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Ice bath for basification Options
 
Gwn
#1 Posted : 5/19/2017 9:09:58 AM

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During my ACRB extraction I utilized an ice bath to temper the exothermic reaction during basification. I'm surprised I have not seen this suggested in any of the teks I've read. I know there is some risk of the jar breaking, but I don't feel it's that significant with a high quality canning jar.

Does anyone have experience with performing this step as well? Has anyone broken a jar using this method?
 

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cyb
#2 Posted : 5/19/2017 10:48:33 AM

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Extreme heating of glass and then rapid cooling ... is not a good idea.
Glass can handle the temp if it's thick enough...it's how they are cleaned in the manufacturing process.
We try to reduce All risks to a minimum here. Wink
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pitubo
#3 Posted : 5/19/2017 11:49:20 AM

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In one word: DON'T.

This is a real safety issue. I have had the bottom of a flask falling out from dissolving lye in it while holding it in a bucket of fast moving water. Luckily, the bucket served to contain the hot concentrated lye spill (and of course I was wearing safety glasses and gloves). Since then, I dissolve lye in a tall slender stainless steel pan. If you must use glass, at least use a glass coffee or tea pot. These are made from thin borosilicate glass, the same glass that laboratory beakers are made from. Some pots even have a "Schott Duran" logo.

Always use a secondary spill container, eg. a bucket. Not only while dissolving lye, but also to hold the extraction container. Put the extraction container in a sturdy plastic bag while you are shaking the layers. If an accident happens, it will be largely contained instead of splashing over the tapestry and your clothes (or even you).

Besides the safety issue, it is a bad idea anyway to dissolve the lye directly into the plant sludge. The dissolving lye creates local pockets of superheated and very strong lye solution. These are incredibly corrosive and their effects on the plants and molecules has a negative effect on the quality of your extract. My experience is that using pre-made lye solutions gives a much cleaner end product.

cyb wrote:
Glass can handle the temp if it's thick enough...

AFAIK, actually glass is better able to withstand temperature gradients if it is thin. As an illustration, the only thick laboratory glassware are vacuum filtration flasks and vacuum dessicators, and those are not intended for temperature gradients, only pressure gradients.
 
Jees
#4 Posted : 5/19/2017 3:52:20 PM

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pitubo wrote:
...it is a bad idea anyway to dissolve the lye directly into the plant sludge...
Very true! Yet we miss details, Gwn could be pointing to an exothermic reaction from just pouring an already liquid base in a liquid acid. Gwn will tell us if it was solid base or liquid base Pleased
 
Gwn
#5 Posted : 5/19/2017 6:08:40 PM

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If I told you that I made an aqueous solution it would be a lie. I will certainly take this information to improve my technique in the future. I did have PPE, secondary containment, and acetic acid for neutralization. The tek I was using did not specify aqueous, and I wanted to be as accurate as possible.

cyb - it was not extreme heating then cooling, the reaction vessel remained in the ice bath for the duration of mixing. Reaction temperature did not rise beyond 60degC.

I'm quite disappointed with the prospect of reduced quality due to my addition of solid sodium hydroxide. Thank you for all the information.
 
pitubo
#6 Posted : 5/19/2017 7:25:45 PM

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Jees wrote:
Gwn could be pointing to an exothermic reaction from just pouring an already liquid base in a liquid acid. Gwn will tell us if it was solid base or liquid base Pleased

Oh, that's true. But since I so often see reports here of people who mix solid lye in with the plant sludge during stb teks, I assumed this was happening here as well.

Gwn wrote:
I did have PPE, secondary containment, and acetic acid for neutralization.

Very good! By no means did I intend to doubt your general safety practices. I just like to spell it out again and again when discussing the use of lye. Not everyone is aware of the risks and of the simple measures that can be used to prepare for accidents. Many people will read these postings and perhaps some will pick up a few tricks.
 
Jees
#7 Posted : 5/19/2017 8:51:10 PM

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Your intuition proved right pitubo.

Gwn I think ice cooling might lower temperature indeed but still be unable to counter the small local heat pockets around the 'melting' hard lye, as mentioned. And also unable to counter the extreme chemical conditions in those pockets. So it might be a kind of harm reduction philosophy but not preventing the harm from existing at all. The making of a lye solution in advance in a metal pot then let cooling down, only then add to the acid brew, then there's no such a harm to deal with from the start.
Breugel made a good picture about it, how it might feel for your dearest brew when pouring in hard lye:


 
Gwn
#8 Posted : 5/20/2017 6:32:16 PM

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Hahaha that's quite the visual! Aqueous it is from now on!
 
downwardsfromzero
#9 Posted : 5/21/2017 10:04:20 PM

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pitubo wrote:
I dissolve lye in a tall slender stainless steel pan

Asparagus pans can be had for a fairly good price this time of year. That little stainless steel basket also seems useful.

Never thought of dissolving lye in my asparagus pan, though! I even ended up cooking asparagus in it. Let's face it, it's fairly rare that I end up using any kitchen item for it's designed purpose - but asparagus is Drool

Large stainless steel pans also make good containment vessels if there's a risk of glass jars fracturing. Which there always is.




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