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Poor Yields with Heated Heptane Extraction? Options
 
atom45
#1 Posted : 7/5/2009 8:23:20 PM
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Hey guys,

I'm trying to do an STB extraction on roughly 125g of MHRB powder. I used 1500 mL of water along with 7 tablespoons of NaOH. I heated my heptane to around 80 Celsius and extracted all of it. I then let it evaporate to make the freeze precipitation easier. I resulted with less than 100 mg of DMT. Might I add, the heptane took on a rather yellow color during the extraction.

Thanks in advance.
 

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West-en
#2 Posted : 7/5/2009 9:03:46 PM

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Insufficient information. Please tell us more about the procedure. Like, how did you mix the heptane with your barksolution? How many grams are 7 tablespoons? How much heptane did you use? Did you evaporate or freeze precipitate (didn't really got it)? And lastly, did you only do one pull?
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Jorkest
#3 Posted : 7/5/2009 9:16:00 PM

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um....how much heptane did you use? and how long did you mix the heptane into the lye tea?
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atom45
#4 Posted : 7/5/2009 10:14:28 PM
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I used roughly 175 mL of heptane. To mix the solution, I turned the solution end over end and swirled for 5 minutes. I mixed around 5 times in a period of 60 minutes. I kept the reaction vessel in a heated water bath that was around 50-70 degrees Celsius. Seven grams should be around 105 grams of lye. I used freeze precipitation, but prior to precipitation I evaporated some of the solvent. I did only one pull.
 
tryptographer
#5 Posted : 7/5/2009 10:16:54 PM

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Quote:
I heated my heptane to around 80 Celsius and extracted all of it.

How do you know you extracted all of it? Why heat only the heptane and not the tea, the heat will be distruted over the whole - if you heat, heat the big teapot.
Not enough info to say anything useful about it, too many variables. How cold is the freezer? Is the MHBR good?

Edit: you beat me to it, we were typing simultaneously Smile
Still, what about the MHBR, sounds like you should have gotten more indeed!
 
atom45
#6 Posted : 7/5/2009 10:26:58 PM
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I ordered it from Secret Herbals. Although it was my first purchase from there, I hear their root bark generally is of high grade. My freezer can freeze ice creame rock hard.
 
SWIKiljosh
#7 Posted : 7/6/2009 5:26:35 AM
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I just got a batch from their ebay store and was able to pull some. I only used 40g and evapped wrong so I think I turned most of my spice to N-Oxide because Naptha was used(apparently cant pull N-oxide)and a fan was blown on it. I ended up with ALOT of brown goo, so there is something in there. My extractions got progressively bigger, the first pull was evapd to check spice content and I got barely anything. Try it again!

I am a noob but from what I have read here if your pulls are low try heating the whole thing up and add some more lye water.
 
funkatron9000
#8 Posted : 7/6/2009 7:13:24 AM

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I swear I thought I read somewere that you can't freeze precip from heptane? (anyone else remember seeing this? I've never tried heptane as my main solvent before so idk)

Lol, try using naptha first to pull from the bark, then you can evap that down then freeze precip it. take your spice and recrystalize it in heptane if desired/needed to clean it up. I know that works Smile

Has anyone ever tried FASA with heptane? I know it works with Xytol but idk bout heptane.
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West-en
#9 Posted : 7/6/2009 2:46:56 PM

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funkatron9000 wrote:
I swear I thought I read somewere that you can't freeze precip from heptane? (anyone else remember seeing this? I've never tried heptane as my main solvent before so idk)

Heptane works fine. Actually, I used heptane to the first 100g and then I found light naphtha (hydrogentreated, whatever that means) for the next 100g (half the price of the heptane). And I have to say, heptane was way better. It does not pull much things except DMT and it's really soluble in it. You can get pure white crystals without washing or recrystallization. If you can afford pure heptane, my advice is, use it!
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funkatron9000
#10 Posted : 7/6/2009 4:50:02 PM

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Very nice, I was going to have to go buy some more naptha soon but I still have a fair bit of heptane left so i'll try that. thanks for the insight mr. west-en Cool
Do you treat it just like naptha or do you do anything differently with it?
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Ignore my presence and go about your Earthly business.
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West-en
#11 Posted : 7/6/2009 11:14:26 PM

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funkatron9000 wrote:
Very nice, I was going to have to go buy some more naptha soon but I still have a fair bit of heptane left so i'll try that. thanks for the insight mr. west-en Cool
Do you treat it just like naptha or do you do anything differently with it?

Treat it just like a very luxury naphtha. It's expensive but gives very clean yields!
You may also use smaller amounts, since it's way more soluble in heptane. If there's a big price difference between naphtha and heptane (aka, you have access to both) I recommend pulling with naphtha and recrystallizing with heptane to purify the product. For this, heptane will last for a very, very long while!
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