Any idea what may have happened?

[EzekielCain]

Hope endless sees this

So I'm still in the process of my big extraction and have put in about half a pint of already yellow naphtha plus a bit of new naphtha to my big jar and after rotating, swirling around and leaving it sit for a day, I noticed a LOT of my solvent has straight up disappeared.

Is it possible it just hasn't found its way back to the top yet? There is some solvent on top but not near as much as I put in. I added a bit more water and rotated again but so far its not coming back to the top...

Any ideas as to where it went to? :surprised

 

[Compound37]

You did leave the jar closed right? Naptha evaporates rather quickly.

Other than that, probably still separating out. Do you notice bubbles or an emulsion below the naptha but on top of the basified mimosa? This could mean you were a little too vigorous in your turning shaking etc when adding the naptha.

 

[۩]

Add more base and let it sit overnight see if it clears up.

And when you are using jars, it's better to use some aluminum foil with a rubber band or something tight than to use the actual lids, as they contain rubber seals, and aromatic hydrocarbons are basically rubber sealant removers.

 

[DMT777]

Try adding more lye and or non-iodized salt. A heat bath may also help. Ive had this happen a couple of times, adding a lot of salt helped it separate.

 

[EzekielCain]

No bubbles or emulsions at all. There IS a layer on top, but not as much as went in.

Jar remains sealed.

No, haven't wrapped an extra wrap around the top. I'll give that a go after I add some non iodized salt to the mix. I just thought it was funny not seeing much more solvent. So far my pulls have been exceptional.

live and learn!

 

[Noman]

What tek are you using?
It's hard to say what happened when we don't know what you did.
If it's an STB, chances are that your naptha is stuck in the bark.
You need to let the mix sit for awhile so that the bark is saturated with the lye/water solution. Otherwise, the naptha soaks into the bark and won't separate.
It could also be the problem that happens with STB's when not enough water is used.
In either case, add more water. Salt might help, it certainly won't hurt. If you used enough lye in the first place, adding more won't do anything.
Post back with your procedure, and we'll be able to help more.

 

[EzekielCain]

Thanks Noman!

As crazy as it sounds I'm not using a tek. :?

I did my first 100g test extraction using your tek and through my own rushing botched it up, so I started over again with a bigger glass container and my own common sense and weighed nothing but the bark powder and the lye. My last few pulls I did when "something" told me it was ready...

I'm just being more patient and attentive and going by the look, consistency and smell. When my solvent is good and yellow I pull it out and put it into a pyrex brownie dish and evap it in front of a fan in an industrial fridge at 34 degrees until a noticeable amount has evapped and its a milky yellow and stringy white clouds form when blowing on it. Then it goes uncovered in a walkin freezer at -10 for 24 hours until very little or no solvent remains and then it does another air evap after I scrape the product up and let the few drops of that solvent evap as well.

 

[Noman]

Well you ARE using a tek - an STB tek.
You need to post your procedures so we can better help you out.
More water will probably do the trick - if the naptha soaked into your bark, you may have to go to some lengths to get it back out.

 

[EzekielCain]

I've got some pics up in the "yellowish yield" thread.

I don't so much have a problem getting product but this disappearing solvent has me thrown...

I use pre-powdered bark, it's very fine with just a little coarse fibrous material. I've taken great care in the mixing thoroughly before and after basing and gotten product before.

I'm getting ready to pull what I've got in the next few mins... I'll grab some pics and show you everything.

 

[Noman]

Quantities! Ratios! Procedures!
That's the info we need.
Your problem is very likely not enough water.
Was the bark at the top of the aqueous or the bottom before you added the naptha?

 

[EzekielCain]

Well THIS is totally phucked.....


I got water boiling and down to 160 degrees.

I poured some non-iodized salt into the jar and proceeded to put the jar into the hot water bath when I heard a *crack*

I go to my jar and lift it...the bottom falls right out and my entire mixture dumps right into the goddamn hot water bath!!!

I quickly grab a strainer and a large pot and dump the boiling mixture into the strainer to get the intact glass bottom from the jar.

I'm pissed as hell at this point until I notice the mixture bubbling and spittin' and I notice there's a SHIT ton of solvent appearing from the nether-regions of the mix. I grab my baster and salvage 2 pint mason jars of EXTREMELY golden yellow solvent and accept my loss of the bark since I have NO other container to funnel the boiling hot mixture into, even though it's still rapidly producing solvent from below....

*sigh* I have no idea why this sturdy, thick glass jar's bottom just busted right out of it, but the hot water it went into caused this thermonuclear war and was dumping gobs of naphtha out (the missing solvent!)

So that's all I've got left. I'm friggin' pissed off cuz I was going to try and get at least 6 pulls done off this huge batch. :thumb_dow :x

What's the BEST glass to use, anyway? This sucker should have lasted the Apocalypse!


And Noman: After I tried being meticulous in my process only to have melting product, I didn't measure anything at all except the 378g of MHRB and lye. It sounds crazy but all the grams of product I have thus far are a result of not really following a tek at all but just watching what the mix has been doing and what it looks/smells like and what my solvent looks like. Doesn't matter now anyway since it's all gone except what I managed to siphon from the pot.

 

[mush_mage]

From what I've read here all is not lost. Once you've removed the solvent from the broken glass hot water bath mix you can still recover the dmt. It might take a bit more lye and reducing but the goods are still in there. Simply add more solvent, mix and extract.

I once spilled a gram of dmt that was suspended in solvent in a shot glass all over the bench. I screamed a string of obscenities and then grabbed the closest thing to me which was a paper towel and soaked it all up. I knew I had a paper towel full of dmt so I extracted it again and hey presto I ended up with 900mg or so.

Never throw away anything!

 

[EzekielCain]

I got quite a bit of the bubbling dark yellow solvent but alas, I had to cut my ties and take the loss since I had no other container to move it into. *insert the cries of a thousand babies*

Now I've got to order more (doing shredded this time) bark and try to find a sturdy glass vessel to start all over again.

I'm grateful I got what I did but sooooooooo pissed off that I had to dump the batch when there was obviously so much more solvent coming out on top of the mix. I just can't believe it cracked before my eyes and there it went....

 

[Noman]

I notice there's a SHIT ton of solvent appearing from the nether-regions of the mix.

the hot water it went into caused this thermonuclear war and was dumping gobs of naphtha out (the missing solvent!)

I told you that adding water was the way to fix it.:lol:
I'd have gone about it a different way myself though.

Count yourself lucky that the vessel with the hot water was big enough to hold everything - you could be in the hospital right now explaining to the cops what you were doing with that much lye and naptha.

Use more water next time and don't put cold untreated glass in hot water, no matter how heavy duty you think it is.

 

[EzekielCain]

For sure!

Best thing to use is a wine carboy?

Yeah, its unfortunate what happened but I'll chalk it up as a learning experience and do it differently next time. I'm fortunate there wasn't an explosive reaction that left me blind and I still managed to save a ton of solvent in addition to the product that's already been successfully extracted.

I've got enough to last me for quite awhile.

So what's the best and most low risk glass to use with little to no chance of breaking?

 

[Noman]

Lab glass.
A wine carboy won't work either.
But if you're doing your extraction right, there is no reason to have to heat it beyond hot tap water anyway.
If you insist on doing large quantity extractions, you should consider an A/B.

 

[EzekielCain]

Will do, Noman.

I was going to try an a/b next round anyway to be able to compare the 2 and see what's most effective for me.


Looks like it's time to start researching lab glass!


Something like this maybe? 1 Gal Amber Glass Jugs w/ Black Phenolic Cone Lined Caps


I'm not really finding "lab glass" in gallon size jars. Well, I should say...not that I'm going to spend $700 on.

 

[EzekielCain]

Any thoughts/ suggestions noman?

I highly regard the advice of a professional of your caliber!

 

[Noman]

Yeah yeah yeah.
My advice was that if you do your extraction properly, there is no need to heat the solution beyond a hot tap water bath and to use an A/B for large quantities.

 

[EzekielCain]

Noted.

I'll start over again in a few weeks and try the a/b to see if that makes it any easier. I'm not looking for shortcuts, just properly doing it the first time...