About
Community
Bad Ideas
Drugs
Ego
Erotica
Fringe
Society
Technology
register | bbs | search | rss | faq | about
meet up | add to del.icio.us | digg it
Go Back   Community > Science > Laboratory Tips
FAQ Members List Calendar Search Today's Posts Mark Forums Read

Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists.

Reply
 
Thread Tools Display Modes
 #1 
Old 2004-01-23, 01:27
Regular
 
Default Meth Synthesis Information Thread

Methamphetamine Synthesis Fundamentals by-Jamiroquai

Chemicals Ratios by weight

(pseudo)ephedrine/iodine/red phosphorus

Ephedrine Iodine crystals Red Phosphorous When to use

1/1.5/1 Tincture or poor quality of chems --- Matchbook RP use 2x -3x normal amount

1/1.5/0.6---> My favorite uses excess iodine- this insures a spontaneous reaction, and complete conversion of E to Meth

1/1.0/0.33--> 4 oz or more good chemicals ratios

1/1.0/0.20---> Lowest amount of RP used to convert 6+ ounces

1/1.2/0.7---> What to use for less than an Oz

Remember the second time around for the RP it will contain Iodide unless well cleaned and dried , and therefore the actual amount of the RP is much less.

Because of the Iodide weight . So add 2x the RP if it was pre-used and not cleaned.

If the RP was washed in acetone and water then dried it is almost good as new add 10% more RP for used.

Some bad news 92% is the top yield of chili by weight, theoretically possible.

It is common to obtain between 50% to 75% chili by weight and rarely 85%.

The addition of aluminum to the reaction reduces the amount of RP needed, 5-6 soda can pop tops per-oz of E<----Is this some typo?! No. Things change, methodologies change but some things forgotten.

Water

The reaction may go without any water added, this is true if using iodine from tincture, or if the humidity is high the E and RP adsorb enough water to fire the reaction.

The common mistake is adding too much water, and not getting any reaction. Mix the reagents dry, if the reaction does not fire, then add

1-3 ml distilled water /ounce of E.

The mixture should be very damp, a thick mud, but not wet.

As it fires off , the first thing that happens is it liquefies, and becomes wet, so you want to start out as a thick mud, then let the reaction thin itself out.

This is such a touchy part of the reaction, experience is the only way to be sure

If the reaction still does not fire, Use heat, do not add more water, yet.

If heat does not do it or the mixture is very dry still add another 1-3 ml of water/ oz of E

Then try heat again .

Keep alternating until it is goo like melted taffy. this should fire with heat. for sure.

At that point re-evaluate your three main items ( E/I2/RP) are any of them the potential problem? If not

The last resort is to reflux it for a few hours.

The quality of the water is extremely important to the quality of the chili, and to the yield.

Always used distilled water, and for even better results run the distilled water through a Britta water filter to remove metals, and other trash.

Hydrogen Peroxide

If using recycled phosphorus some suggest using a capful of hydrogen peroxide also.

I suggest you avoid using peroxide at all, if possible. The reason is peroxide in an acid environment will digest many organic molecules.

In addition peroxide will oxidize the RP,

In the reaction the peroxide will change HI into I2.

Any HI that is not mixed in with E and RP is useless in the reaction and is escaping This includes all the HI that is above the reagents. The HI is only of value while it is being recycled within the reagents.

The bad aspect of heat, is that it tends to vaporize the HI . HI has a boiling point of 117 C but this is a 58% solution with water.

The concentrations of HI you are using is many times above that. 4 to 6.5 molar

By adding peroxide some of this HI may be washed down into the flask as I2.

Peroxide will also strip off organic molecules that may be stuck on the RP like wax, this refreshes the RP at the same time providing I2,

and may be enough to kick in a dying reaction.

Additional heat is my preference. But try it and judge for yourself.

Cautionary Notes

Be prepared, the RP hitting the I2 will often start the reaction.

It may be impossible to see inside the flask, either from vapors or the rise of reactants. Either way, if the surface of the reactants contents can not be seen, act fast, because seconds count, shake it hard., or swirl the contents Keep swirling until you can determine what is going on. Look for a nice easy bubbling. If you fail to shake it down you will end up with very little, because the thick smoke indicates a fire is going on in the flask, this will destroy the E, or the contents of the flask may have expanded and are going to soon blow down the hose, Hard shaking will stop both of these situations allowing you to regain control, If you hesitate all will be lost

If the mixture starts to rise up, too high, swirl it lightly

Shaking before it blows out of the flask will save your whole reaction

Keep the wet towel handy, it will turn a potential disaster, into a laughable "won't do that shit, again" story.

Phosphorous fire confined to a flask

Too hot of a reaction

Place your wet towel over it ,

You want to avoid the contents, that may be tossed out of the top of flask

Get you and the flask to a safe area, away from all flammables,

The fumes are not a deadly toxin, but they are not healthy to breathe

vaporous HI acid

and Phosphine (not phosgene)

Phosphorous fire not confined to a flask

Phosphorus is hell to extinguish once it catches fire. Do Not Touch, Phosphorous will stick to whatever it contacts and burn

The amount of smoke is unfathomable, and will draw attention..

Toss your wet towel over it, this will cut off its oxygen, and buy you time, maybe a minute. (don't worry, you will be moving at the speed of light,)

Wet dirt is the best retardant, water may just blow it around if a lot of RP is on fire.

But water will put it out if you flood it

The worst thing to do is to run away, leaving it out of control, probably will result in a fire , injuries, and your arrest.

Most Fire extinguishers are not very effective against a phosphorous fire

SWIM was drying RP in the oven, unattended , when the glass bowl broke, fortunately the RP was damp

The first sign was an odd smell and difficulty breathing

Then the smoke was obvious

Two fire extinguishers were emptied onto the 4 oz of RP and had no effect ,. the wet towel slowed the fire and the garden hose finally controlled it, by flooding everything.

SWIM took a break.

While cleaning up the mess SWIM noticed there was still RP on fire and flooded it again it, and there were still spots on fire after that.

The Reaction . . . . This reaction is exciting, and rapid. You must really focus your attention at this point. It is of -primary importance, that you have your wits about you. It is most difficult sometimes to determine if the reaction went to completion, so observe as much as possible and you will be able to make a determination.

The mythical chili of the ancient gods, as legend has it, is that the mixture is so perfect that the energy provided by the light of a star was sufficient.

The sun god preferred to mix at night , when the first ray of light at dawn struck the flask the reaction began.

Most were satisfied to prepare the mixture during a storm and then step to a window and allow the light from a lightning bolt begin the reaction/

Today we modern people are more scientific, and most rely on the sound coming from a Lynrd Skynrd CD.

Here that it becomes hard or impossible to follow along as a recipe., and to see the step by step reaction again. So use the recipes provided, improvise as you see fit. As you become more familiar with the process, eventually you will have the steps memorized, then you will be able to note subtle differences between the procedures, You will appreciate the explanations here, they will seem to suddenly answer many questions you have.

Preparation and initiation of the phase one reaction[i]

Weigh out the Ephedrine and I2, in a ratio of 1.0(E) : 1.1(I2) , place in reaction flask.

Mix the E and Iodine together. Keep them dry, They may liquefy don't worry about it at all

Place the flask of E and I2 in the freezer for a few minutes while you weigh out your phos (5 minutes or less). The chems are slightly chilled so you will have time to mix the RP in well

Variations are as numerous as the number of cooks, no two cooks use exactly the same methods and some cooks never do the same thing twice. However certain details are always the same no matter who does it.

Some mix red and I2 first , some mix e and red, some add water at the beginning others add it later.

some mix the reactants for hours, some barely mix them at all before beginning the reaction

Heating the reactants before mixing is very dangerous and is 10 x as dangerous if you are using free base E. It will blow. The free base has to be handled carefully and not forced to react in any way.

If doing [i]over 1/2 oz and if not familiar with the free base, react the HCl salt instead.

Prepare a pan of hot water to heat up the flask, or use an electric stove, SWIM uses an electric WOK filled with sand with a temperature controller

Some use a warming tray, hot plate, or the stove, some heat is usually needed to get the reaction to go to completion..

Avoid using an excessively high temperatures.

Variations -my latest heart throb is the use of sand placed inside of a wok or pan on the stove the reaction flask is placed in a depression in the hot sand and partially covered up. The value is the glassware does not contact the excessive heat of the stove top. Even heating, .A milder heating the sand takes a while to warm up so the reaction temperature slowly rises , This works great when evaporating solvents because the tendency toward over heating is reduced. The sand I use is the standard 60 or 30 pound washed silica sand from the hardware store it cost a couple of dollars for a 100 pound bag, the bag may not be easy for some to to carry, or even to pick up, so get some help if your not muscular . This is the same sand used in the sand filter the 60 pound is probably better it is smaller grained.

Tear 6-10 strips of sheet metal tape 6" long - 1 inch wide and have them ready to seal the stopper onto the flask

Prepare a small cup of water, this will be added to the flask with an eye dropper or a syringe

Remove the E and I2 from freezer and add the Red Phosphorous (chili powder).

Mix it very well, it may begin to react with just dry reactants. You will smell and feel the HI as it hits your nose

If the reaction is not happening or is slow and the flask has warmed to room temp, you want to coax the thing to gently begin

If the reactants are dry Add 2 ml of water /oz of E, shake it around,

Often the reactants will lump up into large balls of chems, watch these balls as they will melt when the reaction is about to begin.

if it is still dry add 1-3 ml more of water / oz E

If no reaction place it on the heat 150 F

If using homemade iodine from tincture you won't need to add any water, usually just mix and heat

Increase the heat slowly until it reacts

SWIM will toss in 3-4 pop tops from soft drink cans for the aluminum, it helps even out the reaction

Once it has begun carefully but quickly put on the vented stopper and strap it to the flask tightly with tape.

Be very gentle with the reaction flask, It is a tense moment as the reaction is kicking in and your still tapping it up , plus you need to be watching for excessive smoking of an over reaction and possible RP fire in the flask. Just take your time and don't break anything, a few fumes won't hurt you, but a lot of them will.

If you cannot seal the stopper in place and the reaction has begun and fumes are getting out of control , pour water in it, to stop the reaction and get away from the fumes, get some fresh air,

This will begin phase one reaction and it usually lasts 30 minutes, This part of the reaction creates very little heat but will push out some gas

Keep the reaction going by slightly increasing the heat if reaction slows

Keep increasing the heat slowly

If the reaction has been flooded with water, and looks soupy ,

add more of the three reactants, or

lightly boil it for several hours

Reaction Signs - Sometimes the two stages of the reaction are very distinct, at other times no

Phase 1 20 to 40 minutes

Initially the thick mixture liquefies, and bubbles. The small bubbles have a silvery metallic sheen on the surface

May notice some gas being pushed into the p/p

Rise in the level of the solution, increases volume,

As time goes on the gas production to the p/p decreases but the bubbling still continues

White fog or light colored mist is OK

continue heat to maintain an easy bubbling reaction.

The heat is not creating the bubbles . the heat maintains the reaction that produces the gas bubbles

Trouble Volumes amounts of thick yellow or red smoke (not good) over reaction, a phosphorus fire in the flask, may reduce yield substantially. Shake the flask as soon as you see this to stop the fuming. There can be an actual fire in the flask with phosphorus burning, initiated by iodine and wax,

Variation - the common variation is to stir or not to stir. Certainly some mixing is desirable and too much mixing will quench the reaction. So somewhere in the middle find your niche between mixing and keeping the reaction alive.

Definitely shake hard if things get out of control.

It is important to be there when the phase two of the reaction kicks in, a little stirring here to keep the violent nature to a minimum and keep the reaction going is the critical link for a great yield or a pile of nothing at the end.

Left to its own turbulent nature , if it is in a large flask the reaction will yield on the low side 50% to 70%.

With optimal mild swirling to control the turbulence , the yield will approach 70% to 90% depending on the pills and other factors.

Over stirring the reaction may not complete and you receive only Ephedrine as a product.

Variation the application of heat is another area of differing opinions , some use heat no matter what others avoid it like the plague. The best method I believe is to simply add heat for a minute of two when needed to keep the reaction going.

Use more if needed.

All agree that too high of a temperature is not good for results.

Phase 2

After 30 minutes or if the bubbling begins to slow

If you held back some of the RP then Add the remainder of the RP, mix in well , add a capful of water if you think it is needed.

Optional: add a few grams of I2

Increase the heat very slowly, plan on taking 20 minutes to raise the heat to to 200 degrees F.

200 F is internal flask temperature, the outside temp will be higher. Somewhere near 180 F phase two begins

At first you will notice that the metallic sheen on the surface of the bubbles will be silvery ..

Soon the metallic sheen on the surface of the bubbles is no longer silver but is either yellow, greenish and even reddish.

The entire atmosphere in the flask has this color change.

The small bubbles seem to collapse in large holes (pac-man sign, like the game pac-man is munching big holes in the surface)

This mixture will slowly become more turbulent, loosing the small bubbles, the reactants rise, suddenly all hell seems to be breaking loose. (It is a charge and a half to see this.)

Once seen you won't forget it, turn off the heat as this begins, if you remember.

If you have followed the guide for flask sizes you have nothing to worry about

"IF" it is going to blow out of the flask it will do it now. so be prepared to give the flask a light swirl before it gets even close to the top. or a hard shake, if needed .

If you are concerned that you have too small of a flask, have some heat resistant gloves on, and eye protection

shake once or Swirl the flask to keep it down below the 3/4 point of the flask

Major amounts of heat and gas are produced , it is a swirling maniac

the mixture expands , and may oscillate (expand and contract) several times

The push/ pull - will be pushing very hard, bubbling big time

At the end a tremendous pull may be noted .

When complete -

The turbulence quickly stops, you did it, you have chili, there is no doubt about it.

Reactants do not stick as tenaciously on side of flask, depending on dilution .

The hue of the mixture changes from reddish purple to more dull or drab red purple color.

Tilt the flask if the reactants very slowly flow off the bottom , and no longer are stuck to the bottom, you are finished.

If uncertain heat it up to a easy boil , If nothing happens it is probably completed.

Filtering and Purifying the Product -- GaKK Patrol

Dirty glassware, poor reagents, sloppy technique, from this point on affect your product in a big way.

If you use soaps or detergents on your glassware, you introduce a sulfate that will turn your chili black and stinky when smoked

Wash glassware with water and rinse with acetone, if something is stuck on the inside wash with acetone and salt, swirling the salt as an abrasive then rinse super good

At the end of the reaction you may have heard of the chili being called an oil, well it looks golden, like an oil,

but at this low pH (acidic), it is actually a water soluble salt of iodine.

Are you still withme?!

Procedure Continued

Add 100 ml of boiling/scalding-hot-as-fuck---->water for every ounce of initial ephedrine after the reaction mixture has cooled.

Boil the solution in a stove top safe glass bowl for 5-10 minutes, this will save you time by not having to refilter the mixture several times as noted below

Filter using coffee filter and cotton ball plug gently pressed inside the tip and pre-wet all filters always and forever religeously.

Re-filter through the same RP and filters again, continue refiltering until it is clear as a bell. It may take three filterings.......it may take fifty but do not proceed until it is clear or your ass is gonna wish it did come time to get high!! You will end up with a clear yellow or colorless solution that can have many different odors. If you don't refilter you may leave iodine in the stuff. Recycle the red phosphorous it is still good.

Trouble - If it refuses to filter and it seems like iodine is everywhere!!! STOP, the reaction did not take. It is still possible to save your batch and obtain a good yield .[i]

[i]Collect the fluids, RP and iodine put back in flask, add more I2 and RP, and a condenser and begin boiling lightly for many hours (4 at least). You can even boil it in an open flask. You want to boil away most of the water. At the end of the boil,. it the contents are allowed to settle, there should be RP on the bottom and a yellow fluid on top. The yellow liquid is almost as viscous as motor oil.

SAVE everything until you are done and sure you have your chili Use a large glass or plastic vessel to store all the discharge in (a empty gallon water container is perfect)

Notes

In the Russia and in much of Europe this is the final product, it is called Meth/acid. It is sold as a liquid , for injection, ingestion, or snorting. Now although the iodine is gone, it has been converted to iodide as a salt and some is still HI. They notice that after taking speed this way their joints are sore, muscle aches, skin eruptions, and a severely hungover feeling after coming down, They are lucky to be alive. The next step of basifying the mixture removes all those nasty iodides and most of the water soluble contaminants, and in Europe people will add bicarbonate to reduce the acidity of the mixture. Needless to say, they were sent the full instruction on how to clean up the meth/acid.

After normal filtering, Take a strong flashlight and shine it through the mixture, look for reddish particles indicating phosphorous is still present. If it is there- Put a plug of a paper towel in the funnel a few coffee filters and filter one more time, your flashlight test will show no more phosphorous.

Procedure Continued

Create the chili free base (oil soluble) by raising the pH of the water soluble layer to pH 12.5-13,

Slowly add a cold (put ice in it) 20% Sodium Hydroxide solution( 200 gm of NaOH dissolved in 1000 ml of d-water).

Add the NaOH slowly, Swirl the flask or shake lightly, Hard Shaking will create an emulsion and it will have to sit for hours before ot clears

Important- All pH measurements are made only on the water layer (lower layer) or polar solvent. To take a pH reading on the non-polar, upper oil. solvent is useless.

Solubility, ions, polar, non-polar

Variation- as to when to add the nonpolar solution is a common point of contention, you want a nice debate, this will get you into the middle of a fanatical argument.

Generally it is a good idea to add the non-polar before adding the base, the non-polar attracts the free amine (free base) E and M and helps them move more rapidly out of the polar solution..

However there are times when you do not want a non-polar compound mixed in, Steam distilling , contamination, or to observe the E and M changing solubility.

The non-polar is not absolutely needed most of the time , it depends on concentration, it may give a better yield, and does move the E and M much faster.

But unless you have a specific reason to not do so, most newbees would be advised to add some non-polar prior to adding the strong base. Experiment when you have a few cooks behind you.

CAUTION adding NaOH too fast, to a hot solution is dangerous. Many bees premix a 20% NaOH solution and then add ice cubes to that, others add it straight .

The idea is to get the pH up above pH 12.5.

Contrary to some literature in Erowid's site, only the amines and very similar compounds have this unusual ability to freely change solubility from water to oil base when the pH is changed.

Morphine, codeine , heroine, and cocaine are common examples they have CH-CH skeletal structures with the N-H and OH groups exposed.

The CH hydrocarbon(hydro--hydroGEN/CARBON--CARBON-hydro/carbon(CH)<---get it?! ) chains and rings (aliphatic and aromatic) are what is a non-polar polar molecule like methane-(CH4) or benzene-(C6H6)

The -OH(oxygen/hydrogen) adds a degree of ionic polar like quality as in methanol CH3-OH, or phenol C6H5-OH.

But it is the mainly the nitrogen =NH changing to =NH2+ in the presence of excess H+(acid) that gives the legendary Hydrogen bonding and full water(polar)(ionic) solubility, along with attracting anions like -Cl.

Hydrogen bonding is an ass kicking ionic bond that is 1/5 as attractive as a full bore covalent bond.

Now that is some stickiness. You will find hydrogen bonding when N, O or Fluorine are present.

Generally these three atoms determine if a hydrocarbon will be water soluble.

Procedure continued

Depending upon concentrations , The chili floats to the top, or will be seen still in the water as a thick white cloudiness

Check the pH when above 12.5 Add a non polar solvent (Coleman, Charcoal lighter fluid, toluene, xylene, naphtha, ether, hexane ..etc.) at least 100 ml then 50 ml for every ounce.

Shake Lightly. this should clear out much of the cloudiness from the lower layer as the chili moves up into the non-polar

Adding rock salt (as much as will dissolve) causes the water to drop all remaining chili, releasing it to the oil and increases your yield.

Swirl at this point , or shake easily .

Allow the mixture to layer, 10-30 minutes or more, then separate, discarding (but saving)the lower water/lye layer.

Lye Lock

Watch out for a solidification of the lye/water layer (lye lock) too much solid material in the water lye , as it cools from the heat released by adding the NaOH, the NaOH begins to solidify. One good thing is you know the pH was high enough.

probably close to pH 13.7

Dilute it with warm water before it hardens, and begin draining out the lower layer, contine diluting, or it will harden then it is more difficult to keep dilute

keep it separated (don't shake)

Remove the lye solution

Depending on concentrations there may be a whitish waxy looking substance at the lower layer of the nonpolar, looks sorta like emulsion, This is often not speed . This is emulsion which rarely has anything of value in it. If in doubt as to where exactly to make the cut off between emulsion and non polar flush the lye /water layer and leave the emulsion with the non polar.

After the initial water wash is drained swirl the separatory funnel very strongly , a snow storm of whitish globules will descend to the bottom. dump these they are emulsion, swirl repeatedly to remove this nasty gakk it is dependent upon pH and concentrations and 95% of the time is gakk at is best.

Wash with water again and repeat the swirl to get after this emulsion, it is an impersonator of meth but is tainted because it is an altered molecule containing properties that place it in between polar and nonpolar, and is best removed because it tends to pull anions and cations with it and these will really taint your shit. This gakk will have properties similar to chili but not identical.

Wash the free base and fuel solvent with d-water 3 times and separate each time ( using 1/2 the volume of water as the the oil ). Shake it well when doing the wash, but do not over shake. Add this wash water to your discard bucket along with the lye water

After three washes- make the salt of meth

Add d-water again ( a smaller volume than the fuel), it is easier to evaporate the less water you use.

If you want to gas dope simply take you Liquid Fire Sulphric acid found at plumbing supply stores and the like and Rock salt. These are your precursors for the Hcl gas now go buy an aereator stone for aquiariums anda microwavable baby nipple with a 1/4-out-diameter vinyl tubing with a OLD MILWAKEEE QUART-WIDE-MOUTH BOTTLE OR OF SIMILAR DIAMETER NECK AS THE NIPPLE FITS PERFECT OVER IT AN YOU RUN THE TUBING THROUGH THE NIPPLE NOT DOWN THE TUBING!!! Sulphuric acid is much tamer than aluminium foil and muriatic acid and gassing is superior to titrates any day of the week. Put a cotton ball an inch-and-a-half outside the tipof the nipple inside the tubing and any possible "splash-ups will be absorbed and stopped from running into your chilli which is soon to become cottage cheese.

Or add HCl(muriatic acid) drop wise, shaking lightly, test the pH add more HCl until the water layer tests between pH 7.0 and pH 8.0 . This is about 6 drops of 30% HCl (muriatic) per gram of expected product,

this makes the chili a water soluble molecule again, and moves it down into the water layer.



If you are consistently getting dope that smokes burns dark and gakky , consider the source of your HCl probably also contains sulfuric acid, and you might consider gassing it instead or distill your HCl first.

Separate the water from the non-polar again ,saving the water layer in your boiling bowl

Evaporate the water away, using heat, and a hair dryer. The hair dryer will improve yield , it actually cools the solution by evaporation.

But the hair dryer will add debris from the air, so don't use hair dryer on severely dusty, smoky, or smoggy days.

If the pH goes below pH 6.0, go ahead and evaporate the water away then wash the crushed crystals with acetone, to remove the acid.

In this HCl water soluble form, it is usable

Adding the HCl

Add an 1/2 volume of d-water again

Toss in a couple healthy squirts of HCl.

A bit less HCl than is needed, that will be 1 ml of 30% HCl for each gram of expected product

Shake well

allow to form into two layers

Separate and save the water layer in your boiling bowl

Evaporate the water away

Enjoy the great crystal chili that pops out

then do another pull

Add more d-water to the non-polar/meth

Couple more squirts of HCl

shake well,

allow to layer

separate and evaporate

Continue in this fashion

Eventually you will get to the last pull,

you will know it is the final pull because a great deal of nasty HCl vapor will come off when evaporating the mixture ,

You will have to wash the excess HCl out of the crushed crystals, of this final pull, with acetone.

All the pulls are the same and great chili even though the pH was at 10 , 9, 8 or 7 when the shit was dropped out of the non-polar.

WHY?

Most of it happened with in a small pH range of pH 10.0 to pH 8.5 As the chili takes on a H+ attached to its nitrogen, it is capable of hydrogen bonding . Once it accepts a Cl- ion, it becomes suddenly very water soluble.

It is related only partially to the pH because if you were very careful about any ions you could concievably maintain the freebase at pH 7.0 but the -OH would interfere .

In this case it is the Cl- that is the primary factor affecting formation of the water soluble salt. That is why it is very important once you have the freebase form, to only use very pure distilled and deionized water to wash the freebase clean. because any negative ion , is going to cause a loss of product when washing the free base, depending upon the pH and a dozen different concentrations of whatever ions are present,

The pH will drop with each washing. The pH of pure water is 7.0, distilled is often 6.8 , tap water can be up to 8.5+

The less foreign ions present the better control you will have.

Better yields

Better dope

De-contamination procedure For cleaning up Chili quickly

Crush up, the chili in a bowl with minimum of dry cold acetone ( no water)

Pour crystals and acetone into a filter

Wash crystals by flushing with more dry acetone, until they are white, this removes the acetone soluble junk

Optionally wash them with any of the non-polar solvents to remove non-polar soluble junk

Wash off the non-polar solvent with acetone.

Change to a clean collecting flask

Keeping crystals in the same filter. Add denatured alcohol to dissolve the chili and leave most salts and insoluble crap behind.

It may take 10 minutes for all the chili to fully dissolve

For a quick clean evaporate the alcohol away

For a major purification use recrystallization

Boil the filtered alcohol/chili mixture until a slight skin begins to form on the alcohol, add about 10 ml of fresh alcohol to dissolve the skin again and add 20 ml of acetone, cover the container and place in freezer for 6 hours or more up to 24 hours, the longer the better and bigger will be the crystals.

After the 6 hours, Filter the crystals cold and quickly, rinse lightly with a very small amount of ice cold alcohol, after the residual alcohol evaporates from the surface of the crystals this will give you some of the finest chili you have ever had.

After washing with the alcohol as noted above , it is fun to place the crystals on a dark surface , spread them out to help the residual alcohol escape. Pull out the digital camera, and snap a few pictures of your beauties. These photos will be a source of enjoyment. Simply because it is rare to see so much stuff, looking so good. Soon it will be bagged and such and looses that magic quality of the untouched pure crystal. You will be one person in 1/2 of a million in the US that ever gets to see this.

Water Soluble Sulfates

If your chili looks clean and white but when you vaporize it leaves a nasty black residue , then you have water soluble sulfates that can be removed using the recrystallization method

Glass like shards and crystals

To get the bigger clear glass crystals, the final stage of drying should be slow, from dry alcohol seem best,

with a little acetone added, then was with alcohol only

Recrystallization

This is the same as presented above in De-contamination procedure

Re-crystallization of chili using methanol, denatured alcohol, or 91% isopropyl alc. will grow some very pretty, large crystals and will make your product more pure and much more potent. This is one procedure that is simplicity itself and always produces a major improvement with surprisingly little loss of product.

Super pure crystals, using denatured alc. and vision ware

After the chili was pulled out of the toluene (non-polar solution) using HCl and water, It was run through a filter and placed in a vision ware bowl for evaporation. The water was evaporated leaving the crude raw Crystals.

These were crushed and washed with ice cold dry(25%-cooked-epsom salts-inside-the-acetone-container/75%-acetone) acetone. Using a filter with cotton-ball-tipped and five or ten filters, use this to ensure the acetone is 100% stripped of not only the water which may have condensed, but the dessicant used inside!! The epsom salts. It should pour a clear liquid. Don't getsloppy here now ya hear?!

The washed Crystals were then dissolved in hot denatured alc. the alcohol was boiled away until the first sign of skin forming or the first sign of crystallization noted. Remove from the heat add enough alcohol to remove the skinning so no more crystallization can be seen then add 20 ml of acetone, if it turns cloudy add alcohol drop wise until it is clear again cover and place in freezer 6 hours or more( overnight is great) you will return to find crystals floating in the liquor.

Rapidly filter out the cold crystals , then wash them with a little cold alcohol to remove any gakk on the surface and in the outer crystal layer, set out to dry..

All three steps were performed without ever removing the chili from the vision ware bowl.

Recrystallization details

The Chili is dissolved in a minimum amount of dry alcohol, this is heated, USING a Safety fan (Always)

as needed to get it to dissolve , bring it to a soft boil . Continue boiling until you begin to see the chili form crystals on the surface of the alcohol.

This is a super saturated solution . Add a little alcohol to dissolve the skin again, and add 20 ml of acetone

Then cover and set in freezer, as the temperature drops, crystals will form .

Leave in freezer for 6 to 12 hours or even longer. Generally the longer in the freezer the bigger and better will be the crystals.

The chili re-crystallizes as the temperature drops, the alcohol won't freeze.

As time goes on the crystals "digest". Digestion means the crystals are slowly re-modeled, the outer layers with impurities are stripped away a reform without the impurities.

In addition the smaller crystals dissolve and become incorporated into the larger crystals because of volume(cubic) versus surface area(square) considerations

After which the resulting crystals were quickly cold filtered , washed with a little cold alcohol and dried.

The crystals should be rinsed lightly with alcohol wash off any of the mother liquor that is stuck to the crystals, and to remove the outer layer of crystal which is slightly impure

Note-for even better results:

The super saturated solution(dissolved in hot solvent) forms crystals faster than the hot but more dilute solution , but the more dilute allows better digestion and more pure crystals.

Life is such a trade off in every way.

Appearance:

The resulting crystals were sparkly, 1 cm x 2 mm x 0.5 mm very clear

up to 1 inch long and chunky

BioAssay:

Performed repeatedly, and it was determined that the resulting product was far superior to the original stock. The taste was greatly improved . Any nasty residue was essentially nonexistent. The overall potency was increased significantly. Enough to warrant the use of this technique in future productions.

Final thoughts

I could say more but this is enough for most to get fair shot at it.

I realize I repeat myself over and over many times, for you to retain the information in long term memory it must be repeated three times.

85% of what you read will be forgotten within a few hours

If at first you don't succeed , before you try it again, analyze what went wrong first!!!! Other wise you will repeat the same error and will have learned nothing

At first you may have failures, I did, mostly due to equipment or chemicals

Remember at this point you may still be a little green, but you have taken the the plunge and you know much more than you suspect you know. The amount you have learned at the hive is enormous , so don't kid yourself into thinking your not getting it, more likely than not your are so close, and just one little thing is stopping you.

I estimate that at least 30% of you are tossing out good speed because they are not sure about something.

Take advantage of a failure to learn maximally from it, A failure is an important tool, use it!!

To figure out what went wrong, Backtrack to the point that you first noticed something was not right, there is more than enough descriptions of what to look for and when you did not see what you expected to see, The error occurred immediately before that.

Believe in your own skills is what I am saying, because there is no way you could have gotten this far without developing major amounts of savvy about this stuff.

One main cause of initial failure is your Chemicals, everything at first is OTC because you have not yet developed the connections for supplies., and the OTC stuff has to be re-made to suit your needs.

The ephedrine must be clean and the govt. is constantly tweaking the stuff. They screw me over at least two times a year with their concoctions.

The Iodine the main source of energy for the reaction is touchy , if made from tincture , wash it repeatedly by shaking it hard in a 2 liter container (and not in a 4 ounce jar or by running water over it in a filter) I will wash it with major amounts of tap water for maybe 4-5 times , then finish it off with distilled water,

Use an excess of iodine 1.5x to 2.0 x ratio if unsure.

RP is only a problem if match-book stuff is used, you need a shit load if from match strikers because the contaminants , glass specifically alters your weighing. I have never used the matchbook RP but I have listened to those that have, and it will work, from the amount of glass and trash that is likely to have remained in the RP it is a good idea to use an equal weight of MB RP and Ephedrine

The Equipment will be OK if you follow the sizes used here, once you go to nano-sizes or to larger sizes you will begin to have problems, all the equipment needs resizing together, you can not just get a bigger reaction flask to make bigger batches, every step of the way you will be dogged by size problems, if you do.

.

To prepare everything properly is a pain in the ass , if doing it all OTC for the first time it may take you several days to clean up the E and Iodine and RP., but it is the formula for success, if it were easy anyone could do it, but everyone can't do this, it takes a special touch, you either have it, or you must learn it.

Once you make a batch you become a major asset and people want what you can create , stuff begins to come to you as if by magic, I am amazed at what people will trade for a gram of this shit. They begin to bring you better chemicals, or you pay them in speed to acquire chems for you. and "Viola" your home free. then it is as easy as measuring it out and mixing it together.

As time goes on you become intimately familiar with the properties of these Chemicals, and it will seem too easy, you will know what to do instinctively,

You have seen it all now, at least once, so the best thing to do is to get some experience behind you, and start cooking away, be a good observer..

Once you have a successful reaction, 90% of the screw ups are fixable easily, it is getting the stuff to react that should be your primary focus. Once made you will get it out of the solution, believe me you will find a way.

Save everything until absolutely sure that you have product or until you know what went wrong.

I still save everything until I have all the final product accounted for.

And even the nasty lye water contain recyclable Iodine

Haste makes waste and

materials

1) 1000 ml 2% Iodine tincture = 2.5%I+2.5%KI in etOH and H2O =-

2) 100 ml Muriatic acid = 34.4%HCl

3) 475 ml Hydrogen peroxide = 3% solution of H2O2

4) 1750ml Distilled H2O

In a 1 gallon container (plastic or glass),

mix 1 liter of 2% tincture of iodine

with 250 ml of Muriatic acid

stir and allow to sit for 15 min.

Add 475ml of a 3% hydrogen peroxide

stir and let sit an additional 15 min.

Add 1750 ml distilled H2O

shake and let sit for 15 min more.

An orange water layer appears on top of a dark gray layer of I2.

Pour off most of the the orange water

Add fresh distilled H2O shake and let sit

Pour off most of the the orange water

Wash a total of three times with distilled water

On the last wash pour the I2 into a stack of 5 coffee filters

Wring it dry

roll the iodine ball into 5 dry coffee filters

Wring it dry

Roll it into 5 more dry filters

wring it dry

Put the I2 in a small clean glass jar break up the iodine ball

place the jar of I2 on a piece of cardboard, cover the I2 with a larger jar

put in freezer for several hours

Remove jar of I2, seal it tight, with cellophane then screw on the cap store it in a dark cool environment

Potential problems

Not rinsing the I2 enough with water to remove the chlorine and salts from the tincture Not drying the I2 out enough and adding it too wet to your reaction.

If in doubt at all re-wash the iodine with distilled water in a filter and wring out, The iodine is only very slightly soluble in water, you lose very little washing with water. If it is not clean and dry you can lose a lot more in a failed reaction.

The Solution

There are only three chemicals involved in the reaction, make sure they are top notch in purity and integrity

1. Ephedrine - the free base reacts stronger than the HCl salt

2. Iodine - use more if you are not getting a reaction 1(E) : 2(I2)

3. Phosphorus- use more if doing a small amount 1:E/0.8:RP

It hurts to see a couple of hundred dollars in chemicals go to pieces in front of your eyes..

So do not get fiendish and attempt a flawed batch, think first, before acting rashly

This is a proven, no BS procedure for cleaning up RP. This is not the procedure used to get the RP off of match strikers.

The use of Sulfuric acid and/or Hydrochloric acid is recommended only in severe cases if nothing else will work.

What happens to the RP,? Some gets oxidized in the reaction and is gone. Most will get a waxy build up after a few uses,

It gets course and grainy because the powdery stuff, is what reacts the best, large surface area for a small volume.

Screen

Run it through a fine stainless steel screen, (kitchen utensil - grocery store) to remove debris, and breakup chunks

Acetone

put the RP in a funnel with coffee filter pour acetone through it until the acetone is a light yellow

Solvents

Any of the following familiar solvents have been safely used to wash the RP

methanol, ethanol, denatured alcohol , isopropynol, toluene , xylene

Rinse with acetone again to remove non-polar solvents

If you want a solvent that gets thatfucking glue off with effiecincy and efficacy then go and buy you some:"Goof Off". It is manufactured specifically to disolve and remove glues of all fashions.

It contains xylene sure enough but it seems to be that methyl carbitol and surfacant mixed in along with itthat makes it a most usefull four or five bucks the for usual purchase price.

And some of us prefer to grip on a nice old Old Timers pocket knife and scrape off each striker one at a time. There is at the end of this session no paper and 99% of available striker-surface is collected. I say striker surface so as to imply and reming this mass is no more than 50% P4/red phosphorus.

It is a good habit to form in getting vigilant with boiling/soaking/refining your collected striker-surfaces and be smart and weigh the s-s-mass before refining and then after. This will be your guide and future refrence for knwoing when it isas ferined as humanly possible.

The more ANAL you become on CLEAN AND PROPER PRECURSORS, the less R.P. needed and the more product there will be when its time to acidify that which was basified(with NaOH/Lye)

And its only a matter of 15% more effort to net 50%+ more of a refined and cleaner contaminate-free ingrediants/precursors so that the redution has no free-radicals to throw shit in the spokes of the wheels in motion in respects to the mechanics of this reaction.

Water

Final Washes with warm or hot distilled water

Sulfuric acid wash (rarely needed)

If the RP still has an abnormal coating

Soak in warm dilute H2SO4 10 minutes

Add equal amount of HCl for 10 minutes

let settle

pour off the acid

repeat until clean

repeat the Acetone and water washes

Dry it

An oven at 150 F to 200 F just barely on,

I have had the glass bowl break while baking 1/4 pound of RP in the oven , the RP was fortunately still wet , it started to smolder about 15 minutes later the house was full of smoke.

Threw the towel on it , that slowed it down, pumped two large fire extinguishers into it with no effect , secured the garden hose and with wet towel finally put it out, began the clean up and there was still areas on fire, the extinguishers ruined the RP and made a nasty mess

Screen and powder

Usually screening it will be is enough ,

Powder with mortar and pestle or use your imagination.

CLEAN E/I2/RP=CLEAN--->[CRYSTAL<-->METH]

quote:



1/1.5/1 Tincture or poor quality of chems --- Matchbook RP use 2x -3x normal amount"

Ok, just so I got it straight, where the ratio for red phosphorus is 1(grams?), I would use 3(grams?) if I were getting it from matchbooks, correct?



No. That is referring to using two-three times as much R.P. as you would if you were using Lab Grade R.P. Look at what I wrote again and you'll see where you overlooked what I was saying as it is almost natural to think we need a 1-part R.P. to that of the E-net. weight take a look---->

quote:



:"1/1.5/1 Tincture or poor quality of chems --- Matchbook RP use 2x -3x normal amount

1/1.5/0.6---> My favorite uses excess iodine- this insures a spontaneous reaction, and complete conversion of E to Meth

1/1.0/0.33--> 4 oz or more good chemicals ratios

1/1.0/0.20---> Lowest amount of RP used to convert 6+ ounces

1/1.2/0.7---> What to use for less than an Oz



<----see that?!

quote:



what on the matches does it come from? Does it come from the match head or the striking pad on the actual pack?



{b]The striker is the strip of abrasive surface located on the side of match boxes or at the bottom of paper fold over matches(you know these are what usually comes to mind when you think of matches).[/b] The tips do not contain R.P.

quote:



How many packs of matches are needed? [Obviously a shitload but just a rough estimate]



I'll spare you the usual overly-estimated figure of what is normally answered here and give you the more realistic figure to shoot for as this is the net weight of R.P. after refinement. Not the gross weight of the scraped-striker-mass.Figure on .250g's(1/4-grams)per box of 100 matches if scraping paper matches. As to what brand to use all I can recommend is to shoot for the ones which look nice and redish in color. Off-reddish ones are ok. Brownish ones are not. Some say they are but of the six grades of red phosphorus, none represent a brownish color. [b]If you are doing a nanowhich is 1-3 grams I recommend buying the new DIAMOND BRAND-FIREPLACE MATCHES IN A SILVER-CYLINDER CONTAINER.Note:If money is limited buy the store brand equivalant Cylindrical Fireplace Matches Give it a good soak as the glue is more prevailant having more surface area to bond to as the striker is circular but go and take a look at that bright pretty red R.P.!! And it ain't clay making it that pretty red!! I recommend this for a nano because the R.P. is good and you won't have to put haste in your precursor-refinement because of the tedious tasks involved causing you to want to "hurry-up" and take short-cuts.

At the store the other day all of these matches were jacked of their strikers. lol!!! Whcih would be easy as they pop right off but stealingin this fashion is not endorsed or encouraged.

As to how many to buy, I would recommend five. To take care of that glue on them buy some:"Goof Off". And soak for an hour and I recommend using a sharp pocketknife over a razor any day of the week as they scrape just as effectively in regards to scraping down to the paper but cutting in deeper is hardly ever an occurance you'll have to worry about. Shit just glides right off with a knife. Those Swiss Army knives the smalllest ones they sell with the tweezers and tooothpick are perfect here.

If you think you got the patience then go ahead and save you some money by having such patience for those Fireplace matches are $2.25-per and scrape you 400-matches(on average not a set amount now so don't come complain later it took more) per One-gram of refined pseudo. Or 4 boxes of 100.

quote:



psudeoephedrine - any particular brands that are better than others?



Well stay away from extended releas pseudos being a newbie and forget the red hots(30mg's regular Sudafeds red-coated) snd go pay your $2.98 for some Equate AntiHistabs(48-60mg's=2.88g's net-wt.) at Wal-Mart. And while you are there buy a coffee gringer. A one time investment that will save you the hassle of pill-powderizations for future extractions/reactions.

sitbcknchill is correct in Dollar General or Family Dollar selling budget-pseudo.

Money adds up with a quickness when precursor hunting & gathering.

So look out for places which might sell one particular item you could use which is sold there cheaper than anywhere else.

Like 88-cent iodines which are sold in a little brown bottle right next to other little brown bottles and in the Antiseptic aisle. Where Isopropyl alchols and Hydrogen Peroxides and Band Aids are sold.

I intend for this thread to be an all-in-one sythesis thread where we can direct any future simple to moderately complex questions about methodologies and fundementals.

So anyone who sees something which is not included and should be by all means post it.

This ain't my thread this is yours. For informational purposes.

It might end needing to be comprised into two threads as a thread with 1000000 replies is hard to sit through and read unless one has kept up with a regular frequency as to whats inside it.

But you guys please refrain from the usual flames on the kindergarten questions pertaining to Rxns.

We'll just answer them and they only need answered once so it's not like we'll be repeating ourselves and in theory we will be spared them(questions) being asked over and over again.

So again, just like sitbcknchill did above me here in answering a couple questions please do the same.

This thread is nobodys to claim and everybodys to use.

Jam.



Jamiroquai

Moderator posted 12-31-2003 00:31



quote:



With the new questions concerning the woods, the koalas, and the squish between your toes. Does this mean all swims back to research and re-research



Now thats pretty cool Princess! I must say that I'm glad I remained silent on the matter for you asked for me!!

I am the last one to be all anal and act like a dickhead in the name of whatever but I must ask that all of you guys delete your replies above here in the name of keeping this thread releveant to its purpose.

I ain't irritated or anything like that just trying to make a thread here at totse that for once is informatively homogenous.

In the future instead of Rhodium re-directs......you cann give this: http://www.totse.com/bbs/Forum26/HTML/003491-2.html For it will answer anything and everything.

None of us got to where we are without our own efforts of self-education.

And nothing is different for any person new to the whole scheme of things.

And since this is in fact totse, Sources and being explicit is totally included so as to leave no room for questions.

But anything in this threaad must be from an experienced point of view.

Conjecture and speculations or speculative proposisitions are to be kept for posting on the Board. But bare in mind man that it must be somehwat logical and not something a tweeker buddy tweeker talking has said.

Let him himself come post his rhetoric if he beleives in what he has to say.

There are some more additions to this I am going to punch-in which involve forgotten methodologies that need including as I am sick of this bullshit of there is only one way to rock!!

HA!!

Nobody can dictate only ONE WAY IS BEST!!!

For back when RP was labgrade all over, the dope produced in 45 minutes was just as clean as 48 hour long-wets.

Why this is so is what I intend to bring to light.

Lab Grade precursors can be acheieved from a crudely made resource.

And incoorporating waxpaper into your iodine refinements can greatly improve abilities to "handle" your messy-stain-y I2 which is never discussed in pertaining to a reliable route to a righteous refinement and DRY DRY DRY!!!

all contaminants can be removed from wshing your polar and non-polar solvents which your meth freebase is camping in!!

And if those contaminents are soluable in one or the other(polar or non-polar) then who can say the shit still hangs on to the end?!

So this is what's motivated me to simply bring back a forgotten mentallity and forgotten quicker way to strip that fucking pseudo of its one oxygen molecule and doing so with no contamination.

It can be done.

Pure precursors produce pure products.



I hope I never have to type this much in one setting ever again in my life!!! lol!!

Nor edit this many words man.

Talk about no wonder I hated fucking school!!! Don't miss this part of it a bit.

Jam.
 #2 
Old 2004-02-11, 10:12
Regular
 
Default Re: Meth Synthesis Information Thread

<A HREF="http://users.telenet.be/eforum/emoticons4u/violent/sterb163.gif">http://users.telenet.be/eforum/emoticons4u/violent/sterb163.gif" width="90" height="90 (http://users.telenet.be/eforum/emoticons4u/violent/sterb163.gif" width="90" height="90)</A>
 
To the best of our knowledge, the text on this page may be freely reproduced and distributed.
 

totse.com certificate signatures
 
 
About | Community | Bad Ideas | Drugs | Ego | Erotica | Fringe | Society | Technology
Hot Topics