Baking Soda

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Bagasso
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Re: Baking Soda

Post by Bagasso »

Bourbon_Greg wrote:Anyone ever used baking soda in a thumper when the still has the mash? It seems this would be OK to boost the ABV and compress the heads when trying to get a neutral.
I'm not seeing it. The chemistry behind esters and baking soda says that a pot with alcohols and acids (what you have in your boiler) yields esters (not counting those that are created during fermentation) and that, in the presence of an alkali, esters can be hydrolyzed (what would end up in your thumper).

The question is, how much time would the bicarb in a thumper have to work on the esters? In Tomb's post he is thinking about the entire heat up time before the temp is high enough for the esters to boil out of the solution but in the set up you describe the esters would be driven into a thumper that is hot enough to drive them off before the bicarb has much time to hydrolyze them.

Also, esters are just one type of congener that keeps distillate from being neutral so, unless you have a column on the thumper, and you are running it correctly, you will not be getting anything close to neutral out of it.

Using bicarb isn't about compressing heads but about breaking down the compounds that makes heads what they are.

Then there is this graph which, if correct, shows that heads are made up of different things depending on what the ABV of the still charge is:
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Re: Baking Soda

Post by Bourbon_Greg »

Thanks for the info!
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Re: Baking Soda

Post by Spriit Tisler »

Can baking soda be substituted with sodium hydroxide? Looking it's chemical properties it should sort of do the job much quicker, possibly during heat-up of strip wash. Basically we're looking for cutting esters and reversing ethyl acetate - acetic acid - ethanol - cycle.

For comparable results, making 2 batches, one for soda and other for lye and refluxing them could be done.
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der wo
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Re: Baking Soda

Post by der wo »

I never tried baking soda, because it's not very soluble. Washing soda is much better. 5g per liter low wines solve after a few minutes on a radiator and rise the pH to 11.
Sodium hydroxide is much stronger and perfect soluble. 1g per liter will rise the pH to 12, 2g per liter to 13. Be careful, wear gloves when working with it.
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Re: Baking Soda

Post by rad14701 »

der wo wrote:I never tried baking soda, because it's not very soluble. Washing soda is much better. 5g per liter low wines solve after a few minutes on a radiator and rise the pH to 11.
Sodium hydroxide is much stronger and perfect soluble. 1g per liter will rise the pH to 12, 2g per liter to 13. Be careful, wear gloves when working with it.
+1 on the washing soda... You can get a box of Arm & Hammer Washing Soda pretty cheap just about anywhere here in the US...
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Re: Baking Soda

Post by Spriit Tisler »

Does anyone have practical results on how each works, and which gives better results? There's NaHCO3(baking soda) which gives Na2CO3(washing soda) and water when heated to +60C and then NaOH(lye), which does make washing soda when reacted with carbon dioxide so the chemicals are very closely related and *should* do pretty much the same job, lye only being more powerful. Both are easily and cheaply available in all forms where I live + I've already got few kg's of both so that's not a factor. I don't think and hope I wont be needing them with all-bran spirits but I'm keen on testing for hobby's sake. :mrgreen:
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der wo
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Re: Baking Soda

Post by der wo »

I have here 1 liter heads from a feints run with pH 12 and one with pH 13. With sodium hydroxide one week at room temp. The one with pH 13 smells significantly cleaner, less fores. The higher the pH the more complete the fores reduction. But I don't know, how the ss-boiler of my still reacts with such an extreme pH. Up to now I only distilled max pH 11 with it. Next time running feints I will distill pH 12, but it will be in autumn or winter.

Important information for chemical novices: Between pH 11 and 12 or between 12 and 13 is a HUGE difference.
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Re: Baking Soda

Post by Bagasso »

der wo wrote:But I don't know, how the ss-boiler of my still reacts with such an extreme pH.
I had the same concern. I have a paper thin 555 SS pot as a boiler, made in India.

I would just use a bit of citric acid or hydrochloric acid to bring the pH down to under 10 pH before running.

After coming across the idea that the heat in the boiler might make the conversion work quicker I decided to try at over 12 pH. Instead of letting it sit for a week, I let it sit for a day then run.

My cheap pot looks the same as it did before the 3 or 4 runs that I have done at extreme pH but, as always, YMMV.
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Re: Baking Soda

Post by FreeMountainHermit »

Cheap ain't good. Get a keg.
Blah, blah, blah,........
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Re: Baking Soda

Post by Bagasso »

FreeMountainHermit wrote:Cheap ain't good. Get a keg.
Well, I emphasized cheap because, despite being that, my boiler is still holding up.

Besides, I wouldn't know where I can get a keg where I'm at. I can't even think of a bar that has kegs in my small central american town.

On topic: After looking around for more info I noticed that ester hydrolysis seems to be a thing on more than a few chemistry syllabi. Can't seem to find any hard info on the conversion rate but most of the things I've come across measure reaction rate in minutes, some even seconds (although they run into the hundreds), even at room temp. Maybe it has something to do with them using concentrated chemicals.

I have read that alkali also break down other compounds so, maybe sitting for a week is doing more than just ester hydrolysis.

From my experience, I can add sodium hydroxide or, my current go to, calcium hydroxide and I notice a change within minutes. It's like the sharpness of the smell of my low wines disappears and I end up with something earthier, tailsy. it seems to be something that has always been there, they are low wines after all, but it seems like something moved out of the way or was neutralized and the other smells are more noticable.

Maybe it's ketone and aldehyde hydrolysis that makes a difference in the week long alkali treatment. Seems like "The more you know, the more you know you don't know".
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Re: Baking Soda

Post by Spriit Tisler »

It appears to me that most stainless steel are resistant to mild (up to 20%) solutions of NaOH under 65-80C depending on source. When we are talking about 0.5% solutions(5g/l), there should not be an issue. Basically pH scale ten-folds every step, so one higher is 10 times more alkaline, and one down is 10 times more acidic, so difference between pH 12 and 14 is 100-times. In woodleg logic this would mean what would take a week to work should go in less than 2 hours.

http://www.bssa.org.uk/topics.php?article=34" onclick="window.open(this.href);return false;" rel="nofollow

Stainless steels are weak against chlorides so hydrochloric acid should be kept away from SS boilers at all times. It will form sodium chloride (table salt) upon reaction with sodium hydroxide, but I would rather use citric acid, or if one comes to it, even sulfuric acid, since it generates very inert end products (sodium sulfate).

So a 0.1M/l NaOH solution (where 1 mol is about 40g, 0.1 coming to 4 grams per liter) would give pH of 13, where a 1M/l solution would give pH of 14. For a boiler load of 10 liters this would result of 40 grams of NaOH needed to get pH 13. For getting pH 12 with NaOH, apparently only 0.4g/l is needed. Since all reactions go exponentially faster the higher the temperature, I suppose that what will happen in days in room temp, will happen in even minutes under 80C of reflux.

For sodium carbonate (washing soda) the 0.1M/l pH is 11.26 ( http://www.aqion.de/site/191" onclick="window.open(this.href);return false;" rel="nofollow ), where 1 mol is approx 100 grams. 1 mol solution would be just a bit over 12pH, and this would require a mere 100 grams per liter? This sounds quite a bit compared to the usually suggested 5g/liter.
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der wo
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Re: Baking Soda

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Spriit Tisler wrote:So a 0.1M/l NaOH solution (where 1 mol is about 40g, 0.1 coming to 4 grams per liter) would give pH of 13, where a 1M/l solution would give pH of 14. For a boiler load of 10 liters this would result of 40 grams of NaOH needed to get pH 13. For getting pH 12 with NaOH, apparently only 0.4g/l is needed.
Those numbers are for NaOH in pure H²O? To get numbers for NaOH in low wines or feints you have to measure, not calculate.
Spriit Tisler wrote:For sodium carbonate (washing soda) the 0.1M/l pH is 11.26 ( http://www.aqion.de/site/191" onclick="window.open(this.href);return false;" rel="nofollow ), where 1 mol is approx 100 grams. 1 mol solution would be just a bit over 12pH, and this would require a mere 100 grams per liter? This sounds quite a bit compared to the usually suggested 5g/liter.
To solve 100g washing soda in 1 liter low wines is not possible I think. I would not try more than 10g.
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Re: Baking Soda

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So I've used salt, sodium bicarbonate and sodium carbonate in low wine distillations and here is what I've observed:
Salt I use in my spirit run primarily to try to compress head/tail cuts. Salt certainly seems to help keep the tail pinned in the boiler longer but you have to add a fair amount of it to really change boiling points significantly.
Sodium bicarbonate I've used interchangeably with salt. It doesn't appear to do anything more or less than regular salt, my spirit runs off tasting the same with or without it.
Sodium carbonate produced a visible series of affects, much more than either salt or baking soda. Firstly, adding sodium carbonate actually dries the spirit some and visibly entrains the water from it forming a heavy, oily mixture that settles to the bottom of a glass vessel. This can then be decanted off and will give up to a 10% proof bump. When I tried running the spirit after decanting off the water/soda solution the spirit ran off tasting quite different. The heads could only be described as having a flatter flavor but the tails came off tasting like hell fire. Whatever the carbonate did to the tail wasn't good, even early tails were far more foul than they would normally be. The last observation here was that the usual oily slick left in my boiler after a spirit run had visibly changed to a crusty orange/brown deposit caked to the inside of my boiler that was a pain to get off. Basically it did more to hurt my final product than improve it and left a nice mess to clean up.
The conclusion for me is that using salt is acceptable but trying to split the esters with a base does not produce good results. If the spirit is still too heavy after a second run then run er' one more time with more cuts, that'll clean it up better.
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Re: Baking Soda

Post by Alchemist75 »

Oh, and as a quick little trick if you're into using sodium carbonate:
Heating sodium bicarbonate in a dry metal dish up to about 650 degrees with stirring (open gas flame works) will convert it to the carbonate form. Heat it up to about 850 degrees and you'll get your hydroxide. It all starts with baking soda....
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Re: Baking Soda

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Alchemist75 wrote:Sodium carbonate produced a visible series of affects, much more than either salt or baking soda. Firstly, adding sodium carbonate actually dries the spirit some and visibly entrains the water from it forming a heavy, oily mixture that settles to the bottom of a glass vessel. This can then be decanted off and will give up to a 10% proof bump.
I have used sodium hydroxide quite a bit and have also seen how it causes a cloudy precipitate. I'm not sure I would call it oily but honestly I don't remember actually feeling it. I'm also not sure about it giving the AVB a bump but I did have a bit of a problem with my last run being a bit high, compared to the calc on the parent site, but I couldn't remember if I had made a wash with a little extra sugar or not and then I started thinking that the connections on my hotplate might be a little oxidized and maybe the wattage temp was a little lower. So many variables.
When I tried running the spirit after decanting off the water/soda solution the spirit ran off tasting quite different. The heads could only be described as having a flatter flavor but the tails came off tasting like hell fire.
I have also noticed that ph treating causes a bit of an off taste but I feel that it is something that is in the product even in the wash and it just comes forward when the esters are removed.

What do you mean by hell fire? The reason I ask is because in my experience sodium hydroxide pretty much eliminates the lip numbing, solvent feel/taste of the product. I mean it usually has something off but it isn't hot, solventy, lip numbing. It just smells/tastes bad. Hell fire sounds hot.
The last observation here was that the usual oily slick left in my boiler after a spirit run had visibly changed to a crusty orange/brown deposit caked to the inside of my boiler that was a pain to get off.
I have never had this happen. I have noticed a darker than normal dunder but it is always just liquid with some sediment but nothing caked on.
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Re: Baking Soda

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So the "oily" description has more to do with the way it looked in solution. Actually when I felt it with my fingers it was slippery like dilute hydroxide and smelled like hydroxide as well. I assume it was an aqueous solution of the carbonate that had partially ionized to hydroxide and was insoluble in the higher ethanol solution.
The "hell fire" thing does indeed describe a hotness. Normally my tails have a certain heat to them but not to that extent. Usually early tails are somewhat bitter sweet but actually impart a bit of a nice taste. Later tails get progressively more an more bitter. With the carbonate that bitterness was replaced by a hot, nasty punch in the palate that was neither bitter nor sweet, just foul. It tasted like hell for lack of better term, burnt or scorched. I run bain marie so the likelihood of actual burning or scorching is quite low. In terms of that crusty deposit I have no explanation. The carbonate appeared to be almost completely insoluble in the low wines so perhaps some amount of it precipitated out as I boiled it down and caked to the inside of my cooker.(?) I only know that it did my end product no visible favors other than perhaps made the tail cut crystal clear simply because the tail tasted exceptionally horrible.
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Re: Baking Soda

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I think despite the fact that I do a spirit run with a little deliberate passive reflux to lighten the flavor the presence of the naturally occurring esters imparts a positive character. My stuff comes off tasting closer to what they would call vodka in Russia vs. What Americans think of as vodka. It has a hint of its origin to it though it is very light. Using the carbonate just didn't help improve the flavor I guess.
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Re: Baking Soda

Post by Kareltje »

Quite an elaborate description you posted ten days ago, Alchemist75.

Yesterday I did a slow run of a collection of heads that were sitting a month on washing soda. Despite vigourously shaking the soda was not completely dissolved in the 60 or 70 %ABV heads. Because I feared the bad influence on the boiler, I put the heads with soda in the thumper and diluted to about 36 %ABV. I put clean water in the boiler.
In total I had about 2.5 liters of absolute alcohol and by running slow I collected about half of that in very nasty smelling heads again of 89 or 90 %ABV. This I discarded for later use as firestarter or burning alcohol.
After that I fired up a bit and got about 850 ml (about 1/3 of the total) pure alcohol in seemingly clean hearts of 78 to 64 %ABV. The rest will be tails, I guess, but they seem to smell rather clean too.

I forgot to check for the oily feeling, but I definitely did not get the hellish smell or taste in the tails.

As said: it was a collection of almost solely heads. It does not seem illogical that the result of such a run strongly depends on the composition of the feints. So I got a whole lot of nasties and no tailies.
When there are esters in the tails, they are broken down by the soda and might result in nasty smelling/tasting acids and alcohols.

I did not compare a run with or without soda, alas.
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Re: Baking Soda

Post by Alchemist75 »

It might be a phenomenon unique to my particular ferments. Perhaps something in the tail of my stuff reacted strongly with the carbonate/hydroxide ions and gave an powerful flavor or perhaps removing some of the esters actually unbalanced the otherwise light, grain like character of my finished product. I don't know precisely what occurred but it wasn't good in my case. I might be open to trying it in smaller batches with different ferments....
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Re: Baking Soda

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The drying affect was probably the coolest part of my experiment:
I found that you could add the dry carbonate which would entrain the water in that oily looking mass, decant that off, add another round of dry carbonate and decant again. I think I was able to do it 3-4 times before no more water would entrain and I got about a 10% proof bump after doing that. Cool trick that....
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Re: Baking Soda

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Alchemist75 wrote:I assume it was an aqueous solution of the carbonate that had partially ionized to hydroxide and was insoluble in the higher ethanol solution.
Sodium hydroxide is freely soluble in ethanol so it can't be that.

There is stuff dissolved in our distillate besides fusels. The essential oil forum here got me looking in that direction and it was an eye opener.
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Re: Baking Soda

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Well whatever it was it was an insoluble aqueous solution containing some measure of hydroxide ions plainly detectable to my nose. Hydroxide has a distinct odor. I'm sure it was more carbonate ion than hydroxide anyway which isn't terribly soluble. It didn't feel exactly like and essential oil, it was slippery like a strongly alkaline solution and it washed readily from my skin so it was water soluble but not ethanol soluble.
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Re: Baking Soda

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Also, it might help to point out that I used powdered carbonate, not pre dissolved which promptly formed an insoluble, crystalline mass which sunk to the bottom of the flask. The oily mass formed and clung around it.
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Re: Baking Soda

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Alchemist75 wrote:It didn't feel exactly like and essential oil, it was slippery like a strongly alkaline solution and it washed readily from my skin so it was water soluble but not ethanol soluble.
I wasn't implying that it was an essential oil. What I meant was that while looking into essential oils I learned that steam from plain water carries oils and hundreds and even thousands of compounds that end up in the collection jar. Just because something looks clear doesn't mean that the change cause by carbonate or hydroxide won't cause these things to precipitate.

I get the same fluff (what I call it) even when using dissolved hydroxide. I usually filter out. There is a pic of one example in this thread on chemically treating tails.
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Re: Baking Soda

Post by Alchemist75 »

OK, I misread. Yeah, the chemical make up of the blob at the bottom of the decanter is a little mysterious to me though I know it had a lot of water in it. As to why it adversely affected the flavor may forever be a mystery. Maybe what I'll do is try the same experiment with some cheaply made brandy and see what changes: do a spirit run with and another without.
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Re: Baking Soda

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Ya know, looking at your smurf poo goop makes me wonder if the crusty stuff stuck to the inside of my boiler wasn't some kinda copper complex. I considered that possibility but your results suggest that might be the case. Maybe some complex series of reactions occurred giving my final spirit that hot as hell tail. Goodness only knows how many possible reactions can occur with a mix of organic and inorganic molecules bumping around. One pot synthesis, quite literally
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Re: Baking Soda

Post by Kareltje »

When I decanted my sodaheads I had some rest with the undissolved soda and put it in my freezer. Today I took it out and the fluid was unfrozen, clear and uncolored, but the soda on the bottom was blueish. It had not been in contact with any metal since it came out of the condenser in the previous run!
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Re: Baking Soda

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There must be trace amounts of copper in anything condensed on copper. Maybe not much but perhaps enough to produce that blue color. I know some stills are designed in such a way as to avoid condensing the vapors on copper. A short column packed with copper with a ss condenser coming off the top is intended to alleviate possible copper contamination. Some aspects of my gear can accomplish this as well....
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Re: Baking Soda

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Did my stripping run into a corny key. Ran quite long until only a few percent alcohlol was left. This resulted in about 30% at a ph of 4.6. (Also a fair amount of stinky stuff)

Added about 1 teaspoon of sodium carbonate (pool ph+) that raised the ph to 7.6. (This must be strong stuff?)

This is a 20 inch deep keg with a surface diameter of about 8 inches, with about 16 litres.

After some mixing an amount of blue “scum” formed on the surface. This can be removed with a few strips of paper towel.

I am guessing this is some copper compound that the oils float to the surface. (2”column with marbles and concentric condenser and copper product cooler. No reflux on stripping run)

Waited a couple days and then did the stripping run on the same rig to 94%.

I am also guessing this is a good thing that I got the blue stuff off. (This was actually only a trace amount in 18l of 33%)

Anyone else see this when they add sodium carbonate?


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Re: Baking Soda

Post by Forest Beekeeper »

This is a great conversation to read through.

Thank you so much :)
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