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Testing the SPP

These usually have the means for returning the spirits to the column and usually allow metering of the take off to help in the reflux.
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rkr
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Re: Testing the SPP

Post by rkr »

Here are the first results of my tests, a complete report is available in ARC forum.

"Let's start with liquid holding capacity. I took a 13.5cm piece of 54mm column that just holds comfortably 3 brand new potscrubbers. These scrubbers weigh 55.2g when dry. So I wetted them, let them rinse for a while in a sieve and weighed them again for 85.7g. This means that they held about 30g of water.

Now I took that piece of column and filled it with SPP. The weight of those SPPs was 209.3g. I then wetted the SPPs, let them rinse in a sieve for a while and measure again. The weight was now 246.3g which means that they held 37g of water.

That means that they hold 23% more water than scrubbers. This is getting really interesting, SPP really seems to have some potential. The only minuses so far is that they are hard to handle (I had to use a spoon to pour then in to column and still got many small SPPs bouncing around the table and floor) and weigh a lot. The handling part shouldn't be a problem once they are in place inside the column."

"Well then, the reference run is done now - I think. I had some glitches in the run so depending on the next run I may need to reconsider. The original plan was to use ethanol water mix, but as I had low wines all ready sitting on the boiler I thought I'd give it a go. First problem was fluctuation when running at 2kW. With VM-E-ARC these fluctuations are absorbed but with LM they are not good for measurable run. So, after taking the probe out a bit without effect, I switched to 1kW and got steady readings. So far so good, I think the LM reservoir was causing the trouble as the ID of the hole was only about 23mm. The next problem was high concentration of heads. This forced me to remove some 600ml before the temperature ceased to rise. I then set the thermostat at stabilization on +0.1C off. The strictest setting in order to bring out performance differences as well as possible. Here are the results:

13:24 - Opened the valve
13:34 - Had collected about 300ml, the buffer that had accumulated in the column during stabilization.
13:44 - ~400ml
13:54 - ~500ml
14:04 - ~600ml
14:14 - ~750ml
14:24 - ~950ml

The accurate measurement showed 980ml. So pretty much what we can expect from scrubbers considering the tight thermostat setting. Worth noting is that at the beginning there were quite a lot of fluctuation which towards the end of one hour period had evened out. There were still heads present so I reserve myself a right to do another comparison using ethanol water mixture if needed."

"Then some results with SPP:

14:37 Started the run
14:47 ~300ml collected
14:57 ~450 ml
15:07 ~600 ml
15:17 ~700 ml
15:27 ~900 ml
15:37 1120 ml

So the increase in output was 14%. Not quite as much as the increase in liquid holding capacity, frankly I was expecting more from this packing. I must say that I wasn't very happy with the way the thermostat was functioning, it may have generated quite a lot of inaccuracy for this test. I think I'll rig up that CU100 + PID for my next run.

It is also possible that the SPP was operating below it's optimum vaporspeed. Next thing I'll try is to set up the trusty old Thorshammer with CU100 sensor and check how it works with SPP and 2kW.

The conclusion so far is that this SPP seems to be better than pot scrubbers but the HETP is only in high 40s mm based on my first test."

SPP-close-1.JPG
SPP-close-1.JPG (142.33 KiB) Viewed 10611 times

SPP-holder-1.JPG
SPP-holder-1.JPG (127.43 KiB) Viewed 10613 times


Mod edit. Deleted one of the photos, made the text unreadable. Please repost a little smaller

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Re: Testing the SPP

Post by rkr »

And some more photos.

Slainte, Riku

SPP-in-column.JPG
SPP-in-column.JPG (455.21 KiB) Viewed 10733 times

test-still.JPG
test-still.JPG (445.09 KiB) Viewed 10720 times

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Re: Testing the SPP

Post by jake_leg »

So far so good.

Very thoughtful to provide size comparisons in multiple European currencies. :D
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Re: Testing the SPP

Post by punkin »

Looking forward to further testing. Some of the claims are for overclocking as far as abv is concerned, are you monitoring for that?

Also the pickling was mentioned as being essential for high performance, have you completed it?
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Re: Testing the SPP

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I went and measured the ABV, it was showing 96.5% with 21.7C temperature. Given the usual inaccuracies in alcohol meters (I broke my old one that was giving correct readings) I'd say that this is azeotrope so no magical past azeotrope figures here. Of course the spirits (1120 ml) had been in a gallon jar overnight so if there was any magic overclocking it should have diluted down by now.

I haven't planned any etching process since I want to get figures from SPP as you can buy it. I will probably use these column pieces for continuous stripping afterwards and that should corrode the surface to some extent.

Slainte, Riku

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Re: Testing the SPP

Post by kiwi »

It would be interesting to see the difference between etched and unetched...

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Re: Testing the SPP

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rkr wrote:
I went and measured the ABV, it was showing 96.5% with 21.7C temperature. Given the usual inaccuracies in alcohol meters (I broke my old one that was giving correct readings) I'd say that this is azeotrope so no magical past azeotrope figures here. Of course the spirits (1120 ml) had been in a gallon jar overnight so if there was any magic overclocking it should have diluted down by now.

I haven't planned any etching process since I want to get figures from SPP as you can buy it. I will probably use these column pieces for continuous stripping afterwards and that should corrode the surface to some extent.

Slainte, Riku



Your 96.5% measurement was probably very close. It should be measured at exactly 20.0C. So there's a tiny bit of error there (probably not worth worrying about).

And something else to consider...

A long time ago I did some research on the difference between ABV and ABW (weight) of ethanol. There are calculators out there that change one to the other, but they are useless at spirit measurement. They're meant for low-proof beers, and the constants of 0.8 and 1.25 only work for beer. The comparison scale is NOT linear, and when you get near azeotrope the difference is quite a bit smaller. I've been caught out with that one in the past.

The figure of 95.6% that we use for ABV is actually closer to the true figure of 95.53% ABW that is derived from the CRC Handbook for Chemistry and Physics, which gives the vapor-phase molar fraction y_1,Az = 0.1030 (the 1 is water).
That 95.53% A/W figure calculates out to 96.5% Alc/Vol @ 20°C.

So there you have it. Our ABV figure for azeotrope is in reality ABW. But the difference is so tiny, and the importance so irrelevant, that I think we can dismiss it and continue on as we always have. We're not making lab grade spirit. We're making booze. Nor are we being forced to pay tax on the absolute values. In fact the TTB can't measure such a tiny discrepancy after the spirit is diluted to measuring strength.

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Re: Testing the SPP

Post by Hammers »

Nice chronograph, rkr.
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Re: Testing the SPP

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Hammers wrote:
Nice chronograph, rkr.


We could probably start a poll to see how many people recognizes chronograph from the photo :D

Anyway, I ordered the packing from this guy lipskitechmar@gmail.com - just in case someone else wants to try it.

I hope to conduct some 2kW tests this week.

Slainte, Riku

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Re: Testing the SPP

Post by Harry »

One of our newer members, who can't yet post in this thread, has sent me a message. It contains a chart link and I think it is relevant here. It appears to be the source of the so-called 'overclocking' that's been mentioned. Chart looks genuine and valid, so a repost...

Harry wrote:
The figure of 95.6% that we use for ABV is actually closer to the true figure of 95.53% ABW that is derived from the CRC Handbook for Chemistry and Physics, which gives the vapor-phase molar fraction y_1,Az = 0.1030 (the 1 is water).
That 95.53% A/W figure calculates out to 96.5% Alc/Vol @ 20°C.

So there you have it. Our ABV figure for azeotrope is in reality ABW.


Or do bourbon, or a good vodka (Belvedere, Absolut). Azeotrope is 95.6% ABW I 97.2ABV It is not enough because the SPP instead of HEPT at 1.7 cm to 3.1 cm and it is already almost a second behind.

http://en.wikipedia.org/wiki/Azeotrope
Here, for your convenience are the conversion tables
http://akas.tuba.com.pl/azeotrop/tablica1.jpg
Na zdrowie (slainte)
Regards Jancio53

PS In the end no matter what you drink, you mistreated each
:wink:

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Re: Testing the SPP

Post by Abstinent »

Hi!
rkr wrote:
Hammers wrote:
Nice chronograph, rkr.

We could probably start a poll to see how many people recognizes chronograph from the photo :D

Indeed, at this moment I noticed it.
But, it’s simply: the obvious similarities of male hobbys attract like magnets :D .

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Re: Testing the SPP

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Jancio tipped me that tapping the column compresses the packing. I tried that and was able to create some 30mm additional space in a 500mm column piece. Naturally I filled that with new SPP :) All in all I was able to add some 110mm worth of new SPP to the column. The Thorshammer is now ready and loaded but I still need to fix the PID for the next run. In my regular runs with scrubbers I've been able to get 2-2.2 liters/hour neutral azeotrope. With more low wines I was able to reach 2.75 liters/hour which I believe is close to the flow limit of my valve. If we assume that same 14% increase that would then be around 2.3-2.5 liters/hour. If I can hit 2.75 liters that would mean 25% increase which is close to the increase in liquid holding capability. Of course there are several unknowns at play here. At the beginning the speed is likely to be flow limited and the packing efficiency steps in only as the ABV in the boiler decreases. On the other hand the increased liquid holding capability should increase the pressure and thus increase the speed. I guess it's best to stop speculating and fix that bloody thermostat :beer:

Slainte, Riku

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Re: Testing the SPP

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I fixed that for Jancio Harry.
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Re: Testing the SPP

Post by punkin »

Dog's Master wrote:
Dear Colleagues, distillers and rectifiers
I promised to do a little esse about SPP and I fulfilled my promise.
See it in attachment.
Sorry for my English, if somebody can correct it I will be grateful
Maybe there you will find some answers you want to find
Cheers!

I realized that pdf is not acceptable, so here is my esse:
Why I prefer to use spiral-prismatic packing.
Before you do anything, should clearly define the objectives, the costs of
achieving these goals and desirable ratio for the price - quality.

Outlined below - my personal opinion. But they are backed by a reputable
literary sources (Stabnikov, Krehl, Bagaturov) and personal experience, and
therefore may deserve consideration.
If we are talking about the spiral-prismatic packing, we mean that our goal -
to obtain a neutral alcohol of high quality. When we have special needs and use
special modes of operation of the column - we can produce fruit and grain flavored
spirits also.
Q-1 What characteristics should have a packed column and
the actual packing?
1. Minimum resistance for vapor. Packed column working in film mode.
The flow of the film reflux unseparably, laminar. Flow regime - waveless.
According to experimental data, the optimal rate of steam is about 1.5 m /
s, ie very little. This means that the cross-section of the column should be free to
the maximum.
2. With a minimum of volume our packing should be characterized by a
maximum surface. We know that the interaction occurs at the interface between
liquid and vapor.
3. The surface of the packing must be very good for retaining fluid.
4. Packing should have a good heat conductivity. This is dictated by the
fact that good thermal conductivity makes it easier to transfer heat to liquid film,
and it is easier to evaporate.
5. Packing must be chemically inert, should not make harmful impurities
and to change the taste of alcohol.
6. Easily washed when needed.

Q-2 What we must avoid when designing a packed column.
1. Should fully weaken the influence of wall effect, ie the desire to fluid
flow along the walls of the column. For this purpose it is necessary to arrange
high-quality insulation and direct the flow of phlegm in the center of the column by
means of special devices.
2. Avoid creating channels for the fluid in the packing, so-called “preferred
paths”. This can be achieved only with the help of correct choise the shape and
diameter of the packing with a well-wetted surface.
Channeling stops when dc / dp> 10 (dc-dia of column, dp-dia of packing)
Specialists in laboratory distillation knows the so-called "rule Hubert",
dc / dp = 10-30.
3. Should not allow non-uniform, layered styling packing. It also causes the
appearance in the column “preferred paths”.
4. When selecting attachments aspire to the angle of the surface tension was
minimal, as the surface tension forces are entirely determined by shared properties of
the mixture.
In stainless steel angle of - 83 degrees, with frosted glass - 20. But glass
loses in the heat conductivity, and therefore, our decision is to use steel, that conducts
heat well, we have to do specially prepared (grass) surface of the packing.
5. Afraid as a fire nonvertical installation of the column. Otherwise, fluid
will flow mainly on the walls. You just guaranteed this inconvenience. Use a plumb
or level when installing the column into position!
6. Must provide an needed amount of phlegm in the correct place. It is also
easily solved. In the upper part of the column phlegm feed tube, preventing its contact
with the wall.
Column necessarily need to be divided into parts. Phlegm in partitioning
have to be redeployed again in the center of the nozzle.

It makes sense to do, since the workload on the column partitioning can
reduce the HETP. Partitioning can reduce the height of the column while maintaining
the quality of separation by 30%.
This, in particular, are devoted to Kazan, who investigated the near-wall
effect in the laboratory. Effectiveness of its non-partitioned column on the
separation of a mixture of hydrocarbons was 18 HETP. After dividing the column
into three sections, it increased to 24 HETP. With spirits the situation is better.

Q-3 What can we obtain, using spiral-prismatic attachment.
Consider a column of 40 mm in diameter. Its cross section is equal to 12.56
cm2. Let us remember that figure.
Let’s see what facilities we will be able to work using a variety of packings,
if the optimal rate fo vapor is 1,5 m / s, and at 1 kilowatt heater power produce around
45 liters of vapor per minute, or 750 cm 3 / sec.
If the column is empty, then we are at a speed of 150 cm / s in 1 second
would have let through the cross section of the column 1884 cm3 of vapor, which
corresponds to the power of 2.51 kW.
At this stage, are visible benefits of properly made spiral - prismatic
packing. It is, on average, leaving 86% free cross section of the column, that is, allow
us to work with a power 2.51 x 0, 86 = 2.15 kW.
If in the same column load glass balls 4 mm in diameter, often used by
artisan distillers, they will occupy 74% of the cross section of the column. This means
that the maximum capacity will be in the case of balls of 2.51 x0, 26 = 0.65 kW, which
is in excellent agreement with experimental data.
So the first conclusion in favor of the spiral - a prismatic attachment: it
allows equal power to use a less diameter tube, that means - to save on material.
Becomes clear why is unacceptable use of expanded clay, broken glass,
pebbles, marble chips and similar materials. They almost completely cover the
cross-section of the pipe, or vice versa, leave it too loose, often crack from
temperature fluctuations and crumbling.

Usage of scrabbers made off stainless steel looks better. But there is too big
risk of channeling fnd simply buying low quality chinese production made from
unknown metal and with unknown surface, that makes almoust impossible to
accurately calculate the parameters of the column.
A few words should be said about the surface area of SPP packing. Virtually
the same will be the interface between two media - the gas and liquid.
• In the first approximation we can say that the surface area of packing
contained in a unit of volume determine the separation ability of column.

And that’s exactly the aim for which we are doing the column.
At the same time, the balls 4 mm in diameter, which we mentioned earlier,
have a surface area in one liter of 0.9 m2.
Very expensive glass Raschig rings in one liter of surface separation are
equal to 1.1 m2.
The second conclusion in favor of the spiral - a prismatic packing: it
provides a separation in 1,5-3,5 times better than its nearest competitor.
Q-4 Retention ability of packing.
After properly designed experiments it appears that the spiral-prismatic
packing can hold 94-96 grams of water per liter . This is when the packing thoroughly
blowed out, imitating the passage of steam. If you do not blow, then the retention
capacity raises up to 200 grams.
In addition to static retention, spiral-prismatic attachment is characterized
by a dynamic of containment. For a theoretical plate, this value comes to 3.5 grams (
according to Krehl).
Static retention capacity of spiral-prismatic packing, etched properly, only
slightly inferior to the static retention frosted glass and higher retention of china.

Q-5 Thermal conductivity.
The thermal conductivity of stainless steel is 35 W / (m • K) that is higher
than the thermal conductivity of glass (the most common material for making beads,
Raschig rings and some other types of packing), which is equal to 1.15 W / (m • K)
Consequently, the steel packind is about 30 times better conductor of heat
from hot vapor to a liquid film that completely compensates for its lack of wet ability.
Q-6 How much does it cost?
If the height of the filled volume of the column of 1 meter, the volume of
the nozzle is equal to 1.26 liters. I remind you that we are talking about a column
40 mm in diameter, optimal for domestic usage.
Volumetric weight of the packing after etching and seals - about 900
grams per liter. Price of stainless steel wire 0,2 mm thick in our area - about $ 20
per kilogram.
On our column will need wire for 22 dollars 68 cents. Etching will be
worth about $ 6 - reagents are dangerous, they must be thoroughly neutralized and
rinsed. The process of neutralization is much more expensive than the actual
reagents. Manufacturing does not cost anything - you do it yourself!
Equipment for one usage is worth almost nothing, because at the end of
the process the machine will be dismounted. Even if you buy at the flea market the
remains of an electromagnetic lock, sealed switch, a small permanent magnet (for
example, to keep the doors of the cabinet), these expenses do not accurately pierce
a hole in yours budget.
Total packing cost 6+ 23 = 29 dollars. Inexpensive, since it allows you to
make a completely professional equipment and save a decent amount of money
thanks to reducing of the diameter of the main column, adapters and fittings.

Thanks for yours attention!




Riku, what Dm seems to be saying here about the efficiency bebnfits of different packings seems to be to be best tested by finding the limit of packing height or hetp. That's the claim, that the hetp is better for spp.

So i'd be thinking that the best way to test if this was tue would be to use a modular column. One that clamps together in sections...

Do a run with scrubbers in a 600mm column, do one with spp. If both pull 95+, take 100mm of packing out of each. If neither get 95+ add 600mm more...

This will quickly draw the lines as to how high a hetp is for each packing type and how much more efficient it is. :|


Seems to be more sense than measuring output volume.


I was actually trying to find where he discussed the application and theory of the etching, i was sure he gave figures for the increase in surface area and hetp and that they were very significant. Can't find it with a scan of the 7 pages though, i'm thinking it may be in another thread.

He did say it was nessercary to derive the maximum benefit.
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Re: Testing the SPP

Post by rkr »

I think people are putting too much weight on the term HETP. As a matter of fact we can well achieve sub 40mm HETP with pot scrubbers or mesh type packing. As the reflux ratio is increased the HETP is decreased. Then the HETP is also dependant on vapor speed (optimum gives higher HETP) and reflux spreading (after certain column length HETP starts to drop). Let's take Mike Nixon's experiments as an example, he was able to achieve 91.5% ABV with 150mm column filled with pot scrubbers - quite hard if the HETP really was in the 80-90mm range.

Now that being off my chest, I did a 2kW test run yesterday with Thorshammer. The results were positive but I noticed several things wrong with the run (low wines with excess amount of tails + too little alcohol, hairline crack in the column connection that leaked, new PID that took some learning to use, lots of oil in the boiler) that make the results unreliable. I can just tell that I got faster run than usual and that the end result was 96.5% stuff at 17.5C temperature. The SPP doesn't seem to mind the increased power either.

The etching will of course increase the surface area and thus increase the liquid holding capacity of the packing. However, I think that's beyond the means of many here so I'll try to test something that everybody could use.

Slainte, Riku

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