Steam Distillation
Purpose Steam distillation may be used to purify meth , after the reaction.
Advantages over A/B. It eliminates the headaches of 1) a Separatory funnel, 2) a non-polar solvent 3) shaking 4) multiple washes. 5) Waiting for layers to separate 6) to do multiple pulls of crystals 7) no more lye lock You can still 8) You can still gas with or without a non polar
Method The reaction mixture is filtered, then lye is added to bring the mixture to pH 13, this creates the freebase Steam is bubbled through the mixture, the steam carries pure e freebase to a cooling condenser and a collection flask. Can't be much simpler All you do is add lye, and out the other end comes purified meth freebase. Steam distills at the temperature of steam 100C . If you were to attempt to distill at the boiling point of Free base meth i it would take considerably higher temperature.(250 C)
The steam unit is like an assembly line and requires a bit of room, It can extent laterally for 3 to 5 feet long. It is composed of four(4) simple units joined together 1) The Steam Generator(pressure cooker or a glass flask) 2) The Steaming Flask - holds the reaction mixture 3) The Condenser
4) The Collector In addition you will need a heat source for the steam generator A warming tray for the reaction mix A water pump or water source for the cooling condenser Various rubber tubing Some glass or copper tubing
Principles involved
Steam Distillation works off the property of vapor pressure Vapor . Press is similar to the boiling point, but is a different property .
Vapor pressure occurs at the surface and can occur at temperatures below the boilinnt, . increasing the temperature, increase the vapor pressure ,.
Here is a simple and effective unit The product comes across to the collector in the form of a clear free base oil, floating on top of distilled water
Making Meth HCl salt If HCl is added as a liquid or a gas, the freebase layer will disappear, the HCl salt is produced, and the solution may be evaporated to give the solid product.
You can separate the freebase from the water, then gas the freebase, or add a non polar and gas the freebase
Some Finer details . A pressure cooker is not needed because the apparatus does not need high pressure just a steady flow of hot steam, with average pressure. The steam is allowed to bubble through the alkaline reaction mixture carrying Chili free base and steam to the cooling condenser, and into the collector vessel. To make the process more efficient the steaming flask is warmed up Like the above example in a hot water bath on a warming tray is used. It is important that the steam is very hot and kept at a constant temperature, So keep the distance between the source of the steam and the flask short, and well insulated.
Super heated steam An advanced form of this device would use super heated steam , which , brings more product and less water to the condenser. It is quicker more efficient. The steam is re-heated or super heated by a gas flame before it enters the steam flask, A nozzle that creates a broad flame is used on the torch. This is easy to make with some heavy sheet metal . This directs the flame to a glass or metal tube for super heating
Temperature control Also the steam flask is enclosed or surrounded by steam or hot water to maintain it at the high temperature.. With out heating the reaction mixture , too much water condenses in the reaction mixture. These two modifications will give a more pure free base and will allow less water into the condenser , as well
as make the process much faster
.
Splash head Use a large steaming flask and don't fill it past 1/2 way to prevent the alkaline solution from splashing up and contaminating the steam in the condenser. You may have seen the term splash-head . A splash-head is designed to prevent the alkali solution from splashing up into the condenser. A simple splash head can be made from an elliptical piece of plastic (Tupperware) with a hole in the middle so it fits over the oncoming steam tube. It should be placed to block the splash from hitting the
tube leading to the condenser. . It should loosely fit ,(that is why elliptical) in the flask so the steam will flow around it , yet the splash, will hit it.
pH considerations Finally you will need to check the pH of th solution periodically. Precaution #1 If you turn off the heat to the steamer you will creatye a vacumn in the Steam generator. If you look closly you will notice what a great siphon tube you have created, the reaction mixture will be drawn rapidly into the steam Generator. So either put in a bleeder line and open it up before turning off the heat ( a picture is forthcoming), or pop the top off the Steam generator. It does no good to pop the top on the reaction mixture, unless you also pull the entire steam tube out of the mixture. Monitor the amount of free base collected . As time goes on, the pH drops and the rate of collection of free base decreases, There will is still be freebase in the flask. But because the pH drops the amount of free base coming across is lessened. So turn off the steam apparatus and carefully add more NaOH to the steaming flask to bring it back up to pH 13 and resume steaming. You will see a large amount of free base start coming across again , this usually needs to be recharged only once or twice. But incremental small recharges of NaOH is probably best
Well, if no NaOH is crossing over into the collection flask why does it need to
be replenished??? The Answer is below, you can think about that one for a minute.
Warnings of potential danger A word of caution,, If Murphy's law follows you around, Beware This thing will get excitable and get hyper fizzles, Be-careful when adding dry NaOH if too much NaOH To get it to blow you need an excess of dry NaOH that sits in the bottom as a solid . Once the steam heats it up it may go ballistic, and start shooting out every office it can find. Not good for yields, in fact it trashes your product because it will be on the ceiling , walls, and floor. To place a picture in your mind of what to watch for here is a story SWIW was distilling 6 oz of product The first three came through just fine and it was time to do a recharge, So SWIW poured in the dry NaOH, then in true tweaker fashion, decided to go with a larger diameter tubing all the down the line. SWIW fired up the steamer, the larger tubing seemed perfect, not realising that the NaOH on the bottom was getting super steamed, , IT started to slowly build pressure and then it blew the reaction mix up the hose into the steam generator and out the top SWIW watched 3 oz of final Chili product fizz everywhere, just thankful only a little alkaline solution was getting on SWIW. The shower was a very welcome relief from Na OH. Actually SWIW was lucky because SWIW had already done the first run and pulled out 3oz of product, When it blew 1.5 oz was recoverable from the three flasks 1.5 oz was on the floor, ceiling. walls, cabinets,
so actually recovered 4.5 oz Oh Yeah almost forgot, SWIW am sure you already have, or soon would have, realized that the pH decreases because the freebase Chili is alkaline and as it comes over the pH is decreasing. T What remains is primarily Na-I and NaCl in water ,
