Volatile Reaction Using Washing Soda

Other discussions for folks new to the wonderful craft of home distilling.

Moderator: Site Moderator

Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Volatile Reaction Using Washing Soda

Post by Avalir »

So I had decided to make an attempt to distill my saved up heads with washing soda to see what the buzz is about. I've tried my best to see if I could find explains to what I was experiencing, but couldn't find answers or stories from people with similar experiences. From everything I read before I tried, seemed like a normal enough thing to do. From what I could tell theres a good number of people that will put it right in the boiler with their low wines/heads/feints and not have any issues, but obviously I am.

So in a 5 gallon charge of heads dilluted to ~30% abv, I added just 1 tablespoon of washing soda. It fizzed for a little bit, then stopped. I then began to run it. It all started fine and dandy, but about a half pint in, I began getting some surging. I figure this may be normal, but the more I ran it, the more violent the surges got. So violent, that aside from shooting out the condenser and hissing, it was even managing to squeeze out from under the lid seal and pour down the side of the boiler. Naturally I turned it off at this point (I have since checked and ran other liquids through it with no issues to verify there's not a leak to cause this).
After it cooled a little and I was confident the ridiculous surging was over, I took the lid off to take a look. Washing soda looked brown in color sitting at the bottom of the pot. I decided to try to make some scientific (sort of) observations. The brown distillate seemed to like to pull towards each other and bunch up. If I briefly turned the heat on it would evaporate decently quick, then precipitate out just as fast when I cut it off.
I poured some more washing soda in to see how it may act, it just kinda moved and bunched up with the brown washing soda precipitate that was already in there.
I then decided to actually boil it (with the lid off) to try to find the cause of the surging. Turned the heat on and of course it readily dissolved. Not to much longer I could see the start of boiling bubbles at the bottom of the pot even though I haven't reached boiling temperatures. Within about a minutes, I have these bubbles starting to rise to the top and as soon as they break the surface, they make a loud bang and rattle the pot.
Can anyone possibly explain what the heck I had managed to make that's reating this violently? All I can think it the washing soda reacted with some ester and/or minerals in there and formed a compound that has a lowish boil point and seems to be volatile when introduced to air/oxygen.
I can't imagine this is a normal occurrence seeing how wildly unsafe it seems when I use it, yet there's lots of people that seem to use it happily with no problems remotely like this they care to talk about.
Any thoughts on what compound formed or what's happening, or maybe someone wanna tell me I'm not the only one that's had this happen?
"I am a man. And I can change. If I want to. I guess." ~Red Green
User avatar
Salt Must Flow
Distiller
Posts: 1921
Joined: Sat Jan 29, 2022 2:06 pm
Location: Wuhan China (Novel Coronavirus Laboratory)

Re: Volatile Reaction Using Washing Soda

Post by Salt Must Flow »

Washing soda/sodium carbonate/soda ash is not the same as baking soda/sodium bicarbonate. You should be using baking soda/sodium bicarbonate. That could be the problem right there. I wouldn't try to understand exactly what happened because exactly that will never happen again.

When I've used baking soda, I drop it directly into the boiler with the diluted low wines right before I fire up the boiler. There's a guy on the Still Dragon forum that did much testing with baking soda and his findings were that you don't have to wait and it works during the boiler's heat up.
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

I do understand they're different. From the readings I had done, people had specified they used washing soda/sodium carbonate. If the people that made these posts were mistaking the name, I couldn't say. I'll probably avoid it from now on, but was definitely curious.

I figured I'd also add my still is 304 stainless, since that's probably relevant for if it was some kind of potential metal reaction. I also didn't take a temperature reading for when it did form these volatile bubbles and for obvious reasons, I don't much care to recreate the experiment to get one.
"I am a man. And I can change. If I want to. I guess." ~Red Green
User avatar
Salt Must Flow
Distiller
Posts: 1921
Joined: Sat Jan 29, 2022 2:06 pm
Location: Wuhan China (Novel Coronavirus Laboratory)

Re: Volatile Reaction Using Washing Soda

Post by Salt Must Flow »

You are absolutely correct. Sorry, my bad. I just tried to pull up my references for baking soda and discovered one link where they mention using either.

I've only ever used baking soda and nothing ever happened. I never waited before running it either. I'm still trying to find that link too.

EDIT: I think this is the link.
Sleighahh
Site Donor
Site Donor
Posts: 22
Joined: Mon Apr 05, 2021 9:26 pm
Location: New Zealand

Re: Volatile Reaction Using Washing Soda

Post by Sleighahh »

Are you sure your washing soda is pure sodium carbonate - does it contain any detergents, soaps, or sodium percarbonate?
User avatar
Demy
Master of Distillation
Posts: 3084
Joined: Fri Sep 04, 2020 1:45 pm

Re: Volatile Reaction Using Washing Soda

Post by Demy »

From my readings on the forum, sodium bicarbonate should act for a few days while the sodium carbonate will act immediately in the boiler ... this is what I have read, I have not delved into the chemistry enough.
User avatar
still_stirrin
Master of Distillation
Posts: 10337
Joined: Tue Mar 18, 2014 7:01 am
Location: where the buffalo roam, and the deer & antelope play

Re: Volatile Reaction Using Washing Soda

Post by still_stirrin »

Demy wrote: Thu May 19, 2022 1:11 pm From my readings on the forum, sodium bicarbonate should act for a few days while the sodium carbonate will act immediately in the boiler ... this is what I have read, I have not delved into the chemistry enough.
The esterfication using the carbonate (base) is catalyzed with heat. So, it is much more active when introduced into the boiler. However, it does not produce CO2 or any other “bubbly” action. It shouldn’t increase the volatility in your boiler at all. If anything, it would raise the boiling point of the boiler charge (slightly).

Perhaps, you were simply putting too much heat into the boiler, especially if the low wines were on the high %ABV side of the ledger. Without doubt, that would make it more volatile, possibly even explosive, compared to other, more conventional spirit runs.

But, the question remains … “what was actually in the washing soda” you added? It quite possibly did contain other “stuff”, ie - detergents, or otherwise. I don’t think I would want to add that to my spirits.
ss
My LM/VM & Potstill: My build thread
My Cadco hotplate modification thread: Hotplate Build
My stock pot gin still: stock pot potstill
My 5-grain Bourbon recipe: Special K
zapata
Distiller
Posts: 1664
Joined: Fri Jul 07, 2017 1:06 pm

Re: Volatile Reaction Using Washing Soda

Post by zapata »

I've used washing soda and not experienced anything similar.

Did you mention heat source? Not that I have an answer, just trying to think through it all with you.
User avatar
Yummyrum
Global moderator
Posts: 7653
Joined: Sat Jul 06, 2013 2:23 am
Location: Fraser Coast QLD Aussie

Re: Volatile Reaction Using Washing Soda

Post by Yummyrum »

Demy wrote: Thu May 19, 2022 1:11 pm From my readings on the forum, sodium bicarbonate should act for a few days while the sodium carbonate will act immediately in the boiler ... this is what I have read, I have not delved into the chemistry enough.
Thats how I’ve always understood it too Demy .
Washing Soda ( Sodium Carbonate ) is done in five minutes,
Bi-Carb Soda ( Sodium hydrogen Carbonate ) takes several days to a week to do it’s job .

Anyway , only done it once with Washing soda and can’t say I noticed much , but it was back in my early days when my senses were not so sharp .
Regardless , was no big froth up like OP .
bluc
Site Donor
Site Donor
Posts: 437
Joined: Thu Nov 12, 2015 12:32 am

Re: Volatile Reaction Using Washing Soda

Post by bluc »

Is it just a base neutralizing acids to stop esters forming?
User avatar
Demy
Master of Distillation
Posts: 3084
Joined: Fri Sep 04, 2020 1:45 pm

Re: Volatile Reaction Using Washing Soda

Post by Demy »

bluc wrote: Fri May 20, 2022 2:29 am Is it just a base neutralizing acids to stop esters forming?
From what I know yes, the precursors are somehow prevented from interacting by forming esters, so neutralizing the acids should slow down the reaction.
Anyway, that "fizzy" reaction is not normal, I suspect like others that the product used by the OP contains other ingredients
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

The box of washing soda claims the only ingredient to be sodium carbonate (and water, not so sure that matters--was a powder), so I'm guessing they're full of crap. Was using arm and hammer brand.
"I am a man. And I can change. If I want to. I guess." ~Red Green
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

Either way, I'll probably stay clear of additives in the boiler after this. Probably just stick to my good ol reflux, aquarium charcoal, reflux again for the heads.
But others may want to avoid the arm and hammer washing soda.
"I am a man. And I can change. If I want to. I guess." ~Red Green
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

My best guess at this time is I may have been lied to about what metal my stainless is. Claimed to be 304, but I believe made in China, so take that with a grain of salt. First issue I've ever had with it though.
"I am a man. And I can change. If I want to. I guess." ~Red Green
NormandieStill
Site Donor
Site Donor
Posts: 1738
Joined: Wed Dec 30, 2020 10:17 pm
Location: Northwest France

Re: Volatile Reaction Using Washing Soda

Post by NormandieStill »

It could be something as simple as the crystals providing a nucleation site for boiling. I've found that exceptionally clear washes in my keg boiler will boil explosively at times due to (I assume) the surface quality not providing enough nucleation sites. Once a rolling boil is established there's no further popping noises.
"I have a potstill that smears like a fresh plowed coon on the highway" - Jimbo

A little spoon feeding *For New & Novice Distillers
User avatar
Salt Must Flow
Distiller
Posts: 1921
Joined: Sat Jan 29, 2022 2:06 pm
Location: Wuhan China (Novel Coronavirus Laboratory)

Re: Volatile Reaction Using Washing Soda

Post by Salt Must Flow »

Avalir, your original post reminded me of a time when I heated water in a big aluminum pot and added calcium hydroxide (hydrated lime). It violently foamed and made a mess. At the time I didn't realize that caustic base materials react with aluminum. I'm not claiming your boiler contains aluminum, but if you wanted to do a simple test, you could add Baking Soda/sodium bicarbonate to water, heat it up and watch to see if anything happens. If nothing happens then something else was likely the cause. This test could also put your mind at ease about your boiler potentially being the culprit.
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

Salt Must Flow wrote: Fri May 20, 2022 5:07 am Avalir, your original post reminded me of a time when I heated water in a big aluminum pot and added calcium hydroxide (hydrated lime). It violently foamed and made a mess. At the time I didn't realize that caustic base materials react with aluminum. I'm not claiming your boiler contains aluminum, but if you wanted to do a simple test, you could add Baking Soda/sodium bicarbonate to water, heat it up and watch to see if anything happens. If nothing happens then something else was likely the cause. This test could also put your mind at ease about your boiler potentially being the culprit.
Not a bad idea. If not the boiler itself, I don't know how they went about their welds. Works really well just running my washes and low wines, but it's definitely possible aluminum or other metals were involved in the manufacturing.
"I am a man. And I can change. If I want to. I guess." ~Red Green
zapata
Distiller
Posts: 1664
Joined: Fri Jul 07, 2017 1:06 pm

Re: Volatile Reaction Using Washing Soda

Post by zapata »

Arm and Hammer is the brand I have repeatedly used, both for this purpose as well as other chemistry related purposes. I have always found their washing soda, as well as their other products to be reliably pure. The water is "water of crystallization" and is an essential thing that makes washing soda washing soda, as opposed to other forms of sodium carbonate with fewer molecules of water in the crystal structure.

In the chemistry world this problem is called "bumping". IME it is rare on solutions that are or recently were foaming, and more nucleation sites should reduce it, not cause it.

An interesting test would be to see how the saturated solution with no solids behaves. There should be more than enough in solution to keep esters from forming and it would at least eliminate pot compatibility and quite a few potential explanations.

I think this would be a great thing to post over at www.sciencemadness.org/whisper/ and see if any of the chemists have any thoughts. Please link here if you do.
ThomasBrewer
Swill Maker
Posts: 233
Joined: Wed Dec 02, 2020 9:24 pm

Re: Volatile Reaction Using Washing Soda

Post by ThomasBrewer »

Definitely weird, especially with the loud pops you referred to. It could be nucleated boiling, followed by the violent collapse of the vapor bubble as it cooled outside the heated zone, but that is just a WAG.

The fizzing is also weird. Usually the carbonate is added to low wines from a stripping run, which wouldn't contain any free acids to neutralize. Don't add it to the wash.

Edit: I re-read and see that you added it to a feints run. There really shouldn't be any free acidity. That is puzzling for sure. Maybe your heads started turning to vinegar? So many weird questions.
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

Really hard to say. I'll generally store heads seporate from tails. Heads I reflux and tails I toss in the pot still. Both are stored in sealed glass jugs, usually for at least a couple months, in this case a quarter of the heads were fresh. All of the heads still smelled the same as fresh off the still, but never bothered taking a ph meter to it or any distillate for that matter.
I do recall the boiling bubbles being dramatically larger than you'd normally expect from boiling anything. Anywhere from quarter size to nearly the size of the boiler near of shortly after it began boiling. Odor was like hand sanitizer, but that's probably because hand sanitizer is just these same reject alcohols/denatured alcohol. Either way, whatever reaction, chain of reactions is definitely not safe if it builds to pressures that causes spills out of a leak-free boiler (it did combust with my heat source, so either high proof alcohol or highly flammable compound of sorts).
I'm probably gonna discontinue trying to solve the logistics of what happened and not revisit adding sodas to the boiler until I build my own rig and can be certain of materials and welding process, and maybe not even then because I wasn't much of a fan of the idea of salts in the boiler regardless.
"I am a man. And I can change. If I want to. I guess." ~Red Green
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

If nothing else, I hope that my experience may at least act as a warning to anyone else that may have a problem like this before they start a fire or hurt themselves. I'm definitely leaning towards the impurities from a questionable manufacturer as the likely culprit. But if anyone has this problem, I'd say to stop and that running your rig with baking soda or washing soda is not a good or safe thing to do with your equipment.
"I am a man. And I can change. If I want to. I guess." ~Red Green
User avatar
NZChris
Master of Distillation
Posts: 13062
Joined: Tue Apr 23, 2013 2:42 am
Location: New Zealand

Re: Volatile Reaction Using Washing Soda

Post by NZChris »

Check the pH.

If you're experimenting with adjusting the pH of anything to do with distilling, check it and keep records to refer back to. You don't need a meter for the accuracy you need for this type of experiment, strips will do.

I've got a grape feints experiment waiting for me to get around to running it. The pH was about 8 last time I adjusted it with slaked lime, but I'll check it again before I run it.
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

A thought I just had... I'll sometimes clean my equipment with a citric acid solution. Though it's thoroughly washed and rinsed afterwards. But if there were somehow some residual citric acid left, I suppose that could account for the fizzing when sodium carbonate is added. However the creation and presence of sodium citrate wouldn't explain the volatility.
"I am a man. And I can change. If I want to. I guess." ~Red Green
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

I just got around to examining the little bit of distillate I collected before things went horribly wrong and I dumped the boiler. Only collected two jars (3/4 full pint jars) and I will say the second jar collected, despite my surging still pouring into it, smells pretty darn clean. Put a couple drops to my tounge and there was no urge to vomit or chemical burn; the first jar even smelled only mildly offensive (I discard first pint off pot still spirit runs as foreshots and not worth my time to salvage heads). So I am at the very least impressed by how well it broke up the esters and gave me a clean spirit before it went horribly wrong--kinda makes me more sad that I had to dump the whole boiler. I've never had that clean of distillate that early on without adding something to the boiler for my heads run. Maybe it could be worth my time to try to investigate... or maybe I should just go ahead and start planning to upgrade my rig early since I'm still thinking it's likely a matter of impurities in my boiler.
"I am a man. And I can change. If I want to. I guess." ~Red Green
User avatar
NZChris
Master of Distillation
Posts: 13062
Joined: Tue Apr 23, 2013 2:42 am
Location: New Zealand

Re: Volatile Reaction Using Washing Soda

Post by NZChris »

That makes it sound like you were giving it too much heat and gave up too soon. Dumping the charge without keeping a sample doesn't help as you can't investigate what was in it, wrong with it, etc..
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

I had also let it rest and cool back down to room temp before attempting again with the surging beginning right away... won't fully dismiss that thought though, I recently moved and this is the first I've done this on a gas range, so it may be possible I just brought the heat up too quick.
"I am a man. And I can change. If I want to. I guess." ~Red Green
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

As a test, maybe I'll attempt to distill some water with washing soda, or maybe baking soda, in the pot. Can check for unwarranted fizzing and see if I have any out of the ordinary surging. Can also get a better feel for the range vs the the old electric I was familiar with without risking wasting a whole load or have to worry about combustible vapors or liquids spewing out.
"I am a man. And I can change. If I want to. I guess." ~Red Green
User avatar
NZChris
Master of Distillation
Posts: 13062
Joined: Tue Apr 23, 2013 2:42 am
Location: New Zealand

Re: Volatile Reaction Using Washing Soda

Post by NZChris »

If you have any feints, you could put them in too. My pH adjusted experiments have been using heads and tails and I've I had promising results without any scary reactions.
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

Well, looks like I'm in the market to upgrade my rig... I don't know how, but the lady knocked down the boiler and apparently hit the ground just right to bend like hell. I made a short attempt to bend it back into a shape that the lid could fit and seal, but honestly it felt almost brittle and like it would break before it would bend back. I feel like brittle feeling "stainless" and the fact it even managed to bend the extent it did may support the impurities theory.
Oh well, I'll call it divine intervention. I'm past due for an upgrade and would have drove myself mad trying to figure out what was happening with that. Gonna start the search so I can get back to it. No more 5 gallon runs for this guy, gonna look at 10-15 gallon options. Can also ensure this time that I trust the source and material.
"I am a man. And I can change. If I want to. I guess." ~Red Green
Avalir
Swill Maker
Posts: 224
Joined: Sun Jan 31, 2021 3:26 am

Re: Volatile Reaction Using Washing Soda

Post by Avalir »

Should be getting a nice 60L stainless milk can and a 2" bulkhead to fit it with so I can continue to utilize my columns and condensers. Goodbye 5 gallon capacity and questionable Chinese manufactured alloys. It may take a little while to get everything together, but I fully plan to revisit the washing soda on my new rig once I get a stockpile of heads and/or feints saved up. I'm sure it'll go better this time around and I'll try to remember to report back... I should also probably get some 30+ gallon fermentation barrels if I'm making that kind of jump in still size.
"I am a man. And I can change. If I want to. I guess." ~Red Green
Post Reply