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the
Hive BB ![]() Crystal
Meth ![]() Low
Yields? -> -> Hi Yields !!! (Page 1)
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| Author | Topic: Low Yields? -> -> Hi Yields !!! |
| Worlock Member |
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 |
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, |
| SunriseSpecial Member |
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 |
He-he, very funny, It was not my idea, as you well know. Just standard lab procedure, General Chem 101 All too familiar, |
| Worlock Member |
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. ************ 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. 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. 22 grams / 187 MW = 0.12 moles Meth-Cl Percent Yield by mole Percent Yield by Weight 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. The drawback to this method is the reaction signs of bubbling, gas
production, and internal heat production are not as obvious |
| Android Member |
Excellent |
| gemini33 Member |
Worlock, you handsome wizard...got a question for ya... On 09-05-99 04:29 PM 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..." 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.
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| Hematite Member |
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 ) ------------------ |
| Worlock Member |
Hemetite you will get your wish I ain't worried, Gemini Gem 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. Granted slow and easy, can be such a pleasure as compared to quick and
over soon. I wish I really knew the answer. 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. I enjoy a very intense situation that requires quick decisions and fast
action, it just seems so awesome. Whatever it takes to get the desired result.
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| gemini33 Member |
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: Gemini |
| Worlock Member |
Thank you for the kind words while I defend my ...... rights Hematite was only teasin', right? pal?, buddy? I gotta go |
| Hematite Member |
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. ------------------ |
| FMAN Member |
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 |
| FMAN Member |
possible reaction papameters of interest 1 Lighting conditions |
| Hematite Member |
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
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| FMAN Member |
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 |
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. ------------------ |
| FMAN Member |
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 |
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 |
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 |
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. ------------------ These proceduress are presented for testing by Bees only. You will not
obtain |
| Worlock Member |
that is a "Clever" bee. I don't know what a cleaver bee is? |
| Hematite Member |
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 " ------------------ |
| mysticsrock Junior Member |
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 |
You missed it entirely. what he said was quote: The fact that we're all about experimentation completely voids out any 'hive standard method'..
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| Worlock Member |
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. From now on , if this is not objectionable to anyone, I will use the phrase:
quote: Examples: Air Polution Footnote 1 quote: And now I wasted all that fucking time and space, I'll report my findings on increasing yield some other day. Briefly The hive always has the more advanced, updated, experimental
information. |
| Worlock Member |
Hematite, Imagine, if you will, a pill additive that is similar to ephedrine, and
is safe to consume. |
| Worlock Member |
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 |
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. ------------------ |
| mysticsrock Junior Member |
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 |
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 . ------------------ |
| mysticsrock Junior Member |
Herm: Had nothing to do with you... a late reply on my part from a few posts back...sorry. |
| Worlock Member |
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 |
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. Problem was 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 |
| Worlock Member |
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, Ratio 1(E) : 0.4(RP) : 1.2(I2) |
| Hematite Member |
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 ! ------------------ |
| FMAN Member |
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 |
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. ------------------ |
| Worlock Member |
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 |
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 |
Hey Worlock, NL brand pills, 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 |
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 |
cases? stop it, i'm drooling! ![]() ' ' ' _ 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 |
damn, the drool didn't line up under the ![]() ![]() ' ' ' _ |
| Hematite Member |
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
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| FMAN Member |
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 |
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. |
| Worlock Member |
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 |
Spitball a recent photo
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| Worlock Member |
Heme from the solubility tests I did I figure I have been had by Povidone quote:
adding acetone at this point the |
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