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Synthese_PLUS

After the completion of the reaction, add 200 ml - 400 ml of water, then boil for 5 minutes. This should result in a clear fluid with the RP settling to the bottom( a few aluminum potpies from soft drink cans, helps remove any excess iodine, when boiling). Filter the RP out of the reaction mix, , Begin adding base or a Sodium hydroxide solution. Observation is the key, just watch what happens. First the solution turns white when the lye hits it, then it clears , With more additions of lye the water layer becomes milky white, and stays milky white for more than 30 seconds, you are very close to the alkaline pH level. The milky white is what?? A white precipitate?? It can only be that which you are looking for. Chili in the free base form, loosing its water solubility, coming out of the water layer Mix it well and observe closely for the whiteness to go away a little bit, leaving the water layer cloudy Add another dose NaOH, this puts it over the line, right where it needs to be add your non-polar solvent. You can be certain because 1. the chili was seen becoming non polar. 2. additions of NaOH do not form any added white precipitate in the water layer. 3. you may see a "lye lock", solidifying the water layer. Wait a few minutes then test the pH of the water layer just to be certain it is over pH 12.4 Toss in some table salt if you wish. 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 Washing the chili After removing the lower water layer Wash the non-polar/meth with about 1/2 volume of d-water This means add water, shake fairly well, let it layer, and fully separate and remove the water layer Repeat the d-water wash three (3) times 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 Considering the shitty quality of muriatic acid, it would be great to distill your own. If you are consistantly 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 onstead or distill your HCl first.