Author Topic: New Straight to E -- a novel extraction tech.  (Read 68722 times)

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tpower9s2003

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thanks VE, ...and realizes it had another problem
« Reply #120 on: July 07, 2003, 07:41:00 AM »
It was commercial pool grade 98% sodium(oops) carbonate without indicating what the inactives were but just that the remainder 2% was inert. SWIT also remembered that its particles seemed really big, larger than any RD-lye, and even with vigorous stirring/shaking for about 5 mins most mostly spent time on the jar bottum, so he suspects better results with some surface area by grinding the pebbles to more of a powder then the oven dry. Still probably opt for excess amounts maintaining ratio with NaCl unless 99% IPA is available. Cant wait til tomorow funn shoppin, cause a 7+g rxn4 is underway


platcat

  • Guest
red bottle=yes
« Reply #121 on: July 07, 2003, 12:20:00 PM »
go ahead and use it.swips favorite.PC


mickyfinn

  • Guest
proceeding by the book - even then issues pop up
« Reply #122 on: July 07, 2003, 02:03:00 PM »
Okay, SWIM is going absolutely by the book, except for the glass stir rod (bamboo sticks) and the flask used for the initial boils is a 500ml rb boiling flask.

6x24 count generic 60's (half of SWIM 60's pillstock)

It took forever for the pills to dissolve on the hot plate and the initial 1/3 solution was at a rolling boil. At least 10-15 minutes, probably more like 30 and still some pills had not fully dissolved.

SWIM finally pulled the solution and filtered. Looks like he started with 130ml or so and ended up with...50-75 if that...

The next two 1/3 solution boils go more according to what appears to be spec...not much loss in volume, but some pills still have not fully dissolved.

And upon filtering the last 1/3rd SWIM found needles at the bottom of the glass used to contain the 3 pulls. The solutions was then filtered again into another container and then everything is being left alone; covered with saran wrap but left alone till some kind bee can clue SWIM in as to wtf is going on. The needles that were filtered out look like sugar, sparkling and in density in the filter but clearly looked like fred in the solution.

Trying to do this thing just as written but this doesn't seem to have been covered. ??

Off to sleep and dream of honey...someday


xboXer

  • Guest
anhydrous isopropyl
« Reply #123 on: July 07, 2003, 02:05:00 PM »
The big drug stores have it, you know the EMPORIUM sized stores. 99% can also be had at electronics supply, and easiest of all, internet drugstore pages.
The method STE is hereby nominated as technique of the year, catagory: extractions
For simplicity, and yeild, it is the best by far and away for pulling psudo. Fast and easy, thanx VE

(Also works with zyrtec 5s heheheheheheh)


ici_rhi

  • Guest
THANKS PC
« Reply #124 on: July 07, 2003, 03:06:00 PM »
rhi thought so..but was pondering, while waiting on oven fresh epsoms....
SwiM--on pills...what were inactives and what % ISO--91%,99%, as in drugstore not auto type(red-bottle)? Those needles you are describing,,,this info may help..Sound familiar but most may need that info just in case....


Scottydog

  • Guest
Yes micky
« Reply #125 on: July 07, 2003, 04:06:00 PM »
Yes micky!

There "May bee" pfed in both the filter and what passed through the filter.  :o

Want to know for sure?

Separate the contents...

Take the contents left in the filter and redissolve in meoh, shake and let settle. Also allow the contents that originally passed through the filter to come to room temp and refilter that solution. Take the now 2nd filter of pseudo + gakk and redissolve this portion in meoh, shake and let settle.

What is the common denominator between both piles?

They both MAY contain some gakk. (Esp if SwiY follows write-ups or attempts to modify it like Swim did)

Pfed is soluble in methanol, most of the gakk remaining at this point is not. Edit:(PEG or POV would bee)

Swim ended up having to do this in the end. There was insoluble sediment because Swim chose to pool everything together. *(Which he shouldn't have)*

Swim ran 4 extractions total. On one of them (the last one) he had to peel a plastic layer off the top of pfed. (exoskeleton plasti-gakk) That became a clue that a recrystalization was necessary. For some bees the gakk may not bee as obvious?

He then syphoned the meoh solution, run through funnel with Charmin and re-evapped for pristine needles.

Lost a little weight in the end. But makes for an excellent finishing step to make sure that you know exactly what you got.

Now it has been covered.

But then again remember, Swim didn't follow the extraction verbatim as was instructed.

He used 120's and if he would have pre-cracked the tombstones with acetone and filtered through a fine mesh metal screen (filtering off the plasti-exoskeletons) and dried the powder prior to extraction with dried IPA/naptha, this may not have been necessary.

Hope this helps with the 120's.

Some people discover helpful tips after the fact.  ::)


ici_rhi

  • Guest
Poor V/E
« Reply #126 on: July 07, 2003, 05:02:00 PM »
Seems like the S2E is becoming more complicated than it should on a daily basis!


geezmeister

  • Guest
not paying attention--damn
« Reply #127 on: July 07, 2003, 07:05:00 PM »
Why is it I get those offers to be a playground for idle hands when I'm not online here? Damn....missed again!

On a more somber note,  Scottydog's experience with the 120's suggests an alcohol soluble binder in the shells I think. I extracted some of these 120's by straight to E and realized something other than pseudo was in the pseudo. It was nice and white, but too hard, too firm, whatever. I did a xylene clean of the pseudo with about 5% loss in weight but no problem with the reaction (other than an unsatisfactory yield, which might be cured on the third pull if the extra is there) and no contamination of the product. Mirror interface, no emulsion. There seems to be a need for a little polishing up on the pseudo extracted from the 120's.


wareami

  • Guest
Crackin Skulls
« Reply #128 on: July 07, 2003, 08:46:00 PM »
Okay Geez:
Ibee had some real eye-openers regarding the difference between Large-Scale production and small testing scale nano size extractions.
Only til you're faced with such dilemma's, the problems solutions don't require much thought.
When working with 1000 tombstones, Ibee's method of skull bashing with a mortar and pestle are outta the question.
Mnkyboys Cracked Pearl technique is good if using anhydrous tone, but it takes a humongous strainer and some shit still gets through.
Most bees still chuck shit in the blender on large scale and this lets some shell through as well.
Here is Ibee's suggestion for such cases.
Ya Ready........STRAP IN....I mean it!!!!!
Take two pieces of hardwood plywood and wrap them individually with packing cellophane. Pour out yer tombstones Onto one of the sheets so all lie individually flat. Put the other piece of plywood on top and run a strip of cellophane around the sides! Then completely wrap both sheets together!
Lay the fucker flat in the driveway(preferably concrete or blacktop). Hop in the ride....strap in and drive over the bitch to crack all the tombstones!
Once cracked, the tombstones can be strained with a strainer.
The pillmass will fall through the strainer and the shells will be left in the strainer!
Just a thought....I think! ;)
Ya really want to eliminate those shells prior to a liquid phase extraction.
Peace of the reaction

Have FUN-Bee SAFE



mickyfinn

  • Guest
Pre Xylene phase psuedo crash - good fred
« Reply #129 on: July 08, 2003, 10:06:00 AM »
Scottydog:
Thanks for the insight as to most of SWIM's issue...the first needles that caught in the filter weighed 4G dry and when place on foil burned slowly with much white smoke and left zero residue. SWIM has been finding previous fred to turn orange on foil when heated. There was a familiar scent to the smoke...but SWIM doesn't know exactly why or what. Working on pulling the settled needles.

SWIM still has outstanding questions in regard to the length of boil and pillstock. SWIM is going to save the pillstock in case he may have to mix another batch of elixer since the pills didn't all fully dissolve even after 1 seriously long rolling boil and the 2 standard 1-2 minute boils for which s2e called.

It seems like the timing of the first boil was off spec and if someone can tell SWIM that a 500ml rb boiling flask instead of an elemyer made a difference then he will suffer his questions in silence, but it doesn't seem that it should matter for that part of the process. SWIM is using a 2000ml (yes 2L) filtration flask for the xylene crash phase...this allows plenty of room for the fred to crash, yes?

Off to filter the settled needles and do the first vm&p pull of SWIM's nano that's been sitting for 8 hours....how's that for patience?

EDIT 8 hours later

The second needles that had filtered *through* were very similar to the needles that were caught in the charmin plug initially. SWIM is going to add the xylene to the combined fluid and continue as per s2e.

However, SWIM thinks that the nearly 6G in needles that are already out will be dissovled in methanol (when procured from the store...the "HE*T" auto product is satisfactory, yes?) , as per scottydog, to see what appears to be fred.

Then, should SWIM do a xylene precipitation to be sure they are clean needles? Seems as if it would be a good idea...

He's tempted to just throw the damn 6G in a new rxn but will remain patient to be sure he doesn't jump the gun erroneously.


geezmeister

  • Guest
pill coatings
« Reply #130 on: July 08, 2003, 05:58:00 PM »
Mickeyfinn: Have you considered the fact that the pills you had may have been coated with a compound that does not dissolve readily? There are several brands like that. For those, you do not benefit by boiling the alcohol off before the coating dissolves and the pills fall apart. Might as well crunch them up and powder them before you add them to the solution, or at least let them soak to dissolve the coatings before you boil them. The pseudo is extracted by the alcohol; if you evaporate too much of it off you do not have anything to extract with, or not enough to extract with. You have to use enough alcohol to extract the pseudo--and that much has to be in the solution after filtering or you did not get it all.

Boiling the solution is more critical to gakk avoidance than it is to extraction. The boiling is only an indication that you have the solution hot enough for the naptha to do its job. There is no benefit to be obtained by boiling the pill solution and evaporating the alcohol while the pills are intact. Most crumble readily in the hot solution, but if they do not, break them up before you put them in the solution.


mickyfinn

  • Guest
by the book one time I recall...
« Reply #131 on: July 08, 2003, 11:13:00 PM »
Okay Geez...SWIM was trying to do this as Geez directed "just one time" by the book since he had used the microwave before so he just opened the packs and dropped in the pills. It didn't say to GUP them so SWIM didn't. These same 60's dissolved quickly in the microwave S2E two weeks ago...don't know if these are a different lot.

Just checked the manufacturer...they are perrigogos, white 60's not 120's but they are perrigogos. Will go over scottydog's methodology and attempt to follow the best course of action from here. Will also check to see if he went with GUP initially.

SWIM has 8 x 24 perrigogo 60's to run next and he will go GUP...then 60 count national brand 120's with blue writing are batting clean up GUP.


chronic_cook

  • Guest
SWIC came across some 99.9% dry ...
« Reply #132 on: July 08, 2003, 11:20:00 PM »
SWIC came across some 99.9% dry isopropanol and n-hexane, ths mixtures percentile is racemic. This quickly caught SWICs eye. n-hexane is a nice np. And 99% isopropanol is very valuable in the method of STE also. SWIC is very curious as to how nice they would play mixed together. Another curious question is, how would they fair with the introduction of ketones?  SWIC appreciates any info about this. It was defanitly something he wanted to look into.

ChemNewbie

  • Guest
Plastic coated 60's
« Reply #133 on: July 09, 2003, 03:53:00 AM »

Mickeyfinn: Have you considered the fact that the pills you had may have been coated with a compound that does not dissolve readily?




Fackin Aye. The 60's Swic uses have a plastic shell on em' that swell up like a fackin balloon when they are boiled, but absolutely refuse to break open, and allow the pfed to come out. Swic has ta crack em' open before hand to get at the goods, but when he does, the STE works just fine. He had the same problem with the Tyvek pulls he was doing till he figured that out. Speaking of tyvek, somma ya that have been havin' problems with gaak comin through should wrap yer goods in tyvek and tie a good knot in it to keep the PM in, and I guarantee that the gaak won't come through the tyvek, no matter how long, or how hard ya boil it in the alky/naptha. Just try it. It works, and does away with the need to filter the alky for the most part.

CN




mickyfinn

  • Guest
missed reply
« Reply #134 on: July 09, 2003, 01:07:00 PM »

SwiM--on pills...what were inactives and what % ISO--91%,99%, as in drugstore not auto type(red-bottle)? Those needles you are describing,,,this info may help..Sound familiar but most may need that info just in case....




Sorry ichi, missed this earlier...

actives are fred=60mg and Chlorpheniramine maleate=4mg
the inactives *listed* are minimal:
magnesium stearate and microcrystalline cellulose

IPA used was 99% (this particular bottle was L*ngs Dr*gs -{bustarhymes with wrongs bugs} blue bottle - SWIM won't use anything less than 99% (he obtained a quantity of various 99% IPA when he realized how badly he wants to be completely anhydrous) SWIM also doesn't depend on the truth in advertising so he takes the bottles and dumps them in silica gel to be sure they are h20 free as possible.




mickyfinn

  • Guest
no coating like that on these 60's
« Reply #135 on: July 09, 2003, 01:25:00 PM »

Fackin Aye. The 60's Swic uses have a plastic shell on em' that swell up like a fackin balloon when they are boiled, but absolutely refuse to break open, and allow the pfed to come out. Swic has ta crack em' open before hand to get at the goods, but when he does, the STE works just fine. He had the same problem with the Tyvek pulls he was doing till he figured that out. Speaking of tyvek, somma ya that have been havin' problems with gaak comin through should wrap yer goods in tyvek and tie a good knot in it to keep the PM in, and I guarantee that the gaak won't come through the tyvek, no matter how long, or how hard ya boil it in the alky/naptha. Just try it. It works, and does away with the need to filter the alky for the most part.




Well, these 60's didn't do that...they just didn't dissolve real easily...zero swelling.

However, SWIM will take up the tyvek gauntlet again, (SWIM actually posted this question about tyvek wrap way back in the first threads but nobody answered) since it will save a mess and now knows it will keep the gaak back. SWIM entered the game a month after the tyvek trials...and swim loves tyvek...HOORAY!

GUP in tyvek will be the only modification to s2e with this next batch of 60's...should be able to run it tomorrow sometime...would do it tonight if flippin nano would've given up it's goods...off to check the evap...

Well, strike that...if the nano would flippin evap...looks like SWIM will have some honey in the morning...light crusty rim tasted salty and made SWIM's mouth water.  :)  

Damn, that's "a spicy meat a' ball"




geezmeister

  • Guest
Zyrtec-D
« Reply #136 on: July 09, 2003, 06:22:00 PM »
SWIG was the grateful receipient of 214 Zyrtec-D tabs yesterday evening. These were extracted by this method. Yield of pseudo HCL was 82% (21 grams of 25.5 possible). This pseudo seemed exceptionally clean. The yield could likely have been increased with more care on SWIG's part, who suffered some loss in yield to a little spillage of the alky/naptha/pseudo mix, some pseudo lost in the filtering process. These pill extract nicely by this method, it appears. SWIG did not do additional cleaning or polishing of the pills. Bioassays scheduled for Thursday-something.


ChemNewbie

  • Guest
Zyrtec?!?!
« Reply #137 on: July 10, 2003, 12:46:00 AM »
Holy Schniekeys that was some expensive ass pseudo! Maybe it'll like double itself in the rxn flask or something to give ya twice the meth.


ici_rhi

  • Guest
NO prob
« Reply #138 on: July 10, 2003, 11:24:00 AM »
No problem mickeyfinn...I have those same pills, generic, same exact "stated" inactives....Don't have 99% from drugstore so platcat says ISO 'red' is ok...My comment re: needles was just make sure it is not MCC.....Sounds tho your method will take care of that...plus like moi you always burn test on foil!!!!!


Look_Away

  • Guest
Red-Hot 30s + STE = ?
« Reply #139 on: July 12, 2003, 01:43:00 AM »
This is my first post, but I haven't had any fun dreams yet, so no flamage!

I read about this guy's dream where he followed the STE process exactly as written. He used 15 (24 ct) boxes of various red-hots. However, he did not de-red them as no mention of that in the write-up.

As some have experienced, the first pull didn't do much to dissolve the pills, so manual crushing was employed as the temp increased to boiling. (Maybee too little solvent mixture?) A splash of ISO was added to keep everything fluid.

More pulls and completion of what is written. Much attention was paid to ensuring the 105C was reached and not exeeded.

In the writer's dream, the end result is very reddish/pink and upon spreading out the filter for drying it does look much like moist, chewed up paper (as someone else dreampt).

I not only USFSE, but I have coded them, so give me a break. I just have a couple questions about this specific method.

1. Would anyone suggest that this method works better with non-red pills or de-reded ones? I've read that some red-in-yur-fred doesn't cause that big of a problem during RXN.

2. VE - Did you leave out any settling or cooling steps? In the guy's dream, he just moved along without significant settling or cooling.

3. Can't seem to locate a recent thread on recrystalization of fred. This seems like a must. Can someone point me in a direction on that?

4. After combining the remaining solvents in a trash jar, noticed an oily looking layer on the bottom. Is this fred?

I'm really looking forward to a dream about a mid-nano RXN and am very pleased to have stumbled upon this. I think I've read nearly every post thus far. Well, skimmed.