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2nd extraction attempt, help please! Options
 
dodgemalodge
#1 Posted : 2/23/2012 4:15:50 PM
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Hi Guys,

This is my second attempt at an extraction.

I have earlier on mixed 100g of lye with 1.5l water and shaken until it all dissolved. I have then added 100g of mhrb powder and shaken the bejesus out of the glass jar I am using. It has been left still for 2 and a half hours.

I have just added 50ml of heated naptha to the mixture. I have then gently rolled the jar on the floor for 2 minutes.

I have then waited another roughly 5 minutes and can see a very thin layer (roughly 3mm) of naptha near the top but on top of it is another layer of the black gunk stuff (roughly 2mm) on top of that.

I have tried gently pouring off, I have tried using a syringe but I'm really struggling to get the naptha out :-(

This other black layer on top? Is that an emulsion? Should it be there or is that my problem?

Help please, I'm not sure how to tackle this.
 

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dodgemalodge
#2 Posted : 2/23/2012 4:29:20 PM
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I have images but cannot see how to insert them either, sorry. I f someone could tell me I'll post what it looks like.
dodgemalodge attached the following image(s):
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DSC01049.JPG (2,780kb) downloaded 159 time(s).
 
tony
#3 Posted : 2/23/2012 4:32:15 PM

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I'm not familiar with exactly what tek you are doing, I only use a 5th of that amount of water and I don't use heated naphtha... but whatever tek you are doing the two layers should be completely separate before you try to remove the naphtha. You don't want to pull *any* of the black layer out when you are removing the naphtha. I think you just need to leave it sitting for a while to let the layers separate then get the naphtha out with your syringe.

EDIT: From looking at your pictures, are you sure there is a thin layer on top... cos that just looks like a trick of the light to me. You'll have difficulty getting such a small amount of naphtha out of such a wide container IMO.
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dodgemalodge
#4 Posted : 2/23/2012 4:35:40 PM
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Seems I figured the photo's out at least. Thank you Phog, I know I definitely don't want any of the black layer, it just seems so difficult to get just the naptha! I think I need a taller, much more narrow bottle but I am still concerned. This layer doesn't seem to going anywhere it's just floating on the top.
 
Global
#5 Posted : 2/23/2012 4:38:26 PM

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I agree with PhOG that you'll probably have to just wait a little for it to settle itself out. I don't use this tek, but when I mix the naptha with my basified bark, I mix the naptha for at least 30 min to make sure I've got everything. The problem you're having is one of the big reasons I don't use a tek with lye in it. I tried it once, was successful, but man was it a pain. You'd be much better off in the future trying out Q21Q21's lime/vinegar dry tek. You won't have to worry about this problem of separation. You'll be separating solids (or semi-solids anyway) from the naptha, and worse comes to worse, you just use a coffee filter and only the naptha will get through without any sediment to worry about.
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dodgemalodge
#6 Posted : 2/23/2012 4:43:20 PM
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Many thanks for the advice Global, I may well try that next time. It's also invaluable advice to know to mix it for longer. Best bit is, PhOG is right, I just dipped a stick into the top of the mixture and it came out with no black on it so it must be a trick of the light. It sure does look convincing!

Currently looking for a more suitable container to transfer the mixture.
 
tony
#7 Posted : 2/23/2012 4:45:21 PM

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Here is a pic of my last extraction, plus a pic of what came out of it when I finally pulled out the solvent and evaporated it. I wasn't doing the same way as you though, I left the solvent in it for like 2/3 weeks at room temperature (xylene, not naphtha). But yeah, as you can see the container I'm using makes for much easier removal of solvent, and to get every last drop of solvent I filled it with more water causing the last little bit of the solvent layer to go right up to the neck of the bottle where I could get it even easier.
tony attached the following image(s):
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dodgemalodge
#8 Posted : 2/23/2012 4:51:44 PM
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That's very interesting PhOG, which Tek is that? I'm not sure whether I can get xylene in the uk. Yeah, I've totally chosen the wrong type of container. Struggling to find something else suitable, though I guess it can wait?

Does anyone know if PET plastic bottles are safe? I know HDPE is but don't have any at the moment.
 
tony
#9 Posted : 2/23/2012 5:02:24 PM

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Yeah man you can get xylene from ebay, I'm in Scotland and had no problem getting it. Very cheap, but it stinks. It's not a particular tek I'm using. I started out following a different tek using naphtha, then bought xylene to try and pull some jungle dmt... then decided it's easier to just use xylene for the whole thing since xylene doesn't need heated (I'm poor, heating is out of my price range just now Laughing ).

My tek is:

Get a 1 litre milk jug. Add 600ml of water and add 100g of lye. Let it dissolve then add 100g of mimosa. Shake it like crazy. Leave it sitting for a day and then add xylene (I don't use a particular amount, I just pour a load in). Leave it sitting for a couple of weeks, shaking it every time I remember (basically every time I go into the kitchen I give it a shake) and then pull out the xylene with a syringe and let it evaporate.
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dodgemalodge
#10 Posted : 2/23/2012 5:14:39 PM
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Excellent food for thought mate. I may well give that a go next time. And buying my solvent off ebay is much more preferable to looking like I've got a serious problem keep buying cans of lighter fluid in large numbers from poundland!Rolling eyes

I particularly like the idea of taking one's time over these things. My first extraction was a bit of a cock up really and was 9 and a half hours of pure hell through lack of proper pre planning and allowing myself the space and time. It seems I'm missing / getting wromg the most obvious of things (like the dimensions of my container!) but I will get there. We've all got to start somewhere.

Got 1.5g's of yellowy powdery crystals from 150g of MHRB from my first extraction but haven't properly sampled it yet as I'm not convinced it's clean enough so going to re crystalise it first.

Just wanted to have another go as I have improved some of my equipment, though obviously not enough!Embarrased

Many thanks Smile
 
Electric Kool-Aid
#11 Posted : 2/23/2012 6:20:07 PM

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So what I see here from your STB is your jar is too large. You need a smaller jar. The smaller jar will help keep the liquid level up and increase the depth of the solvent you need to pull. Thus making it easier if you have say a half inch of liquid rather than 1/4 inch (3 cm rather than 1cm) type thing. Also suck up the liquid with an eye dropper, not a baster if your solvent is shallow. Also place the dropper on the side of the glass where he water retention is, this way it won't suck up any base mix. Also another thing, I leave my solvent in for 12-24 hours rolling every now and then, then let sit for at lease 2-3 hours or more to settle after rolling. Then do your pull and put more solution in the jar. Then stick the pull in the freezer for 12-24 hours, drain off solvent, put dish upside down with bottle cap tipping up one side. Come back in 2 hours and take out of freezer, seal container and let it heat up to room temp. 1hour later (30min) and open, scrape... Smoalk!

Edit: this was for naptha pulls... Oops!
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dodgemalodge
#12 Posted : 2/23/2012 7:25:41 PM
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Thank you Electric Kool-Aid,and indeed this whole community.

I was so frightened to ask such stupid questions but already things are becoming so much clearer thanks to your help.

I have transferred the solution to a more suitable container and managed to siphon off 35mls of the original 50mls of naptha which is currently residing in a small flat ceramic dish at room temp with a piece of paper covering it. I plan to transfer it to the fridge in another hour or so, then after a couple more hours the freezer.

I have just added another 50mls of heated naptha to the solution which itself is in a heat bath.

I was planning on doing another pull as soon as I can see the layer but will definitely follow your advice on the next pulls and wait longer.

I've just been using a 10ml syringe (instead of the massive 50ml one I thought would be helpful) but I reckon the eye dropper will be much easier and should free up one hand making it much easier.

Just to check, when you said "I leave my solvent in for 12-24 hours rolling every now and then, then let sit for at lease 2-3 hours or more to settle after rolling. Then do your pull and put more solution in the jar." I take it you mean do your pull then add more solution for the next one? Not add more solution during the pull? I think that is another stupid question but would rather ask.

One other question, is the heat bath really necessary? I'm getting mixed signals. I guess that's for people trying to do a "quick job" but if you just leave it longer the same or better effect can be achieved regardless of heat?

Thank you for making this so much clearer for me. I've been reading for months yet still somehow obviously hadn't quite got it.

Huge respect to you guys,

Dodge Smile
 
tony
#13 Posted : 2/23/2012 7:39:45 PM

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dodgemalodge wrote:


One other question, is the heat bath really necessary? I'm getting mixed signals. I guess that's for people trying to do a "quick job" but if you just leave it longer the same or better effect can be achieved regardless of heat?



For naphtha heat is required. DMT is not really soluble in naphtha at room temp. Other solvents like xylene and d-limo can dissolve DMT at room temp and so require no heat.
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Electric Kool-Aid
#14 Posted : 2/23/2012 8:21:18 PM

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Correct. 1st pull, then put that pull aside and add additional naphtha for the next pull in to the main mix. Roll that around and wait a few hours and pull. I found 12 - 24 hours best. But I am no pro. Heat baths might speed things up. I have heard that the heat bath can be used for later pulls. But again I am not a pro. I read about it an did my extraction, plus tried methods mentioned like small dropper for easy pulls. Good luck!
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dodgemalodge
#15 Posted : 2/23/2012 9:33:23 PM
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Thank you both for your replies.

I get what both of you are saying but am confused at the conflict of heat?

PhOG you are saying that heat is necessary for the naptha to take on the spice but Electric Kool-Aid if I am not wrong, you are saying that you use naptha but leave it for a long time so I am guessing you do not use heat or do you keep heating the mixture as and when you can whilst also agitating it?

Thank you for your patience Rolling eyes
 
Electric Kool-Aid
#16 Posted : 2/23/2012 10:29:22 PM

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2 methods
1) Heat agitate (roll) and pull = fast method
2) Agitate (roll) every now and then, let sit for around 12 hours then pull. = long method but lots of spice comes out.

No method is better or worse. Try it with one pull heated and another waiting. Compare.

Cheers!
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dodgemalodge
#17 Posted : 2/24/2012 12:37:14 AM
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Thank you for clarifying that Electric, that's exactly the course I'm planning on taking now. The first pull having moved out of the fridge already looks quite interesting and now it's covered up in the freezer.

If it doesn't turn out to be an embarrassment I'll post pics!Laughing

Cheers,

Dodge.
 
dodgemalodge
#18 Posted : 2/24/2012 12:15:42 PM
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Well I guess this has to be a success?
First pull from last night.

Not much of a yield at 0.25g but I reckon there's a few pulls left in there yet!

Just out of interest, what is it meant to smell like? It doesn't smell of solvent or anything, more like a slightly plastic / fish smell that I can't quite place. To be fair it smells pretty much like the mixture did from the moment I added the MHRB, though not so strongly. Is this ok?
dodgemalodge attached the following image(s):
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voodoobutter
#19 Posted : 2/24/2012 6:13:40 PM
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Looks yummy! 0.25g from from your first pull isn't bad. Just keep at it until nothing percips on your dish!
 
dodgemalodge
#20 Posted : 2/24/2012 7:34:34 PM
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Thank you Voodoobutter :-)
 
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