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.