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Offlineneuro
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Interesting observation.
    #2869773 - 07/08/04 08:03 PM (12 years, 4 months ago)

Okay, so I'm in the middle of a mimosa hostillis rootbark extraction. Right now I'm trying to filter out the particulate matter that i didn't get out during the initial pouring into containers (yes plural, as i didn't have one large one).

What I found interesting was that left over xylene that I managed to let slip through my seperatory funnel does not go through the filter paper and just sits in the funnel with the paper.

So what I'm hopefully saying here is that one doesn't have to worry about being very meticulous about getting just the aqeuos (alkaloid) layer because one can get rid of the excess organic layer through filtration it seems, but this may only be true with xylene and some heavy particulates.

I don't know why but i thought i'd note that. Maybe i'll try to snap a picture with my shitty cam.


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Invisibleblink
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Re: Interesting observation. [Re: neuro]
    #2869838 - 07/08/04 08:22 PM (12 years, 4 months ago)

do you mean that the sediment and the xylene remain in the filter?
this is during the extract, and not the defat correct...?


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Offlineneuro
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Re: Interesting observation. [Re: blink]
    #2869892 - 07/08/04 08:40 PM (12 years, 4 months ago)

Yes the sediment and the xylene remained in the filter. I suspect this was due to the amount of sediment that accumulated on the filter and it just made it so that the xylene couldn't go through.

This was just some step i through in the middle of what i was doing to get rid of extra sediment. I'm not following any specific tek though i bet it's the same or similar to some that are written..


What i did:

Made acid and base.
-Mixed HCl with some distilled water to get a 1L solution that had a pH of about 1

-Mixed 1mole of NaOH to 1L distilled water to get a 1M solution of sodium hydroxide

Powdered and gently boiled the rootbark in some quantity of the acid, did this a second time and combined all liquids and lots of gunk too (shitty strainer)

Mixed with xylene and took only aqeuos layer (bottom layer in my case)(alkaloid layer) but some xylene inevitably gets through.

Poured liquid through filters to get rid of extra sediment and noticed the xtra xylene stayed in the filter and didn't drip through probably due to the sediment (just thought it was neat)

Next I'm going to gently boil with some activated charcoal to decolorize the solution. Currently it's a dark red and hopefully it will come close to clear after the charcoal.

From charcoal step base is added until all acid is titrated (checking with litmus paper).

Crystals that form will be vaccuum funneled and washed with water to remove any base still on them.

After this i may choose to recrystalize, but i won't be able to do it with water as water boils at 100C and DMT-HCl will melt at 80C, thus i'll have a problem of oiling out as mentioned in my thread about recrystallization.


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Re: Interesting observation. [Re: neuro]
    #2869978 - 07/08/04 09:05 PM (12 years, 4 months ago)

Quote:

neuro said:
Next I'm going to gently boil with some activated charcoal to decolorize the solution. Currently it's a dark red and hopefully it will come close to clear after the charcoal.



That's a great idea, I assume you can skip the washes on the xylene cause the charcoal will pull the gunk out.

Have you ever used naptha or any other low BP solvent to clean them up?
I've followed no specific teks either, and had incredible results... my problem is in the organic solvent... I'm going to read your thread on recrystalization to see if I can salvage what I have already. (I used camp fuel just to see if it would work as expected and there was a blueish green oil to them, high BP "rust prevention" crap.)

Ans lastly, you are right when you say the sediment is blocking the xylene, it's happened to me the same using water as well (with larger particles)


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Offlineneuro
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Re: Interesting observation. [Re: blink]
    #2870005 - 07/08/04 09:18 PM (12 years, 4 months ago)

>>That's a great idea, I assume you can skip the washes on the xylene cause the charcoal will pull the gunk out.

Not exactly, the xylene will get out the plant fats and things that became dissolved in the acidic solution because of solvent partitioning or partitioning index or whatever it was called.. Mole Fraction X = [concentration in water]/[concentration in organic solvent] (or the reciprical i can't remember).

The charcoal only serves to decolorize so i can see the crystals fall out when i add base.

>>Have you ever used naptha or any other low BP solvent to clean them up?

Naptha would redissolve my DMT Base, quite easily and probably lots of other things too, i wouldn't choose naptha as a recrystallization solvent.

Also check out my post about Acid/ Base Extractions


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Re: Interesting observation. [Re: neuro]
    #2873005 - 07/09/04 03:18 PM (12 years, 4 months ago)

Just for us ignorant folk, what is a mole of sodium hydroxide in grams? I've seen the formula. It's molecular weight but I'm way too lazy to look it up. Matter of fact, I would just use the crude extract of the rootbark myself and skip all the mad scientist part. That is mostly the laziness talking but also some fear of contaminants in chemicals and solvents not meant for food processing. The pure solvents themselves are questionable in their long term use and it can be hard getting rid of all of it. I don't mean to throw cold water on anyone's favorite tech. I'm sure there is a lot of satisfaction in obtaining pure crystals. About the most high tech extraction I've done is an alcohol and water soak. I've got loads of glassware but doubt I'll use any of it.


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Offlinefelixhigh
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Re: Interesting observation. [Re: neuro]
    #2873346 - 07/09/04 04:34 PM (12 years, 4 months ago)

i've had once had problems with paper filters neuro, i've solved that by using cotton balls into a funnel for filtering...
other problem that you might be running into that i've seen before - too much alkaloids for too little solvent. saturated alkaloids don't pass well through filters.


FH


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Offlineneuro
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Re: Interesting observation. [Re: Stonehenge]
    #2874157 - 07/09/04 09:18 PM (12 years, 4 months ago)

>>what is a mole of sodium hydroxide in grams?

~40g

>>Matter of fact, I would just use the crude extract of the rootbark myself and skip all the mad scientist part.

That's fine and all, but the product won't be as pure and you won't get the same effect. Since the chem you're after is diluted so to speak in a bunch of tarry crap.

>>The pure solvents themselves are questionable in their long term use and it can be hard getting rid of all of it.

Not if you know what you're doing.


>>I've got loads of glassware but doubt I'll use any of it.

You should, it's fun. But i'm a chem nerd so that's just me.



Felix:

>>other problem that you might be running into that i've seen before - too much alkaloids for too little solvent. saturated alkaloids don't pass well through filters.

I know that's not my problem, what happens with pouring saturated solutions through filters is that as soon as it hits the filter it induces crystallization in the filter which you don't want.


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OfflineOpenminded
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Re: Interesting observation. [Re: neuro]
    #2876644 - 07/10/04 10:04 PM (12 years, 4 months ago)

I think the xylene is not passing through the filter simply because the filter is soaked in your aqueous layer. In order for the xylene to pass through, it would either have to mix or emulsify with the water, neither of which are favourable energetically, ie, they will not happen spontaneously.
Or it could kinda push the water out of the way using capillary action, but in order to do this it would have to touch the filter, which it can't do because it's soaked in water, which is held there by capillary action...
Also I'm guessing that the filter is cotton-based, which would rather be soaked in water than xylene due to all the OH's in cellulose. So perhaps water could get through a filter soaked in xylene?

Stonehenge, you should use your glass man! I can tell you that NOTHING is more satisfying than taking some plant material and ending up with glistening white crystals, it's like holding a vial of pure magic. True, it can be a bit wasteful if you want it really pure, but it is so much fun (if you're a chem nerd :smile:).


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