Liquid/Vapor phase diagram for ethanol/water solution

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Liquid/Vapor phase diagram for ethanol/water solution

Post by rubelstrudel » Tue Sep 10, 2019 3:04 am

I am using the liquid/vapor phase diagram for ethanol/water solution all the time. It gives me all the information I need about my still by just measuring the temp in the top of the column while running. I found this nice chart by googling:
Image

This chart is not perfectly accurate, but good enough for me. But I would like to make a prettier one for print, and it should be prominently placed in the wiki to in my opinion.

But I have not been able to find (or understand) a better description on how to generate this chart. Or a tool that could calculate the data. I'm guessing that this is a common enough thing that needs to be calculated in the process industry, so there are certainly tools out there that could do this. But where? And how accurate are they?

Do any of you guys have a mathematical formula to generate this chart? Or know of a tool online that could do it? Or a better search term so that I can find it myself?

When searching for "ethanol water phase diagram" I do not get the results I want except one instance of the same chart as above with F scale, and in horrible quality. When searching for "alcohol water temperature diagram" I get something similar. But it is all rather low quality images, no generated graphs.

The best resource I have found so far would be this:
http://stupidityshouldhurt.com/reference/org/calc.htm
But the author is unsure about the validity of all calcs.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by MtRainier » Tue Sep 10, 2019 4:43 am

Maybe this will help. I found an old post here with an old reference to vapor/liquid phase for different concentrations. I can't find it now, but the author had done OCR on the old paper after scanning it in. I put it in a spreadsheet then took the relevant columns and fit a formula to them and used it to calculate my own graph on the second worksheet. It's what I use when I'm trying to figure out what to expect and what is left.

The formula gets wonky up near azeotrope, but I'm not operating up there much anyway. 8) At least it has columns of numbers you can use to generate whatever graph you want.

It's attached here.
Brau.xlsx
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by rubelstrudel » Tue Sep 10, 2019 1:37 pm

That is some solid work MtRainier, thanks a bunch. It is all numbers though, no formula as you say, but it is just what I was looking for. Basis for a nice looking graph that I can put up on the wall. The formula wonkiness is just the approximation breaking down as I can se it, not to worry about anyway.
ethphasediag.png
This is the graph from your data. Great stuff.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by richard1 » Tue Sep 10, 2019 6:29 pm

Hi @mtranier I am being a bit stupid with that VAPOUR formula on the excel sheet. Can you more simply write the exact formula used.

I am not sure whether you are referring to EXP for E or an alternate / other value and whether x is the power value of the EXP.

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Hügelwilli » Tue Sep 10, 2019 11:59 pm

There is no real formula for this. The formulas of those calculators and graphs are polynomes and base on only a few values. Like the "Equilibrium data" list in the stupidityshouldhurt-link.
This one from member hefezelle is much better:
viewtopic.php?f=1&t=10158&sid=ece93a526 ... 0#p7558917
Based on much more values and connected with spline not a polynome.

I have spent a lot of time with programming distilling calculations. It's fun for me like solving crossword puzzle. :D

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by rubelstrudel » Wed Sep 11, 2019 8:30 am

Hugelwilli, thanks for the link. My Google-fu is failing and I was unable to find that old thread.

But you appear to know your things. Would you be willing to write a wiki article explaining this stuff to us plebeians?
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Mr Sippy » Mon Sep 16, 2019 6:23 am

The vapor liquid equilibria you find online you see are generated from readily accessible equations. At a base level they are simply algebraic. At a refined level it is a little more.

I have made a study of this for the last year or so and maybe this will be helpful. This learning is solidly in the realm of thermodynamics but don't be intimidated by it.

The liquid line is a graph of the 'bubble point' calculation. You'd input the known molar fractions of the liquid and atmospheric pressure and derive the vapor fractions and temperature. The vapor line is the 'dew point' calculation. Here you'd input the known molar fractions of vapor and pressure to derive the liquid fractions and temperature.

The simple form of bubble point needs 4 equations:
1) conversion from ABV to ABW.
2) conversion from ABW to molar volume. I am using Edwin Croissants' algorithm.
3)Antoines Equation. This establishes the saturated vapor pressures at its boiling point. It's an iterative solution.
4)Raoults Law. To solve for the vapor component fractions.

The Raoult calculation is valid only for an ideal mixture.

I believe that the Brau data and the excellent work done by Mr. Ackland (and Husker) are valid only at standard atmospheric pressure although they do account for non ideal. I would be delighted if someone could confirm this.

The refined solution uses an additional activity coefficient in Raoults Law. This coefficient is determined by a half dozen or so empirical models. The one most appropriate for water/ethanol seems to be the Wilson Model, which I am using. Wilson is not a simple calculation but it is necessary if you are interested in any kind of accuracy or control.

After some head scratching I abandoned the notion of solving this as equations of state (temperature). 10 unknowns; 10 simultaneous equations. Far easier I think to solve for each mol fraction of liquid mix and generate a table. I am doing these calculations in C.

I have to run now but later I will provide a couple spreadsheet oriented solutions that have been enormously helpful in my learning.

Cheers

I'm glad to see other folks interested in the science of distillation.

edit to post links
The first is a sophisticated spreadsheet that will calculate the VLE for a binary mix. The advantage of this one over most others is that atmospheric pressure is an input parameter and the results reflect the (typically) lower boiling points. If you look closely at the cell arithmetic you can see Antoine, Raoult, and Wilson at work.
https://www.cheresources.com/invision/f ... fficients/

The second is a video how to set up a spreadsheet to do the calcs yourself. It uses a different binary mix but substitutions are easy. It also emphasizes the temperature dependence of molar volume.


To me- what is elemental in all this is atmospheric pressure. Nearly every one here will experience a different set of boiling points for an identical mix. If you want to generate a single polynomial that is specific to your circumstance you might take the pertinent range of data from the first spreadsheet and the use Excels LINEST function.

Hope this helps anyone interested.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by rubelstrudel » Mon Sep 16, 2019 1:12 pm

Great information. Love this.

Will the changes in atmospheric pressure really be that significant? I guess mountain Highland conditions will make a difference. But most people live more or less at sea level with air pressure in the 950-1050mbar range.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Mr Sippy » Mon Sep 16, 2019 3:41 pm

I guess it would depend on your level of desired accuracy. For most, probably not.

For instance I am in the Great Lakes region. Elevation ~700 ft. Using the aforementioned spreadsheet at 1 bar and 0.984 bar the difference in boil point is just under .5 degree C. If you are using rtd for measurement, that may be significant. If all you care about is precision, then maybe not so much.
I think there is one vendor here that includes a pressure sensor in their e-parrot for just that reason. Odin has hinted as having one in the works. I have not investigated how much difference daily perturbations make but I imagine it is measurable. My goal ultimately is control hence the rigorous method. One day I will have a sensor for my controller. :D

I must mention that the equations are not Laws (except for Raoult) but empirically derived, i.e., it'll be a squishy number. But it will be as close as one can reasonably get. With the spreadsheet and 5 minutes you can generate an accurate table of temp/purity values for your situation. You'll still need to convert for molar back to ABV.

According to the Compleat Distiller, not accounting for the non-ideal nature of water/ethanol mixture makes about 4% difference. Altitude difference of course will vary.

Hope this helps.

edit: there is one more piece of software that maybe useful. Freeware. It's called Thermosolver developed to augment Oregon State's ChemE and Thermodynamics textbook. What I like about this program is you are not limited to a binary mix. You can add acetone, methanol, propanol, etc. You still have to know the ratios.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Kareltje » Tue Sep 17, 2019 7:29 am

Thanks a lot, Mr Sippy! Been looking for such a good fit for some time.

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by rubelstrudel » Tue Sep 17, 2019 10:31 am

I downloaded thermosolver and it is a great tool to visualise this dense mass of formulas that is thermodynamics. Maybe not the prettiest, and I am having problem entering numbers correctly since the software is not consistent in how it handles decimals. As long as you're using . (period) as decimal separator you're golden. But with us who use , (comma) as decimalseparator it doesn't play nice. I had to change my windows configuration to get it to work properly. Then I could make nice graphs at once.

https://cbee.oregonstate.edu/education/Thermosolver/
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Hügelwilli » Tue Sep 17, 2019 11:50 am

The problem is, ethanol water mixtures don't behave ideal. Those formulas are good to have a starting point, if you want to know something about mixtures without data. But we have datasets of ethanol water mixtures.

https://en.wikipedia.org/wiki/Azeotrope
A solution that shows greater positive deviation from Raoult's law forms a minimum boiling azeotrope at a specific composition. For example, an ethanol-water mixture (obtained by fermentation of sugars) on fractional distillation yields a solution containing approximately 95% by volume of ethanol. Once this composition has been achieved, the liquid and vapour have the same composition, and no further separation occurs. A solution that shows large negative deviation from Raoult's law forms a maximum boiling azeotrope at a specific composition.

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Mr Sippy » Tue Sep 17, 2019 11:52 am

Nice work 8) :thumbup:

Remember the x axis depicts molar fractions. Do you have a utility to convert to ABV?
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Mr Sippy » Tue Sep 17, 2019 12:07 pm

Hügelwilli wrote:
Tue Sep 17, 2019 11:50 am
The problem is, ethanol water mixtures don't behave ideal.
That's what the activity coefficient does. I refer to Raoults but if the coefficient is employed its called the modified Raoults Law. I've lost my file but I would refer you to a paper:
Simple Batch Distillation of a Binary Mixture, Housam Binous, Mamdouh Al Harthi.
The data fit is very good. You can also a see demo on Wolfram depicting the fit using the various models.

Cheers
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by VintDist » Tue Sep 17, 2019 1:34 pm

Hi all,

I simply use the CRC Handbook of Chemistry and Physics. Lots of useful info in there and it's verified, unlike many other sources.
Boiling points of aqueous ethanol.docx
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Boiling points of aqueous ethanol.docx
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by rubelstrudel » Tue Sep 17, 2019 2:08 pm

Mr Sippy wrote:Nice work 8) Image

Remember the x axis depicts molar fractions. Do you have a utility to convert to ABV?
No, I don't. I was looking at that problem now. Going to ABW should be easy enough, but ABV is a different matter. Right?
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by VintDist » Tue Sep 17, 2019 2:55 pm

To convert ABW to ABV the really rough guide is multiply by 1.25, but these are not quite linear equations at higher abv's as you'll all already know. Not quite sure why you are worried by all this. If you want precise figures, really the only way is to analyse the samples you've produced by the industry standard methods - and few of us hobbyists have that kind of kit and lab accreditations (or money!!) to do so.

Also lab methods are slightly different between say US and Europe/ Asia and so on, so results can be slightly different by different methods. Raoults Laws and others are all based on ideal inter-molecular predictions that do not really account for ethanol/water hydrogen bonding effects, so don't get too hung up on all that stuff. Go for industry standard tables and so on that are based on real measurements..........e.g American Society of Brewers etc (sorry I'm used to metric untis, so can't get my head around all the Imperial units they use, so personally don't use them)

As everyone has already said previously - accuracy and precision depend on all sorts of factors, and ethanol isn't particularly well behaved.....it's all a best approximation really

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Mr Sippy » Tue Sep 17, 2019 6:35 pm

rubelstrudel wrote:
Tue Sep 17, 2019 2:08 pm
No, I don't. I was looking at that problem now. Going to ABW should be easy enough, but ABV is a different matter. Right?
Have a look at Edwins paper.
On the Conversion of Alcohol r1.pdf
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PM sent.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by rubelstrudel » Tue Sep 17, 2019 11:06 pm

Mr Sippy wrote:
Tue Sep 17, 2019 6:35 pm
rubelstrudel wrote:
Tue Sep 17, 2019 2:08 pm
No, I don't. I was looking at that problem now. Going to ABW should be easy enough, but ABV is a different matter. Right?
Have a look at Edwins paper. On the Conversion of Alcohol r1.pdf
PM sent.
Absolutely fabulous. Thats just what I needed. THanks a lot.
Previously when doing estimations on ABW/ABV I've assumed volume to be constant regardless of mixing rate. And for the range 30-60% that is "good enough" for bottle labeling purposes. However, the intricacies here are facinating in it self.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by rubelstrudel » Tue Sep 17, 2019 11:09 pm

VintDist wrote:
Tue Sep 17, 2019 2:55 pm
sorry I'm used to metric untis, so can't get my head around all the Imperial units they use, so personally don't use them.....
..... ethanol isn't particularly well behaved.....it's all a best approximation really....
You and me both VintDist. You and me both.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Hügelwilli » Wed Sep 18, 2019 3:12 am

Mr Sippy wrote:
Tue Sep 17, 2019 12:07 pm
Hügelwilli wrote:
Tue Sep 17, 2019 11:50 am
The problem is, ethanol water mixtures don't behave ideal.
That's what the activity coefficient does.
This coefficient looks at the behaviour of the components heavily diluted, that the molecules don't affect much each other, and this tells how the components perhaps behave in less diluted situations, right? So you measure something total different than you want to know. But this method helps the industry. Because they want:
Plan a system or machine for distilling cemicals, noone knows exactly how they behave. The formulas give a starting point. When the machine runs they measure everything and correct the settings.
But we want: Look at the temperature of our still and calculate the temperature into abv. We will not measure and correct something.
So I think, tables with measurements are the best option for us.


Here are three online calculators and simulations in German language I have made with other distillers, based on the data of member hefezelle:
https://hobbybrennen.ch/Rechner/Destill ... chner.html
https://hobbybrennen.ch/Rechner/Destill ... ator1.html
https://hobbybrennen.ch/Rechner/Destill ... ator2.html
It's revised versions of the calculator page of my forum I will upload there soon (I revise the whole calculator page currently. Currently all calcs are on one page. In future there will be one page for each calc).

The first one is able to calculate also vacuum distillation. The two simulations are set on normal pressure. Perhaps I will add the pressure function there too.
Also the calculation for the pressure relies on data. Unfortunately there is conflicting data about how much more or less pressure does transform the vapor-liquid diagramm. We had to pick out the information, what looked best for us, and also looked at formulas (Antoine and Frost-Miller).

All calcs can calculate or simulate rectification. But it remains theoretical, because we cannot calculate how much rectification your still provides.

Also the other calcs are interesting perhaps (dilution with contraction for example). And we are working on a few new ideas.
(If the mods don't like links to other homedistiller forums, feel free to delete them).

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by rubelstrudel » Wed Sep 18, 2019 4:09 am

Hügelwilli wrote:
Wed Sep 18, 2019 3:12 am

Here are three online calculators and simulations in German language I have made with other distillers, based on the data of member hefezelle:
https://hobbybrennen.ch/Rechner/Destill ... chner.html
https://hobbybrennen.ch/Rechner/Destill ... ator1.html
https://hobbybrennen.ch/Rechner/Destill ... ator2.html
It's revised versions of the calculator page of my forum I will upload there soon (I revise the whole calculator page currently. Currently all calcs are on one page. In future there will be one page for each calc).
This gets better and better. As you say Hügelwilli, these are the calculators us hobbydistillers need and want. These calculators really ought to be translated to reach a wider audience. Great work.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Mr Sippy » Wed Sep 18, 2019 4:46 am

Hugelwilli... those are the best calculators I have seen so far. Very nice work and thank you. :thumbup:

edit:
From your site "The consideration of the air pressure or the altitude can have a significant influence on the result. When specifying the air pressure, the calculation is very accurate, given the altitude and the outside temperature, unfortunately, very inaccurate, since weather fluctuations can have a greater impact than 300 meters. Therefore, it is strongly recommended to enter the current air pressure for calculations. This can be found on sites such as wetter.de without much effort."

I had acknowledged earlier that the results of calculation are a 'soft' number but I always believed the difference to be quite small through proper modeling. For those of us with controllers who want to display real time purity; I wonder if the error of calculation is preferable to tabulated data that doesn't accommodate weather fluctuations (without updating). Thank you.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Hügelwilli » Thu Sep 19, 2019 1:46 am

All data for the basic diagram we used base on normal pressure (1013.25hPa).

For implementing the influence of pressure on the boiling temperature, we compared the common formulas like Antoine and Frost-Miller with data we found and decided for Frost-Miller. But we finetuned it, that it matches exactly 100°C at 0%abv and 78.17°C at azeotrope 97.18%abv at normal pressure, what are the most trustworth values we think.

The influence of the pressure on the difference between abv in the boiler and abv in the vapor we looked at measuement tables and tried to draw a line between the points. From the line we took values and feed our calculator with it. Not very scientific, but it doesn't need to be exact, because the influence of pressure on the abv difference is very small compared to the influence on the temperature. At 800hPa (2000 meters above sea level perhaps) the azeotrope is 97.39%abv according to our calculator. Not much difference to 97.18. But it boils at 72.3°C instead of 78.17. This is an important difference.

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by MtRainier » Thu Sep 19, 2019 4:39 am

I've been following along with this thread and clicking on the links. Looks like lots of interesting info. What I really like is a simple chart of numbers with three columns at normal atmospheric pressure: temperature, liquid, and gas.

I'm not thinking about using it to drive anything automated so it doesn't need multiple decimal places of accuracy. It's just up on the wall so I can read a temp on my boiler or in my vapor path and have an idea of what's happening. 8)

Honestly, I mostly use it to figure out when I should turn down the power because I'm close to boiling the wash and also after the fact what my ABV in the wash was when it boils at a certain temp. I also use it as one input to decide when collecting anything else wouldn't be worth it.

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Hügelwilli » Thu Sep 19, 2019 11:20 am

Main benefit of making those calculators is the high chance to learn something really new.

For example we tried to make a proper liebig condenser calculator. The one on hd is pretty primitve and simply wrong in most cases. But we failed too. It's possible and easy to calculate the cooling water and also possible to calculate the physics of the outer jacket, but not possible to calculate the steam, air and condensate filled inner jacket. The only way would be to build a dozen different sized liebigs with sensors and experiment with different water amounts and temperatures, different angels and different heat inputs. A condenser calc based on measurements.
But we learned a lot about designing and running liebigs.

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by OtisT » Thu Sep 19, 2019 12:18 pm

Mr Sippy wrote:
Mon Sep 16, 2019 3:41 pm

Freeware. It's called Thermosolver developed to augment Oregon State's ChemE and Thermodynamics textbook.
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by hefezelle » Fri Sep 20, 2019 12:34 am

rubelstrudel wrote:
Tue Sep 17, 2019 2:08 pm
Going to ABW should be easy enough, but ABV is a different matter. Right?
I used the formula for density of water/ethanol mixtures suggested in this pdf to wirte a tool for converting between abw and abv:
abv<->abw.zip
contains two 64bit windows executables
(554.21 KiB) Downloaded 48 times
Unpack the zip, open your command line (Windows->Execute->type in "cmd" and hit return), navigate to where you unpacked the exe files (eg: type "cd C:\\Users\Frank\Downloads" and hit return), and use them like this:

Code: Select all

>abvfromabw.exe
Usage: C:\\Users\Frank\Downloads\abvfromabw.exe ABW[%] TEMPERATURE[°C]
>abvfromabw.exe 33.3 25
33.3 ABW = 40.0637 ABV at 25°C
>
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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by MtRainier » Fri Sep 20, 2019 12:59 pm

I finally found the chart I liked the best again. It's Hookline's PDF chart in this .zip file.

viewtopic.php?p=7024977#p7024977

Not dissing the calculators. They're cool. I just always want a nice chart to look at while I'm doing it.

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Re: Liquid/Vapor phase diagram for ethanol/water solution

Post by Hügelwilli » Sat Sep 21, 2019 6:27 am

Yes, everyone has his own habits. I understand that during the distillation it's easier to look at a paper.
Because of that it's one of our future plans to make a html for producing tables and diagramms automatically.
Something like you type in your pressure and your rectification and you'll get within a second a downloadable and printable diagramm with the curve of the wash, the curve of the vapor above the wash and the curve of the vapor after rectifcation.
Or you type in the pressure and you'll get a downloadable and printable table with perhaps 50 temperature values and the corresponding abvs in the vapor.

hefezelles abwfromabv.exe is our source of data, when we have to switch from abv to abw or otherwise within our calculators.

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