Glass Marbles for Reflux Column Structured Packing

[rad14701]

I have been meaning to stop by the local Michaels' to see if they have these in stock... Smaller than standard marbles, which are 16mm|5/8", so I'm guessing in the 12mm|1/2" range...

[SoMo]

I have been meaning to stop by the local Michaels' to see if they have these in stock... Smaller than standard marbles, which are 16mm|5/8", so I'm guessing in the 12mm|1/2" range...

The ones in your post are the ones I'm getting at hell*mart just on a 2-1/2lb package.

Hell*mart has 5/8's and 1/2" in the craft department, 6$ for 2-1/2lbs clear glass going to get mine today. They also have the flattish ones that are already etched for a buck or two, I remember someone saying the flat ones weren't as good tho.

[cob]

They also have the flattish ones that are already etched for a buck or two,
I remember someone saying the flat ones weren't as good tho.

no one has yet posted real experience with the flattened marbles. so good or bad is still just conjecture.

[Red Rim]

I tried packing my one inch column today. Learned a few things. First, I tried a wad of fine copper with sets of six marbles, then wire, then marbles with a total of ten levels. Thinking that each set of wire may work as a plate. Finished it up and poured some heads through it and it barely drained. Ugh. Then tried blowing through it and it was really hard. Damn.
So then I unpacked it and tried sets of twenty marbles then wire, then marbles. Much better this time however, the wire would wrap around the marbles and almost plug the hole. Much better flow, but I think I will drop back and try a third step.
This time I am going to wrap a coil of 12 or 14 gauge wire to separate the levels. If that doesn't work, I will just go with all marbles and a wire start and finish.
The wire I have been working with is so fine it looks like I am stuffing a redheaded step child down the pipe. Odd really.

I also understand that since I am using a one inch pipe for my column, that I won't get near the level of abv or the speed of take off, but what the heck, it's worth a try.

[SoMo]

I believe on other threads PP found use two different types of packing in the same column was counter productive.

[Red Rim]

I believe on other threads PP found use two different types of packing in the same column was counter productive.

Thanks for the input, as much reading as I have done, somehow I missed that.

[ozone39]

Very interesting post....Think the essential variables are unlimited and calculating the packing consistency and the heat transfer (or non transfer capacities for that matter) would involve a math formula two pages long or longer. I have dabbled in this experiment a bit in my time only I was using only 3/8" and 1/2" s.s ball bearings I got from a buddy of mine. (aprox 3" depth in an 1 1.2" column, makes for a heavy column but what ever). It worked great, in my personal opinion it worked better than the copper "wool" I normally use. I ran a couple runs with this, but I do not use columns that have packing any more. My opinion on the variables using small spherical packing. Material = resistance to heat, Diameter = surface area and size of voids between the spheres to allow vapor migration. Location = obviously higher up the column the more heat that is diffused by the column itself and temperature distribution of the packing itself. Just my two bits....If it works for you, run it....

[Red Rim]

For what it's worth.
Ran my bastardization of a modification this weekend.
In a heads/fores/tails/thumper waste run.
One inch column by 4 feet tall, copper mesh at the bottom, marbles all the way up.
18 inches of cold finger sitting above for a condenser.
To really screw things up, I have an undersized thumper to finish it.

After taking a gallon and a half off, for perceived fores/heads, I started right into 175 proof and worked my way down in 5 proof increments per quart jar.
I ended up with three gallons of product waiting for cuts, out of an initial 13 gallon batch at 30 proof.

As a disclaimer, this is my first time working a reflux column, and it is night and day different from working a pot still with a thumper. The thumper I could drive blind, deaf and naked and still run better than anything you can buy in a liquor store. So before I can give a conclusive performance evaluation, I will have to get a few runs under my belt, both at low abv (8%) and spirit runs. Also I need to do a side by side comparison with copper scrubbers or Copper wire.

For now, taking a pot still. That I would get 135proof and increasing it to 175 proof in a few short modifications, simply by stuffing it with marbles and running a reflux over itsn't a bad deal.

Thanks Rad for your ideas and I will keep you posted..

[waster]

I can assure you that my rig is getting better than 8" HETP's...

Rad, how does one measure HETPs for a column, experimentally? I'm pretty close to having my set-up ready to test (marbles, rings, scrubbers all in hand, heating power avalable 40,000 BTU/hr, test wash ready.....). Since I'm interested in high throughput + high purity, I thought that the procedure should be:

1. Run the system, increase the heating and cooling until flooding. Back off by a margin. Stabilize with no reflux.
2. Measure cooling power (flow of cooling water * temp difference in to out). This tells me the throughput, which is confirmed by step 3.
3. Open the RR valve fully, let it siphon out the reservoir, then measure the rate of flow through the open valve. Unless the valve is limiting things, this should confirm the same power number as step 2 when multiplied by the heat of vaporization.
4. Again with RR valve fully open, collect 250ml (or a hydrometer flask full) and measure ABV at calibrated temp. This ABV should give the zero-reflux HETP

For steps 2 and 3, with sample numbers, the calculations look like:
[tr][td]cooling water rate[/td][td]0.5L/min[/td][/tr] [tr][td]delta CW temp[/td][td]30 C[/td][/tr] [tr][td]cooling power[/td][td]15,000 cal/min[/td][/tr] [tr][td]conversion[/td][td]4 J/cal[/td][/tr] [tr][td]wattage of cooling[/td][td]1,050 Watts[/td][/tr] [tr][td]wattage of cooling[/td][td]1,050 Watts[/td][/tr] [tr][td]heat of vaporization of eth[/td][td]39,000 J/mol[/td][/tr] [tr][td]density[/td][td]0.79 g/cm3[/td][/tr] [tr][td]mass[/td][td]46 g/mol[/td][/tr] [tr][td]production[/td][td]1.57 ml/sec with no reflux[/td][/tr] [tr][td]production[/td][td]5.7 L/hr with no reflux[/td][/tr] For step 4, the procedure comes from the mass balance equation from the parent. For example, again assuming no reflux from the head:

starting liquid ABV 10.00%
condenses to 55.02% after 1 plate
condenses to 81.00% after 2 plates
condenses to 87.50% after 3 plates
condenses to 90.23% after 4 plates
condenses to 91.88% after 5 plates
condenses to 93.02% after 6 plates
condenses to 93.87% after 7 plates
condenses to 94.55% after 8 plates
condenses to 95.10% after 9 plates
condenses to 95.56% after 10 plates

Once we measure the actual number of plates, then its just a question of dividing the actual packed height to get HETP. Is this the best/right way to experimentally measure HETP? I realize I'm approaching this rather simplistically (ie, assuming product is 100% eth for many of the parameters), but I'm just trying to get close. Anyone who has a better procedure for evaluating packing (specifically marbles) for both HETP/purity and productivity, I'm all ears.

PS: Rad's and Lester's experiments give 3-4" HETP with reflux, which might correspond to 4-6" at zero reflux.

[googe]

No.matter how much calculation and theory you do, it will not give you any answers, every still, packing, heat, wash, atmosphere, water, material is different, eg, rad doing this for years and starting this thread, you don't know until you do it.

[Bagasso]

Since I'm interested in high throughput + high purity, I thought that the procedure should be

I think you just need to time step 4 to get the throughput.

Since you still have heads, hearts and tails even at 95%, I guess comparing purity from different packing would mean measuring how much is kept and how clean those fractions are.

[ozone39]

well said googe....i agree completely.

[Bagasso]

well said googe....i agree completely.

We can all agree but waster was asking about measuring his real world runs to get an accurate comparison.

[googe]

well said googe....i agree completely.

We can all agree but waster was asking about measuring his real world runs to get an accurate comparison.

give him an example then Bagasso, his still type would be a good starting point .

[Bagasso]

give him an example then Bagasso, his still type would be a good starting point .

An example of what?

[waster]

Thanks Bagasso--I agree that step 4 is the key. But thinking about it last night, I had two thoughts. First, the preceeding steps are needed to make sure there is no reflux (ie, comparing cooling power to zero-reflux production). I think this is important because my product arm is 1/4" tubing--I can imagine fittings/valve that restrict flow, which would create reflux and lower productivity numbers. Step 3/4 must have no reflux.

Second, starting with 1000mm of packing seems wrong. If the wash is 10%, and the HETP for marbles is 150mm, I should have ~6 plates in my 1000mm column. The problem is that I'm in the flat part of the curve, near azeo. Its going to be inaccurate to judge the number of plates when 6 plates is 93.02% and 7 plates is 93.87%. It seems like the accurate way to measure HETP would be to use a shorter column, only 2-3 plates worth. For the same 10% wash, 2 plates is 81% and 3 plates is 87.5%--I should be able to measure that accurately. Its even better for 1% wash.

Bottom line: I'm looking for a protocol to accurately measure HETP for marbles. It seems that the lowest ABV wash and a partially filled column (maybe only 300mm of packing) will give a better measurement. I have no idea how the SPP-istas measure 20mm HETPs unless the are using 40-60mms of packing. Maybe Rad's hybrid column in short mode is the ideal tool for this....

[SoMo]

Isn't the point of this to produce a higher % at a higher take off speed? Comparing the different media structures against one another? The same wash ran over different packing which will produce the highest at the highest take off?

[waster]

SoMo,

Yes, certainly. But if we are going to say that the gospel numbers on the parent site for HETP of marbles are wrong, we need to measure the HETP accurately. Also, if I saw 1 ft of column packing produce, say 65% ABV with one packing and 85% with another, at zero reflux, that would be way more convincing than comparing 94.3 against 94.6.

[SoMo]

But your excluding the variable of speed which is also a limiting factor.

[SoMo]

My .02$. You guys are way over thinking this, it's pretty simple. Make one wash or mash big enough for two or three runs. Set up and run a specific amount of wash using the different packing materials, marbles, scrubbers whatever. Maintain highest purity at the fastest take off possible. Post results it's pretty simple none of the hetp plate stuff will matter as the results should show the difference. It's up to the member to be honest and not inflate or deviate from the results their experience produces.

[waster]

neat

http://www.amazon.com/gp/product/B00H0B68XK/" onclick="window.open(this.href);return false;" rel="nofollow

[Hound Dog]

I can agree with SoMo's $.02 but keep in mind that % does not = purity. Not by a long shot to my taste buds. I think this all started with Rad pointing out that he got good results with a really clean tasting product. That is the important part. I can brew up some 95%+ that really tastes like crap if I have the wrong setup working for me

[Bagasso]

I can agree with SoMo's $.02 but keep in mind that % does not = purity.

Add to that the fact that he says he was taking it off at a fast rate.

It isn't just about HETPs.

[SoMo]

Purity, speed, for neutral spirit. I want to use them for purity speed and high flavor, now flavor being my variable. Odins pure corn whiskey via Smiley.

[rad14701]

I'll reiterate that I have zero interest in what HETP's I'm getting with marbles, or SS scrubbers for that matter... Speed, %ABV, and taste, are what I'm after and that's all that counts... My 1.25" column filled with 5/8" marbles doesn't look like it should perform as well as it does... In fact, I was half expecting to have even worse results than with scrubbers but have been surprised by the amount of overall improvement... I'll leave it to someone else to play with HETP comparisons...

Probably stated previously but simply being able to run faster, attain higher purity, have a larger hearts cut, and cleaner neutral spirits, provides me with enough satisfaction to wish I could run my rig more often... Might be time to bump up my boiler to be able to take a full 6 gallon wash... I've trimmed enough run time to where I can probably run 6 gallons off in about the same amount of time I used to run 3...

[rager]

well here is my contribution to this thread

I picked up 600 5/8ths marbles from the "dollar tree" cost was 12.78 . not bad

I filled my 2 inch column up to the site glass "44 inches" . ended up using 575 or so.

total weight was 6.75 pounds.

that should help some people

I will post results of sac run when the time comes

rager

[Setsumi]

After long hours behind my 2 inch boka I started looking into alternatives to speed things up. Bigger column or inline thumper or strip runs?? My VM head does not produce faster, but then I have a 3/4 elbow into the column as splitter to take off. Gues I will try marbles for my next run, only thing is no one realy explain why it work so well. I agree with the guys mentioning thermal mass and drainage both these are present in bublers and inline thumpers (to a degree). Wonder if a short thicker column packed with marbels under the 2 inch could act as thumper, any one venturing an comment?

[ksarrow]

They have marbles 1 mm and up..
https://www.rainbowturtle.com/mobile/Ca ... 818&page=3" onclick="window.open(this.href);return false;" rel="nofollow

[700G]

I'm gonna give marbles a try on a neutral run. I loaded up my 4" borosilicate column with 30-35lbs of 5/8 glass marbles. I've gotta say, it looks pretty badass! I'm hoping to get at least close to the same performance as lava. Marbles will be WAY easier to clean. I'm gonna run on Wednesday, I'll post results.

[still_stirrin]

I'm watchin' ya', 700G.

I use those same marbles in my column. +1 to the cleaning ease. It's the truth.

So, when you run it, could you take a video and post it? I'm terribly curious what the column insides looks like when running. Mines copper so I can't see inside. Thanks.

And I bet they were easy to fill and didn't cost an "arm and a leg" either. Maybe not quite as efficient as scoria, raschig rings, or SPP, but who can argue with simplicity, easy on the pocket book, and easy to maintain?
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