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Author Topic:   Low Yields? -> -> Hi Yields !!!
Worlock
Member
posted 09-28-1999 09:05 PM     Click Here to See the Profile for Worlock     
One way to combat a low yield is to prepare your filter paper for use by washing it down with some clean solvent before use.
This way the solution of goodies can just filter thru instead of being taken up to wet the filter paper.

Stonium
Member
posted 09-28-1999 11:53 PM     Click Here to See the Profile for Stonium     
A very good idea, Worlock. Now why didn't I think of it first? Heh, always thinking, aren't you Worlock?

Sure makes me happy...

Toodles,
Stonium

SunriseSpecial
Member
posted 09-29-1999 12:37 AM     Click Here to See the Profile for SunriseSpecial     
I dream about small production. In these dreams I use a 2"id PVC pipe with screw on end cap with a hole the size of the id of the pipe. Cut out coffee filters so they fit inside cap. Screw cap down tight and whahlah! You have a nifty filter that doesn't absorb alot of your stuff.

Worlock
Member
posted 09-29-1999 06:21 AM     Click Here to See the Profile for Worlock     
He-he, very funny,
It was not my idea, as you well know.
Just standard lab procedure, General Chem 101

All too familiar, I give up

Worlock
Member
posted 09-29-1999 01:41 PM     Click Here to See the Profile for Worlock     
Using the "Cold" "Dry" HI/RP/E method, is often filled with surprises, and an occasional low yield.
To improve and consistently obtain decent yields it is important to avoid burning the ephedrine.

************
A 2000 ml Florence flask was fitted with a stopper, three(3) feet of 1/2" hose, ending in a push/pull unit made from two five(5) gallon water bottles.
Forty-five(45) grams of I2 were added to fourteen(14) grams of RP.
With slight mixing a reaction started that began producing a dense yellow-red smoke. The flask was immediately placed in a ice bath, the reaction chilled, then removed and allowed to react and bubble normally without the production of the thick fumes.

After twenty(20) minutes thirty-three(33) grams of E-Cl salt were added and allowed to react normally with-out the production of thick fumes.
Small amounts of water were injected into the mixture and a hot water bath was used to enhance the reaction rate.

After 45 minutes the mixture was removed from the hot water and heated to a slight boil and allowed to cool, the mixture was again brought up to a slight boil, at which time it appeared that the thick "burgundy mud" was no longer adhereing to the sides of the flask, and was flowing to the bottom of the flask with ease.

After cooling, filtration and extraction of the product using ether as the non-polar and standard A/B technique produced 22 grams of exquisite white Meth-Cl crystals.
The crystals were vaporized and otherwised tested the quality was very high.

22 grams / 187 MW = 0.12 moles Meth-Cl
33 grams / 201 MW = 0.16 moles E-Cl

Percent Yield by mole
.12/.16 x 100% = 75%

Percent Yield by Weight
22 /33 x 100% = 66%

These percentages represent the yield obtainable under most situations.

If the ephedrine is allowed to burn producing volumous thick colored smoke the yield decreases substantially.
To increase yields beyond this point the Ephedrine Cl salt would need to be replaced with the E freebase or the E-I salt.

The drawback to this method is the reaction signs of bubbling, gas production, and internal heat production are not as obvious
as when the heavy fumes are present.

Android
Member
posted 09-29-1999 04:41 PM     Click Here to See the Profile for Android     
Excellent

gemini33
Member
posted 09-30-1999 08:31 PM     Click Here to See the Profile for gemini33     
Worlock, you handsome wizard...got a question for ya...

On 09-05-99 04:29 PM
You said,"fast reaction=better dope"

I had posted, "If the reaction goes fast why do you think the quality is better? Less time to produce crappy molecules? Less degradation of the final product? What?

In my dreams, it seems like the reaction goes too fast and I have been thinking of ways to let it go longer. My thinking is that a longer, slower reaction..."

Now, on 9-30, you write, "...The flask was immediately placed in a ice bath, the reaction chilled..."

Are we working on the same principal? Are you saying slower (cooler) may be better than faster (hoter) as you had originally posted? I have thought this for a while, but I have not experimented with it in great detail....

Thats really cool.
gem

Hematite
Member
posted 09-30-1999 09:01 PM     Click Here to See the Profile for Hematite     
Gem, the cooling water bath is used in the dry mixing and subsequent reaction between I2 and rp, once the reactive mixture has begun it must be chilled or one fills their house and a couple of the nearest neighbours places with stenchy thick plumes of yellow/purple yucky smoke.
In this variation the E is added last of all and then the use of a hot water bath is needed to help the much less violent reaction along.
I'll be trying tomorrow and will post results for better or worse. I NEED A VAST IMPROVEMENT IN YEILD AND I"M LOPPING OFF WORLOCK"S LEFT NUT IF I DONT GET IT>
( I'm sick of taking the blame )

------------------
Regards,Hematite.

Worlock
Member
posted 10-01-1999 12:45 AM     Click Here to See the Profile for Worlock     
Hemetite
you will get your wish
I ain't worried,

Gemini
you will get yours, probably when I get my wish.

Gem
There seems to be a destructive reaction involving fumes and heavy smoke, that is what
we want to avoid when cooling the mixture.

The good reaction that makes meth is not destructive and does not sweem to produce smoke.

Once again you pull out this now familiar noose to be placed around my neck, and once again I'll attempt to slip away.
You will never tire of the process and I love it. Someday we will know for sure then one of us can gloat.

Granted slow and easy, can be such a pleasure as compared to quick and over soon.
But with a fast yet very satisfying reaction one then has time to perhaps run a second third or more, leisurely reactions.

I wish I really knew the answer.
I have seen them fire off and be complete in the blink of an eye, super good quality.

I have been on long term grinders that were 1/2 E.

I say you did the preparation, go in, do the deal, and get out.
When that reaction starts you are vulnerable, because you want to be sure it completes without interuption, or you could loose the whole blessed thing.
No use having your behind, sticking out where anyone can kick it, any longer than it has to be.
Enough time has been spent in preparation for this one moment, the crisis, the denoument, the moment when all is revealed. That moment should be savored and not become a chore.

I enjoy a very intense situation that requires quick decisions and fast action, it just seems so awesome.
What if it just does not matter, either way works out the same, then which would you prefer?
What if you can set it up to work either way, which would you choose?
It is nice to be in control and to have the choice.
What ever it takes to complete the process, extraneous activity is wasted energy without purpose, and involves a risk just because it is prolonged needlessly.
And that can be a real kick too.

Whatever it takes to get the desired result.

gemini33
Member
posted 10-01-1999 12:11 PM     Click Here to See the Profile for gemini33     
Hematite:
Please don't lop off anything of worlocks (especially his nuts,...I really like them!)
Good science takes time and also many failures. I am reminded of a famous quote, one of my oersonal favorites. Thomas Edison, ran 15,000 experiments to invent the light bulb, and he said..."...now I know 14,999 things that don't work". So, bottom line is that there is no 'bad' data. Data is data, it all adds to the final outcome. hang in there.

Worlock:
My adorable, sexy wizard...I did not mean to put the proverbial noose aound your neck. I just meant that I have thought about the hot/fast, cold/slow thing. One thing I did do was freeze the flask before adding the ingredients, (like a chilled beer mug), then I added the stuff. Because the flask was cool, it took the reaction a few minutes to start, and it was slowed down a bit, it produced some very kind results. (no burn). becuase of the condensation, I didnt need to add any water either. May not much much sense, but I havnt had a batch as good as that since then, but I really need to do it again, and maybe use a water bath. That is why I was wondering. I wasnt planning on gloating or reveling in good results, I was just thinking about science and the bees and what works or will work the best.

Gemini

Worlock
Member
posted 10-02-1999 05:33 AM     Click Here to See the Profile for Worlock     
Thank you for the kind words while I defend my ...... rights

Hematite was only teasin', right? pal?, buddy?

I gotta go

Hematite
Member
posted 10-02-1999 02:02 PM     Click Here to See the Profile for Hematite     
OK, the nut stays ! At least for now, and only because of an unexpected extraction disaster that indicates my pill supply has been upgraded despite no label change and now contains something I did not enjoy.
Anyway, I got over 50% return of great looking crystal and excellant quality. Sad but true is that 50% even would be enough to make me happy and your splooge sack to remain unsplit ! (note: I think spitball has.
Na fuck it, I'll only get him started earlier than usual)
Thankyou and I'm off to try some different starter and will report back tomorrow.

------------------
Regards,Hematite.

FMAN
Member
posted 10-03-1999 12:32 AM     Click Here to See the Profile for FMAN     
negative or positive pressure is simple thing really to control is fun.

Positive DIPHRAM or GAS DISPLACEMENT with a liquid or Positive air pressure or negative pressure or GAS PRESSURE like propane or simmilair
---Aim thy fist first then dig---

FMAN
Member
posted 10-03-1999 12:42 AM     Click Here to See the Profile for FMAN     
possible reaction papameters of interest

1 Lighting conditions
2 flask meterial condition
3 tempature of flask and log of tempature
4 the most stable will be formed by step up and scientific notes unless ya gona run live vidio or audio it???
5 the thing most likely to suceede in improving or decreasing result ellectromagenetic pulse laser
6 equipment design
7 equipment configeration and time intervolts therin
8 ambient tempature and gas
9 all kinda variables
Make a stair case for the gas PP
ok so one bottle is slightly higher than the next, the entire is filled all the way then as the water is pushed out oh tank on does not necessarly drain all the way important.

Hematite
Member
posted 10-03-1999 11:08 PM     Click Here to See the Profile for Hematite     
Good ideas there Fman, love the stair case push/pull and in fact had a crazy vision of a basement almost entirely filled with the reaction flask(special order from a glassblower)and tanks on every stair of the spiral staircase going up . Somehow that didn,t seem as lame in my thought as it does now written down !Forget it , and Fman dont post silly stuff like that again please

------------------
Regards,Hematite.

FMAN
Member
posted 10-03-1999 11:38 PM     Click Here to See the Profile for FMAN     
actually the push pull is stimulating stuff

The bigest problem I see is it mainly gets rid of some chomped up stuff like free ammonia shreads

The thing has about zip advantage over a distilation setup refluxing

It is economicial from a start up point

It is incrediably dangerous if not knowing the pitfalls like the contact fires and such created by missinformed fellows

Wear a asbestos slicker the silver kind

use gloves tape them on so there is no crevice and they can be removed instantly

Have a fire extinguisher with some cold propellent cause if fire starts it aint gona go out

use at least a thin polycarbonate face shiels and a hard hat

cover your shous with damp cardboard or likewise cover yourself with a damp clothing, this gives you a few seconds before the serious burning ensues

in that little time you must spray off and strip before it burns a hole clean through you

the push pull should be done in a par bomb device like shooting bullet into water

it has been described in detail upside down 55 gallon barrel filled with water and a plexi view port it is secured forom the inside I have seen them set with wet glue and run the can is upside down and in explosion you kinda kick back and watch

most of the force is spent launching the can off the ground in this example upside down water glass trick

Oh and the coolest valves and stuff are attanable for precise control of some of the variables

I dont think this is a new method allthough it may be the most famous for causing dissabilitating eye injury even when a person is in full body armor

I wear goggles and sunglasses underthat just to be shure

I got vidio of not me doing the human glass stretching thing with his hands in full armor while another guy torches him with a flamer to keep everything nice and warm

Guy likes to mave glass hot and with interesting manipulative efforts that go well beyond the ussual????

Anyways good luck with the bomb

Hematite
Member
posted 10-04-1999 02:46 PM     Click Here to See the Profile for Hematite     
An interesting discovery hase been noted during expeditions into these new methods. This discoverywas of a whitish powder impurity that although not wet, would never feel quite dry and was able to be smeared flat with one's thumb and look more like a paste than powder would. I am hoping this is key to a long standing problem I've had with low yields and a constant need to recrystallise to get get crunchy dry feeling crystals.
The ones above were crystallised via Worlock's ph/sep and evap method and looked very nice though a hint of yellow and resistant to final drying. Bio-assay was;
Very good but dulling/heady and definately not right.
Some of the seperated powder(an amount of parent crystal was dissolved in iso for recrystallisation in acetone, and this impurity wasn't happy with the iso) was dropped by chance into a strongly basic soln and revealed a secret it was keeping by sinking and returning as droplets that I first assumed were solvent, butnow am wondering if perhaps it is some pill additive that is doing it's job and holding the liberated freebase oil apon basing or something. Unfortunately I've not been back to the work area yet to further investigate, but I invite comment on this and it's possible that a technique I am very familiar with and have repeated time and again is incorrect, so dont hold back on the comments of a simple and seemingly obvious nature please.
Clean and dry recrystallised product was superb quality and free of any side effects as noted previously. The heady confused state induced by the initial test was actually not unpleasant he,he. But lets face it, you dont take meth to go slow hey !
A couple of points noted in the pastthat may correlate information here are;
Often found product degredation over several days in terms of worsenning of and minor sense of impurity.
One batch was in sep funnel and getting close to basic with NaOH addition and mixing.
Addition of NaOH then saw good portion of oil seperate as I then shokk the mix to liberate it all.The final seperation was less oil than I had first witnessed before mixing ! This is a strong indication that the impurity I have just found is something happening at this stage and that I am indeed an amatuer.

------------------
Regards,Hematite.

FMAN
Member
posted 10-04-1999 07:10 PM     Click Here to See the Profile for FMAN     
I wouldent joke around about this but I think it is a mecury or paladium salt? And it is also in the microcellulose package

FMAN
Member
posted 10-04-1999 07:20 PM     Click Here to See the Profile for FMAN     
I domt know which method ya follow but this is the shit?

Anyways I am into crystal growing man and the impurity can be removed, it been posted

My prime susspicion is that after the impurity is removed and isolated you will have absolutly no question what the impurity is

I dont want to say because the impurity is in everything all kinda pills and such, this impurity may not be all that harmfull, but it makes for some real shit fall in final crystalizations

You do know what the impurity is?

the solution to the impurity is sought after discovery of what the impurity is?

The impurity almost allways increases with the use of fresh solvent!!!!!!!!!!!!!!

The impurity will always be present at least a portion is allways in there, steril aint perfect there is allways something in there of this nature and elliminating it is worth your time.

The impurity will be discovered in allmost everything if targeting issolation for the impurity use a metal like aluminum in solvent, weight of the alluminum could be a critical factor if attracting the equal ammount of impurity, I have susspected that static forces may be employed to activate the foil and laser is necessary if only for a few seconds through the chilled stuff????

Hope this helps???

---A010---

FMAN
Member
posted 10-04-1999 07:35 PM     Click Here to See the Profile for FMAN     
ya find a similiar looking stuff in spent cruciable

the stuff is attracted to salt out in the ellectro

The stuff is sometimes incorporated into the lattice of the ellectrode, it often turns green or other colors when dried or removed from solvent

Honestly I think it is a conglometare of spent crystalization, the waste of crystalization, prevents crystalization, unless reactivated, how to reactivate UV or LASER in solvent cold layerd and real fussy situation

You got a better method to remove the stuff that is simmpler????

Please how did ya arrive to seperate the stuff

I plainly see the discover of some stuff but how was dirt issolateed??????

Worlock
Member
posted 10-08-1999 09:29 AM     Click Here to See the Profile for Worlock     
Yes Gemini,
You cleaver honey bee, you are correct about the slow reaction producing a higher yield.

As you pointed out adding the cold reactants to your vessel, and waiting a few minutes the reaction will begin, using a cold water bath if too much smoke is produced will slow it down a hot water bath to speed it up.
The yields are way, way, up.
If one watches the reaction mixture and sees slight bubbling it is moving along, you may not see any white or yellow-red smoke, but it is there. Prove it to yourself and open the reaction flask, the fumes will billow out so be carefull.
This of course adds a half an hour or more to the reaction time, and it is well worth the wait to get 80%-90% yields / mole.
In fact to increase the yield, many aspects from pill prep to purifying the meth respond to waiting, allow things to react, separate, cool slowly, and settle, taking your time increases yield and quality.
Very good assesment and right on the beeam,
Wonderful, just what this bee was looking for.
Thx

------------------
disclaimer
Due to the public's expectation of shrink wrapped procedures, regardless that the
Hive is based upon experimenting with new techniques, please be advised that:

These proceduress are presented for testing by Bees only. You will not obtain
favorable results if unfamiliar with the hive's standard methodology. In other words,
if you fuck it up, you only have yourself to blame. None of these experimental
approaches are to be used for performing illegal activities.
Worlock

Worlock
Member
posted 10-08-1999 09:35 AM     Click Here to See the Profile for Worlock     
that is a "Clever" bee.

I don't know what a cleaver bee is?
Well, maybe I do know, it is actually a
Beever Cleaver,
The cleaver used on Beevers (that is your basic American beever, and not the European beever)

Hematite
Member
posted 10-08-1999 11:31 AM     Click Here to See the Profile for Hematite     
The 'cleaver' bee is like the sgt. at arms for that particular hive, you fuck with any members or speak badly of the queen and this is the bad dude that's all over your face with it's stinger.
Excerpt from;
"great bee bikers of the '60's "

------------------
Regards,Hematite.


mysticsrock
Junior Member
posted 10-08-1999 02:07 PM     Click Here to See the Profile for mysticsrock     
Is the standard hive method the same method Warlock references on his website? Just want to make sure I have been studying the correct one being the beewannabee that I am.

spitball
Administrator
posted 10-08-1999 02:23 PM     Click Here to See the Profile for spitball     
You missed it entirely. what he said was
quote:
.. the hive's standard methodology..

The fact that we're all about experimentation completely voids out any 'hive standard method'..


-spitball-
The Hive's standard for assholes.

Worlock
Member
posted 10-09-1999 11:06 AM     Click Here to See the Profile for Worlock     
Let me define the term "Standard procedures" such that it will still not fall into agreement with those that desire to be anatomically anal sphincteric(see Footnote 1) in attitude.

There are procedures and chemicals that are "commonly in use" by most bees.
Procedures used repeatedly by the vast majority of bees, and reported over and over, such that it is "common knowledge" that this is the method or substance being used and is not needed to be explained in detail to be understood.
This is "standard of the memer bees of the hive."
The hive is a forum and the standards are those that are "commonly used" by the forum members.
The administration of the hive has influence over the form and general topics, the fact that influence is also exerted over the content of the forum, makes the member bee standards synonymous with the hive standard.
If the administration of the hive chooses not to influence content this would not be the case.

From now on , if this is not objectionable to anyone, I will use the phrase:

quote:
"the more basic adjunctive procedures commonly employed, known, and accepted by member bees. These are procedures and reagents that are utilized in conjunction with the experimental procedures and are considered part of a bee's armamentarium, some of which are also a standard of the hive."

Examples:
Red Phosphorus
---------------
No one doubts that match book scratchings are not considered suitable.
So we have a minimum standard of using a quality grade of phosphorus.
This is a policy aggressively promoted by the hives adminitrative staff and is a Standard of the hive.

Air Polution
------------
The hives policy and promoted by the administration is to avoid poisoning the air. Advised is a gas collection device even if it is kitty litter to absorb this stuff.

Footnote 1

quote:
The anal sphincters are two circular muscles a primary and secondary that pinch off each individual turd as we shit.

And now I wasted all that fucking time and space, I'll report my findings on increasing yield some other day.

Briefly
A consistent 90% by mole, 83% by weight, return of meth from pseudo-ephedrine/HI/RP, is obtainable, with no loss in quality and in fact improvement in quality.

The hive always has the more advanced, updated, experimental information.
The web page is updated long after the information is presented to the hive forum for discussion.

Worlock
Member
posted 10-09-1999 11:33 AM     Click Here to See the Profile for Worlock     
Hematite,

Imagine, if you will, a pill additive that is similar to ephedrine, and is safe to consume.
The only difference is an added side chain on the aromatic ring of ephedrine. This side chain is such that if subjected to certain chemicals, the molecule becomes a cumulative toxin.
Hence it is safe unless it is treated a certain way. Such a molecule the will also be toxic under many other condition, since it is difficult to predict under all conditions.
This molecule would only be found in some brands of pills, namely those brands under the control of a corrupt organization who are seeking control of the population.

Worlock
Member
posted 10-14-1999 07:35 AM     Click Here to See the Profile for Worlock     
Heme,
The additive just found me it followed the E thru Acetone, methanol, water, toluene, HiRP reaction, A/B extraction, sand filter. The shit turns into an oil, wax, and powder.
Managed to clean it from meth but not E yet, by running freebase meth from toluene into water as a Cl- salt with the pH above 9.1.I think it will also get caught in a serious freeze.

Hematite
Member
posted 10-14-1999 09:27 AM     Click Here to See the Profile for Hematite     
Yuk !
Have you managed to isolate anything with regards to the source ?
I bet it's consistant with at least one common label I see on shelves.

------------------
Regards,Hematite.


mysticsrock
Junior Member
posted 10-14-1999 09:50 AM     Click Here to See the Profile for mysticsrock     
I know you realbees get tired of the wannabees but I do believe that each of you were wannabees at one time. Is it possible to keep that in mind and thus avoid being a prick when answering? See Spitball's message for what not to do. Thanks Worlock for responding in an appropriate manner. Now I understand why Gem is all over you!!

Hematite
Member
posted 10-14-1999 11:21 AM     Click Here to See the Profile for Hematite     
I'm a blufferbee at best , which is no doubt why I dont have a clue what you mean.
If I have inadvertantly offended anyone....
then deal with it!!
Hematite does not post with this intention.
Unless it's to get spitball out of that damn closet .

------------------
Regards,Hematite.


mysticsrock
Junior Member
posted 10-14-1999 12:04 PM     Click Here to See the Profile for mysticsrock     
Herm: Had nothing to do with you... a late reply on my part from a few posts back...sorry.

Worlock
Member
posted 10-14-1999 03:03 PM     Click Here to See the Profile for Worlock     
mystirock,
The whole thing was misunderstood by me, until after I wrote the response.
A perfect example of the language barriers that exist.
As you well know it takes a while to develop the knowledge and skills to do this.
I am frustrated that I can't even begin to write down all the important details, and the site is already overly large.
Everything there has been tested and is not BS.
It is best to take what you need from all the authors here, that way understanding will be more clear.
Some of the best improvements have come from reading comments from:
Gemini
Methhead
Dwarfer
Spitball(Hematite

Worlock
Member
posted 10-14-1999 03:37 PM     Click Here to See the Profile for Worlock     
Hematite,
I'm still fighting that funk, have some stuff frozen that look real good, and some stuff in naphtha that may be a better solvent than toluene when this grease is found.

The pH thing worked, but I had to separate the water/HCl/Meth-salt layer from the toluene between pH 9.1 and pH 8.3. This reduced the residue to zip. Suprisingly the yield stayed fairly good(but not great). The goodies are as tasty as can be, and plenty speedy.
I was never able to achieve pH 7.3 because at some point around pH 8.0 the thing would let go and the pH went to pH 2.0ish

Problem was
This gook seems to mask the true pH of the solution, and form a sludge. After each addition of HCl, I would shake it, then come back later(20-360 minutes) to test the pH and adjust again. This continued on and off for 2 fucking days.

My feeling is that the funk is a combined form consisting of the Ephedrine or meth and a molecule that may be replacing Chlorine as the anion.

In other words it is seems to be some bastard molecule that can form a salt with meth in some situations, and it possesses a similar structure and properties, so it can also mimic meth.

I am thinking of a meth "like" molecule with a side chain that is a carboxylic acid -COOH. Because of it's lipid like qualities it takes time for the grease to peel off the meth when adding HCl, nothing seems to move smooth or fast, with this stuff clogging up
the plumbing.

Worlock
Member
posted 10-14-1999 04:01 PM     Click Here to See the Profile for Worlock     
Thanks again to "Gemini" for coming up with the following method that has worked very well for me in obtaining 90% returns(by mole)
She suggests placing the reactants in the freezer prior to use, then combining them cold this gives you time to mix and shake them very well in the flask.
The reaction often will simply begin on its own, or a drop or two of water will start it up(dry climates). A Hot water bath is used, and an ice bath is kept handy in case the reaction begins to produce excessive colored fumes indicating it is eating up the ephedrine.

A rise of reactants to 2x - 3x volume is expected. Avoid "excessive" additions of water, always add less instead of more than you think you should.

If not satisfied that it is reacting correctly(many causes, usually goo in the pills) and it appears to have too much water,

Very cautiously open the flask,
Add 1/4 the original amount of RP and I2 and more E(E is optional), give it a blast of heat to fire it up, swirl the mixture and inject 2 mls of Hydrogen peroxide into the hot swirling mixture, that sucker will go.
That is heat above the BP of water, just enough to cause the solution to boil. It may cost 10%-20% in yield but there will be a yield.

Ratio 1(E) : 0.4(RP) : 1.2(I2)

Hematite
Member
posted 10-14-1999 10:15 PM     Click Here to See the Profile for Hematite     
Worlock,
Had a good close look into frothy troublesome and tedious gunk layer that occurred when basing post rxn mix.
Visible whitish sludge layer if shaken and in wide container, however it goes back into solution if slowly poured into narrow vessel.
Toluene took up some of it and after solvent removal, there remained a bright yellow oil with strong odour that failed to give a ph reading(or perhaps the paper was uneffected)
This oil began to dry, refused to dissolve in clearly acidic H2O, strongly basic H2O, and even turned it's nose up at solvent !
I pondered the sludge as possibly unreacted material in a form between E and M, that has characteristics of either molecule and can move everywhere but belongs nowhere.
I have questioned numerous times the possibility of something with a conflicting ph joining in and crystalising with a HCL salt and effecting the quality and resulting in degradation of the product over a short time.
I still haven't a clue about so much with chemistry and the variables we create for ourselves by the routes we are forced to take, that everytime I think I have something determined and understood, it seems I merely have gained enough knowledge to comprehend the true scope of possiblities and variables
Fun stuff hey !

------------------
Regards,Hematite.


FMAN
Member
posted 10-14-1999 11:24 PM     Click Here to See the Profile for FMAN     
Its proally an alum salt YA got to issolate the alum salt the half ya want to be rid of in layering solvent and add catalyst, hopefully it will like bunch up in the soap layer, and the goods will be else where???

Um yep its crud for shure no doubt about it.

---Amethystium---

I might of added a bit more rumoids than suspected, thinner or other turpintiunes to resolve the gunk out of the thing.

I got some shit looking with the commoner techniques the issolate is like 1- 3 % or base meterial a real bugger hugh?

Hematite
Member
posted 10-15-1999 12:02 AM     Click Here to See the Profile for Hematite     
FMAN,
Layer the solvent and add catalyist ? I dont quite follow. Do you mean layer the solvent prior to NaOH mix ?
Tried many variations, no solvent and 20% soln.
Solvent layer and 20%soln, straight dry pearls, chilled soln etc.
I can build an engine and make it scream and enjoy screaming, because I understand them .....but I only partially understand even the simplest chem activity so my chemistry engine keeps throwing rods and punching holes in the yield casing.

------------------
Regards,Hematite.


Worlock
Member
posted 10-15-1999 12:37 AM     Click Here to See the Profile for Worlock     
Heme,
The stuff is an ingredient of certain brands of pills. Definitely forms a milkshake, messes with the pH readings, is present in a minor amount, but the way it coats everything you would think there is a lot of it.
Added naphtha and toluene to lye water and meth the crud settled between two layers in a thin layer that was removable.
I ran accross it with the NL brand(red and white) pills, but only in some of the lots not all the time. The first time I ran across this, I lost the whole batch, it did not react. Now I can get the reaction, but it is slow, extraction of the meth was messy, and slow. It has taken days to get 1/4 of the anticipated yield.

Worlock
Member
posted 10-15-1999 12:51 AM     Click Here to See the Profile for Worlock     
FMAN
It gets tough keein' that valve train together once you start cranking up the RPMs
Hot Cams leavin' that valve sitting open to kiss der ole piston. Ah it's only another head gasket and valve , hopefully.

shiznasticus
Member
posted 10-15-1999 08:29 AM     Click Here to See the Profile for shiznasticus     
Hey Worlock,

NL brand pills,
NL = national? or
NL = company name or abbreviation?

Just curious because I have some pills (60mg/100ct) that come in a white bottle with a brownish-red label that I am now wondering if they caused a problem similar to the one you and Hematite are discussing here that I had previously attributed to something else. NL is no indicator of the company name (AP-Adv. Pharm. is what they are) and the label looks brown to me but could pass for a shade of red. Thanks.

shiz

Meth-X
Member
posted 10-15-1999 09:07 AM     Click Here to See the Profile for Meth-X     
have any of you tried the Psuedo 60's the come in a blue\yellow\white labeled bottle 60 count\60mg pills for 5.99$ and the local quick stop shop on the corner????? or the Mini-Psuedo Thins. I can buy cases at a time where I live.

shiznasticus
Member
posted 10-15-1999 06:21 PM     Click Here to See the Profile for shiznasticus     
cases? stop it, i'm drooling!
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They sound like pills that I've come across once or twice and were pretty durn good if I recall correctly. Best thing to do is fuck around with what you can get and figure out which ones you like the best while avoiding guifassin(sp?) and acetaminophen(sp?) and probably some other stuff that I can't remember right now.

shiz

shiznasticus
Member
posted 10-15-1999 06:22 PM     Click Here to See the Profile for shiznasticus     
damn, the drool didn't line up under the

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Hematite
Member
posted 10-15-1999 09:47 PM     Click Here to See the Profile for Hematite     
Well folks if you find this slimy fuck of a problem locking up your solvent and goodies in froth, here's a method that worked today.
Pour solvent/basic H2O mix into a vessel that tapers into a narrow neck and let it sit for as long as you wish. Then pull apart and fluff up a few cotton buds and plop them into the solvent/sludge layer and move them around to suck up the whole layer.
Then gently submerge them with the 'poke at things' tool and you can release the solvent fairly easily without it re-gunking

------------------
Regards,Hematite.


FMAN
Member
posted 10-16-1999 02:13 AM     Click Here to See the Profile for FMAN     
Roamans use sponge for a drink didnt they?
Ya de activate an alum with electro, um figure this is what they cut with its what it is? or soap um the thing works again and allways did?

Lets move on to Ammonia thing!

Worlock
Member
posted 10-16-1999 04:34 AM     Click Here to See the Profile for Worlock     
NL is a brand, the label has a logo with (NL) in the center, white bottle, mostly red and black label. Only pseudo is listed as an ingredient
Not all of the NLs are a problem, if you look at the expiration date 11/00 or 04/01 or 07/xx are the bad batches.
Otherwise they are great 60 mg come in 100s and 60s
06/xx and 03/xx were good dates.

Managed to come out of the whole mess OK, it took a long time for the milkshake to layer out, ID the crud and remove it.
If I run into this again, I hope to be able to extract it from the ephedrine and not the meth.

Worlock
Member
posted 10-16-1999 05:22 AM     Click Here to See the Profile for Worlock     
http://www.catrachas.com/alkaline/start.html
Recent Update 10/16/99
Reaction Page - info learned in the last month.
Includes changes needed to increase yield into the 80%.

Worlock
Member
posted 10-16-1999 05:26 AM     Click Here to See the Profile for Worlock     
Spitball a recent photo

Worlock
Member
posted 10-16-1999 09:20 PM     Click Here to See the Profile for Worlock     
Heme from the solubility tests I did I figure I have been had by Povidone
quote:
Pharmaceutical grade Poly(N-Vinyl-2-Pyrrolidinone(PVP) is known
generically as Povidone. It is biologically compatible polymer of low
toxicity that has a large binding capability! It's soluble(10% at room
temperature) in alcohols, acids, ethyl lactate, methylcyclohexanone,
methylene chloride, chloroform, ethylene dichloride, amines, glycols,
lactams and nitroparaffins. It's insoluble in hydrocarbons, ethers,
ethyl acetate, sec-butylacetate, 2-butanone, acetone,
cyclohexanone and chlorobenzene. It's viscosity in water and
alcohols increases with solid concentration in a nearly first order
fashion. It is thought that it exists in solution as a tightly coiled
helix. Its heat of solution is -4.8kj/mol (-1.15 kcal/mol). Heating with
ammonium persulfate at 90 degrees centrigrade for 30 minutes
insolubilizes PVP. Oxidizing agents (eg dichromates) and diazo
compounds in the presence of light will cause gelation. When heated
with strong bases such as sodium metasilicate or trisodium
phosphate, PVP precipitates irreversibily. Pyrogallol and resorcinol will
precipitate PVP from water solution. Complexes with iodine are very
stable, and according the manufacturer, GAF, in Bull. 2302-112,
unable to be extracted with solvents. Iodine can be isolated from
seaweed by boiling with sodium carbonate solution, precipitating
alginic acid with hydrochloric acid, neutralizing the filtrate, and
evaporating to dryness. The resulting sodium iodate can
redissolved(or only evaporated to saturation), reacted with the
calculated amount of sodium bisulfite, which causes the iodine to
precipitate. It may be purified by sublimation. A good sublimation
apparatus can be made from a test tube with a stopper drilled for a
long and short tube, creating a cold finger condenser, and another
stopper holding the cold finger in a larger test tube containg the
impure iodine which is heated. Stoppers are best drilled with a drill
press when frozen.


I found that by
extracting with methanol,
drying it,

adding acetone
adding lye mix to form the freebase
povidone gels up,

at this point the
ephedrine is soluble in acetone and ether,
povidone is not soluble in either.

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