be a good way to come to the wrong conclusion with confidence :?


I love that, "When I did a thought experiment".... Be careful now, only on Sundays. And I think you are on to something there. Hundreds of small chambers where hot gas meets cooler liquid.

Badmotivator makes the great observation of extended pathways. That's a very credible explanation for multiple HETP

Joneymac you need to do one of those thought experiments on what effect inert mass is having on volume. Fill a 3" tube with solid objects and you restrict flow. Equivalent to an inch or less? But.... Venturi effect will accelerate gas flow, liquid will percolate slower
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Re: Glass Marbles for Reflux Column Structured Packing

Postby joeymac » Sun Apr 02, 2017 4:22 am

casper the Irish wrote:
RedwoodHillBilly wrote:
joeymac wrote:...

Joneymac you need to do one of those thought experiments on what effect inert mass is having on volume. Fill a 3" tube with solid objects and you restrict flow. Equivalent to an inch or less? But.... Venturi effect will accelerate gas flow, liquid will percolate slower


I'm not sure what you are meaning by "inert mass". I had taken a section of 3" column and filled it 5/8" (~15mm) marbles. I then filled the section full of water and measured the amount of water. The water needed to fill the marble column was 42% of water needed to fill the empty column.

The venturi effect only describes any potential pressure drop due to the increase in velocity caused by a constriction. It's not the venturi effect itself that causes the velocity increase but the requirement to maintain a constant mass flow rate. You've got the same amount of crap to shove through a smaller tube in the same amount of time and if the velocity didn't raise to maintain the necessary mass flow rate, the boiler pressure would continue to rise (which would be bad). Furthermore, quantifying the venturi effect (if any) in a situation like this is specious to begin with because we have phase changes happening everywhere... our gas compressibility factor is quite literally as far from ideal as one could imagine. Going to need more than a thought experiment.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby casper the Irish » Tue Apr 04, 2017 11:45 am

Glass can have little thermal exchange happening here, in that sense it's sheer mass is taking no part except to restrict flow, narrow the effective diameter by at least 58% on your ready reckoning. Gas flow and heat input are therefore less than it could be in an open 3" column.

However, the marbles do have other effects which as we can observe are remarkably positive and begs for some explanation. Three ideas raised on this thread so far will bear further thought.

Surface area. This is exponentially smaller than mesh, so it shouldn't work as well as it seems to.

Interstitial Spaces. Hundreds of small interstitial thumpers. That's gas bubbling through liquid. This would need a flooded column to work, which the experts have agreed will not add HETP. But maybe.... needs some thought.

Pathways. A greatly lengthened pathway as gas is accelerated around the smoothe spheres like an aero foil wing. Also, this acceleration meeting condensed liquids might be atomising it, sucking fine droplets out of the spaces and surfaces back up as they exchange heat, the Venturi effect.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby Bagasso » Wed Apr 05, 2017 9:29 am

casper the Irish wrote:Glass can have little thermal exchange happening here

Maybe that is what helps. Instead of a third element taking part in the interaction it is mainly the liquid and vapor doing their thing.

I think that adhesion has something to do with it. I remember a post where someone (googe) running lava rock said the rocks in the bottom of their column had crud sticking to it after a rum run.

Obviously there is more to it than just surface area. Just because we can't say what it is doesn't negate the results people are getting.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby joeymac » Wed Apr 05, 2017 9:45 am

Personally, I don't really care why it works, if my column is less than 10w from flooding out the top, or if someone's theory/model says my packing is "inefficient"... if I can run a ton of power pulling high takeoff rates at 95%+ with clean flavor and use a packing as cheap and common as marbles then that's all that matters.

I'm curious and plan on trying SPP some day... but a 3"x40" column is going to cost a lot to fill and I not displeased with marbles at the moment.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby casper the Irish » Fri Apr 07, 2017 2:51 pm

joeymac wrote:Personally, I don't really care why it works ....if my column is flooding ...I'm curious and plan on trying SPP some day... but a 3"x40" column is going to cost a lot to fill and I not displeased with marbles at the moment.


SPP or Odins improved helical packing? Small medium or large? Fine if you buy from Odin, he will know. As for me I cannot pay hundreds of dollars for it but maybe, if I understood better how marbles work them I will buy marbles. Should I buy polished or frosted? White or coloured?
For a 3" column do I order 6mm or 14mm? If I can answer this because I know the difference, then my column can be a lot shorter. The right packing will allow my column to be no higher than 30", deliver purity at twice the rate and use half the energy.
I reckon on a column vol of 3l which is 12,000 6mm marbles costing $70.
With that knowledge, it may even be possible to walk a local beach to pick up pebbles of the right size for free
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Re: Glass Marbles for Reflux Column Structured Packing

Postby T-Pee » Sat Apr 08, 2017 4:38 am

casper the Irish wrote:With that knowledge, it may even be possible to walk a local beach to pick up pebbles of the right size for free.

Spoken like a true Scotsman...oops. :oops:

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Re: Glass Marbles for Reflux Column Structured Packing

Postby casper the Irish » Sat Apr 08, 2017 9:32 am

Scots-Irish. The best of both and the worse of either.
With plenty of Dutch blood.

Odin says he used basalt beach stones to great effect before he experimented with SPP then started making improved helicals.
Both basalt and SS metal differ from glass in that they absorb and emit heat quickly.

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Re: Glass Marbles for Reflux Column Structured Packing

Postby joeymac » Sat Apr 08, 2017 10:00 am

casper the Irish wrote:
joeymac wrote:Personally, I don't really care why it works ....if my column is flooding ...I'm curious and plan on trying SPP some day... but a 3"x40" column is going to cost a lot to fill and I not displeased with marbles at the moment.


SPP or Odins improved helical packing? Small medium or large? Fine if you buy from Odin, he will know. As for me I cannot pay hundreds of dollars for it but maybe, if I understood better how marbles work them I will buy marbles. Should I buy polished or frosted? White or coloured?
For a 3" column do I order 6mm or 14mm? If I can answer this because I know the difference, then my column can be a lot shorter. The right packing will allow my column to be no higher than 30", deliver purity at twice the rate and use half the energy.
I reckon on a column vol of 3l which is 12,000 6mm marbles costing $70.
With that knowledge, it may even be possible to walk a local beach to pick up pebbles of the right size for free


Stick with 1/2"-5/8" (12mm-16mm) and clear smooth... not the colored or rainbow iridescent. They should be about $1.50/LB and 6 bags or so should fill a 3" column. I just rinse mine off in foreshots, boiled them in water briefly, and they were ready to go. You can probably get away with a 30" column but closer to 36"-42" would be a bit better for optimum takeoff rate. As for the power though, a fast takeoff rate and the need to maintain a high reflux rate actually means you need MORE power with marbles. SPP and marbles seem to LOVE power and become better and better right up until the column floods out and makes a mess.

I just did a column run last night with 3"x40" uninsulated stainless column. I have a sight glass over the packing and while heating at full power, 5500w created a violent splashing pool of distillate 3" and rising over the packing. :shock: I dialed it back to 5000w and the pool of distillate became less crazy, but it was still slowly rising. Maybe it was imagination, but I was getting nervous anyways... so I turned it down again to 4400 watts and the standing pool on top of the marbles disappeared below the surface. Not quite ideal, but I figured I'd better get on with it since it was getting late anyways. So I held 4400W for 30 more minutes to equalize but I think something like 4700 might have been better, if I had more patience to babysit flooding in the sightglass.

I tried to maintain a takeoff rate of 1.1 mL/sec (4L/hr) and the column held 78.4/78.5 degrees C easily for about 20 of the 24 jars I pulled off. I didn't really play with the takeoff rate and reflux ratio to see how fast I could have gone before my temperature started climbing... but pushing 4400W into an uninsulated column I reckon I probably had 3000W of condensation at the head giving me in the neighborhood about 3:1 refux ratio. Next time I'll be more diligent in measuring my condenser temps and flowrates. I was tired and just wanted to get on with it.

==> If your interested, 1kW of power condensed produces 1.6mL/second ethanol liquid (example: 5500W acually condensed makes 8.88mL/sec pure ethanol)
==> The power you condense at the head to make reflux is often drastically less than your power into the boiler unless you insulate EVERYTHING ery well. Only way to know is to measure the water flowrate through the condenser and the temperature change. Power condensed by water coils = 4.81 Watts (times) water flowrate in mL/sec (times) ΔC coil inlet-outlet temp change.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby casper the Irish » Wed Apr 19, 2017 5:52 am

OK I've just measured the vol of 1m 3" tube at 3.4litre
I have sourced clear glass Matt or polished balls with a choice of diameter from grains thru 1mm steps to 100mm. In other words they need to know to the nearest millimetre the size I want.
Price posted is 6€ per kg and I will need 5kg or 11lb
Some research papers agree with Odin that the diameter of packing should be optimised between 1/10th and 1/15th of column diameter. It is not clear how size affects velocity stability nor flooding/power
The same research papers say that some flooding is required. Efficiency depends on greater than 20% and less than 80%
They also say that thermal conductivity plays no significant role.

I note comment above on how much easier it may be to flood with less power onto smaller packing. My current gas burner delivers a max 2.8kW so less power required is good

Q1. What dia balls will be optimal? 7mm is 1/10th. 6mm is 1/12th Any smaller will look like they will sift thru mesh, a nightmare to contain!

I picked up some basalt and marble stones from the beach yesterday, have them graded into 6mm and 12mm so will now do a few runs to assess and report back
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Re: Glass Marbles for Reflux Column Structured Packing

Postby joeymac » Thu Apr 20, 2017 9:29 am

Most of us are using 1/2"-5/8" (12-16mm) marbles for column diameters 1-1/2" to 3"

If you're going to use 6-7mm marbles you'll be in uncharted territory, I think. Best to just experiment with some 30% clean low wines and a sight glass over the packing.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby casper the Irish » Fri Apr 21, 2017 6:27 am

And with good reason, I suspect.
I know beach stones are not perfect spheres so the interstitial spaces are not a straight comparison, but here is what I've observed on a few runs so far.
3" SS column, 40" with CCVM Tee. I have a 36" copper pipe normally fitted under to provide column height of 60" and normally packed with 12" copper mesh, the rest SS mesh
I normally get 92% abv at TO
For this experiment I've dispensed with the copper section so my column is 36"

Packing 5mm stones.
Vapour speed- 3kw heat rises slow, takes about 180 seconds to get from bottom up to RC
RC lowered for full reflux but fine stream of 92% TO which I can't stop unless power turned down to minimum. I have no sight glass but suspect column is flooded. Sound is a gentle roar even during stabilisation. Turning up power abv drops to 87%
Decided to stop and change packing. Some glass balls I had placed at the bottom were mixed thru so evidence of flooded fluid bed throughout the column with packing moved around.

Packing 10mm stones
Again from heat entering column base it takes several minutes at full power for heat to reach the RC
95% fores and heads,
dropping to 92% with power and lifting the RC/opening the TO to lyne arm
Drops to 89% with full power (3kw)

This is identical to what I was achieving with my original 60" +mesh configuration except that volume is much better and column is a far handier height. (Doubled to a gallon an hour)
but the purity may not be as good, this is a 12 gal batch of corn low wines but my first 4 quarts are not so clean, has that ash taste of fusels from the start. I normally get sweet spirit by my 3rd quart. Stopped after 5 quarts. I think I'll toss these to the still and run again, next time with 18mm stones. And finally with mesh as a control.

Keep u posted.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby casper the Irish » Mon Apr 24, 2017 12:22 pm

I will tell you what I see and hear, and can measure abv, etc but I do not know the math how to gauge packing efficiency.... even my power input is a gas valve, no # kW markings.

Using the Bigger packing from 1/2" up to 3/4" basalt pebbles, still 36" of packing
Things going much better. At last the rig is responsive and controllable.
1. There is definitely a min and max. By that I mean between 20% and 80% flooding raises ABV. As BP is reached I can hear deep bubbling like progeny or corn mash. Increased power as column starts to flood sound changes to a distant roar, steady. ABV increases to 95% If I max the power (2.8kW) liquid reaches top of packing. Sounds like fried grits. ABV falls
2. Power seems otherwise to make no impact on purity (CCVM).
3. RC position (=TO valve) makes no change to ABV
3. I am getting steady 92% running down to 87% before tails

This result is the same I was getting with tight rolled SS mesh, 60" column. So an improvement.

Tell me, are glass marbles similar for you? 16mm with coloured eyes
Anyone with a CCVM can advise how to improve ABV?

Mind you, I'm running rum, Bourbon and barley whiskey so anything above 80% must be nearly too pure to be good for me!
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Re: Glass Marbles for Reflux Column Structured Packing

Postby spiff » Tue Apr 25, 2017 6:51 am

Just wanted to update my last response to this.. using a plate as a platform for the marbles isn't as great as I thought. First couple times it worked great but then I started having flooding issues. So its apparently hit or miss depending on how the marbles stack on the plate. This was always with the downcomer hole covered with a wire X.

So I'm making a dedicated marble holding plate.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby der wo » Tue Apr 25, 2017 7:12 am

spiff wrote:Just wanted to update my last response to this.. using a plate as a platform for the marbles isn't as great as I thought. First couple times it worked great but then I started having flooding issues. So its apparently hit or miss depending on how the marbles stack on the plate. This was always with the downcomer hole covered with a wire X.

So I'm making a dedicated marble holding plate.

Perhaps you remember, we had this flooding problem with a perforated plate as a packing platform four weeks ago:
viewtopic.php?f=17&t=65942&start=30#p7466130
He used scrubbies, so he probably doesn't need a platform at all. But with heavy marbles of course you need. I would think about sawing long holes in a plate, perhaps 1/3 of marble diameter. Or solder/weld on the bottom of the column a few wires.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby Klein » Thu May 11, 2017 1:41 pm

Klein wrote:It was months ago since I have read this thread so I don't remember if it has already been stated.

Just incase anyone wanted to know how much to get.
The 2lb bag of marbles from hobby lobby will fill 19" of 2" copper pipe. :)

I made a mistake as I just filled my column and 6lb filled 39"

I need another pound to fill it all the way. :/
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Re: Glass Marbles for Reflux Column Structured Packing

Postby maritime » Tue May 16, 2017 4:19 pm

i removed my SS scrubbies today and filled with 1/2" plain glass marbles.
running a Birdwatchers tomorrow.
interested to see if the output speed changes, as some have suggested. i have only run scrubbies in the past.
2" slant plate. 3' of packing, 8" space, then the plates and coil.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby Klein » Mon May 22, 2017 9:07 am

Just a quick question
I'm using marbles in a 2" ccvm for the first time as I'm typing this. How much power are you guys/gals using and what size column? I'll be doing some rereading as soon as I'm done getting this stuff ready and I can sit down lol.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby Spriit Tisler » Mon May 22, 2017 10:33 am

I havent' been able to source suitable sized glass marbles so I'm gonna test out soon the ceramic raschig rings I have had lying around for good time. I unpacked the SS scrubbers and they were in perfect condition, corrosion-free. I suppose rings shouldn't do that bad on side of marbles?
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Re: Glass Marbles for Reflux Column Structured Packing

Postby Klein » Mon May 22, 2017 1:13 pm

2825w on a 2" copper column, 39" of marbles (14mm) + ~5" of rings 96.5% abv at about 2 litres per hour.

I had about 6" of space on top of my marbles so I used about 5" of stainless raschig rings on top. (Had them right beside me when I was filling my column and figured why not.)
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Re: Glass Marbles for Reflux Column Structured Packing

Postby Rod » Mon May 22, 2017 4:26 pm

Spriit Tisler wrote:I havent' been able to source suitable sized glass marbles so I'm gonna test out soon the ceramic raschig rings I have had lying around for good time. I unpacked the SS scrubbers and they were in perfect condition, corrosion-free. I suppose rings shouldn't do that bad on side of marbles?


one of many

http://www.ebay.com/itm/Crystal-Clear-G ... 2259054434

by the way I had significant success with the marbles in my reflux still
Last edited by Rod on Mon May 22, 2017 5:33 pm, edited 1 time in total.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby Klein » Mon May 22, 2017 4:51 pm

I ordered them from hobby lobby and had them shipped to a warehouse in the USA. Not sure If they ship outside USA or not.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby Spriit Tisler » Thu May 25, 2017 12:07 pm

Tested raschigs today, had similar output rates to scrubbers but the abv was still limited to 93% at 1.2l/h and it would not rise higher than that.
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Re: Glass Marbles for Reflux Column Structured Packing

Postby yakattack » Sat May 27, 2017 3:16 am

What size column are you running tisler?
And are you going from a wash or low wines?
HDNB wrote: The trick here is to learn what leads to a stalled mash....and quit doing that.
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