Nooo! Something went wrong

[gualapa]

ok shit something went dead wrong. I'm doing q21q21's tek (I had another thread started for questions before the extraction. I decided I needed a new thread to solve my problem).

The problem occurred during my first pull. I waited about 4.5 hours after adding Mrs. Wages Pickling Lime and it seemed to be dry and crumbly enough. Maybe I didn't wait long enough but I believe it may have been that the mix wasn't hot enough or I didn't use enough base (from reading other threads*** link at bottom of post). See the pictures below for the consistency I had. (I didn't want to upload because I would've had to resize it but I wanted to make sure there was enough detail for you to see the consistency I started out with)

The holes are from me poking with chopsticks for the past 4.5 hours to check the consistency after adding the lime/base:
Picture #1 (With Flash)
Picture #2 (Without Flash)



After I took those pics, here's what I did:
I put the boiling water in the ginormous bottom bowl so that it went to the top level of the jar that I set in the bottom bowl. I added 125 mL of naphtha in the top jar (123g of powder initially)... I stirred for about 20 min.. nothing. All that had happened was the mixture absorbed all the naphtha when I had first poured the solvent in. No separating occurred at all.

Now here's where I royally screwed up: I freaked out and boiled more water, emptied the cold water and put the new boiling water in, thinking I hadn't had hot enough water...I didn't want to add too much naphtha since there was already some in, so I added an amount that was probably around 50-70 mL... don't know what I was thinking. I know I shouldn't have done this, I should've just waited but I had no on-hand advice so I just went for it...

From reading the thread I linked below, Tele said that the tomtom (OP) should boil two batches of water. The first to warm the mixture for about 10 minutes, then dump that water and add another batch of boiling water and add the naphtha. Stir for 30 sec, then cover 5 min, then stir for 30 sec, then stir for another 30 sec, then cover. Then swirl the naphtha and pour it off into precip container.

Am I screwed or can I fix this scenario and get my friend dimitri out of the mix? Did I not add enough base (I used 150g of lime for 123g of powder, also acidified with probably around 200 mL of vinegar but I had to keep adding vinegar so I don't have an exact # for vinegar)? Or was the mixture and naphtha not hot enough? Or, was it the mixture might not have been dry enough to begin with?


*** source for the info I read on someone else who had a similar problem: Q21Q21's Tek stole Swims naphtha - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus

*** Q21Q21's White Fluffy Funfest for reference: Q21Q21's Vinegar/Lime A/B Extraction Tek - DMT-Nexus Wiki

 

[Evariste]

Getting a mixture basic enough with lime can be difficult. It is also thickens the mixture enough until emulsions are a problem. I have made this mistake with caoh and strictly use naoh now(koh would work as well.) I am not familiar with the tek, but I have had little success with lime(bad emulsions and low yields at best.)

Is it wet now or dry? if dry is it crumbly or hard?

If is crumbly I would add more naptha and try to pull like the tek says. I dont think your vinegar could have dropped the ph too much. If you get nothing, then I would abandon to a wet tek(the last thing I describe.)

If it is hard I would try to scrape it out, crush it, add a little water, then add caoh to get it crumbly again.

If it is wet(from vinegar) I would switch to a wet tek; thin out with water(shoot for a consistency between blood and dish soap) and add a strong base. Shouldn't need more than 10g/L, but since we have no idea what the ph is now you may want to get an indicator of some kind. get it thin and basic, then do pulls. (this will take time you could try to dry it back out with caoh, then do pulls, but like I say caoh has just barely the pka needed.)

give me info on how it goes. I hope this helps. It will always be salvageable if you are patient. I have gotten hasty and frustrated and thrown salvageable mix away.

 

[gualapa]

ok, thanks for the advice evariste. I'm gonna cap it and decide what I'll do next tomorrow.

anybody else have any advice as well? I'd like to get multiple people's advice before move on just to make sure adding more lime would work.

I shouldn't have put the lid on, there was condensation on the walls of the jar when I woke up so I took it off and I'm going to let it air out for 2 hours. I'm most likely thinking of doing what evariste said to do-to just put more lime in (another 150g?) and distilled water (regular temp water?) if needed. This time I'll allow it to naturally evaporate. Then I'll do the double boiling water technique that tele described in the thread I found.

As my mix is drying out, it's currently very dark and not dry at all but moist, looks a lot like a jar of dirt. I'm guessing the naphtha needs to still evaporate on its own?

So my questions are:
-Does anyone else have other suggestions or think I should do something else?
-If not, should I just use another 150g of lime, or a smaller amount? (I remember everyone saying that you can't hurt the mix by adding too much lime)
-Also, if I need to use water, should it just be at regular temperature? (I ask because the only time I added water was when the tek called for near-boiling/hot water during acidification (in step 1 right after the vinegar).

 

[Vodsel]

Hi gualapa,

Don't panic.

I don't think you screwed up anything at all. Your goodies are there. According to the pics you posted, I'd say that your mix was simply too dry and it sucked in most of the solvent you poured. But there's nothing wrong with having heated again the mix by placing the container inside of a larger one with boiling water, or whatever. No alkaloids will burn or disappear by warming up the mix.

The amount of lime you added should be enough. The only thing you have to do is to get the mix to the proper consistency. If you were trying consistency two, go by the description - consistency of an apple crisp, or if you want, slightly clumpy soil. To achieve that consistency you simply have to change the water content of the mix. So if it's too dry, just mist or add a little distilled water, small amounts, and keep stirring to distribute it evenly until it looks like it's supposed to look. If it's too wet, just wait for it to evaporate until it achieves the right consistency.

Then you can give it a little warm bath, or warm your solvent a little before pouring it (remember to be careful with any fire sources, if there's still solvent in your mix it will be evaporating slowly and those vapors can ignite) and do the pull.

But reading your post, I think the only problem you have is that you've wasted a little solvent.

 

[gualapa]

Ah Vodsel, perfect person for this topic. I read your approach a few times but decided to stick with q21q21's original tek without your alterations.

Going off what you said, I won't add any more lime like I planned. You're right. The major problem I had was that I, for whatever reason, thought of a dry/almost chunky crumbles of apple crisp not the normal crumbly apple crisp. I definitely dried it way too much.

I placed a siran wrapper on top of the jar and poked large holes all throughout it, merely to insure no flies get into the jar (I have a few flies in my place right now).

I'm going to allow the mix to dry more. The current consistently as best as I can describe it: completely crumbly, no big chunks. It's like a very light soil that feels nearly neutral in regards to moisture and dryness. I have an appointment to attend to but I will be back in two hours, hopefully it doesn't dry too much but if not I'll use your advice.

I could care less about solvent loss, I'm just happy the sacred bark mixture has not gone to waste. Thanks for your reply!

 

[Vodsel]

No worries if it gets too dry, it would be fast and easy to rehydrate it. As a rule of thumb, I'd say it has to be loose, but not too much; with plenty of crispy clumps of the size of a small chickpea. If solvent is not a big concern, no worries. You'll get what you're looking for.

And never mind flies, I heard they don't like very alkaline mixes

 

[HippiePilgrim]

Hi gualapa,

Don't panic.

What a lovely reassuring way to start a post on a thread such as this

 

[gualapa]

gothcya. I'm just glad to have my jar of bark, or jar of dirt as jack sparrow would say haha.

I've a question though. If a solvent is absorbed because the mixture is too dry, what happens to the solvent? Does it slowly evaporate out? I'm just wondering b/c my mixture is very dark colored even 20 hours after the first pull (it had a lid on for about 8 hours so it probably didn't evap as fast over night, assuming I'm correct that it does evap).

What about having to moist a mixture? Would the same thing happen?

What a lovely reassuring way to start a post on a thread such as this

I agree! I applaud you Vodsel

 

[Vodsel]

Don't applaud me for the reassurance, applaud Douglas Adams 8)

The solvent absorbed by the mix will indeed evaporate out slowly. Some of it will stay there for hours, though, specially if the mix was not too dry and particularly if you covered the container with a lid, so don't think about opening it the next day with a cigarette in your lips if you appreciate your eyebrows.

The dark red-brown color is normal and I presume has to do with either exposure to oxygen and/or the cooling of the mix. If you rehydrate and warm up the admixture, once you get your spoon or chopsticks and stir it you will see some of that original greyish tone coming back.

And of course, after you moist the mixture the water will slowly evaporate too, but since water is much less volatile than aliphatic hydrocarbons such as the ones in naphtha, it would take much longer.

 

[gualapa]

okay well it looks like its too moist right now so I'll keep checking on it but at the rate it's going it'll probably take 1 day or 2 (The mixture still smells of the overpowering naphtha smell).

I'm guessing it's fine to just leave it out for days on end?

 

[Vodsel]

There should be no problem with setting it aside for a day or two, people often extend the pulls during the period of a week. Just make sure you leave it in a spot with good ventilation.

Although my bet is it'll be ready in one day or less.

 

[gualapa]

There should be no problem with setting it aside for a day or two, people often extend the pulls during the period of a week. Just make sure you leave it in a spot with good ventilation.

Although my bet is it'll be ready in one day or less.

Ok, thanks.

One more question expert Vodsel

When I do get the right consistency and pour the naphtha in, will it just sink to the bottom of the mixture? Would a good way to see if the naphtha's not absorbed be to just tilt the jar sideways and see if naphtha comes out of the mixture onto the side of the jar? I just wanna know how to gauge how well it's working when I go for my next pull.

Also, when you're doing a pull a week later, I'm guessing you just have to add a little water, stir it up to the right, and go forth with the pull (assuming one doesn't put too much water and make the mix too moist)?

 

[Vodsel]

Yes, and yes.

But most of the pulls can be done in a couple days. Remember to squeeze a little the mix against the bottom after swirling the solvent around before pulling, you will pour it more easily.

And Im no expert, I just had my eyes very open when I did it right...

Good luck

 

[gualapa]

Yes, and yes.

But most of the pulls can be done in a couple days. Remember to squeeze a little the mix against the bottom after swirling the solvent around before pulling, you will pour it more easily.

And Im no expert, I just had my eyes very open when I did it right...

Good luck

Perfect, thanks!

Then I guess I shall call you Vodsel, the experienced. haha

I'll report back to this thread if I run into problems again. If not, I'll start a new thread to report my success. Thanks again!