What 's wrong with this?

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Author	Topic: What 's wrong with this?
Osmotic Member	posted 10-21-1999 06:18 PM Can someone please tell me what i'm doing wrong......? I started out with 900 Wally-world 30mg. red berries, put in blender and ground to a fine powder. next put powder in a quart jar then added acitone about 3 to 4 times the amount of powder. Shook like hell then let it settle for about 30min. Filtered through coffee filter. (saw the nasty stuff in the filtrate) then let it dry overnight... My powder was still pink. went ahead and put it in the quart jar and put the same amount of Denatured Alcohol this time. Shook it like hell again the alcohol was very pink. Filtered it through a sand filter charged with d-nat. (drink bottle with washed play sand, about 5 or 6inches of sand with a screen and 2 cottonballs.) After waiting on this the filtrate was still pink. I let this dry overnight every thing still pink but full of crystals. I thought maybe another Acitone wash might get out the pink so i did the same procedure as in my first step...(still pink) So i did another Acitone wash.. you guessed it still pink. I decided to just go on and try to figure it out.. After completely dry i put the powder back in the jar and this time using same amount of Distilled Water (chilled) shook up let it settle for 1 hr. A bunch of gunk formed and floated around on top of the water and a little bit of crap on the bottom. I used the sand filter again (charged with very cold d-water) the filter took out a lot of the pink and all the gunk. When i dried it out still all i get is pink crystals and pink globs popping up all over the place. I tasted it and it is very-very bitter so i know the E is still in there. Can someone please tell me what i'm doing wrong. And how i might can salvage my work (I haven't done any thing else to it.) All help greatly appreciated..(in advance) Still Dreamin..... Osmotic
Android Member	posted 10-21-1999 07:37 PM Gotchur back, baby! Ok, pay attention. Up a little to the right of your screen is a thin rectangular window. Put your cursor on the arrow and click(just once) your left mouse button. The window will open to reveal a list of options. The last 100 days is good start. Open that and start at the top and read thread. When finished, click next oldest thread and repeat. Hope this helps!
Snotbrain Member	posted 10-21-1999 07:50 PM So whassa little pink?? Been one of my favorite colors ever since i discovered GIRLS! I don't know what play sand is gritwise, but it is unlikely to be 30 grit size or smaller: 30 grit is more like beach sand: 60 grit is better. Get $5 worth of 30 grit and throw away your "play sand" most likely it's useless. The red should be left behind in the basification extraction process.
placebo Member	posted 10-21-1999 08:07 PM Are you planning on using P/P method if so you are better off using freebase of E. So surely you plan on basifying anyway and allegedly this rids you of the coloring. Sounds good thus far anyway. Good work! ------------------ Placebo.... Remember it's all in your mind!
aqua-girl Member	posted 10-21-1999 08:52 PM All is not lost- I've used "play sand" in 1L bottles with good results (read: no MCC). Pink is no big deal. Hit the pile with some cold acetone to make crunch crystals.
Osmotic Member	posted 10-21-1999 10:51 PM Placebo, Yes i am planning on using p/p method. I was going by the instructions at the (honduras web site) via Worlock. Doing all the ph "stuff" at the end of rxn. Aqua-girl...., What's a crunch crystal.....?????? Thanks for the input!!!!! I'm still lookin at the drying pan and reading old posts, haven't done anything else to it..... Still Dreamin.....>>>>> Osmotic
manic Member	posted 10-21-1999 10:53 PM hey aqua-girl, what's the percentage of the I in concentrated I. My soft coral is looking a little lame. Pink tastes like cake icing. ------------------ -right to remain unknown-
SkitterBlitzer Member	posted 10-21-1999 11:40 PM I used the same pink ones and went with d-natured first, then h20 then acetone and it was still pink, did the acetone again and once again it was pink. Figured the shit loved the colar so why fight it, out of a hundred pinks i got 5.5 gms of xtals.. Peace! Skitter
aqua-girl Member	posted 10-21-1999 11:41 PM Crunchy crystals = dry pfed. Different I solutions have different concentrations. Hit the local pharmacy for 7% tincture, or Lugols (if you can fanagle it without a script). If you have a vet, get a script for I crystals. ~$25 per Oz from Humco. Still more expensive than from chem supply, but if it's the only way... Xenia sp. and Anthelia sp. seem to respond very well to free iodine additions. Gotta dissolve I2 in a KI solution to get it to go into H20. Gotta be careful not to OD the tank or else you get a nasty cyanobacteria bloom. Hope this helps...
Gadget Member	posted 10-22-1999 12:32 AM Do an A/B on it the pink will stay behind. I wish I had done the alcohol washes first, like you did. I jumped straight to water,filter, A/B and lost most all my stuff to nasties. I have proved the fact that it is VERY prudent to stay the hell away from dh20 till you pretty much have only crystals to play with.
Worlock Member	posted 10-22-1999 02:00 AM The pink is not any problem. But to be rid of it dissolve it in a very small amount of D-water 900 x30 mg = 27 grams of E nice you will want to be rid of the pink with that amount of E dissolve the powder in water Add 100 ml of toluene, ether, or warm lighter fluid. Add concentrated lye/water solution, shake, make sure pH is 12+, let it sit for a while dump the lye/water, the freebase E is in the toluene. Wash the toluene/freebase with d-water once or twice. Then filter the toluene/freebase, no cotton ball, just a coffeee filter. either evaporate the toluene to obtain the freebase or add d-water then drops of filtered HCl until you get a pH in the water layer between 7 and 8. Separate, filter, and evaporate the water you will have some very nice E.
Gadget Member	posted 10-22-1999 08:21 AM Worlock: Re the dh20 wash of non-polar, I found when I evaped the wash water there were a shit load of crystals in there. Only explanation I could come up with is that the dh20 had absorbed CO2 and made a little acid from it. So, question. Would making the water a little basic effect the wash very much? Maybe add just a little bit of baking soda, or other alkalie? I know, I know. keep the fucking lid on the dH20 and I won't have this problem
Worlock Member	posted 10-22-1999 02:58 PM Gadget Yes indeed adding alkali to the solution will solve the carbonate problem, However the amount of Lye to add is a problem since it appears that at pH 10.5 your going to start loosing product to the carbonate. The reason for the wash is to remove these nasty tasting lyes that combine with oils to form a soap that will ruin your stuff if your a smoker and is potentially deadly to shooter. The simplest solution is a light boil on the distilled water for fifteen minutes in a covered glass pot. This will effectively drive off the CO2. Cool by placing hot water in a flask with a beaker over turned to cover the opening and prevent CO2 from getting into the flask. A stopper will be sucked into the flask as it cools, damaging your equipment.
Worlock Member	posted 10-22-1999 03:14 PM Gadget, Very good idea to evaporate those washes and look for product, I do not trust the store distilled water so I always evaporate the washes. I have not yet had any problem with a fresh jug of distilled water. Since the amount of water used for the wash is small, a 1 or 2 liter sealed container could be kept aside separately for CO2 free distilled water.
Gadget Member	posted 10-22-1999 04:03 PM I will admit I may have left the lid off the jug overnight, Ooooops Thanks for the advice, didn't realize just boiling it would resolve the problem!
Osmotic Member	posted 10-22-1999 05:21 PM Worlock, just got back from the store. I have mixed my lye solution (20gm./ 100ml.) hope that's right. As for disolving the powder in d/water i am assuming 100ml. Have touline but not sure of how much of the lye sol. to put in.???? I will be using push pull so does it matter if i go ahead and lower ph and dry in to crystals or should i go for the freebase??? I don't have my RP yet so i may have it around a few days.. As always thanks for the input Still Dreamin........ Osmotic
Osmotic Member	posted 10-22-1999 07:53 PM O.K. i put my powder in jar, added 100ml. of d/water.It disolved nicely into a reddish liquid. Next added 100ml. of Touline then the lye sol. a little at a time. the ph strips i got are the 3 way pool strips they only go up to 8.4 (red) anyway i ended up putting the whole 100ml. of solution in. Then shook up..... What a fuckin mess. I have 3 layers.. on top is very clear but there is only enough of it to barely cover the middle layer.. the middle layer is pink and all puffy lookin and a little over an inch thick... the bottom layer is the same reddish color that i started with.. I tested what i could get to of the clear and the best i got is a rose looking color. PLEASE HELP ME !!!! Dazed and Confused..... Osmotic The middle layer
readyeddie Member	posted 10-22-1999 08:29 PM Osmotic you should of added around 300ml of solvent instead of 100ml for that amount of pseudo.After you add more solvent shake it up for a few then suck up the top and solid middle layers now filter and repeat them steps again.When you get both extractions done pour some fresh solvent over the solids in the filter.
Worlock Member	posted 10-23-1999 12:55 AM Your doing fine add a little more toluene let the sob settle for an hour or so to see if the middle emulsion breaks up it contains a lot of ephedrine, toss a little table salt in i,t when the middle layer is gone then separate the two layers. If the middle layer still exists try to break it up or wait it out. as the middle breaks up, the E in the middle goes up, the rest goes down, some crud may stay in the middle. If after 6 hours it is still there then flush the lower two layers out and work with the top layer, most of the E will be in the top after 6 hours.
cantstanditanymore Member	posted 10-23-1999 01:17 AM Read somewhere in this tangled web, but don't quote me. The red is for not, just goathead with the reaction and finished goods will be red free. Somewhere from git to go it is gone...
Android Member	posted 10-23-1999 03:09 AM Ya gotta love the passion here
Worlock Member	posted 10-23-1999 06:44 AM The pink crystals were no problem, Osmotic mentioned "pink globules", and again the pink is no problem but "globules", now that has to be something besides E. RP and I2 being hard to obtain it seemed like a good idea to be sure the E was clean and would not fudge up the RP so it can be used a second time. In addition this is good practice for the upcoming meth extraction If the emulsion goes away then he has good E. If it remains then it could be something like what Gadget showed us in his picture, the povidone, or something like wax that slipped by. Either way the loss of E 10% will be minor compared to the loss of E 80% if the reaction fails, and the loss of I2 and RP.
Osmotic Member	posted 10-23-1999 01:01 PM O.K. i'm going to go ahead with it. Thanks for the confidence. I guess i was over reacting last night it's just that i want my dreams to come out right..Reading threads and reading more threads is important but it doesn't mean shit until you get the chance to do it "hands on". I'm glad there are those of you out there who realize that not every- body is born with the talents and wisdom that a lot of the Bee's here possess. Thanks for the time that you are willing to spend on helping newbees like me... I will post results when all my "stuff" settles and can be seperated. Thanks again..... Still Dreamin....... Osmotic
Osmotic Member	posted 10-23-1999 01:30 PM I can't believe what i just did. instead of touline i grabbed the acitone jug instead and put in 200ml. Hope i didn't fuck it up. The good news is that now i only have 2 layers. The top is clear (just a hint of cloudyness) the bottom is red and is still partly full of gunk. Gonna let this settle for a few hours and see if anybody can tell me what i should do now.... Human Error...aint life a bitch!!!! Osmotic
skuller Junior Member	posted 10-23-1999 01:43 PM place the pinks in a collander add ice swirl and rinse with distilled water.this should remove the dye from the getgo.
Worlock Member	posted 10-23-1999 10:01 PM Ephedrine-HCl salt is insoluble in acetone. Ephedrine freebase will dissolve in acetone. ******** Separate the layers and treat the top toluene layer as though it contains the Ephedrine freebase. ********* Place the water and acetone solution on a hot plate to help evaporate the acetone(just in case). Acetone is often added to break up the emulsion. Adding Acetone to a hot lye solution can be dangerous, it will effervesce strongly.
mrr pyrex Member	posted 10-24-1999 04:05 AM Hey sir worlock, was just wondering where are you getting the solubilties of chems your mentioning, I mean I only have a Merck which is nice but is limited on solubilties, was just wondering what your source is. Pyrex out
Worlock Member	posted 10-24-1999 04:21 AM The E-freebase reacts much more rapidly than the E-HCl salt. This is because the freebase will form the Hydrogen Iodide salt in acidic medium. The freebase has an advantage of eliminating Chlorine from the reaction, and the freebase is easier to make (evaporate the toluene) The HCl salt (pH in d-water between 7-8) Generally it has been is easier to purchase a different brand of pill, and avoid the A/B extraction all together. However this whole pill extraction process is becoming a major part of the work involved, we all may be doing a version of the A/B soon The freebase will have very much happening right away, a fairly tense start-off. freebase is lighter weight than E-HCl, so multiply the weight of the freebase by 1.3 to get an approximate weight to use in the calculations for the ratio of E : RP :I2 The HCl may need to be kicked in the ass to get it to go and may require a bit more RP and I2 ti initiate a reaction.
Worlock Member	posted 10-24-1999 04:33 AM I have been fortunate to have the opportunities to observe most of these solubilities first hand. Like trying to wash freebase crystals in acetone and seeing them vanish instead. You see I figure I've made almost every mistake there is , but Not even close I still find plenty of new ways to screw it all up.
Android Member	posted 10-24-1999 09:09 AM I made a gas bubbler once to preticipate the product from the solvent in the final step. It pumped crystals out like confetti. When I tried to wash them in acetone, they went bye-bye! I chose to assume they were never really there in the first place. At least not the ones I was after! Did you ever figure it out?
Worlock Member	posted 10-24-1999 01:23 PM Android, Perhaps your acetone mutated to monoxide dihydrate, or ethyl hydroxide Reminds me of a guy who offered to clean up an 8-ball for me by recrystalization. I should have watched him because 10 minutes later, the meth tasted like it had mutated to 50% ephedrine. When I asked what was the fuckin' deal? He replied that "he heard acetone could change meth back to ephedrine". I tossed his ass out, after I finshed laughing in his ugly face for ten minutes, recrystalization,? acetone? the crooked bastard.
Osmotic Member	posted 10-24-1999 07:36 PM Well after letting it settle overnight i had 2 well defined layers and just a fraction of gunk. I separated with a turkey baster and a syringe (what an adventure). I took the almost crystal clear top layer, filtered through a coffee filter into my drying pan, then added light heat. After a few minutes it started to evap. I took off the heat and have been watching the biggest crystals pop up all afternoon. I dont want to add anymore heat due to the thickness of the drying crystals. When they all dry to the SNOW - WHITE (ITS ABOUT TIME) color that is popping up around the edges and on top... I plan to wash with d/water twice,as directed from above.... Almost forgot i evap'd the bottom layer as well, it was all crap with no crystals at all so i guess all my E did go to the top... All input appreciated..... Still Dreamin........ Osmotic
Worlock Member	posted 10-25-1999 04:26 AM Osmotic How come for a junior member you do so well with these lab procedures? If this any indication, it looks like you will probably be successfull on your first run.
Osmotic Member	posted 10-25-1999 07:55 PM I'm not sure how good i did....... I can't get the crystals to dry out!!!!! so i can do the d/water wash... I added just a little heat to aid in drying but the crystals but they just melted into a syrup and began to smoke. The smoke smelled kinda like burning E so i took off the heat. It's starting to crystalize again but it still looks gooey... As for doing well in the procedure perhaps it's that i'm not in any hurry here. I'm in the mid 30's so i have acquired a lot of patience over the years. I've done a lot of reading for the last several months before even thinking of trying this. Knowledge is Power.... Using it takes a little practice... Thanks for all the input...... Any suggestions on my drying problem..??? Still Dreamin...:P Osmotic
Worlock Member	posted 10-26-1999 08:33 PM Since the E freebase is not water soluble you can wash them at any time with fresh (CO2 free) distilled water. It appears that either the Toluene was not pure and has heavy oil contamination or that the red globules noted previously are a wax that is following your E around. It is possible that the oils are slightly soluble in water and soluble in toluene. to wash the crystals in water may help. The chances of a flask fire are questionable with the oil present, not any fun and will ruin the reaction. The E freebase when pure enough drys to a soft crystal. It takes very little contamination to keep then oily. Freezing may harden the crystals and still allow the oil to flow. The E-HCl water soluble salt is easy to create by adding distilled water with HCl about 1 ml 30% HCl for evey 2 grams of E. Freezing the E-freebase and gook, then mixing it with almost frozen d-water/HCl. This may dissolve the E and leave the shit in a hard wax state that can be cold filtered
Osmotic Member	posted 10-26-1999 11:34 PM Worlock...good to hear from you After hours and hours of staring at the stuff I decided to try and help it along. I have kept a small 8in. fan blowing on it constantly. I scraped the pan and mixed the dry with oil and let the fan blow... every few hours or so i go and mix again.. let the fan blow...you know what i mean.. Well it's almost dry...(jumps up and down) I'm hoping when i get home tomorrow it will be completely dry. I have noticed that a couple of small lumps have dried to a red color I just reached in and threw them away. I'll post dryness results tomorrow.... All input appreciated...... till then I'm Still Dreamin... Osmotic

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