Easy method corrects pH(too much acid)

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Author	Topic: Easy method corrects pH(too much acid)
Worlock Member	posted 11-06-1999 09:59 AM Easy correction for too much acid. Have you ever added a little too much HCl and watched the pH of your M drop down to 7 - 6 - 5 - 4 - 3 Can't simply add a base or neutralizer unless you have an affinity for salt and lots of it. Do you dislike the idea of taking it back up to pH 12+ again......, removing the lye, rewashing, and then adding d-water and re-pH the whole mess just to accidently overrun it again 7 - 6 - 5 - 4 - 3. Did I fail to mention "loss of product", and the "loss of your time". Especially since it is totally unnecessary. What do I mean unnecessary????!! Yeah, you don't have to do that shit, it is way too much work!!!! You only over-ran the pH by a little bit, or maybe by a considerable amount, either way, the fix is quite simple. Remove a small amount of the acidic meth/water solution. 20-50 ml is an average amount. Add to this an equal amount of your fresh non-polar solvent. Smack it good with fresh lye solution, be sure you get a pH 12+. Shake. Remove the lye water. Wash with d-water once or twice. Add the non-polar and meth freebase to your separatory funnel Shake Check pH and, hey!!! pH 8.2 , your back in the saddle, slick as slime. All set and Ready to overrun the pH again. For those who have bits and pieces of M, from prior reactions, that were not very tasty, or second and third pulls. This is the perfect time to pull out that container of disgusting powders. Run a quick A/B to clean some of it, then use the freebase to correct the too acidic solution. ***BTW A can of red devil contains 510 grams of lye. In a 1 or 2 liter container add a little less than 1/2 can of red devil, fill container to 1 liter with d-water(Viola) ~=~ 1 liter of 20% lye solution(ideal).
CHEMMAN Member	posted 11-06-1999 04:35 PM This is a great idea.Another one is build a HCl gas generator.No more PH woes and no more evapping water.Use for pill extraction and final product.
Worlock Member	posted 11-06-1999 06:29 PM Have not been too pleased with outcome of gassing, perhaps I should give it another try since you seem to positive about it. What do you suggest Ether, toluene? Bubbling Air through an HCL solution then forcing it through a solid drying agent then the Meth solution is easy enough. Do you use a drying agent on your non-polar solvent first and what works best?
CHEMMAN Member	posted 11-06-1999 07:46 PM Gas gen was dripping HCL onto conc H2SO4.This is passed thru a washbottle of conc H2SO4,and passed into freebase/toluene.Crystals dryed over buchner and washed with a little acetone.Results were good.Next time will take your tip and use a little calcium chloride to dry the toluene first.BTW this was first try of this method .Any ideas for refinements appreciated
Worlock Member	posted 11-06-1999 08:52 PM Sorry, I have a habit of questioning every step of every procedure to be used. I don't mean this to be a pain in the ass, but since your willing to exchange ideas, let's begin. Why use potentially deadly H2SO4 when all you care about is dry HCl gas. A simple air pump through liquid HCl is sufficient. And why dry with H2SO4, it is a nasty bugger especially when it begins that vaporous shit. Ever consider powdered rock salt $5.00 for 50 pounds, a tube filled with this salt, HCl gas passes through the salt but water stays with the NaCl. The rock salt is used because table salt is hydrated and the particle size is such that it will not suck in a lot of water. So it will not tend to solidify in the paper container.
CHEMMAN Member	posted 11-06-1999 09:03 PM Sounds a lot nicer.Im used this method cause I had both acids on hand and got good results Another from Vogel drips HCL onto NH4CL.I will try your method as it seems most safety wise.
Hematite Member	posted 11-06-1999 11:25 PM Using a gas generator for ages, I leapt at the chance of a low odour method to replace it. The lowering of ph using Worlocks method is almost as troublesomme to me in it's own way, It takes me ages to get it right, and then evap the water ! Any ideas folks, any inkling at all how long that shit takes to go away ? Water has become one of my least favoured solvents. Gassed crystal is much smaller in size and is much more uniform in shape, but it is not as good as evapped super solvent after careful ph adjustment and seperation, needs rinsing again or recrysto.. Worlock, have you considered a two solvent recrystalisation of your product ? The resulting needle like crystals are about 10mm long and clear and crunchy. It is a really nice purification in a fine tuning kinda way. I got all ass about. I can make showstopping crystals, of fine quality, unfortunately in about a 20% return. I suck ! but it's so fun to hang out with me that I just put up with myself. Now I have the feeling I am meant to be together and fate set it up well. Worlockian, please mail me sometime soon and I'll answer after I have this little snooze that seems determined that it's time is NOW ------------------ Regards,Hematite.
CHEMMAN Member	posted 11-06-1999 11:48 PM Hematite I have done the water thing and the gas thang.I feel the gas gave a better yield and as you said beats evapping water.Please tell more of your method ie solvents etc Yes those fumes do suck a bit
Android Member	posted 11-07-1999 04:43 AM Choice post, Hematite! The sleep deficient Hematite is quite the literary phenomenon! ------------------ These Irish eyes are smiling!
CHEMMAN Member	posted 11-07-1999 06:15 AM Worlock What were your problems with gassing? I dreamt success first go <beginners luck> Maybe we can collectively perfect this method In theory it has everything going for it .
whoops Member	posted 11-07-1999 04:19 PM Chem GUy is proababbly alot like me and dont waste his time when working.....Um it is ussually the first time it works in my case.....um yep I try abuncha different things with a new rational not simply following directions but adding a diferent approach all together usually....No being how I find sucessfull divedents at about a .25 sucess rate according to theory and wacko at theorums amazingly they work? Ok so thay want to make some {fill in the blamk] um so it works the first time when gassing,,, um does this means ya tried it and we sucessfull in a procedure that is widely applicable, others say I am right over nighty percent of the time in theory and after working the bugs out of it it could be considered over nighty percent good advice.....Humm so not to spoil anybodys fun but how many different things have we um discussed??? Oh the most important ellemental thing is gona be launcehed soon....Do it your own high pressure gas source for air or anything pressurized say hello electricity and gass???? Use I want to run stuff on numatic powered by in from electrolysis of gas and as the resultant haave a side monopoly on the idea of it so all you inventors nnd big mouths start talking we need this numatic powered motor for transportation and all kinda stuff see this is run formm electricity and battery and now ya got another thing to save the thrusters in??? Sounds fun dont it imagine the security if it all them big tanks and stuff might just mind there own buisness aferall.....Ever seen a torpedo of busted regulator go whooshing across a block through a few buildings,,,yes I am taling mega potentialand along with the cold fussion stuff ya got it made in the shade
Hematite Member	posted 11-08-1999 04:27 AM Chemman, I tried many solvents and preferred toluene over them all, it must be dried thoroughly with pref.magnesium sulphate or at least allowed to stand for an hour or more before decanting to a clean container. It seemed to hold water very effectively and that causes problems. The bubbling kept fairly slow and the crystal filtered out numerous times rather than going till it is impossible to tell if it's done, always yielded cleanest and greatest yields, this gives the solvent a lttle freshen up when you rinse through the filter cake and add this to the pot. Also, I think you avoid uncrystalised product from getting caught up in the drying cake. ------------------ Regards,Hematite.
CHEMMAN Member	posted 11-08-1999 05:14 AM Thanx Hematite .Some good advise.I did use toluene as it was on hand.You have now given me the answer to a question I havent asked yet<how do I know when to stop gassing?> I must have been lucky as had no water problems. Will be using drying agent next time however....Cheers
Worlock Member	posted 11-09-1999 12:27 AM My first problem with gassing was the gas has no on off valve. A slurry of NaCl and HCl, then adding H2SO4, The vapors were viscious, the bubbling over ran the flask and gassing had to be terminated. Forgot and used a plastic tube instead of glass, so yield was suck, the taste was not great, and still needed filtering and washing, then I wondered about chilling. I have no problem adjusting the pH of d-water and meth, and dislike evaporating water, so I keep it concentrated, when the water is gone the crystals are clean and ready to use. Once you have the freebase in toluene, after removing the waste/lye/water. The crystalization from the solvent is clean enough, I imagine except for the bit of remaining toluene, since nothing else is likely to precipitate upon gassing. With the waterevaporation any remaining waste crud that is water soluble ends up in the product. A definite concern. To get this to a minimum requires, three hot water washes after the lye water is removed. These are done just prior to adding the final d-water that will be pH-ed and evaporated. You have given me an idea, it may be that the final addition of water can be kept to an extreme minimum, so that little needs to be evaporated away, decreasing loss to evaporation, and with the concentration very little impurities may pass into the low volume of water. Once thought that more water would extract the freebase from the toluene better. But that is not the case multiple small extractions of the meth HCL from the toluene using d-water will be much more efficient, using much less water. But may present a problem setting the pH with each extraction. Unless the water can be preset to the correct pH that will saturate it with meth(it can), just keep extracting with 1-5 mls of acid water till the pH of the water coming out begins to drop and your done. The potential here is awesome no mo' pH hassle, set your water concentration at a certain HCl level, add little amounts of HCl/water to the toluene, run the water passed the digital pH unit as it exits the toluene. Can even imagine a drip system where acid water drips in the top and drips out with meth below. Even if I don't switch to gas. Discussing this final process is well worth it. Certainly it has already produced details that will be of genuine benefit, and quite unexpected. Thanks for your comments so far. One of my pipe dreams "assembly line speed" add ephedrine at one end, the automated unit takes small bits of E mixes in the proper amount of P and I2, passing it along heated tube where it reacts, gets filtered, n-p solvent and base are dripped in, separated using a holding tank, the overflow goes to a second holding tank, where it is washed, the freebase on top overflows into a third tank where acid water is dripped in , removed from bottom then evaporated to speed, at the other end.
manic Member	posted 11-09-1999 01:16 AM Now that my dear sir would be the hookup. Im sure once you've worked out the d-tails You will post it. It sounds quite feasable? But speaking from experience, "what do I know" ------------------ -right to remain unknown-
FMAN Member	posted 11-09-1999 02:21 AM Wheather or not the special circumstances will hapen readily from small addative improvements is questionable. Different solvent mixtures will produce notable differences in product, dependingn on crystalizzation tech employed such as evaporating from water, imagine the solvent let cure in a mix of water and solvent, at ambient tempature asistd by fluxing tempate gradient to alow spontanious crystallization within the mixture, as this happens it is thermoinsulated in a colller jug thermos and ttempature is adjusted by allowing heeating and cooling much like outside in the fall. The crystal appear in fluid first and them sublime onto the walls sooner or later the entire is suspended onto the wall of the thermous, this is scrapped and reentrained into solution for final XTYLS, acid can be cleaned prety good this way. The adjusted acid water is alowed to drip on drop at a time from the top and it falls through a more boyannt solution wheater or how many different layers is really dependent on pressure and tempature, it cold well be ya will benifi from sonification process as this causes chemical transformation at an alarming rate considering prressure tempature critical controled equipment, aotomating the device will provide simple and long term benifit for all, ussing the available and simple chemical stuff and rembering this speeds up nearly any reaction where evolved gas is a factor I would not be supprised to se the yeild and constitution of most product to jump. Allowing pressure to build and at the same time causing the solution to ccavitate will result in instantanious reaction, rembering the bubbles formed by vaporazation and allowing gass extracted to be reformed into pure solutions from generated gas by ellectro and sutiable uV light wich also alows for a heat source or sink, dont forget that ancient ice making machine history, the whole thing can be as complex or simple as it needs to be, allowing water to drop through or float or sink is very possible considering tempature and pressure,, the better system is not a technological spagattie maker it is a mix over of simple solutions from ready available products and purification is not necessary, as the volume of the mixxutre is not critical in any regard, having the multi role of each component mapped, becoming famaliar with the different employment techniques, we rach a technological standstill in progress to the avrage denezin of the domain, I am glad it has reached this point of finality I have been waiting I am very proud of all everything having been layed aside and discussed as it should be and from a respectfull and compassionate counterport. I am looking foreward to doing getting back to the discovery phase in the researching area, although a big breakthrough at this point would be a little bit much to ask for, I have had so many of those they seem commonplace now. what we do with these new ideas is put them to critical application this is not allways appreciated, by shall we say most of the mass, so please to use diserfication in your approach to reporting these new developments, as the refining of the past echniques has done much dammage to the avarage denezin of this domain, feel free to employ any idea or all and give credit to whomever it suits at any paticular time, we are good at this, and it is a good thing to do what suits whomever may become appreciative and linger for advancing wisdom dished out sutiable protions to the conceering dispensoary guide. Allthought the advancing technology repot is commencing at an alarming rate and due to past fears having becomee reality do not let fear guide the path to harnessing these new ideas or/ do not imprsionate the idea in fear of retalation, as so has seemingly been used as a raport to deny the truth to those of the mass that would benifit from employ from these benificial and straightfroewad guides be carefull not to limit employment of the overall objective tramsmittal of information be shure tho that the available information is all esentuallity an absolute foundational principle to guide it. A specific example that may cause or curative efect in minuratuallity in relation to individualistic and unique circumstance not well reported and cited as a generic thing and gets a generic an equal thing in return, thus much time and effort is used to guide the thing to get it off the ground, most of this effort is a waste of time the most important considerations and time concerning repetious events and reporting should concern bodily harm that migh tcome to an individual whoo could be nieave in regardss to loss of function from preeforming somewhat complex and crittical procedures that often result in a dangerous event, all in all any advancing technique should empploy the most safe and clandestine method available and especiallly if reporting from a know end to the means, thus much effort and time --is waste of time. is not suited to this forum presently is the opposite reflection of this end tuition that must not be allowed to bear friut, and do not hessitate to add simplification to the problem by taking awide approach, this is ver helpfull for all and I am impressed by this conuanial report as is at is communal in essence the overall token of advancement the greatest weapon will always be diversification and infecting the whole with the benifit of the approcah, the society sufferes greatly as a result due to non diserfication on the applicatory phase of the method employed to keep rule and order to a minimal lode of overburden to a few selective posts, this should be tolerated and is the result of the guides mistakes in providing to narow a path for others to follow, the method is simple and technology employed shold not overgrow the common knowledge, because if it is not common knowledge even if that means with a selective few who want it and have found them selves in company containing the essential foundation for benificary entitlement do not for any reason consider it a waste of time to help such as is fit to be called the critical measure of need, or is someone genuine in there need? Hummn so the enemy is this thing not them who dont what to know nor is it those who want to be secretive about it, the enemy is the effect and equal and oposite reaction needing to be entered into the ballance, this can be manipulate compassionally at will if necessary, but never undermine the power of it or it will take possesion of everything at once and cause ruin from lack of respect ofr whatevr principle it may be, allways be dilligent and wait for a guinine offer for comradery as this is a rare opurtunity to form a monopoly on the critical stuff alowing all to patercipate therin the exchange of it and alowing competent and discerning individuals to add to it as they seem fit to do so at any paticular time. Everone has ups and down and the interesting inviduals invested with power in most situations are those who struggle at it ofteen they have become experts as the result of contunal need for repair and are very experienced it applicatory phases of the whatever it is that is seemingly the problem at hand, other times some may appear to have a peusodo quaility of or about them but it is allways undessirable in the end to end up with the non genuine stuff and this is not allways an easy thing to discriminate, allthough on the surface it seems well enough to jump to conclussions based on a little action or time vested never employ that you have wholey understood even the foundation of what has seemigly been asserted or testified upon the thing that is built in short time and does not bend to suit individual needs and alow diserfication, look around I say and see the whole in extenction just as we experience the growth and flowering bloom of new expectations it is in the application and simple aplication at that that we have become so talented at ussing the common thing to add justification to our end, thus are ways are distinct and the diversity is seemigly narrow, do not narrow this path but make it wide and jump from it as seed to through the wind of time and allow it too, and it will be that what you leave will be better than what you found but the application o this genera may nt well be employed to justify the end to the thing as you might have expected as there seemingly is allways a need to leave things left undone as to the whole we who are nowing and following the thing need still to know the difference between reading and knowing a thing or situation based on some things that are not apparent in the litature, and alot of fakes have become know in through the simple reading and comerce of trading this as a mater of something to regretfull of this the lessersdie of the greatness of the greats because they are allways seemingly in the relaxionary phase after taking credits for the greatness umm we are aware of this conclusion of the discoveries and the discoverories that resulted in ruin of an advancing and wholsome thing of the overall objectivness of the situation and allways take on the guild position to a overzealous seeker, who might benifit from your lead in comming into the truth of it...I must go stop ---Amehtystium---
SkitterBlitzer Member	posted 11-09-1999 11:58 AM Have a quick question here guys, In my dreams the only hydrochloric acid notme can get is the drain cleaner which has a very low amount of acid and alot of other things, the bottle doesn't give details, notme can smell the slight acid content but while trying to add the acid to the lye water/colemans notme can't seem to add enough the cabbage strip stays green to a quick yellow no matter how much notme uses..Is there a way to make this mixture of partial acid more potent by removing the other junk and concentrating it??? thanks.. Peace! Skitter
rev drone Member	posted 11-09-1999 02:12 PM Worlock, Soooo, What are you doing, and how did you get too much acid in there? 'Remove 20-50 ml'? From WHAT?! So, by diluting your meth solution, then adding base, you're hoping to avoid... adding base? Does this not make sense to anyone else? Definately, without a doubt, for salting out phenethylamines, I'm a 'gas fan' until the day I die. Use anhydrous solvents fresh from the can, and you have no worries. Barring that, anhydrous MgSO4 or Na2SO4. Solvent? Toluene, DCM, pet ether, benzene are my choices -- in that order (hate the smell, but love those toluene-precipitated crystals!) Sorry, I have a habit of questioning everything too: quote: And why dry with H2SO4, it is a nasty bugger especially when it begins that vaporous shit. ...As opposed to healthy, nurturing, HCl?! Firstly, its not so much a dehydrating agent as it is simply a nifty trick to move the soluility partition away from dissolved HCl -- the higher hydronium ion concentration means you're already saturated HCl solutions (which is an equilibrium of H3O+ + Cl- <-> H2O + HCl), is going to liberate the gas from the solution. Yes, H2SO4 is dangerous, but so is HCl, and the difference is less than you think. Another method that some people enjoy is gently refluxing 37% HCl. HCl forms a constant boiling aqueous solution of about 10-11%, meaning that the remaining 26% can be utilized. Use an efficient condenser, and dry with CaCl2. ------------------ -the good reverend drone
Cheapskate Member	posted 11-09-1999 03:06 PM I haven't gassed meth, but I have gassed a number of other things and my experiences may apply here to help y'all. When you just bubble air through HCl then dry through salt, you pick up a shitpot full of water from the acid. It all can't be removed by the salt, unless you have a BIG salt column. Same thing applies if you heat the HCl and dry it the same way. Way too much water is transferred. There's a bunch of ways to make dry HCl gas, just look around. The method I use is to drip Sulfuric on HCl and dry the released gas by bubbling through Sulfuric then passing through "Damp Rid" I picked up at Home Depot. Salt helps in the HCl to pick up the water that is in the HCl as well, but it isn't absolutely needed. The dryer the gas and the dryer the solvent, the more crystals will form and not dissolve in the water that is carried over. This bumps yield up a lot without having to spend the time evaporating water. However to Worlock's credit, the gas method is a real pain in the ass and the water method is easy. One of the old time visitors to the hive would place a small container of HCl beside a container of freebase dissolved in toluene with both of them in a large plastic bag. Apply a heat lamp and wait. The HCl will gas the toluene and the toluene will evaporate out of the container and collect on the bottom of the bag. Then, just collect the crystals that form and dry them. Sorta combined the best of both worlds. I tried this and with a couple of tries made it work pretty well. But like I said, I never make drugs so this may not work for y'all. CS
FMAN Member	posted 11-09-1999 05:42 PM i got to go so real quick ya add h2s to a solvent to precipate epsom salt not the other way it dont work that way althoght it might work a little bit if ya desicate the stuff but this ussually drives off an ellement and ya no longer have salt like ya had before if done carefully it does work but never as good as good plain pure gas, see if there aint no water in there then gas just rises out of solution unless pressure is not allowed to escape in that case ya get an explosion or pop o f gas H@S is not dangerous it does stink a bit alot it stinks but it can be ussed safely and does dehydrate alot of different stuff will makes epsom of any amount of water given time.... ---Amehystium-- I check back later SEE YA

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