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first extraction, first catastrophic failure? Options
 
Shiva H. Vishnu
#1 Posted : 2/2/2011 5:26:41 PM

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i know it will be tempting to roll your eyes at the exploits of this neophyte, but i kindly ask that you reserve judgment on the contents of my head long enough to equanimously dole out some constructive criticism. the previous query is not an anticipation of churlishness on your part, but a recognition of my own sophomoric ignorance.

a9apologies. no pics)

i did a 100g extraction of mhrb using roughly 750ml water basified with approximately 100-120g NaOH. added the mhrb to the somewhat cloudy basified water in a ball brand quart jar and stirred until thoroughly muckish. at first i tried just turning the mix, but clumps were forming so i opted to stir it with a stainless steel knife. i added my first 40-50ml of naphtha shortly after to take advantage of the warming effect of the fresh base. turned it several times and let separate. repeated this 3-4 times and then siphoned off the naphtha with a disposable syringe i had in an elaborate first aid kit. it held 10ml/cc so a few tugs on the plunger netted me amber naphtha with no apparent trace of base at all. placed the pyrex measuring cup with the first put in the freezer, turned on low, and tightly covered in plastic wrap.

i repeated the process, but on trying the first pull, the rubber plunger in my syringe pulled loose from the stem, rendering it unusable. no problem, i thought, i does say "single use only" on the package. i had another syringe and so i used it for the second pull, and it broke down right as i was making the last 10cc pull. the rubber pulled free of the stem of the plunger. at this point it didn't occur to me that the naphtha was actually dissolving the rubber plunger. i just thought the syringes weren't made to be pulled back and forth more than once and the materials just gave way under the friction.

i made one final pull, but this time using a clear plastic turkey baster.

i put everything in the freezer on the lowest setting and set the jars next to the vents for maximum encoldification (back off man, i'm a scientist). during the night i noticed the samples got cloudy and a dark amber layer formed at the bottom. i thought this was unusual give the pics i'd seen of the process but did'nt fret too much, as i know spice can be amber. (amber is the only spice ive broken through with).

after work the next day were the lovely globes, but stuck in a layer of dark amber oily muck. i dreid for a few hours and then tried to scrape it all up, which proved quite difficult given the viscouness of the muck and how deeply entrenched were the crystals in this muck. what i ended up with was a substance the consistancy of warm hash that ranged in color from very light amber to very dark brown.

i got on chat and was informed that brown means i got base in the mix. i was very sure that no base got in my mix. unless some of it stays suspended in the naphtha after separation and then freeze precipitates, there was no base. i was very meticulous upon siphoning and observed nothing but clear yellow/amber naphtha.

so i did a re-x. warmed naptha and put it in all of my collection dishes, stirring tomake sure to get the remaining xtals, but not so much the muck on the bottow. i also redissolved my scrapings, but only like 50% of their mass dissolved quickly, the rest formed black chunks that wouldn't dissolved. i poured off the naphtha and got rid of the junk on the bottom. all this naphtha was coollected in one pyrex dish and put in the freezer.

in the meantime i did three more pulls, rather quickly, but using slightly more naphtha. but i was still using this turkey baster to transfer my naphtha to the jar and to siphon it off after the mix. everything went in the freezer.

i was on the lookout for this abominable muck to form on the bottoms of my collection dishes, and when it did, i poured off the naphtha, cleaned the muck from th jar, and reintroduced the naphtha to the jar (side not: this left tiny little xtals in the bottom of the otherjar, so i dissolved them in a little warm naphtha and added them to the jar.

after 24 hours i now have maybe 6 salt grain white crystals clinging to the side of the jar, and a light brown to amber muck on the bottom drying to what might end up being a scrapable powder layer eventually, but atm it's too oily.

i poured off the naphtha and am now evaporating it to get whatever else might be in the. i think the last pulls were to diffuse to freeze precip in my freezer, so maybe they'll manifest after evaporation.

i just can't believe my result were so radically different from those i've seen posted here.

where did i go wrong? was it simply the use of the disposable syringe and cheap turkey baster? would the mere seconds my naphtha spent in contact with these substances have been enough to dissolve plastic and turn it into a dark film in my precipitate? my final product it feel is mostly free of dark muck, but it's still too oily to tell what the final product will look like. is it possible that i still have something usable here, or should i just scrap the whole thing. another 500g o MHRB is already on the way.

i just don't want to admit defeat. i thought this would be easy as pie. perhaps i've been spanked for it.

 

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Shiva H. Vishnu
#2 Posted : 2/2/2011 6:41:16 PM

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addendum. i scraped up some of the amber brownish precipitate from my later pulls and it was entirely inactive. Sad
 
proto-pax
#3 Posted : 2/2/2011 7:15:51 PM

bird-brain

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dont know why it didn't work after you used new naptha, but dont do this:

i added my first 40-50ml of naphtha shortly after to take advantage of the warming effect of the fresh base.

just dont ever do that.
blooooooOOOOOooP fzzzzzzhm KAPOW!
This is shit-brained, this kind of thinking.
Grow a plant or something and meditate on that
 
Shiva H. Vishnu
#4 Posted : 2/2/2011 7:37:11 PM

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proto, thanks for the reply! that sounds like good advice, although i've heard conflicting opinions.

the final collection dish with all my naphtha evaporated about 80-90% last night so i decided to stick it back in the freezer and, what do you know, it started to quicky form white precip. i think my solvent was too diffuse after i did the re-x. it sure isn't now. hopefully i can save at least 50% of my yield. live and learn. my next try
will be much better.
 
Shiva H. Vishnu
#5 Posted : 2/3/2011 12:08:37 AM

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HAHAHAHAHAH! I've done it, by Jove (whoever that is)! My girl and i are about to go take a class on shamanism at the local unitarian church, so i loaded up just a taste to see if i had the molecule. oh, yes, one little hit and i scratched the surface. but my gf wanted to take a full hit, so she did, and blasted into the ether. i'm so happy right now i can't stand it. i'm waiting until after the class to take on hyperspace for real.

thanks for the help i got on chat. in the end i just had to play around with the solvent until i was sure i'd gotten out the impurities that so vexed me, and i had to evap the solvent a great deal before i could freeze precip properly. i've learned a lot through this experience. next time will be much better.

the spice i have is way purer than any i have gotten through dealer friends. i can't wait to share the love.

thanks again nexus..
 
 
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