Author Topic: Problem gassing generic 120's  (Read 36087 times)

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Scottydog

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Problem gassing generic 120's
« on: February 29, 2004, 04:02:00 AM »
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!


ChemoSabe

  • Guest
Bad yeilding Won Twen Tees (Phony Pearly 120s)
« Reply #1 on: February 29, 2004, 11:18:00 PM »
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.


Scottydog

  • Guest
Hydroxide or carbonate form of gakk?
« Reply #2 on: March 01, 2004, 01:39:00 AM »
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.  :o

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.  ;)


wareami

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The Polebarerz vs The Undertakerz
« Reply #3 on: March 02, 2004, 11:57:00 PM »

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" ;D
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 :o  :)
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 :P




ChemoSabe

  • Guest
Unsure of What Brought on Which efx
« Reply #4 on: March 03, 2004, 01:36:00 AM »
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.


weaz1dls

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Digital Typing
« Reply #5 on: March 03, 2004, 04:30:00 AM »
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! ;D

Prepuce

  • Guest
Read any good labels lately?
« Reply #6 on: March 03, 2004, 07:14:00 AM »
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

geezmeister

  • Guest
the new gakk has arrived
« Reply #7 on: March 03, 2004, 06:39:00 PM »
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.


Osmium

  • Guest
Time for some chromatography trials, don't you
« Reply #8 on: March 03, 2004, 06:49:00 PM »
Time for some chromatography trials, don't you think so?


wareami

  • Guest
Drastic Plastic
« Reply #9 on: March 03, 2004, 11:33:00 PM »
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.


CharlieBigpotato

  • Guest
likewise, i'm sure
« Reply #10 on: March 04, 2004, 02:24:00 AM »
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?

Scottydog

  • Guest
Working the bugs out
« Reply #11 on: March 04, 2004, 10:33:00 AM »
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?  ;)


gluecifer69

  • Guest
Thanx for laying it out so simple ScottyDog!
« Reply #12 on: March 04, 2004, 05:15:00 PM »
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.


Osmium

  • Guest
> I agree that is definetly a solution, but
« Reply #13 on: March 04, 2004, 05:45:00 PM »
> 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?


weaz1dls

  • Guest
Geez
« Reply #14 on: March 04, 2004, 06:43:00 PM »
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! ;D

ChemoSabe

  • Guest
Aside from the cranium busting lab books ...
« Reply #15 on: March 04, 2004, 06:53:00 PM »
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.


geezmeister

  • Guest
Strange flakes.
« Reply #16 on: March 04, 2004, 07:01:00 PM »
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.


Rhodium

  • Guest
Basic chromatography
« Reply #17 on: March 04, 2004, 07:05:00 PM »

https://www.thevespiary.org/rhodium/Rhodium/chemistry/equipment/flashpad.html



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.

https://www.thevespiary.org/rhodium/Rhodium/djvu/tlc.zubrick5.djvu

(plugin at

http://www.lizardtech.com/download/

)

http://www.indiana.edu/~orgchem/movies/complt.mov



TLC tutorials to determine the best elution solvent to separate the pseudoephedrine. Also UTFSE for my name and "TLC".


weaz1dls

  • Guest
Geez
« Reply #18 on: March 04, 2004, 07:39:00 PM »
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 (missing)

(weaz1dls: "Lights", Stimulants)
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Post 450895 (missing)

(weaz1dls: "Square", Stimulants)
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Post 466425 (missing)

(weaz1dls: "Tic Tock!!", Stimulants)
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 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.


gluecifer69

  • Guest
Price/ nice response Cheif
« Reply #19 on: March 04, 2004, 07:46:00 PM »
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.