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Not getting anything after first pull
- Thread starter The Gnome
- Start date
Try adding more solvent and when you do the rolls to mix the solvent and soup, make sure you roll it for at least 5 minutes and then let it separate. Make sure you do that at least 3 times before you pull your solvent out.
If that doesn't work, we'll need more info on exactly what you did so we can find out what went wrong.
If that doesn't work, we'll need more info on exactly what you did so we can find out what went wrong.
DMT Gnome said:I do not have any ph strips at the moment. But it was 1gram Lye/1 gram of powdered bark/ 15ml water.
Add lye until the solution turns black.
I also shake my solution. If an emulsion forms then just wait a few hours or until the next day. Also you can gently heat the combined Aqueous/NP solution in a water bath...no open flames though!
Edit...ignore this post if you are doing a STB...
The Gnome
Rising Star
joedirt said:DMT Gnome said:I do not have any ph strips at the moment
Add lye until the solution turns black.
I also shake my solution. If an emulsion forms then just wait a few hours or until the next day. Also you can gently heat the combined Aqueous/NP solution in a water bath...no open flames though!
Edit...ignore this post if you are doing a STB...
Exactly
112 grams of powder RB
112 grams of lye
7 cups of water(1680 ml)
2.15 cups of naphtha(112ml)
hot water bath with naptha on first pull and got 300MG... repeated and got 0 the second and third pull. Also heated the combined mixture at one point.
Hi,
You didn't mention anything about how long you are letting the MHRB sit in the base solution before you wash/pull with your non-polar solvent (NP)--I've found that anything less than 2-2.5 hrs gives low yields (and more than 3-4 hrs starts giving a yellow product). Warming the base + MHRB doesn't (IME) appear to speed up the extraction substantially and pretty much guarantees a more yellow product; warming the solution (including the NP) does pull more material per wash.
You may want to try using less base solution for that amount of powdered MHRB, and adjusting your washing technique. 300-400mL of base for 100g of MHRB should be fine. In that case you would wash the base + MHRB slurry 3-5 times with ~30mL of NP each time. When you wash you want the NP to be completely mixed into the slurry for a couple minutes--try: swirl until the NP disappears, keep it up for a couple minutes, let the mixture separate, repeat a couple more times, remove the NP layer, repeat with fresh NP. Don't combine the NP washes!
As far as yield goes: I've been using whole plantation grown Brazilian bark, chopped and powdered as needed, the technique mentioned above, and getting yields of a little over 0.6% (that's 0.6+ g white-pale yellow extract per 100g MHRB).
Good luck, and take care,
- Tse
You didn't mention anything about how long you are letting the MHRB sit in the base solution before you wash/pull with your non-polar solvent (NP)--I've found that anything less than 2-2.5 hrs gives low yields (and more than 3-4 hrs starts giving a yellow product). Warming the base + MHRB doesn't (IME) appear to speed up the extraction substantially and pretty much guarantees a more yellow product; warming the solution (including the NP) does pull more material per wash.
You may want to try using less base solution for that amount of powdered MHRB, and adjusting your washing technique. 300-400mL of base for 100g of MHRB should be fine. In that case you would wash the base + MHRB slurry 3-5 times with ~30mL of NP each time. When you wash you want the NP to be completely mixed into the slurry for a couple minutes--try: swirl until the NP disappears, keep it up for a couple minutes, let the mixture separate, repeat a couple more times, remove the NP layer, repeat with fresh NP. Don't combine the NP washes!
As far as yield goes: I've been using whole plantation grown Brazilian bark, chopped and powdered as needed, the technique mentioned above, and getting yields of a little over 0.6% (that's 0.6+ g white-pale yellow extract per 100g MHRB).
Good luck, and take care,
- Tse
The Gnome
Rising Star
thanks for the advice. On the first pull, it was less than 2 hours with warm NP... Got almost completely white crystals, and yielded around .3%. The next pulls stayed in longer and longer, second was in there for 4-5 hours and 3rd pull was in there for over a day! Before each pull, the concoction was spun and swirled pretty damn hard at least 4-5 times!!!
What I noticed is no matter how hard you swirl it, if you do it uniformly, it will have little to no emulsions! This little technique worked AMAZINGLY in the past... Have yet to see anything less than off-white come out of it.
Now this bark is about a year old and is good quality. I dont think the age has anything to do with this problem though. It was packaged correctly. The only thing I can think of is the freezer but it seems to be working fine. Noticed possibly a tiny more floaters so Im not gonna give up on this pull!
What is the longest you let it sit in the freezer for you to get positive results?
This last pull is my last attempt on this particular one!!! I did what was advised and swirled the crap out of it for 5 minutes at a time and let it sit, and repreated.
Hey Tsehakla, why is it a bad idea to combine NP washes? Just before reading this, I litterally JUST combined the 2 jars of possibly nothing to free up a jar for this last pull.
thanks again!
PS- what are the rules here about sources? Can we speak of them or no? Ebay was my only place and as many of you may know, no more MHRB on Ebay
What I noticed is no matter how hard you swirl it, if you do it uniformly, it will have little to no emulsions! This little technique worked AMAZINGLY in the past... Have yet to see anything less than off-white come out of it.
Now this bark is about a year old and is good quality. I dont think the age has anything to do with this problem though. It was packaged correctly. The only thing I can think of is the freezer but it seems to be working fine. Noticed possibly a tiny more floaters so Im not gonna give up on this pull!
What is the longest you let it sit in the freezer for you to get positive results?
This last pull is my last attempt on this particular one!!! I did what was advised and swirled the crap out of it for 5 minutes at a time and let it sit, and repreated.
Hey Tsehakla, why is it a bad idea to combine NP washes? Just before reading this, I litterally JUST combined the 2 jars of possibly nothing to free up a jar for this last pull.
thanks again!
PS- what are the rules here about sources? Can we speak of them or no? Ebay was my only place and as many of you may know, no more MHRB on Ebay
4-5 days. I'm using mineral spirits and have never used naptha so I can't offer any comparison between the two. I get a cloudy solution within an hour, over the next few days clumps of crystals begin to form on the sides and bottom of the jar, after 4-5 days the solution has completely cleared of cloudiness.DMT Gnome said:
The first wash most likely gets you a saturated solution, subsequent washes will result in progressively lower concentrations. If you combine the washes you are diluting them... Of course if you are evaporating some solvent off before freeze precipitating it doesn't matter. Also, by keeping each wash separate you can monitor (well, after the fact) the progress of the extraction and use the information to fine tune your technique. e.g.: If you find that (say) the first two washes with the same amount of NP, starting material, and time, always give you the same amount of product you can perhaps increase the amount of NP used for the first wash or combine them without dilution; if you find that the 4th or 5th wash doesn't get you any precipitate you may decide that you don't need to do them or that it is necessary to evaporate them down before freeze precipitating.
[Personally, I don't like evaporating solvents and don't see the point of doing extra washes just to get a few more mg of material.]
I don't recall the technical reasons, but: It is better to do many extractions with less NP than one extraction with the same combined volume--even if you are evaporating to dryness and recrystallizing!
- Tse
I've never had to deal with a cloudy NP layer...
Assuming the cloudiness is aqueous: I would suck it out and place it into a test tube. If it didn't separate I would add about 1/2 the volume of a saturated solution of NaCl and mix it up.
If you've been extracting from a hot-very warm mixture which has cooled, you may have supersaturated your NP and the cloudiness is product starting to precipitate out.
<shrug>
- Tse
Assuming the cloudiness is aqueous: I would suck it out and place it into a test tube. If it didn't separate I would add about 1/2 the volume of a saturated solution of NaCl and mix it up.
If you've been extracting from a hot-very warm mixture which has cooled, you may have supersaturated your NP and the cloudiness is product starting to precipitate out.
<shrug>
- Tse
cyberdream
Rising Star
i had the same problem until i realized that i didn't roll my jar enough
SHroomtroll
Rising Star
I missed if you just freeze precis or if you also evap your solvent after? if you don´t evap it maybe you need to
roll/mix better. Try shaking maybe. if your ph is high enough, which it should be wth your numbers, then there should be no emulsions
use less naphtha per pull, otherwise your solutin won't be saturated enough to crash anything out. If already used large quantities of naphtha try either salting out or evapping some naphtha and then re-trying the freezing. Re-use the naphtha after freezeprecip - it's better for our environment.
from 100g of MHRB I get ~1g of magic.
try to get as much as you can from it - don't be wasteful. this stuff is so precious! just re-use the naphtha and do small pulls in the future to waste as little solvent as possible!
cheers
use less naphtha per pull, otherwise your solutin won't be saturated enough to crash anything out. If already used large quantities of naphtha try either salting out or evapping some naphtha and then re-trying the freezing. Re-use the naphtha after freezeprecip - it's better for our environment.
from 100g of MHRB I get ~1g of magic.
try to get as much as you can from it - don't be wasteful. this stuff is so precious! just re-use the naphtha and do small pulls in the future to waste as little solvent as possible!
cheers
SHroomtroll
Rising Star
Enoon said:
Yeah i always shake like crazy for a minute and then settle and repeat this at least 10times per pull.
Heptane is so cheap so i use alot more than i need and evap freeze then evap the rest.