equipment
* one hot plate or oil bath
* two pyrex boiling flasks at least 100ml per box used
* one pyrex container at least 50ml per box used
* one separation funnel at least 100ml per box used (or other method to siphon off liquid)
* two 1000ml containers with lids
* one 1000ml graduated cylinder (or other liquid measuring device in ml's)
* one 5ml medicine dropper
* one large funnel with charmin filter
* several coffee filters
* coffee grinder
* hot pads or kitchen mitts
* wooden stirring spoon
* small digital scale
* safety goggles
note:
Credit for developing the charmin plug filter is given to the geezmiester. See the thread
https://www.wetdreams.ws/forum/topic.asp?topic_id=1347
for more information.
Reagents
* citric acid - also known as sour salt (used in kosher foods, home brewing and candy making)
* distilled h2o
* kosher salt - sodium chloride (non iodide)
* sodium carbonate – also known as washing soda
* sodium hydroxide – also known as lye
* hexane - also known as n-hexanes or mixed hexanes (found in electronic parts cleaner and some brake cleaners)
* white vinegar - grocery store variety
* vm&p naphtha - used as a paint thinner
note:
Do not substitute for vm&p naphtha. Shellite, white gas, petroleum ether and lighter fluid are not vm&p naphtha. Vm&p naphtha is a combination of aliphatics, xylenes and ethyl benzene and has an unmistakable smell of naphtha (moth balls). Some oz bees have reported the same success with shellite but since i cannot verify this, i cannot guarantee it will work.
Possible optional reagents
* anhydrous acetone
* anhydrous magnesium sulfate or sodium carbonate
how does it work?
Credit should be given to dwarfer for his long investment in researching polyampholytes and uncovering a method to render them ineffective.
Using white vinegar creates acetate ions that will confuse the hell out of the poly ampholytic polymeric amendments which constitute the principle component of most modern pill formulas. At either very high or very low ph, polyampholytes act like polyelectrolytes. By changing the ph slowly in a hot and ironically crowded environment, the poly-electrolytes assume a different electrical configuration.
Added salt ions can screen the repulsion between excess charges. With no added salt, the polyampholyte chain is stretched on its largest length scale by the repulsion between excess charges. As salt is added the length decreases and the repulsion between excess charges begins to be screened. This screening of charge repulsion decreases the chain size and eventually decreases down to the internal polyampholyte length due to the charged monomers. In simpler terms the polyampholytes can no longer hold onto the pseudo.
Citric acid is added to drop the ph to 1.5 in addition citric acid also gets its acidity because of carboxyl groups that are attached. This adds more confusion to the mix.
Preparation
non-chlorinated brake cleaner is commonly a mixture of hexane and methanol or isopropyl alcohol. The hexane can bee separated by washing once with water, separating and then drying the extracted hexane over freshly dried sodium carbonate or magnesium sulfate.
Electronic parts cleaner is usually pure hexane and may bee used as is. If it is mixed with alcohol follow the same procedure as brake cleaner.
First we need to make our extraction brine the basic formula is:
* 100ml of white vinegar
* 35 grams of kosher salt
* 15 grams of citric acid
so to make about a liter we will place in one of the 1000ml containers with a lid the following:
* 800ml of white vinegar
* 280 grams of kosher salt
* 120 grams of citric acid
shake shake shake for about 3 to 4 minutes. It will almost all dissolve but not quite. This is ok. We want it to be saturated at room temperature.
Note:
The brine is really corrosive, so avoid the use of metallic objects.
Next we need to make our basing solution. You'll need about 20ml per box used. This is made by filling a container half the way with crushed ice then adding an equal amount of sodium hydroxide. Stir until dissolved. Place in the refrigerator to cool.
Note:
If your pills contain tripolidine hydrochloride it is recommended you do a prewash in ice-cold anhydrous acetone, filter and dry.
Method
powder the pills in a coffee grinder and place the powder into a clean boiling flask.
For every box of pills used add 50ml of the extraction brine to the pill mass and placed the flask on a hot plate. (an oil bath is preferred) bring the mixture to a boil. Let it boil for at least 10 minutes.
Note:
This calculation was based on a box of pills used = 48 x 60. If you are doing 120's or 240's you may need to increase this to 75ml to 100ml per box to compensate for the additional filler.
Filter the mixture through a charmin plug in the bottom of a large funnel into the other boiling flask. All the collected liquid should bee crystal clear.
Slowly add powdered sodium carbonate to the collected liquid in small portions. Co2 will be evolved so take your time so the liquid doesn't end up on the floor. Stop when the ph is 7 or co2 is no longer produced.
Place the flask with the neutralized filtered liquid back onto the hotplate. Add approximately 1/2 of its volume of vm&p naphtha. Heat until the brine layer just starts to boil (actually a simmer) then slowly start to add the basing solution a few mls at a time using the medicine dropper. You want to do this so the ph change is gradual. You will see the point where the freebase starts to be liberated. Continue to add basing solution. Stop when adding basing solution causes no more change in color or sediment. If you want to be sure the ph of the brine layer at the stopping point should be 11 or 12. Let this simmer for about 5 minutes.
Warning:
Boiling a bi-layered liquid is dangerous. When one of the layers is flammable extreme caution must bee taken. It is not necessary to achieve a full boil. A good simmer approximately 90-95 degrees c will suffice. Do not underestimate the flammability of hot vm&p naphtha. An oil bath is strongly recommended. Do not add more than a few mls at a time of the basing solution. Disregarding this instruction may cause the brine layer to superheat and boil over. Always wear safety goggles and work in a well ventilated area. Never use anything other than pyrex.
Separate or siphon off the naphtha layer into your third pyrex container. Cover and placed the container in a freezer for about an hour and a half.
Take the naphtha out of the freezer and pour off the naphtha leaving as much of the freebase crystals behind as possible. Capture the lose crystals in a coffee filter and return them to the container. Then wash the freebase crystals in ice cold distilled water. Drain the water and freebase crystals into a clean coffee filter. Then pour a liberal amount of hexane through the recovered product. This will wash the water off and help dry the crystals very quickly.