02-29-04 04:02
No 491712
After reading 8ball's most recent gassing problem thread, it reminded Swim to run his own problem by the elders here at the hive for some theoretical help.
Swim has gassed a few times for pseudo after employing ahgreich's patented tetra trap. For the 1st few times he had no problems whatsoever, but now after filtering and washing with tone, is left with a waxy pseudo end product.
He was suspicious that this end product was a mix of both pseudo HCL and freebase. Why? After 3 washes with tone it will leave the tone cloudy as if some of the pseudo is getting washed away. Measuring yield after the fact also confirmed this suspicion. After adding this product to fresh xylene and water 50/50 just to get it ready for further titration, he checked the ph of the water layer. This reading gave a ph of 10. (With most of the pseudo floating on top of the water) Most of it still obviously in freebase form.
After the tetra trap, he isolates the 3 pulls. Washes 3 times with water, dries Xylene over baked MgSO4 and gasses via VE's muriatic and calcium chloride method.
He had gassed repeatedly, over and over again until no more pseudo precipitated in the Xylene. He filtered the pseudo and gassed the NP again. Waiting 20 min after each gassing.
He has been having the exact same problem twice now!
He ends up having to take the precipitated waxy pseudo HCL/FB and further titrate it with muriatic to MAKE SURE he gets the ph 6 or lower salt form. Why is this?
Is this a new gassing gakk?
When he attempted this for the 1st few times he never had this problem. Now it is consistent and reoccurring.
Now he pretty much expects it! The additional titration has become almost mandatory.
After filtering off the gassed pseudo and ditching the gakk ridden NP, he doesn't waste his time or precursor by rinsing with tone. He just scrapes the waxy pseudo "mix" from the filters into a clean mason jar, adds fresh NP, water and adds muriatic til it hits 6. Isolates the polar and evaps for pristine HCL.
Swim has tried to remedy the problem by filtering up to 3 times and gassing it to death well after everything that is going to precipitate does.
Point is, this additional titration shouldn't even bee necessary...right? He has found that at least in his area, with generic 120's it most certainly is.
Anybody have an explanation. This shit is totally bizarre!
Refuse/Resist
(Hive Addict)
02-29-04 23:18
No 491884
A newer Gakk is definitely present.
After utilizing the ancient and currently unfashionable tyvek extraction method the psuedo saturated isopropanol was sent straight in to Geezes xylene psuedo precip technique then followed up by a scottydog-special acetone panning style rinse.
Swim's buddy was routinely getting 16g from the first two pulls of one red bottle of gas-line dehydrator each from about a 4 hour per pull hot alky soak. This all coming from a single tyvek bound (2 medical hairnets) "onion" containing a full 9 boxes of unground 120's. This extract amount had become steadily consistent for maybe 1/2 year until the last time it was attempted.
Swim's buddy wished to get around 20g instead of the usual 16 from the first two pulls so the tyvek onion contained 11 instead of 9 full boxes of 120s.
Bafflingly the 2pull total from this increased amount came to a frustratingly low 12g. Something suspicious was noticed nearly immediately. Quite soon after the measuring cup containing the "oinion" was placed upon the hot plate a subtle cloudy substance resembling fine, transparent oatmeal could be faintly seen circulating in the alcohol. This cloudy stuff could a also be seen in the second pull. (not in the 3rd though)
As a test to see if it was just hyper saturated psuedo on the verge of crystallization the first 2 pulls were placed in a flask and refrigerated. Settling of the fine oatmeal but no crystallization occurred after 2 hours of cooling. Suspicions remain.
If extraction of 120s now results in a portion of that psuedo being mysteriously converted to freebase I'm guessing this freebase should still bee present in the xylene used and should bee recoverable by titration.
Right? I hope it's as easy as that.
It's quite likely that Scottydog and swim's buddy have access to the same pillstocks and I've suspected that they both dwell in somewhat adjacent vicinities (as well as sharing a past love of bands like Anthrax, SOD and the Mentors) for quite some time now.
erections lasting more than four hours, although rare, require immediate medical help
(Hive Addict)
03-01-04 01:39
No 491924
Thanks Chemo, good to know we are on the same page here.
It really is beginning to make me wonder if pre-cleaning 120's is not only a waste of time but precursor as well.
If the newer gakk is in a hydroxide or carbonate form, preboiling in Xylene will pull some of the pseudo into the NP and it essentially gets decanted and flushed down the toilet with some of the PEG and other gakks.
Pre-soaks and boils have become common practice here at the hive. Monkey see, monkey do! The full turps continues to bee passed on from new to old and with this mentality (IMHO) "At least with the the generic 120's" we are encouraging others to waste their precious and increasingly valueable pseudo.
If bees can read between the lines from Swim's initial post, they will see that the game plan for extraction is all inclusive.
Either that or one can just crush, run a tetra trap, evap the NP down to a skin and decant the gakk. Run the freebase as is, or take the now "relatively" gakk free pseudo and titrate with fresh NP and water to get the salt.
Hope this helps others having similar difficulty.
This pillstock is the most widely available form of pseudo, hard to believe there wasn't more discussion.
I guess most bees prefer to "fight" over the popular brands at the grocery chains. Swim would rather work a little harder in the lab then do more traveling.
The gakk chemists can fool most bees some of the time.
Supreme White Powder
(Hive Addict)
03-02-04 23:57
No 492474
Thanks Chemo, good to know we are on the same page here.
The gakk chemists can fool most bees some of the time.
Situations like this thrust all bees on the same page whether we like it or not!
An old saying cums to mind for some reason...
"Misery Loves Company"
As for fooling the bees, that's why they get the big bucks!
Suspicions are confirmed!
It's new!
White 60's as well.
While there are ways to recover the goodz in a Freebase Form From Frontside (Four-F-Club
)extraction, as Sdawg suggests, don't anticipate everything to run smoothly during the back-side extraction....hahaha...just pulled that one outta my ass
The inhibitor will still be present and thwart post-rxn work-up.
Ibee even tried his hand at distilling and while limited skill may have had a hand in the outcome(steam burns! Yeeehaaa!), this gaak was still bee present following all three common extraction techniques! Gassing, titrating, and distilling.
The Freebase appearance while acidifying identifies it as an anti-xtalling agent as well as a pH adjuster.
The gaak is multi-faceted but the area that most will identify with is "Shittydope".
Some Buzz qualities normally associated are present in the end-result, but "Good As It Gets" feel off the back of the bus somehow.
More research is underway.
New Saga.....
The Polebarerz vs The Undertakerz
a little less conversation, a little more reaction
(Hive Addict)
03-03-04 01:36
No 492507
Not being pleased with the amount of precursor acquired swims buddy dipped into his PeG laden rainy day stocks (essentially the residual pseudo buildup from old, decanted acetone rinses) to up the amount. Rinsed the rainy day stock multple times with hot tone but was never able to get it sparkly white. Should have probably redissolved in alc and taken it through a full xylene precip/reX run.
Only ended up adding maybe 3 grams of the rainy day stock to the total for rxn. Rxn was a 37 hour LWR. It got the standard 3x xylene warsh, a kerplunked base-up job, 3 DH2O warshes of the NP and was finally titrated.
Titration pull #1 took ages to evap and so suspicion of PeG contamination immediately arose. After maybe 4 hours of evaporation time about 1 gram white substance was had. (rxn was from 18.5g of precursor) Bioassay revealed it was damn potent but had the classic peg odors during the long and lengthy vap. Attempt to reX proved fruitless.
There is a resonable bit more but it's still sitting titrating. Overall yeild, although not known yet, shows all tendencies to be awful, product seems non-reXable and takes a hell of long time to be coaxed out of non liquidness. Product is surprisingly potent considering all this though but this still ranks in as a somewhat botched batch.
Swim's buddy remains uncertain though if these results might be due to new gakkers or to the fact that the portion of the older psuedo may not have been clean enough. At the moment warami's comments are the only thing that seems available on making a judgement on this so until more 1st hand accounts come in there's not yet a lot to compare with.
Next rxn swims buddy will most likely dig in to his hallowed vaulted precursor reserves as not enough is yet known or understood of this new gakk animal.
PS. My sensibilities tend to prefer to name this particular face off the polecats vs. underdogs but it's all the same really.
erections lasting longer than four hours, though rare, require immediate medical attention
(Hive Bee)
03-03-04 04:30
No 492551
SWIW noticed the same chem found this past summer in the 60's now in the 120's. Weird thing is the exp dates can only be used as part identifier. This particular manufacturer producesgenerics for at least 3 different stor chains locally. The 2 isentifying attributes that are the same across all three have been the differnt design on the foil blister sheets and the font used for the code number on the side of the box. This number is printed with a "retort" or company logo to the left of the number. The boxes as of late that have at least provided a means of extraction and since the incorporation of the Laq thinner the end result as well as the workup have improved. Other than the increase in time, effort, $$, steps for less but cleaner psuedo.....ok it is a pain in the ass but wait til you run into the shit that not only masks it's way past the extraction but then the party in the flask looks a bit peakid and inactive then afet all that fuckin work bam...you get toothpaste green efervecent post reaction moss. Stock up now on the pills with the regular lookin font...the one that has the boxy square digital font will spiral you out of Kansas Dorthy!
(Hive Bee)
03-03-04 07:14
No 492568
Scotty,
SWIP has run into the same difficulty and thinks your speculation is right on. The most recent problem was with red hots bearing the following list of (disclosed) inactives:
ammonium hydroxide, carnauba wax, crosscarmelose sodium dibutyl sebacate, ethylcellulose, FD&C red #4, Al lake, fumed silica, hydroxypropyl methylcellulose, lactose, microcrystalline cellulose, oleic acid, polyethylene glycol, povidone, pregel;atized starch, silicon dioxide, stearic acid, sucrose, talc, titanium dioxide.
SWIP has been having good luck vaporizing FB crystals as though he were doing a sublimation, to get out the residuals left by the Ttrap procedure. He hasn't yet tried it without first combining other cleaning technics but will do so next round.
PP
(Of Counsel)
03-03-04 18:39
No 492676
(Rated as: good read)
Several of us have been pm'ing each other for the last few weeks about what we see as the new gakk. SWIG first saw it in a white 60's brand that was new to his area. Narrowing the hunt down to find out which white 60 was the one with the poison was simple, since Squidippy was having trouble with the same brand.
A test hypo reaction was done with just under ten grams of pseudo pulled from this brand of white 60's, which were pulled with the straight to E method after an overnight soak in xylene to remove povidone, an MEK.jd boil, two naptha boils, and an MEK boil. the pseudo so obtained was polished by precipitating in a mix of xylene and naptha.
The reaction was worked up by a standard a/b with xylene as the extraction solvent. The xylene was divided into two portions, one of which was gassed to salt out the meth, and the other which was titrated. There was no substantial difference between yields from either approach, and the product of each was the same poor quality. Yield was very low, in the 35% range by weight of the precursor.
The extracted meth was recrytallized twice.
Everything worked backwards. This is in fact a damned nasty gakk. It has a different look and smell than OII, does not appear to affect recrystallization to the extent that OII does, but definitely impedes the A/B extraction process.
Here are some observations from SWIG's first full skirmish with the new enemy:
Yields are very low. One batch was contaminated with this gakk, the second full of it. Yield from the first was low-- about 50% by weight; the second was horrible, about 35% by weight.
Quality of product is low Unlike the yield from OII gakked batches, (where the first pull usually nets excellent meth, but not much of it, and subsequent pulls produce almost no additional meth) each pull produced product. Four successive pulls produced product. The quality of the product was disappointing. There was meth in it, but not in high concentration. There are obvious non-meth components in the product. No unreacted pseudo is noted, no familiar intermediates are noted. This product does not produce the effects familiarly found with unreduced intermediates, nor did it have any tweaky characteristics. It is difficult to smoke enough to get high on. Snorting has little effect outside of irritating the sinuses. IV administration was surprisingly effective considering the low effects of other forms of administration, and the effect lasted well, but the quality of the buzz was lower than expected.
Meth in the nonpolar solvent wash water.In the two batches I know have contained this gakk, I recovered meth from the rinse water. I check the rinse water for meth if yield is sub-normal. Occasionally a little meth will find its way there, but I find it in maybe one of ten times I check for it. I found a half a gram in the water used to wash the extraction solvent in each of the last two reactions. This is very unusual in my experience.
rebasing the reaction fluid. Looking for the missing yield, I filtered the based reaction fluid through a single coffee filter. I dried the solids, then mixed them with xylene and allowed them to stand. Later I decanted the xylene and gassed it. I recovered about a gram and a half of product from this xylene. The filtered reaction fluid was clear. This surprised me. I based it with dry NaOH just to see what would happen. The solution went milky white. I added xylene and let it sit for about twenty minutes. I gassed this xylene and recovered nearly a gram of product reaction fluid filtered clearly through one coffee filter.
A second pull produced nothing. I filtered the reaction fluid again. It again filtered to a clear solution. It again went milky white on basing with NaOH. This time it yielded about a half a gram of product. The fluid was filtered again, based again, and gassing produced about a quarter gram of fine spike like crystals that resemble meth crystallized in acetone. These have not been sampled. The filter cake from the latter basings did not produce additional product.
strange crystallization experiencesThe meth from the first four extractions was recrystallized with ISO and acetone. The first pass produced some white powder in the beaker but no crystals. The motherliquor was combined with the acetone used to rinse of this powder, the solution reduced to saturation, and chilled. This produced crystals of a size and shape I usually see on the second time I recrystallize the meth. A third harvest of the motherliquor produced crystals which looked like coconut flakes. (Usually by now all the meth has crystallized out, but this still had meth in solution that had not crystallized). The next two harvests of crystal were what I normally expect on the first crystallization-- as to shape and type of formation. The sixth harvest left very little motherliquor and I elected to evaporate it until very saturated. As soon as the liquor was removed from gentle heat, crystals formed. I added acetone, expecting the whole to dissolve as it will with OII gakk. None of it dissolved. I poured off the acetone and sprayed some TCE into the beaker. The TCE was mixed with the crytallized contents with a glass rod, and it took on a brown color as the crystals turned whiter.
Normally I expect to get good sized crystals on the first two harvests and to get a few on a third chilling of the motherliquor. I had crystals of one type or the other form on each of seven times I reduced the liquor to saturation on the first crystallization. I have never had the crystallization drag out like this.
The second recrystallization usually yields a fast harvest of large crystals that are flat and irregularly shaped, which break into what I call "diamonds" fairly easily. I dissolved the crystals from the six harvests of the first pass at growing crystals in MeOH and reduced to saturation, added acetone, and chilled. Two hours later I checked and absolutely NOTHING happened. I assumed I had not reduced to saturation after all, and gently heated the alcohol/meth/acetone solution. As it warmed white gakk began to precipitate out. This was really surprising. This did not happen the first time I grew crystals, and I added nothing to the crystals but the MeOH used to dissolve it. The stuff falling out of the solution was filtered out twice. As the solution heated more, another precipitant appeared and it was filtered out. Satisfied that the solution was saturated with product, I let it cool, then chilled it. Two hours later crystals similar to those I usually find on a first crystallization had appeared in the beaker. These were harvested, rinsed with MEK (ran out of acetone) and the MEK and motherliquor reduced to saturation. This sat overnight in the refrigerator. To my morning surprise, this produced no more crystals. I had a little over a gram of crystals from the two harvests the night before, and had dissolved not quite four grams of product when I started the second pass. Later I reduced the solution to saturation and noted clear solids forming on the beaker sides, with thin layers of meth appearing on the sides of the beaker as the alcohol and MEK evaporated. Again, this would not produce any crystals on standing and cooling, or on chilling. The solution was again reheated to a thick consistency, but still no crystals formed, even after chilling in the freezer for a couple of hours.
I decided to try to precipitate the meth in xylene, and added MeOH to the solution. I heated the xylene to 110C but the only thing that precipitated was a white powder with no taste that was not meth. The xylene cooled without any crystals forming. Solids appeared above the fluid line in the beaker which were clear; these dissolved in the xylene when it was swirled in the flask. The xylene was placed in the refrigerator overnight. Nothing had formed in it by the morning.
The second pass at crystal formation resulted in a little over a gram of product from what had been three and a half to four grams. It has little taste, does have a mild effect, but is not what I would consider worth smoking.
Odd results from gassing I tested a sample of the extraction solvent by gassing a thirty ml sample; one squeeze of the gas bottle was all it took to turn the 30 ml into applesauce. After I filtered, nothing more came out of the sample. Period. When I gassed half of the remaining solvent, it turned to applesauce very quickly. This was filtered out. Subsequent gassing produced a little product on the next attempt, then nothing else.
Violet tinge? The acetone rinses were evaporated until they were thick and these had a slightly violet tinge (as opposed to orangish color when OII is involved). It has a distinctive smell I cannot describe easily. It is less noxious than OII, almost like it has a sweet hint to an otherwise acrid smell. The odor was distinctively not that of OII.
Quirky a/b effects The other batches I have encountered this gakk in have all had quirks with the a/b method. One is the presence of meth in the rinse water. Another is that the pH of the solution, once based, tends to creep back down; yields are down for the a/b overall. The a/b seems to leave meth in the polar layer, trapped in solids, or not freebased.
Note that this gakk has shown up in pill masses extracted to avoid OII gakk, and that OII gakk has not appeared in either. In these batches, the principle OII gakk breaker has been jd, although in one the basic washes of the pseudo freebase were employed, and the grey emulsion did fall out with the plain water washes.
I suspect this is the new gakk, and it appears to target the a/b extraction process. This one also kills yield, but additionally reduces the quality of the product. Orange II killed yields, but what yield you did get was usually good. This stuff kills yields and fouls the product. I see a future full of bald headed meth cooks-- everyone is going to be pulling their hair out with both hands over this one.
I urge other bees to post the observations they have dealing with this gakk to learn more about it and find a weakness to exploit. OII took some time to figure out. This gakk will likely take more effort to solve than OII did. It may call for new approaches to extraction.
We need to pool our observations to find a weakness to exploit. If we do not hang together, we are all going to be sleeping a lot longer than we want.
mostly harmless
(Stoni's sexual toy)
03-03-04 18:49
No 492680
Time for some chromatography trials, don't you think so?
I'm not fat just horizontally disproportionate.
http://tinyurl.com/3kdu
(Hive Addict)
03-03-04 23:33
No 492786
I have nothing to add to geez's summation as they mimic Ibee's observations over the last 5 weeks!
I do agree with Os's suggestion and those most interested and following the board recently will recall some hinting and urging at bees to start looking more into the chromatography and brushing UP on research in that area.
As a final push, this gaak forced Ibee to include a method of extraction that he wished he'd been doing all along so he'd have a better handle on it now.
I know it's been repeated here countless times about hw simple and fast steam distilling is.
Well out of all the post-rxn extraction methods Ibee threw at this crap, distilling produced the best results!
Albeit....this was the crudest distillation ghettorig imaginable(no small wonder there eh???) But the elders would bee proud of the Kidz if they had seen them in a action.
It would appear that what geez describes as a violet tinge coloration was left behind after distilling. Ibee was too frustrated to attempt bringing the M-oil obtained to a hcl salt and Buzzed around for three days on the washed FB oil obtained from distilling.
Ibee recommends this method of extraction to all bees and it's simpler than you think! Especially now until a workaround is found that completely rids this gaak.
Ibee had mental blocks for the longest time about distilling that kept him from attempting what others had been suggesting all along. It was easier to stick with the old familiar...or so he thought! He was wrong!
And it didn't help seeing all those complicated diagrams of those New-fangled Do-Hicky steaming Rigs others proudly displayed after building.
Distilling is a peace of cake!
If Geez could get that master pick-uptruck mechanic SWIM to employ a distill on the next post-rxn workUP, he'll have a better rounded view of what bees are dealing with.
The next few will result in some new findings as Ibee has some ideas on what might defeat this gaak!
In the meanwhile, Ibee urges AWE bees to follow Osmiums suggestion. Those runs that are contaminated with this gaak, Ibee suggests steam distilling the basified solution, washing the oil obtained with dh2o(follow proper procedure there as Ibee isn't positive about that part) and then extract oil into NP and either titrate or gas to hcl.
a little less conversation, a little more reaction
(goat)
03-04-04 02:24
No 492838
swimmy dreamt of a tetra-trap on 20 gm precurse; first pull was pristine; should have taken it and run, but it was less than 25% of what should have been there.
swimmy's efforts to retrieve the missing motherlode unleashed monsters from hell; which, unfortunately, were added to the first pull for the sake of convienence, considering the nano nature of the dream, and were devilishly unwilling to depart despite all the manipulations of a guy whom is alot like mcguyver.
is it innappropriate to say, in this forum, that
it simply isn't worth the hassle?
(Hive Addict)
03-04-04 10:33
No 492914
Thanks bees for sharing your nightmare horror stories.
Swim has had a couple failed PhosAcid syths when 1st dealing with this gakk. It makes one think that the PhosAcid is old or that too much water was used in the rxn. Bottomline is if this gakk is present, the rxn will fail to kick off.
Swim has theoretically worked out the bugs.
***Short and simple***
A) Grind pills and perform tetra trap (Do all 3 pulls) Vacuum filtration makes ALL the difference
B) Dry over MgSO4
C) Gass out the freebase (Which should really bee pseudo HCL but isn't)
D) Filter the freebase from the now gakk ridden NP
E) Scrape FB from coffee filters into visionware
F) Recrystalize with Xylene by mixing, evaporating to a skin, cool to room temp and decant off xylene/residual gakk combo (Repeat if necessary)
G) Scrape FB from visionware pan into fresh mason jar
H) Titrate with muriatic dropwise until ph of 6 or lower is reached, isolate the polar, filter through charmin and evap to get the salt form.
I) Wash with dry acetone.
50% yields are clean and realistic. Last 60 box dream of generic 120's yielded 77 gs.
The shelves look empty in Swim's area. Makes him wonder how much of it is getting flushed down the toilet in disgust?
Refuse/Resist
(Hive Bee)
03-04-04 17:15
No 492951
Thanx for laying it out so simple ScottyDog! This should help many bees.
Ware, do you mean by following Osmiums advice that all bees should pursue column chromatography? I agree that is definetly a solution, but is beyond many bees dreams.
EDITSwim was referring to the price of a column. Sorry for the misunderstanding.
absorb what is useful, reject what is useless
(Stoni's sexual toy)
03-04-04 17:45
No 492959
> I agree that is definetly a solution, but is beyond many bees dreams.
Why? Because it requires reading a lab chemistry book with complicated words in it?
I'm not fat just horizontally disproportionate.
http://tinyurl.com/3kdu
(Hive Bee)
03-04-04 18:43
No 492966
strange crystallization experiences
With mix batch dreams of late rxtling has been carried out in dh20 and tone. SWIW has been titrating and using a multidish setup in the micro for drying. Sometimes things that would not crystalize in the past with convection heat, snapped right into shape in the micro. Remember that when forcing it dry it gives off extreme heat as it crystalizes. So if you are using an old dish with scratches and scuffs and a wave is crystalizing in the dish as you watch with glee....tick tack BLAM the dish blows into 5 pieces then hits the floor scatering all over. I can't recall the crystals in the past putting off enough heat that there progress could be tracked by touch from the bottom ov the dish. Ouch hot!
after the titrated candy is dried not tone yet, dry it till it forms crystals but one can observe a slight liquid phase underneith in areas here n there. Then with cooling in between each burst hit it in 7 sec intervals till those last areas with moisture buble up like shaving lather...now hit it with tone. Extra will be needed. Often they will apear as you said like "coconut flakes boiling wildly in the tone. Swiw has observed that allowing them to remain in the tone or even a short micro boil in tone brings that phantom of the methera to a halt!
Let the bitch start it's meth nabing a little bit while all is still hot. Quickly pour all through cotton so as to facilitate fast drainage but not a plain surface such as a coffe filter...that acts as a spone hideout. Ever notice when titrating if you filtered the liquid phase through some prewet cotton it would hold back the np that was in the mix. Same principle applies here. Near as swim can tell this phantom does as designed and travels allllll the way through to the end. There in it's (acrylic??) form it disolves in tone even beter when still wet still better yet when overly acidified. Sometimes it will take on a pink hue in acidic conditions. Then there before you eyes it uses the cloak of the tone and snatches the meth (bonding?)that in turn disolves. Maybe it's iodo you say or perhaps it wasn't meth to begin with... Wrong. Swiw has unleased this phantom on the "best stones in the garden" portions of street goods and personal stash have been placed in a few drops of tone..nothing hapens then with a syrenge a drop of the pink phantom was added and low n behold it looked like the wicked witch in OZ "i'm meltng melting!" moor to come gatta run for a bit
Os, I gotta admire you steadfast ability to prestent the masses with a problem solving solution. Swiw swears more study will go in the crmatography direction, aqually spent reading on fermentation and aeriating metaboli...damn.. just read it yesterday and already forgot. Why is it that even with your persistant advice we would rather spit in the wind to better understand such an invisible force that shawers our faces. Could be the deep rooted habit of trial n error. Or in my case just to damn dumb to figure out how to photagraph the solution with a colum!
(Hive Addict)
03-04-04 18:53
No 492967
Aside from the cranium busting lab books what's the bare minimum setup/apparatus one would need to realistically step into the chromatography realm?
Added edit concerning the new bitch-gakk on the block - whatever it is seems capable of getting both the pseudo and the meth confused about whether or not they are a hydrochloride or a freebase. It can tend to bring on somewhat of a chemical identity crisis for both precursor and final product.
erections lasting longer than four hours, though rare, require immediate medical attention
(Of Counsel)
03-04-04 19:01
No 492968
weaz: the one group of odd crystals formed in an alcohol/tone solution as it cooled. I am not forcing crystal formation by evaporation here, but letting the crystals grow in a cooling saturated solution. The last set of crystals fetched from the motherliquor was obtained by evaporating on low heat to the point at which crystals formed when the beaker was removed from the heat.
Unlike the OII gakk, which does have the effect you described of making an meth present soluble with OII in acetone, this gakk was not soluble in tone, and the tone did nothing to it or the meth. It appeared to be at least partially soluble at this stage in TCE. This was taken as one of the confirmations that I was seeing a different gakk
I only saw these flakes once in the process, and they formed in alcohol and acetone-- and were insoluble in acetone when first removed and rinsed with acetone. This told me I had something in the mix I had not seen before, because I have not seen that crystal formation before.
mostly harmless
(Chief Bee)
03-04-04 19:05
No 492969
../rhodium /equipme
As the separation of polar polymers from a small molecule like pseudoephedrine is a breeze, you can use at least 5x more "sample" per weight unit of silica gel compared to their table.
../rhodium/djvu /tlc.zubrick5
http://www.indiana.edu/~orgchem/movies/c
TLC tutorials to determine the best elution solvent to separate the pseudoephedrine. Also UTFSE for my name and "TLC".
The Hive - Clandestine Chemists Without Borders
(Hive Bee)
03-04-04 19:39
No 492973
I'm sure i'm wrong but this sounds simmilar to curve balls thrown at us in years gone by and near as I could tell it was similar in charactor to povidone. Post 470744 (weaz1dls: "Lights", Stimulants): Post 450895 (weaz1dls: "Square", Stimulants):
Post 466425 (weaz1dls: "Tic Tock!!", Stimulants):
Actually in 1996 there was a powder that could be isolated from the pills that acted identical to the ephed..looking back now I would place it in a catagory with MSM for properties.
This is why I sugested forcing it dry. under an overturned glass dish to cath all the steam.
setup; plate on turntable of micro, dish on top of that with and inverted bowl covering all. The steam will condense and run down the side of the bowl...some will escape the side but swiw uses minimal h20 in the first place.
anyway on the otherhand maybe you have run into that smelly toothpaste makin stuff, except you have succeeded where I failed in cleaning it to a point where it isn't so dominant in the end. This stuff wouldn't rear it's head till the adding of the acid to salt out the goods. Upon addition of the acid a floculant would turn the water to oatmeal either yellow or green with a eucaliptis minty chloro sheetrock smell...You will know it if ever you cross it. Also one thing all these botched rxns had in comon were fast n hot (tisk tisk) and exp date past 2006.
damn his typing sucks!
(Hive Bee)
03-04-04 19:46
No 492974
Obviously swim is very ignorant of this process and thought that obtaining the equip would be pricey. Hey Os, it is not because gluecifer can't understand complicated words! Gluecifer has never seen something that he couldn't learn! Please excuse my ignorance, but don't take me for a moron Osmium.
Rhodium provided an excellent response without trying to piss someone off, hmmmmm wonder how he does that? I guess it is just normal for Os to be a smart ass.
Besides ScottyDog has a proven method to deal with this current gakk.
It still works for 120s in my town and ggggrrreat on the 240s.
absorb what is useful, reject what is useless
(Moderator)
03-04-04 20:07
No 492977
(Rated as: excellent)
Here's some more basic information on oolumn chromatography, as usual lab equipment is best, but the imaginative bee will realize that such a column could be improvised from materials they can scrounge up
Chemistry is our Covalent Bond
(Of Counsel)
03-05-04 00:18
No 493024
I get the hint. I think I see the future. At least mine. I believe its time for this old dog to learn some new tricks.
I'm still willing to learn.
mostly harmless
(goat)
03-05-04 15:56
No 493156
gotta admire the old dog spirit, but, by the time sophisticated analysis and seperation techniques are learned for shitty pills, they won't bee available at all.
may as well jump ahead to what lies beeyond the pills.
(Hive Bee)
03-06-04 13:46
No 493405
After trying again with 5 boxes of 30x60mg name brand whities my results were even worse, but i take the blame for that because instead of soaking in np for 12 hrs i went for 6 hrs(waterless a/b). At least this time it gassed but still took 1 1/2hrs to get everything i could and what i got was a pile of sticky goomp. After pouring about a litre of acetone from the freezer through it, it was a little better but not much, so i put the sticky goomp into a 1000ml pyrex chem bottle with approx 400ml dry 99% isopropyl brought to the boil and then added 400ml dry acetone and brought back to the boil, then capped and left to cool to room temp then fridge then freezer. Me being a nosy fucker i didnt leave alone, i shook it and whatever before filtering and ended up with a dirty sticky ball of goomp for pseudo so i rinsed with fresh cold ace(all my solvents are pre dryed) and set aside. The ace and iso i used to rextalise was returned to freezer to see what else would evolve this was 2 days ago. today i checked and to my surprise the chem bottle had pseudo crystals stuck all up the sides of bottle, mine normally settles as a soft blanket in the bottom. After some serious shking of bottle i managed to dislodge the xtals. These crystals were like little 3 and 4 prong prickles. All up i recovered 3.3gms of pseudo out of possible 9.
i think with full 12 hr soak and more gassing or should i say use a lot more np in the a/b to gas the pseudo in. My feeling is maybe this sticky goomp gak saturates the np making it more difficult for the pseudo to be gassed giving it nowhere to go making it bond back onto the pseudo following it all the way through. IMHO i feel the amount of np used in a/b needs to be doubled if not tripled the amount supposed to be used already and likewise with rextalising. I only rextalised the once then returned iso/ace back to freezer to sit for a couple of days and was stoked to see what happened in my absence.
I have kept some of these aside(xtals) the rest is bubbling away at the present, so if anyone is interested in telling me how to upload picture step by step i will post one. I had a look at the upload page and sorry i'm not really computer literate enough to understand properly what i have to do. Xtals are small even minute but they are xtal clear and do not cling together.
I'm not racist,
I hate everyone.
(Hive Bee)
03-06-04 19:08
No 493447
seems you got clean product there eight ball.
Swim doesn't know why more bees are using ScottyDog's method. Gluecifer knows that it works on the 24 hr pillz because swim smoked the meth from them and found it to be up to par! Gluce hasn't even fucked w/ the 120s this week.
absorb what is useful, reject what is useless
(Hive Bee)
03-09-04 10:04
No 493898
Heres that picture of clean pseudo. Recrystallized once.
I'm not racist,
I hate everyone.
(Chief Bee)
03-09-04 10:13
No 493901
Could you please crop out the interesting parts of the picture? I don't think anyone here wants to download a detailed picture of your kitchen bench.
The Hive - Clandestine Chemists Without Borders
(Stranger)
03-20-04 08:58
No 496273
Have a look at http://www.chem.cuhk.edu.hk/labtech/inde
Clutch
(Stranger)
03-20-04 09:11
No 496275
Scotty,
You write
> C) Gass out the freebase (Which should really bee pseudo HCL > but isn't)
Is this what you meant to say? I think I know the answer, but how can it be? How can it be that you gasased with HCl, I assume, and ended up with freebase?
Clutch
(Hive Addict)
03-20-04 11:27
No 496288
CLUTCH Yes, exactly what I said. Swim gassed and got freebase! With the generic 120's, after gassing to the point where nothing more will precipitate, upon adding this crude pseudo "substance" to water and xylene and shaking it up, most of it will float on top of the water.
After then doing a ph test of the water, he got a reading of 10. He believes that it falls out of the solvent at a ph of 9-10. Why it is suddenly doing this, he has no idea but whatever it is, he believes may have something to do with this new gakk.
After all, if it was pseudo HCL, with the amount of water added, it should have completely dissolved in solution.
It requires an additional titration step with HCL acid to get the pseudo salt.
If you don't, well then you are stuck with yellowish paste.
Edit: Swim has narrowed it down to 120 pills with a 07/06 expiration date. These have a new font on a more difficult to open blister pack (thicker foil/plastic)
Swim also noticed on the perrigogo 60mg pills they also have this NEW font, could it bee that these possess the demon as well?
Refuse/Resist
(Hive Addict)
03-20-04 14:01
No 496300
Swim's buddy who can somehow legally mess around with such things passed me this note.
I've noted this same type of behavior in both extracions of psuedoephedrine and in the final reduced product and for lack of any better terminology have been signifying it with the term "chemical identity crisis". Which seems to have the substance in question not being certain if it's a freebase or a HCl salt and under differing environments displayig varying characteristics of both. This, among other things, makes final cleanup and purification by usual means a challenging and as-yet-unresolved process.
a fembee who gives a good hummjob - priceless - for everything else there's MasturbaCard
(Popular Author)
03-22-04 03:15
No 496536
This sounds a lot like something that complexes with and ties up the free base. If that's the case, then on a chromatography column, the product would be stuck to and ride down the column with the gak. Just speculation on my part, but it makes sense.
(Hive Addict)
03-22-04 05:35
No 496550
There will be many noticible differences to come.
The products they are incorporating as inactives, which coincidently are not going to be considered inert or inactive ingredients because they are part of the delivery system, have a shorter shelf life than all the previous inactives!
A few months ago it was relatively common to find 08 exp dates. Then all of the sudden this new gaak hit and now the dates are back down to 05 and 06.
Now we all know that they will pull stock on a secret recall basis everytime they unleash a new foilant.
Worlock was the first to advise keeping a close check on those dates and lot #'s.
When shifts are noted, then it meant trouble on the extraction front.
This delivery system thang kinda sux because it opens the loophole in their favor in regards to "Consumer Right To Know" labeling and non-disclosure if separate permissions are applied for and granted throug the FDA.
Almost two years ago Ibee started a Pill ID/Lot# chart at Chemhead in an effort to develope a system to combat certain gaaks.
It became a monster to keep UP with but alot of the complexities that surfaced taught us much.
We are at a stage now where the lot#'s and expiration dates are crucial to identifying what is included.
After much thought however, Ibee wondered if revealing this crucial data might somehow be reflected back on an individual poster by zeroing in on region or locale.
It's still not known and hence may not be the wisest move.
At present we've gone solely on characteristic behaviors of these gaaks as identifiers and until something consistant and more concrete is known, we'll have to rely on small batch testing to reveal what works on which pills.
Now in regards to lot#'s and batch composition, there may be a further hinderance in identification which may include multiple formulation spanned over whole lots which may taint large batch extraction.
Remember, a little of that shit can go a long way at tearing down the sought after if allowed to travel through extraction and make it's way to the end.
It's those resilent gaaks that they mark and target to avoid detection so they can sidestep even the most thorough extraction methods. Be it through encapsulation or coating, it's very nature and design is to remain one with the main excipient.
This reminder is only to drive home the importance of "Separation and Removal"
That separation process now involves a deactivation step that wasn't necessary until orangeII gaak hit.
Ibee thinks they flipped the switch on this new gaak that now gets activated instead of deactivated when exposed to the same solvents that commonly deactivated it before.
It's relatively safe to bet that there is no such thing as a Universal Cure anymore nor can one bee expected.
But...if it takes five lesser cures to effectively deal with the multitude of denaturants and adulterants until the pills are no more...then by god, the bees will deliver the necessary blows!
"Every mistake We must still be learning....
While My Guitar Gently Weeps"
a little less conversation, a little more reaction
(goat)
03-22-04 07:32
No 496568
wareami,
my friend, i was wondering if your efforts toward cleanliness had ever brought you to detergents?
i feel a wash-day miracle.
blue cheer
(Chief Bee)
03-22-04 16:41
No 496628
[I've] been signifying it with the term "chemical identity crisis". Which seems to have the substance in question not being certain if it's a freebase or a HCl salt and under differing environments displayig varying characteristics of both.
The proper term is "amphoteric" and is applied to compounds having both acid and basic groups. Take the amino acid glycine for example:
NH2-CH2-COOH
It has both a basic amine group and a carboxylic acid group. At very basic pH the acid group will become a carboxylic acid salt, making the compound soluble in polar solvents (water, and to some extent alcohols), and if the pH is adjusted to acidic the amino group will instead become protonated (= becoming an amine salt), also making the compound soluble in polar solvents.
It is just at a narrow pH range (usually close to neutral) this compound will be a freebase in the amino end at the same time as the carboxylic acid end is in it's free acid form. This is called the isoelectric point, and for glycine it is at pH 5.97. Depending on the molecule, this isoelectric point will be at different pH's, so imagine what would happen if they made a polymer with various different acid and basic groups on it, so that at any pH some of them will form a salt - there you have your polymeric gakk behemoth molecule slimying around your pseudoephedrine molecules, impossible to wash away.
The Hive - Clandestine Chemists Without Borders
(Of Counsel)
03-22-04 17:16
No 496636
A couple of us detected Orange I gakk recently in pills that had not had Orange I. These had previously had OII.
It occurred to us that as the extract approach differed from OI to OII to Eudashit, the companies may be compounding extraction by rotating batches with OI,OII and Eudashit in lots, so you never know what you have until you extract it.
Which means you do a test on each lot number, or you extract with the assumption that all three gakks are present.
I actually dreamed about recording lot numbers and listing which gakk was in which the other night. I woke up moaning about the the added steps that a cover-all-the-bases cure took. I can't say there is any real information to support this concept, or enough to even warn about it. It might be wise for each of us to look for the emergence of one of these three gakks when least expected-- for that could indicate if the gakk swapping by lot number is also something else going on that gives rise to more frequent lot numbers.
mostly harmless
(Stoni's sexual toy)
03-22-04 17:38
No 496644
> the companies may be compounding extraction by rotating batches
> with OI,OII and Eudashit in lots, so you never know what you have
> until you extract it.
If that is true then a little THIN LAYER CHROMATOGRAPHY (there is that evil c word again!) might help you in deciding which one is present.
BUSH/CHENEY 2004! After all, it ain't my country!
(Popular Author)
03-23-04 00:43
No 496715
If this was all there was to it, they would act as buffers, and when hit with a gassing they would all be in their acid state, or with xs base, they would all be in their base state...and the weaker base sudo or ephedrine couldn't compete with the strong base NaOH for spots on the polymer, or when gassed, the HCl should preferentially be absorbed over weak acid sudo HCl. In any case, an excess should overwhelm its buffer unless there is something more sinister involved...
I would like to add a further observation to the already excellent physical properties listed on this thread...
When the new pills are extracted after clean up and then gassed, the precipitate and left over solvent(toluene) are more unmanageable than I have ever seen. Rather than filter,
if the gassed toluene is then extracted into water, and after separating the toluene the water is based, crystals of sudo don't appear with Na2CO3 as basifier.
The best methods are always the simple ones. Chromatography will never be teachable to the masses. For this to remain a people's art, a simple and effective method of knocking out all the new adds must be pursued. I'm putting my bets on superheated steam. Regular steam distillation of ephedrine is borderline workable, and with sudo it just sucks. I'll bet steam hotter than it wants to be will carry the product out without wondering if the product in the pills is Orange Gak 1,2 or 3 or Eudrashit...and I'll bet it can be done on a stove top.
(Popular Author)
03-23-04 01:52
No 496735
Just thought I should add...when the Na2CO3 sat water was hit with NaOH, the most wonderful looking(I emphasize looking) flakes of pseudo free base fell out. This was with an orange looking original gassing. If this was all there was too it, it would just be another day. The orange shit stayed in the water. Has somebody discovered this already??
I should read more, but the kids want me to play so my screen time is limited...
(goat)
03-23-04 03:09
No 496751
swim hasn't dreamt a little dream since the one that was over-the-top agrravating and bad yielding; the same one that never did allow a pristine end crystal.
it had been months. swim is seeking a stim; decides, in the spirit of futility and shameless addiction, to mine the mbrp left-overs for a possible line .
this was a 3gm rxn, and swim had already rinsed the rp with boiling water post rxn.
this was a desperate act, like going thru a trash can for an old ciggarrete butt.
anyway, with the crassest chemistry known to man, and no washes, swim evaps down the water to find some gear that was far cleaner than its mother rxn's end product, with 6 washes; acetone cleaning, and several re-chrystalizations.
swim didn't weigh , but the bio-assay was a-1; 2 people, 2 times.
swim was stunned by this, and feels that there must have been something in the post-rxn work-up that brought out the devil the first time; which swim didn't repeat on this crude effort of squeezing a line out of garbage.
i don't get it.
(Hive Addict)
03-24-04 00:36
No 496911
One thing that's consistent across the board with the new gakker is that all seem to consistently report lower than usual yeilds in both extraction and in final product.
The major effect of this gakk seems to be that of making the precursor and the reduced product not entirely polar or non polar in nature. This means that anytime it goes through a process involving either a non polar or polar solvent another portion of it will stay with whatever solvent was used. Any polar or non polar washes will both rob you of yeild.
The advice to "save everything" has never been more applicable than the present moment.
Baby's in the bathwater.
PS Swims buddy recently let a beaker full of the xylene used in the final stages of a psuedo extraction/clean up evaporate fully. At the bottom of the beaker were some honkin' huge psuedo crystals.
Item description: combination hotdog warmer/sugar bowl
(Stranger)
03-24-04 04:30
No 496975
I continue to read the post of long soaks, multiple recrystallizations, a multitude of different solvent washes and boils and evaporations. Feel free to continue doing this, all ye who have success and find ease in this, but I had an ok time extracting pseudo from some red hots with very little trouble
What I did was:
-stick all the pills (306 pills, 30mg each) and placed them in a normal margarita type blender and blended to a fine powder. The red coatings did not break up nearly even closely as well as the inside and I removed the majority of the red coatings by passing through a mesh screen with fine holes. Only a few small flakes of red remained.
-This powder was put in a flask, 125mL of 99% IPA was poured in and flask heated until near boiling for about 2 minutes. This was supernatant was filtered through very finely divided perlite to obtain a perfectly clear slightly pink solution that when somewhat below room temperature begins to precipitate.
-This was all evaporated in the sun (30 minutes or so), scraped up and placed in a flask where an ambiguous amount of toluene (sorry, roughly 100ml) was poured in and heated until near boiling then pipet-fulls of 99% IPA were added while remaining near boiling just until all of the crystals dissolved.
-This flask was then placed on a book and allowed to slowly come to room temp (tons of cotton-like crystals slowly begin to form) , then placed in the fridge and allowed to cool further (more xtals), then placed in the freezer while I prepared a buchner funnel.
-The crystals were then filtered and washed liberally with freezing cold toluene, then allowed to dry. The mass of cottonballs (5.9g) that remained were a very slight pink, with a melting point of 179-183 (theile tube).
-The crystals were dissolved in 15 mL of water and 5M NaOH was added until the pH was around 12.5-13 (crappy pH papers) to obtain a crystalline sludge.
-25mL quantities of toluene were added and stirred vigorously in an attempt to dissolve the freebase (occasionally letting the mixture settle until some of the clear non polar could be sucked off with a dropper). This took many additions of toluene (approximately >150 ml, forgive me but I did not write this down). The remaining water layer was a foggy peach color.
-The foggy toluene that was collected was filtered,dried with sodium sulphate, then evaporated in an open dish under the kitchen hood (
) to obtain 4.4g of clear colorless rectangular crystals with a melting point of 119.(59% yield)
This was cake to perform, the only pain being evaporating the toluene. The crystals look clean as can be and are practically odorless (with a faint, and I mean faint, smell of toluene). Of course, I suspect it will lose that smell soon. I have not yet reacted using this purification product.
(goat)
03-24-04 15:00
No 497034
chemo;
in swim's bizzare find, the surprise wasn't that there was a tiny baby in the bath water, so to speak, but that the scraps were clean...even though the main rxn product was not. only difference was lack of np wash.
a ? on gassing while i'm here:
any one ever try gassing straight from a bottle of muriatic acid, fitted with a tube? or is that HCl too wet?
(i mean, the vapor that comes off the bottle)
(Popular Author)
03-24-04 19:25
No 497066
This gak certainly does have the ability to suck up NaOH. If to the water mentioned in my previous post, an additional portion of NaOH is added, then more square flakes of pseudo free base are thrown out of solution. Total yield of this crude material I would guess at 75% or so of possible.
(Of Counsel)
03-24-04 20:38
No 497073
Chemo's experience mimics my recent experience. I saw pseudo on the side of every container of nonpolar solvent used. Not much, necessarily, but in every beaker, ever bottle. The same thing was true of meth after the reaction. I had some limited success against the demon in the last batch, but still noted pseudo turning up everywhere it normally would not.
mostly harmless
(Hive Addict)
03-25-04 01:15
No 497112
This is the encapsulating effects of this new gaak.
It will settle out given time!
It has an active life and when it dies, it loses it's ability to retain the goodz...either pfed or meth!
If it's pulled along with the goodz when active, it will require alot of naoh.
It will also retain it's ability to hinder xtal formation.
When it deactivates over time, all the goodz will be there and will then again be allowed to xtallize.
Strange stuff!
InRe to charlies ? about detergents since we're on the squeakyclean baby bathwater subject.
The only foreseeable problems with using detergents in extraction are the same as using oils in extraction.
They are a bitch to get rid of once they are introduced into the picture.
There is no gaurantee that the detergent won't contaminate the goodz! Or create emulsions or introduce other locking agents when mixed with these newage co-polymers.
It's like how even soap residue on glassware can reek havoc on experiments outcomes if not removed first!
Ibee likes clean feedstock but doesn't know if he wants to GO the detergent route just yet!
a little less conversation, a little more reaction
03-25-04 04:05
(Rated as: insignificant)
(Popular Author)
03-26-04 02:06
No 497389
A friend of mine had some time to kill so he experimented upon the previous posts concerning this subject. As was noted earlier, if some more NaOH was added to the water precip media for the sudo free base, more fell out...His first move was to pull the old filter out of the freezer, and pour the new batch through the same filter to get them all together....the new batch and liquid(which had been in the fridge settling) dissolved half of the orginal batch of crystals as they filtered through. That really sucked. Then to see if superheated steam would work on sudo free base, he shoved them into a flask, added 20 ml water and a couple chips of NaOH to make sure the gak was based, and then inserted the flask into an oil bath. While it was heating up, a line from a pressure cooker was lead in(plastic connection to glass tube) and the oil was heated to 160 to 180C. As the water boiled down, the cooker started to spout steam. The steam was lead in as it boiled, and then to keep the flask from geting dry, plenty of water was applied. The water coming out smells like pseudo, but not enough to make crystals, nor enough to taste like pseudo. Dead end on this line of experimentation with steam and pseudo. It can be made to work with ephedrine, but sudo is a non starter.
(Hive Bee)
03-26-04 03:15
No 497402
unless i am remembering incorrectly. This property may be useful if the gak you are battling can be steam distilled...
(Popular Author)
03-26-04 03:46
No 497410
I sucked my head into this pathway because I have numerous refs for steam distill of ephedrine, and have tried that one. If you have ref for no distill of pseudo, would you share it? Then forevermore I shall be less of a Raven.
(Hive Addict)
03-26-04 04:26
No 497417
Steam distillation of pfed have failed miserably by all reports and that is what makes that method distasteful to most.
Not one of those accounts however have persuaded The Kidz that it can't bee done.
The problem always seemed to stem from the endeavor pulling all the gaaks and inactives along with the pfed.
Fractional distillation should work but Ibee has never heard of a crafty enough bee building such an apparatus.
He's game as he needs to refine and build on his nonmenclature skills anyway.
It's only a stonethrow away if the imagination doesn't poop out first.
Those unturned stones may seem distasteful at first until a treasure of forbidden fruit is revealed.
It's much like the obstacles to TLC and having the blueprints spelled out before anyone is willing and able to put it into practice in such a way that a method is devised in laymans terms that will lead the pack.
After AWE, two years ago, who'd of thought that a bee would need an equilancy degree in chemistry just to be able to separate a freakin pill from it's adulterants and polymerscience playmates?
Uncle Fester has a head start and it may just be a matter of putting heads together!
I've said it before...the knowledge is available for those that ask the right questions with half a degree of intelligence and a plan of attack.
The groundwork is layed IMHO and now it's time to get to work on some of the stumpers that others fell short on before.
A mini fractional distillation still????
Does any bee think that it would do the job?
If so....let's build one and put it to the test.
Wattayasay?
Ibee's Game!
a little less conversation, a little more reaction
(Hive Bee)
03-26-04 05:23
No 497426
why not try subliming the pills. It wouldn't take much to do this under vacuum (wide mouth flask with a test-tube in it for the cold finger and glass tube in a little other hole attached to a hose and a vacuum pump) doing the sublimation under vacuum would greatly reduce the risk of decomposing the pseudo. The basification preparation to do this probably should involve some magnesium or calcium oxide or hydroxides as these both won't react beyond pH levels (that is to say, they won't make a solution higher than 10 and 12.5 respectively once they reach saturation of the water) with the material when dry, as NaOH would - just add the dry MgO or CaO, a little water to get it damp, then gently heat it over a hot water bath until all the water is boiled back out, and maybe a little higher, but stay shy of 20 degrees below pseudo fb's bp. Then heat it to the bp of the fb and the cold finger will pick up the pseudo and crystallise it.
i can't see why this wouldn't work, unless pseudo decomposed more readily in the vapour phase to the extent of making it impractical, and in that case, vacuum might fix that problem.
I think this would work, because polymers have much higher boiling points than the precious... :D
Maybe do an a/b extraction or an alcohol extraction on the pills, acetone wash, all that, before doing the sublimation to reduce the amount of other things that can easily be removed from being sublimed with the precious.
If there is issues with stability of the pseudo at it's boiling point another means of eliminating damage would be to flood the sublimation container with inert gas, perhaps to be totally ghetto, flood it with your nitrous bulb machine ;D before sealing it up and running the sublimation.
(Hive Bee)
03-26-04 05:39
No 497431
Biotechdude is the king of steam distilling eph but he does it from plants...
(Hive Bee)
03-26-04 08:58
No 497464
haha, if he's the king..., Dwarfer is the QUEEN. Or is that the other way round!? Swix rates himself as the Petty Peasant
Steam distilling ephedrine is labourious and annoying at the best of times; but DOES work. Steam distilling straight pseudo would be even less sucessful, and would require superheated steam (ala Dwarjet) and or fractional distillation if the polygaak is steam volatile as well. However, it MAY work with the variables nutted out properly...
As a side, Swix's thoughts on the new Polygaak surround INTRODUCING a specie to which the poly gaak has a greater affinity for than pseudo. Like if an ugly chick wont leave u alone, introduce her to your ugly mate and leave them to have their fun together while u slink away undetected.
This hypothesis evolved as it seems polygaak does not stick around based on solubility similarities (to pseudo and meth) alone. It seems there is some other attraction forces between the polygaak and our fav amines. Then, if the introduced specie can interact with polygaak and 'bully' out the pseudo etc.., solvent separations may prove more useful.
Just a thought...
(Popular Author)
03-27-04 03:48
No 497614
It's an obvious solution, and probably wouldn't require any fractionation, but there are two problems with the approach. First of all, many folks work on scales of a gram or two or three, and that wouldn't even wet the insides of the glassware. Losses would be unacceptable. Secondly, it's gotten hard to find an aspirator that will pull down to 20 mmHg or so to make it easy to do a clean vacuum distill.
As to my call for references, I've read a bunch of references, and while they always state ephedrine is volatile with steam, I've yet to find one that said that pseudo was impossible to distill with steam. That made my experiment not only a fun adventure, but also an answer to myself as to whether it could be forced out with a lot of heat.
(Popular Author)
03-27-04 03:52
No 497617
I had the same thought myself a couple weeks ago, and wondered if ammonia would successfully compete with the gak. Then I thought about the problems of getting the xs ammonia out of the mix and said there had to be an easier way...
(Popular Author)
04-01-04 00:23
No 498347
Does anybody have a copy of this patent laying around?? I've misplaced mine for the moment. As I recall, the patent mentioned a plan to encapsulate gak onto bags which are primed to open up when exposed to solvent presoak followed by NaOH. As I recall, Eudragit was one of the pus bag fillers mentioned. I may be remembering wrong, but it's floating around my head and may suggest the way to extract without getting that crap into the mix.
(Chief Bee)
04-01-04 02:27
No 498380
We have [
The Hive - Clandestine Chemists Without Borders
(Popular Author)
04-02-04 03:02
No 498560
That patent generally describes what is now on the market, and I will look for more patents filed by likely suspects to see what else they have been up to.
(formless fortitude?)
04-02-04 22:57
No 498730
If what ware says about the shortened shelf life of this new Gak, is so.
Is it possible to somehow accelerate the ageing process?
UV light is the first thing that comes to mind.
Whenever you find yourself on the side of the majority, it's time to pause and reflect.-Mark Twain
(Hive Bee)
04-02-04 23:08
No 498735
this page talks about transport systems and pill manufacture process. Hope this isn't a repeat. Here is a bit followed by the link.
Post 0051 (not existing) In preferred embodiments, the polymer coat (26) will be insoluble in the fluid of a first environment of use, such as gastric juices, acidic fluids, or polar liquids, and soluble or erodible in the fluid of a second environment of use, such as intestinal juices, substantially pH neutral or basic fluids, or apolar liquids. A wide variety of other polymeric materials are known to possess these various solubility properties and can be included in the polymer coat (26). Such other polymeric materials include, by way of example and without limitation, cellulose acetate phthalate (CAP), cellulose acetate trimelletate (CAT), poly(vinyl acetate) phthalate (PVAP), hydroxypropyl methylcellulose phthalate (HPMCP), poly(methacrylate ethylacrylate) (1:1) copolymer (MA-EA), poly(methacrylate methylmethacrylate) (1:1) copolymer (MA-MMA), poly(methacrylate methylmethacrylate) (1:2) copolymer, Eudragit L-30-D.TM. (MA-EA, 1:1), Eudragit L-100-55.TM. (MA-EA, 1:1), hydroxypropyl methylcellulose acetate succinate (HPMCAS), Coateric.TM. (PVAP), Aquateric.TM. (CAP), AQUACOAT.TM. (HPMCAS) and combinations thereof. The polymer coat (26) can also comprise dissolution aids, stability modifiers, and bioabsorption enhancers.
Post 0052 (not existing) When the polymer coat (26) is intended to be dissolved, eroded or become detached from the core in the colon, materials such as hydroxypropylcellulose, microcrystalline cellulose (MCC, Avicel.TM. from FMC Corp.), poly (ethylene-vinyl acetate) (60:40) copolymer (EVAC from Aldrich Chemical Co.), 2-hydroxyethylmethacrylate (HEMA), MMA, terpolymers of HEMA: MMA:MA synthesized in the presence of N,N'-bis(methacryloyloxyethyloxycarbonylamino)-a zobenzen e, azopolymers, enteric coated timed release system (Time Clock.RTM. from Pharmaceutical Profiles, Ltd., UK) and calcium pectinate can be included in the polymer coat (6).
Post 0053 (not existing) A preferred polymeric material for use in the polymer coat (26) involves enteric materials that resist the action of gastric fluid avoiding permeation through the semipermeable wall while one or more of the materials in the core (25) are solubilized in the intestinal tract thereby allowing delivery of a drug in the core (25) by osmotic pumping to begin. A material that easily adapts to this kind of requirement is a poly(vinylpyrrolidone)-vinyl acetate copolymer, such as the material supplied by BASF under its Kollidon VA64 trademark, mixed with magnesium stearate and other similar excipients. The polymer coat (26) can also comprise povidone, which is supplied by BASF under its Kollidon K 30 trademark, and hydroxypropyl methylcellulose, which is supplied by Dow under its Methocel E-15 trademark. The materials can be prepared in solutions having different concentrations of polymer according to the desired solution viscosity. For example, a 10% P/V aqueous solution of Kollidon K 30 has a viscosity of about 5.5-8.5 cps at 20.degree. C., and a 2% P/V aqueous solution of Methocel E-15 has a viscosity of about 13-18 cps at 20.degree. C.
Post 0054 (not existing) The polymer coat (26) can also comprise other materials suitable which are substantially resistant to gastric juices and which will promote either enteric or colonic release. For this purpose, the polymer coat (26) can comprise one or more materials that do not dissolve, disintegrate, or change their structural integrity in the stomach and during the period of time that the osmotic device (21) resides in the stomach. Representative materials that keep their integrity in the stomach can comprise a member selected from the group consisting of (a) keratin, keratin sandarac-tolu, salol (phenyl salicylate), salol beta-naphthylbenzoate and acetotannin, salol with balsam of Peru, salol with tolu, salol with gum mastic, salol and stearic acid, and salol and shellac; (b) a member selected from the group consisting of formalized protein, formalized gelatin, and formalized cross-linked gelatin and exchange resins; (c) a member selected from the group consisting of myristic acid-hydrogenated castor oil-cholesterol, stearic acid-mutton tallow, stearic acid-balsam of tolu, and stearic acid-castor oil; (d) a member selected from the group consisting of shellac, ammoniated shellac, ammoniated shellac-salol, shellac-wool fat, shellac-acetyl alcohol, shellac-stearic acid-balsam of tolu, and shellac n-butyl stearate; (e) a member selected from the group consisting of abietic acid, methyl abictate, benzoin, balsam of tolu, sandarac, mastic with tolu, and mastic with tolu, and mastic with acetyl alcohol; (f) acrylic resins represented by anionic polymers synthesized from methacrylate acid and methacrylic acid methyl ester, copolymeric acrylic resins of methacrylic and methacrylic acid and methacrylic acid alkyl esters, copolymers of alkylacrylic acid and alkylacrylic acid alkyl esters, acrylic resins such as dimethylaminoethylmethacrylate-butylmethacrylate -methylm ethacryl ate copolymer of 150,000 molecular weight, methacrylic acid-methylmethacrylate 50:50 coploymer of 135,000 molecular weight, methacrylic acid-methylmethacrylate-30:70copolymer of 135,000 mol. wt., methacrylic acid-dimethylaminoethyl-methacrylate-eth ylacryla te of 750,000 mol. wt., methacrylic acid-methylmethacrylate-ethylacrylate of 1,000,000 mol. wt., and ethylacrylate-methylmethacrylate-ethylac rylate of 550,000 mol. wt; and, (g) an enteric composition comprising a member selected from the group consisting of cellulose acetyl phthalate, cellulose diacetyl phthalate, cellulose triacetyl phthalate, cellulose acetate phthalate, hydroxypropyl methylcellulose phthalate, sodium cellulose acetate phthalate, cellulose ester phthalate, cellulose ether phthalate, methylcellulose phthalate, cellulose ester-ether phthalate, hydroxypropyl cellulose phthalate, alkali salts of cellulose acetate phthalate, alkaline earth salts of cellulose acetate phthalate, calcium salt of cellulose acetate phthalate, ammonium salt of hydroxypropyl methylcellulose phthalate, cellulose acetate hexahydrophthalate, hydroxypropyl methylcellulose hexahydrophthalate, polyvinyl acetate phthalate diethyl phthalate, dibutyl phthalate, dialkyl phthalate wherein the alkyl comprises from 1 to 7 straight and branched alkyl groups, aryl phthalates, and other materials known to one or ordinary skill in the art.
Post 0055 (not existing) As used herein, the term "preformed passageway" refers to a passageway or passageway precursor that has been formed on the semipermeable membrane by mechanical means, such as by a laser, drill and/or etching apparatus. A preformed passageway is optionally plugged after initial formation, such as depicted in FIG. 6. If a water soluble plug is used, the preformed passageway will increase in size even after all of the plug has been removed from the preformed passageway. The term "preformed passageway" is not intended to cover pores, holes, apertures, channels or other similar structures formed in the semipermeable membrane by incorporation of pore formers, water soluble particulates, or similar materials known to those of ordinary skill, into the semipermeable membrane during manufacture of the osmotic device. The invention does include, however, an osmotic device having a preformed passageway and one or more other pores, holes apertures, channels or other similar structures known to those of ordinary skill.
http://appft1.uspto.gov/netacgi/nph-Pars
also it apears that electrolytes and sodium ions assist in absorbtion of nutrients into the blood through the intestine.....hmm salt water eeh?
Water and Salt:
Most of the material absorbed from the cavity of the small intestine is water in which salt is dissolved. The salt and water come from the food and liquid we swallow and the juices secreted by the many digestive glands. In a healthy adult, more than a gallon of water containing over an ounce of salt is absorbed from the intestine every 24 hours
(Stranger)
04-03-04 10:16
No 498821
So, once upon a time there was a pile of psuedo freebase (extracted from red hots) that was already ok for use (but the hcl salt was preferred) and a pile of hcl needles extracted from generic 120s that I assumed to still need a little help in purification.
First of all, when once the freebase mentioned above was still the hcl salt, it was in the form of fine white cotton like needles. The same method used for crystallizing the hcl from the 120s resulted strangely in larger prettier more pristine looking crystals.
Second, the freebase from the red hots required large amounts of warm toluene to dissolve (about 35ml/g) while the freebase coming from the aqueous solution of the based 120 pseudo seemed to shoot straight into supernatant warm toluene at about half the amount that was required for the other freebase.
Third, when gassing the red hots toluene solution, very fine flakes of pseudo hcl were produced and quite quickly while when gassing the 120 toluene solution much larger particles were formed that seemed to flocculate, were much easier to filter, and seemed much harder to gas out. Both looked the same as a dry filter cake: dense white pearlescent stratigraphic (or flake-like) clumps.
In reality there is no point in stating all of this, because both of the end products seem to be uber-sue and perfectly fine for reactions, but the whole difference in behaviors sure threw me off. I did not measure the amount of tol it took me to extract the red hot freebase to begin with but I vaguely remember it being quite a bit as well, so I do not think that the reason for the difference is that one was above water.
-lux
ps. I've noticed it to be very useful to have the red color from red hots in order to track the degree of purity, and moreover show the relative pH of my solution when titrating (cherry red in acid to weak tea in base). I've actually been thinking of throwing in a few intentionally in batches of 120s before purification so I can see what i'm doing .
(Fragile ego)
04-03-04 10:45
No 498826
Do the standard wash procedure.
Then extract freebase suzy/gakk. Acidify with H2SO4 and isolate the Sulfate salt. Wash this and then extract freebase again and gas.
Just an alternate idea that that poped into my head.
http://www.democracynow.org/ - The Exception to the Rulers
(Newbee)
04-14-04 05:07
No 500717
Scottydog: Please, Any new oppinion's of these new 120's with just methylcellulose,magneisium sterate,silica,talc and cellulose "listed" as inactive ingredients.Or any new break-throughs on your 120's?Mine cause tiny white specs in the rxn of a 'e.rp.I2' cook. Or of the 120's you are working with.Thanks
The Walls of Ears
(Hive Bee)
04-16-04 08:45
No 501045
SWIP has occaissionaly thought about trying detergents, and did so once without much success. In light of recent research, however, it might not be too difficult to remove them from the mix as long as an ionic surfactant is used. Dishwashing detergent is ionic, if SWIP's not mistaken. Ionic surfactants can be more or less easily neutralized, as opposed to nonionics like out old buddy, polysorbate 80.
SWIP would have never guessed he was battling detergent! But the fact is, polysorbate 80 is one of the most difficult to remove from a solution. Many of the others are not.
PP
(Popular Author)
04-17-04 02:33
No 501162
I covered polysorbate there.
Fester
(Hive Addict)
04-17-04 03:17
No 501179
Popi: Ibee says try cracking the shells off 120's and using a fine seive screen or strainer to remove the shells first before doing anything else!
Ibee suspects that the shells are causing the condition described.
Also mnkyboy had a proposal to remove shells by soaking the tombstones in acetone until the swell and then screening the pills.
That write-up can be found here under the title "MnkyBoy's Cracked Pearls (Tomb-stones)"
../rhodium /pseudo.
Prepuce: Our Spudbuddy Charlie had recently brought UP the suggestion of using detergents in extraction.
The more I think on this, the more it might fall in line with my recent proposals to hopefully incorporate Oils in extraction as a first assault and then maybe using a detergent to rid the oil down the line.
Most detergents are effective degreasers!
Let the experimentation begin!
Sheeeeeesh....this could be torturous!
a little less conversation, a little more reaction
(Fragile ego)
04-21-04 19:45
No 502093
[blue]Popi: Ibee says try cracking the shells off 120's and using a fine seive screen or strainer to remove the shells first before doing anything else!
Ibee suspects that t
I think I read somewhere that the shells never dissolve in a full turps cure followed by a dry IPA extraction. I think I remember reading that.
http://www.democracynow.org/ - The Exception to the Rulers
(Of Counsel)
04-21-04 22:29
No 502124
I've taken them off, and left them on, when extracting pseudo from the 120's in a variety of ways. I frankly never found there to be any yield advantage to removing them, or any penalty in the quality of pseudo extracted, leaving them in. You lose some of the inner ingredients deshelling them. You lose some yield leaving the shells in the mix.
So what?
Granted, I usually extract these pills by an a/b process of one form or another, and consider them too gakked to extract with alcohol alone, all due deference to the more painstaking, and time consuming, procedures of Ibee and the Kidz. I'll take a cut-and-slash clean sixty percent yield of four hundred of them processed at one time and leave the shells on.
Mind you my opinion of acceptable yield has a lot to do with the time I wish to devote to that pursuit, to the amount of pseudo I wish to react, to the value of my time itself, and the cost of a gram of pseudo. I will trade five or ten percent of the yield in pseudo for less time involvemnt and clean pseudo. Why work an extra five hours for another twenty dollars worth of pseudo? Just extract more pseudo tablets to begin with, don't work it to death. Leave as much gakk as you can behind with a little bit of the pseudo as gakk magnets or gakk bait.
Struggling for that last five percent of the pseudo in an OTC product typically brings you into the sights of the foilants, and you get your reaction gakked. Its false economy to stress maximizing yields here. If you find a method and means to a lower yield of clean pseudo, take the clean pseudo and run to the bank as fast as you can.
Maybe its philosophy and not science, but some of the time we get so wrapped up in yield numbers that we forget the actual dollar value of what we are extracting and fail to realize that we may be gakking ourselves by insisting on high yields.
When I first started extracting pseudo, I extracted it from the carcasses of pills which had been ground, put in a coffee filter in a funnel, and had MeOH poured over them. One time. There was over forty percent of the pseudo left in the pills, and damn near all of the gakks. I had to fight the gakks, because I was trying to get all the pseudo that was left. The guy giving me his discarded powder--- he never worried about the gakks.
Granted that was years ago, but the principle still adheres. Make sure you aren't gakking yourself by pulling too hard. Its easy to do with any alcohol extraction method. Its much harder to do when you extract by an a/b method.
mostly harmless
(Hive Addict)
04-21-04 23:11
No 502131
Ain't what it used to bee!
I agree with Geez so far as getting in, getting the deed done, and baggin what's baggable with the least stress and exertion as possible. And he's absolutely right about getting in your own way sometimes by being too meticulous and methodical.
The reason Ibee suggests the removal of the shells now more than ever, is because of what they are including in those coatings since introducing the newest embodiment formulations that contain the polymethylmethacrylates and an onslaught of various other adulterants/denaturants.
Pill size hasn't changed!
They gotta put it all somewhere.
Since they have a need to cram as much as they can in each pill(multi-matrix), it's anybees guess as to which area of pill is going to contain what to screw a bees attempt at any given extraction point.
Ibee's philosophy hasn't changed in regards to getting what's Ghettable by removing what can be removed before attempting to isolate the pfed.
In short...it's not about getting the pseudo out.
It's more about getting all the shit outta the way so a pinwheel of light can be seen at the end someware!
>Its much harder to do when you extract by an a/b method.
Ahhhh Yes....but Ibee predicted that the end of the frontside A/B is very near if not hear
Honestly...I hope bees don't think Ibee's been playing with AWE those exotic chems and solvents AWE this time for his health
!Remember the medical device replacements for delivery system invention. It will make the difference when researching what's revealable on the consumer bee level.
a little less conversation, a little more reaction
(Of Counsel)
04-21-04 23:59
No 502140
The reason Ibee suggests the removal of the shells now more than ever, is because of what they are including in those coatings since introducing the newest embodiment formulations that contain the polymethylmethacrylates and an onslaught of various other adulterants/denaturants
Odds are that if it is used in the delivery system, its with the pseudo, not the shell. Think about it. If the pills are formulated as the literature on methacrylates you posted describes, the last place you are likely to find it is the shell. The methacrylates, by the literature you provided, are integrated into the delivery system and are going to be with the pseudo.
I'm not real sure the 120's are gakked with methacrylates yet. I am about to find out for sure.
mostly harmless
(Newbee)
05-02-04 03:50
No 504272
Thanks Guys,Swip has been pulling too hard.Dam !And I know now that the pricks down here are not listing all "inactives"!!There is Providone in them,because it went to gel if there was no soak.Now swip learned another costly lesson!What next:?
all fed up
(Stranger)
05-06-04 01:06
No 505128
Hello Geezmeister and brother Bees ;?D,
New guy here, tho I've been studying quite a lot this past couple of months and I'm ready to give this a whirl (2nd try actually as my first was snafu'd due to pure unadulterated dumbness, lol).
I've stocked up on a batch of generic 120's but can't decide which method to use to extract the P. I used VE's STB and it worked well enough for my first go (got close to 50% yield). But then I've stumbled across VE's STE method which looks just dandy - nice and clean, simplicity and elegance IMO. BUT now I've been reading about the new gakk and wondering now if either of these Universal methods will work??? Yeah, I'm so stuck now, head spinning as I trying to decide which way to go. I also read your last post stating that you didn't think the 120's had been gakked with the methacrylates, so I'd sorely appreciate it if you could point this noob in the right direction. Thanks for any info!
(Hive Addict)
05-06-04 02:15
No 505146
Swim can't advise Swiy as to what method he should use because he is not into conspiracies but the tetra trap extraction method and gassing for the pseudo salt works.
Swim has dreamed with STE on the 120's and results are not nearly as good as with the Tetra Trap. Gakk has a tendency to follow through using the STE on this particular feed stock.
Swim has dreamed with all recent extraction methods using 120's and the tetra trap is most efficient, both in terms of purity and yield. Swim is not sure if the methacrylates have infested this particular feed stock but one thing is certain, Polysorbate 80 combined with PEG and a dry matrix formulation is a bitch in its own right.
The coating on these 120's wreak havoc on the STE, that is of course if you like peeling a plastic top layer off of your pseudo after filtering.
Swim has been mixing his 120's with a particular brand of 60's that are rumored to contain eudragit, when performing the tetra trap with gassing and the extra titration modification step. (Even the most recent lot #'s with these 60's.)
60% yields of clean precursor.
IF "these" contain eudragit, they certainly go through an extraction and rxn, unscathed.
Have yet to dream of Fester's recent development using KOH because as of yet, it hasn't been required.
Hope this helps...
Refuse/Resist
(Hive Bee)
05-06-04 05:00
No 505187
how many times are you rexataling Scotty? Did you read Geez's post on rextal and the new gakk, apparently it lets go after more rextals than one is accustomed to.[
Post 503703 (geezmeister: "Rextals and the new gakk", Stimulants)
absorb what is useful, reject what is useless
(Stranger)
05-06-04 10:15
No 505248
Scottydog,
Thanks a bunch for that input!
Am finishing up the cracked pearl extraction as I type and will let you know how things progress. HOPING this second attempt will yield even a small success (all fingers and toes X'd, lol).One Q though, in your post you said, "Swim has been mixing his 120's with a particular brand of 60's that are rumored to contain eudragit, when performing the tetra trap with gassing and the extra titration modification step. (Even the most recent lot #'s with these 60's.)" Just wondering what eudragit is and if you're mixing the 120's and 60's for a reason, or is it simply what's available?
Also have found the writeup on the Tetra Trap and will be doing some lite reading before I hit the sack ;?D. Thanks again for your help and advice as this newbie sure appreciates the teachers he meets on the path to his Dream!
(Hive Addict)
05-06-04 14:04
No 505277
Fear
"Just wondering what eudragit is and if you're mixing the 120's and 60's for a reason, or is it simply what's available?"
Best info on this adulterant is found here:
Post 493344 (foxy2: "I'm sure this is the denatureing scheme your...", Stimulants)
Past extractions listed here at the-hive stressed that it was not best to mix pseudo pills, definately not dry matrix with a brand that can bee pulled with alcohol.
With the tetra trap it doesn't matter because this method is designed to not bee partial to certain brands or pill types. It is designed to conquer the worst of formulations.
Swim likes to mix pills containing PEG (without povidone) because these pills require no precleaning (soaks or boils) etc.
Swim likes to also match up a 2nd pile that DOES contain povidone because these pills WILL require a precleaning. Some of these pills contain anti-crystalizing agents. Wouldn't want to mix these with the 120's now would we?
You know its a sad day in hell when some 60's are known to bee more gakked then 120's but it is now a reality and has been for quite some time.
One particular brand of 240's contain both PEG and povidone. These can bee mixed with pills containing povidone.
Once you get the Trap down to a science, it defeats most formulations and opens up a window of opportunity to work with a variety of different feedstock, while before it may have been limited? Good point fear, sometimes a bee has to learn to work with what is available.
Newbees should become acquainted with this extraction now while it is still a voluntary choice because in the future, with newer formulations, it may become compulsary just to stay in the game? Something to think about.
Swim can't remember the last time he used a pre-clean with alkie pull. If it is still possible, I imagine the pills are limited to rarely available.
120's USED to work with the tyvek extraction, so yes the formulation for 120's HAS changed. What that change was, who really knows?
We're an underground revolution working overtime...
(Of Counsel)
05-06-04 17:40
No 505323
My current experience with the 120's indicates that Scottydog's way of doing the tetra trap -- with a slow, low heat extraction of the pseudo into the solvent-- results in excellent yields. In fact, I obtained the best yields I ever have from an a/b extraction of 120's--- not quite nineteen grams of pseudo from 24 available grams. I used more xylene to extract the pseudo than Scottydog does, and add acetone used to rinse the pseudo filtered out of the xylene after gassing to the xylene before gassing again. I obtained pseudo HCl by gassing and had no freebase pseudo to titrate. I tried to follow Scottydog's titration step, but got nothing from the process except the pseudo HCl I had before.
As with most things too good to be true, the yield from the method was. Part of the weight is probably OII gakk, and a reaction of half of this pseudo resulted in meth that has signs of some OII type contamination.
The smaller volume of solvent Scottydog used to extract the pseudo may explain why our results were somwhat differnt, why he saw freebase pseudo after gassing in the filtercake, and perhaps why he didn't have OII gakk in his pseudo.
I do the extraction his way again to see whether using less xylene to extract the pseudo limits the extaction of OII. I used enough that I had no freebase pseudo appear in the solvent, and it may be that the precipitation of the freebase pseudo crystals in the solvent is important to the overall cleanliness of the pseudo. More trials to come.
mostly harmless
(Stranger)
05-07-04 23:10
No 505654
Well Swif just got done extracting the E from 4 boxes of generic 120's. Ended up with 5.2g from a (im)possible 9.6g's. Not certain where the rest went to but Swif has some thoughts.
Swif went with MnkyBoys Cracked Pearl method to remove the time release coating. Swif fucked up right out of the gate by not having enuf dry tone to do the job - he didn't realize how much it'd take to cover the pills in the bowl, thought he had JUST enuf and was in too much of a hurry to make more before starting. Ya, I know, DUMBASS!!!
One note, anyone w/XP using the cracked pearl method your input is welcome - Swif noticed that the "pearl meat" didn't just fall out of the tombstones as stated in MnkyBoys method. After dunking, swirling and shaking for 5 minutes in the dry tone, most of the meat clung tightly to the shells. Swif had to take a fork and hit/tap/prod the meat out which was not as easy as he expected and took a total of around 15 minutes. Disentigrated a large amount of the coating gakk in the process which ended up in the pill mass. Swif wonders if this has something to do with a new formulation/gakk?
So the pearl meat sat in the tone for over an hour (might be where some of the yield went, will ck the tone later) while Swif was making more dry tone BUT THEN he read a post about NOT leaving your pill mass in tone too long as it steals E.
Panicking a bit, he drained the tone. Now a second rinse was required and the dry tone wasn't gonna be ready for more than a hour, and Swif could see the pill mass drying up and was afraid any gakk might contaminate the the mass.
Then he remembered Gottagogo's post saying that usually, tone from a brand new gallon can was pretty much dry and he uses it often without drying. So Swif decided that, since he had a brand new gallon sitting there, he'd take his chances and use it. He did the second rinse and then let it dry.
Just as MnkyBoy stated, the next day there was a fairly thick layer of plastic-like crap that Swif peeled off and then used it to play catch the frisbee with the neighbors dog. Funny the dog didn't seem to want to bring it back the second time....;?D
Next Swif proceeded to extract the pseudo using the Tetra Trap - he chose this method on advice given by Scottydog and Geezmeister due to concerns on Swif's part about all the talk about the NEW DEMON GAKK. Now Swif don't know if this is in the pill stock in his neck of the woods, but he didn't want to take any chances after all the work and expense and worry put into getting these danged precursors ! Plus, as Swif has stated in the past, he prefers simplicity (at least while he's getting his feet wet) and the tetra trap looked about as basic as it gets.
Now another note/Q for anyone with XP using the Tetra Trap. After adding the TCE, heating, then adding the Naptha and finally the DH2o, while heating/simmering the pill mass (mixed equally with sodium carbonate), the mix got all lumpy, looked like dry cottage cheese submerged in mostly clear Naptha! Now Swif's assumes this is normal but no mention was made in the synth nor could he find any info about this.
Well after doing 3 pulls (2 w/naptha & a bit of DH20 and the last with just naptha) on the pill mass and filtering this into his pyrex dish, it went into the freezer. 2hrs later Swif decanted and dried the E and ended up with the fluffiest, shiniest crystals he's ever seen. Sparkled like diamond dust!!! Much prettier then what he got from the Str8 to Bee method - no hard shit stuck to the plate or oily residue like he saw the first time. Swif did a bioassay (yeah he smoked some, well tasted it anyway ) and it tasted right and burned SOOOOO clean, not even the slightest trace was left on the foil.
The only let-down, albeit a small one, was the yield - Swif had hoped for a little over 6g's but 5.2g's is in the range. Now Swif's just keeping his fingers crossed that he can do as good a job on the rest of the process!
Now if Swif could just figure out if any of that new gakk is hidden in his lovely crystals....
Thanks for all the help ;?D
(Of Counsel)
05-10-04 18:52
No 506247
My last try with the 120's gave me pseudo that looked and burned very clean. I did not follow Scottydog's method to the letter. I extracted into more nonpolar solvent than he used, and I gassed my pseudo out of the nonpolar without any problem.
I also had pseudo that despite burning clean on foil was full of polymer gakk that impeded the reaction, gave me less than quality product, lowered my yield, and when smoked gave me gas.
Okay. I'm not completely certain about the last part. I am certain that my pseudo was not clean.
mostly harmless
(Hive Addict)
05-11-04 06:47
No 506362
Polysorbate 80 has to bee the culprit.
Swim tried using more NP and less pills per carafe as recommended by Geez and still ends up with pseudo that registers with a ph of 10 after filtering off the crude pseudo and mixing with water!
As mentioned in another thread concerning Polysorbate 80, these end effects match the symptoms.
The added titration step cannot bee avoided with the 120's!
If one simply gasses the NP after employing the tetra trap, filters, dry and then runs this crude product, he may very well end with what Geez describes above.
By employing this added titration step with FRESH NP and dh20, after adding muriatic until the water layer reaches a ph of 6 or lower. Some of this residual gakk will stay in the NP layer, while some of this remaining crapola will form at the interface.
This water layer is then filtered again through Charmin TP and THEN evaporated.
If one just chooses to gas, dry and then shortcut straight to the reaction, of course this residual gakk will find its way into the end product.
There is something to this added, once thought to bee unnecessary, titration step!
Like any of the other write-ups on this board, any shortcuts usually spells disaster.
As Swim has mentioned before, he combines pills of SIMILAR inactives. 2 different store brand 60's containing PEG, mixed with the 120's doesn't pose any problems with extraction.
If all else fails, after doing a tetra trap, evaporate the NP down to a skin, allow to completely cool, decant the yellow liquid gakk layer from the freebase, then titrate this FB to get the salt.
Tetra, 120's and sodium carbonate are still selling out in the aisles, so it must bee working for others. If Swim doesn't wake UP early enough, he has problems with acquisition.
Sorry you had less then superior results.
Refuse/Resist
(Hive Addict)
05-14-04 09:47
No 507093
Swim's buddy had been on a one batch per month schedule this year and had what he had thought were the finished and petered out lye water and naphtha for his March and April batches just sitting in separate flasks in a cabinet waiting for eventual recycling. Just for the hell of it one day he unstoppered the April flask and lo and behold it reeked of that characteristic fishy freebase fragrance.
This April batch had been older era pseudo that was been mined from past but not quite complete extraction endeavors but the batch itself had been tainted by residual gakks (most likely hiding out in the used but still cleaned RP from the March batch.
A titration was done and about 3/4 of a gram was pulled from the old naphta layer. The quality was OK but it was bordering on what I call "jawclentch junction".
Next the older March batch was uncapped and it seemed to reek even more than the APril. So the naptha was separated, rewashed and titrated and this one was a big surprise.
The March batch had been swims buddy's first run in with the new hyper gakks and it is what he is refering to prteviously in various posts within this thread.
He expected its results to be worse than the April batch but he was pleasantly surprised. It was top grade shit!!! Far from any junction of jawclench and rocked up (or is that cracked back?) good and proper in a borosilicate vessel of vaporization.
I think PappyEarthApple had a related but not identical incident occur that he mentions somewhere in this thread.
But it appears that the lye layer holds on to a portion of the yeild that it later releases. And at some point that chunk'O yeild becomes a completely freed former hostage from the super gakks.
So maybe if you let your based rxn just sit around for two months you'll end up with spanking clean product.
The Shiite has hit the fan
(Popular Author)
05-15-04 02:07
No 507222
My God...just this sort of solvent playing is what the inventors of these new generation of pills had planned...it will frustrate you forever. The polymers must be attacked and disarmed, and other approaches are a waste of time. Boiling KOH in alcohol (not anhydrous) does wonders...why back to this solvent approach?? This has worked for me, and others,..why continue this avenue. In reply give specific experimental details.
(Hive Addict)
05-21-04 02:19
No 508510
Swim changed things UP a bit this time and opted to try odorless mineral spirits with a fresh batch of generic 120's.
No pre-cleaning as usual and employed the tetra trap extraction method.
Swim noticed the coffee filters werent as full as usual after having simmered in the NP for 20 minutes per pull.
The extractions pulled alot of yellow precipitates after drying and gassing. After wringing out the sludge and titrating had to decant off a coffee colored gakk fluid.
Swim doubts it has anything to do with the decision to try a different NP but more towards what Geez was saying.
Looks like Swim got the last of the good 120's during the last extraction and the crapola has arrived.
The adulterants obviously hit Geez area first.
Swim is contemplating revisiting the 120's at another time and doing Wareami's "news flash blue streaker UP" prior to the tetra trap to see if this kills the crap.
Ya never know, Swim saw the worst of shit hit the blue 60's before all others. 120's have always been more available, guess it doesn't really matter anymore.
My apologies to Geez and all other bees for a method that without pre-cleaning may have now become obsolete.
Those pill fuckers work quick eh?
Japtetratone/purplepoison...
Refuse/Resist
(Stranger)
05-21-04 10:20
No 508564
Try spending 3-4 hours on mixing vigorously and gradually elevating the heat.
Use a 80:20 mix of naptha and mineral turpentine. He does this to ensure better pfed solvency at all phases of the warming process.
The 3-4 hours is where we differ I think, and I have a feeling you people use larger batch sizes.
tetra isn't used either, clearly such a powerful solvent, miscible with your NP (it is) is going to pull a host of stuff. Just like using alcohol as your basing medium does.
Same with DCM. There is just no way you are going to get a clear extract using something like that, it just makes life harder.
SWIM also uses a sprayer to introduce water over the 3-4hr period. With a mist you ensure that the top layer exposed to the non-polar is based first.
using a skewer to rapidly create narrow lines in the sand also helps with that.
SQuashes the pillmass on the final pull with a coffee plunger.
filters out all the "floating clouds".
separates the tiny basic water layer.
washes with a tiny amount of fresh water once.
horses for courses though, I've been known to get it wrong, but the yields are certainly clean and nothing to be upset about. 60 and well up.
a rinse with wet tone/h2o mix and some fancy evaporation plate shuffling work should make you hit the final opponents for 6 runs.
(But don't look at the crystals too long the glistening pearlescents can damage your eyes when it's too clean!
)
(Of Counsel)
05-21-04 16:29
No 508593
Wow, Shane. You almost describe what you do. And almost tell us the pills you use. And almost tell us what you base with, what you extract into, etc.
All of which seriously limits the usefulness of the information you impart.
I'm not criticizing your method... I don't know what it is. But if you want to chime in and help us with the problems we face... at least be clear enough about what you are doing for us to understand what you are doing. Otherwise, you are just posting advice without practical application.
mostly harmless
(Hive Addict)
05-22-04 01:49
No 508677
The birchers in Swim's area are still cranking out gear.
So I guess eudragit doesn't interfere with a birch rxn?
To stay on topic, then I suppose 120's are still fair game for the birch and it just may bee the way to go?
I suppose more bees will end up switching rxn methods?
Refuse/Resist
(Stranger)
05-22-04 09:30
No 508737
geez, sorry
Na2CO3, sodium carbonate. (As if I'd be talking about NaOH if I'm describing dry basing) The amount of base is the amount specified in the tetra trap method, about one to two table spoons per gram.
'what you extract into, etc'
I clearly state that extraction is done using an 80:20 combination of naptha (or colemans is fine) and mineral turpentine (not pure, not yellow, but residueless mineral turpentine).
The pills are varied, blue and white 60s are the best, because they are ground easily.
De-shelled 120s may work nicely with that method, but I have my doubts, it's like trying to grind stickly lollies, where the small pieces like to clump together.
But it hasn't been attempted because he operates like this: one box for a method, if successful he buys maybe 3-5 boxes of the same brand to aquire enough for a nanoscale.
Oh but, any crystalline gak that appears as pfed.fb does... I'm uneducated on. But nothing like this has effected anything important.
spraying, mixing as vigorously and as often as you have the patience for, time, and extraction solvent is the secret...which is no secret at all, it's common sense.
I thought I was clear, (1) do a tetra trap, (2) skip the tetra, (3) use a sprayer and not a spoon, (4) aswell take 3hrs to build up to temperature with (5) vigorous mixing with a wet skewer.
(6) Decant the first pull in to an appropriately sized glass bottle, fitted with a funnel and using 1 coffee (7) filter to remove the cellulose vessels (floating clouds...are ya with me?)
Now spend about 10-20min on the 2nd and 3rd pulls, again filtering through the same filter paper, which hopefully contained mimimal solids from the first pulls filtration.
On the 3rd pull, decant the NP sitting on top of the pillmass as you had done on the 1st and 2nd...but this time (8) use a coffee plunger or other similar implement to SQUEEZE out any remaining NP from the pillmass.
note this has been shown to also bring a small amount of basic water across which requires separation.
Now...(9) Look at your combined layers in the bottle, observe whether it is clear or requires further filtration.
I mean by all means try passing 120s through this technique, but the result Ill just speculate will contain residues of various colourations and descriptions which require rinses.
LAstly, if you do a tiny h2O wash of the bottle containing your NP, don't add H2O to your acetone for the plate rinse.
Well I do want to help, as you queried, but I didn't know how much detail you needed to get you on your way...
(Hive Bee)
05-22-04 09:44
No 508739
SWIW will try gassing at step g in SWIW’s procedure and post the results. Hopefully they will be a positive note here.