Straight to BEE III - The Pickled P

hAzzBEEn · Tue Jun 28, 2005 9:54 pm

Straight to Bee III – The Pickled P
By VideoEditor 06/02/05

VE here with a radically different approach to pill extraction. Straight to Bee III challenges the current extraction thinking while adding some important features such as no evaporating large amounts of smelly liquids, solvent fumes are minimized and there is no HCL gassing required. All reagents are over the counter and easily acquired.

Note:
Due to the ever changing formulations in pills today there is no one cure fits all. Tests have shown this to work with a wide variety of pills but there is no sure thing. Please run a test batch before committing a large amount of your investment.

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.

This will probably bee the last of the STB write-ups as prohibition seems to bee the next phase in trying to control the diversion of pseudo based products. Please bee safe. If you're out of control please get help. Don't let law enforcement make an example out of you.

-VE out

hAzzBEEn · Tue Jun 28, 2005 9:59 pm

The original thread and discussion on Wet Dreams is located here:

Straight to Bee III – The Pickled P

You must be registered and logged in to view the thread.
There are several pages of discussion about the details of the method.
It's been referenced so many times here that I thought the post was appropriate.

geezmeister · Busy Bee

This approach seems to work well against the methacrylate polymers in particular.

There are a couple of gakks that do find their way through; some work is being done on these. One pernicious type of reaction inhibitor sneaks by even with the pseudo burning completely clean on foil. It can be detected at that point by observing the melted pseudo as it starts to vaporize. With the gakk it will jump off the foil or run from the heat. Without, it will do neither. Recrystallizing the salt form of the pseudo will leave the gakk in the acetone by the second pass.

Reports of complete success wtih 120's suggest the method has great merit.

hAzzBEEn · Fri Jul 01, 2005 6:36 pm

How harmful are the pernicious gaks that make it through STBIII? It sounds serious. Is the STBIII pse reaction quality, or does it still need further processing?

pernicious - Causing great harm; destructive

geezmeister · Busy Bee

Depends on the pill source. No extraction technique is universal anymore. This method works very well against the methacrylate polymers as the combination of ions in the acidic, salt-saturated solution, make them collaspe to their shortest length, making the pseudo accessible to the a/b extraction method. Or so we think.

Combining this with a careful, gradual basing and a hot extraction into the nonpolar solvent avoids other pernicious gakks, like what is commonly referred to as Orange gakk.

Yet the method is not truly universal. Reports are clear that some formulations are impervious to the method, and other reports indicate that some gakk may get through the process. Thus far SWIG has identified only one gakk that made it through, although said he had low yields a couple of tries.

The one gakk that made it through has not been identified. but is what some call "Fool's E." It has a profound effect post reaction when HCl is added to salt the ---- oil. One thing SWIG noticed was that on a single squeeze of the gas bottle, the nonpolar became full of white crystals and had to be filtered after the second squeeze. The filtered nonpolar combined with acetone used to rinse the goods already salted out produced more crystals immediately when gassed; after the second gassing nothing else was produced by gassing the solvent, or by titration.

Yield appeared execellent until it was discovered that a portion of it was just not ----.

The same gakk will have incredible effects on titration. The first pull of SWIG's titration of the nonpolar solvent is usually separated before the pH falls to 8; this first pull is usually evaporated separately; this pull is usually about 35% percent of the total yield, but with the gakk present the first pull will fall to about 10%; the second pull, taken between pH 6 and 7, is large, usually 50% of the total yield, and with the polymer present, the second pull appears to be very good. A third pull usually gives the last ten to fifteen percent of the yield, but a third pull with this gakk present will again appear to be a great yield. The stuff looks like product in the evap dish; it is not NaCl nor is it grainy or textured differently than the product it self. It isn't product, though, and burns with a nasty taste with residue left on glass or foil.

SWIG said he figured the gakk was something which polymerized when the acid was introduced to salt out the product, since one simply does not even see it before that point. The pseudo (both in salt and freebase forms) vaporizes cleanly off foil prior to being reacted... and the only hint this stuff is with the pseudo that SWIG claims to have seen is that in the freebase form when melted on foil it appears to run from the heat.

Post reaction, recrystallizing with alcohol and acetone two to three times will produce product in clean form but low yield; the gakk will be found in the acetone rinses and the last portion of motherliquor. It takes the form at that time of a clear, viscuous fluid that does not air dry, even under a fan, but will dry over low heat in time.

SWIG said he believes that recrystallization of the pseudoephedrine before reacting it several times in alcohol and acetone may have the same effect. Unlike other polymers he has encountered, this one does not prevent crystal formation; it impedes it for the first pass, is pretty much cleared by the second pass, and usually the third pass yields true pseudo crystals. Prepuce suggested that if one were to extract the pseudo and precipitate it as freebase crystals, then dissolve those crystals in acetone and gas for the salt form, one could leave the gakk in the acetone. SWIG planned on trying that the next time he had a supply of those pills.

This gakk is one that will impede the reaction in part. The product lacked the euphoric effect desired, but seemed to have the CNS effects, although in less long-acting quality than expected.

p2e3r4f5e6c7t8 · Mon Jul 04, 2005 8:22 am

Hey ya GEEEZZZZZZZZZZZZ dude, How are ya mate, Long no time no see since the hive & Rhodium's site went away, (fuck it).
Anyway swip was thinking of trying this method, But one question remains and swip is wondering how to sorta incorparate the KOH boil into the STR8 toE 3, Because from what swip has read no one hear has even posted results on yeilds from either method. Rolling Eyes

loki · guinea pig

loki · guinea pig

what i mean is, a synopsis, something like what you already put, plus explaining what is done next briefly.

the extraction method is very elegant, i particularly like how few steps there are to it. less steps means less handling and less handling means less chance for errors (eg, spills) and less mechanical losses.

swim will do a test and writeup using aussie naptha (shellite) Very Happy

loki · guinea pig

Here's a proposed process that swim will use:

make up brine solution with the following proportions:
100ml of white vinegar
35 grams of kosher salt (rock salt is substituted)
15 grams of citric acid

add pills (in this example we are working with 18x120mg in 75ml of solution) to solution in a 125ml pyrex container, microwave for 2 minutes or until pills completely decompose, taking care not to allow it to bump. add a litre of water in a jug sitting beside it on the turntable to ensure it does not rapidly start boiling.

filter with charmin filter, add an extra 10ml of hot brine solution after it completes the filtration to wash through any residuals.

neutralise with sodium carbonate, slowly, the cessation of evolution of carbon dioxide indicates approximately neutral pH.

put about 40ml of shellite on top of the solution and place the beaker onto a hot electric frypan.

add the basing solution with a dropper a few ml at a time (in standard small droppers from 25ml dropper bottles, about 2 dropper loads is 1ml), add slowly until you can see that the solution ceases to change. at this point, let the solution continue to bubble for 5 minutes.

separate the shellite from the brine solution using a separatory funnel into a small jar, dry the hot naptha solution with epsom salts, and reduce the solution until it starts to oil out and add a little shellite until the oil redissolves, cover with polyethylene wrap, and wrap it in cloth to insulate it to slow down cooling (this ensures better crystallisation). in about 2 hours the jar will have deposited all its goodies, decant the solvent and collect the crystals of freebase pseudoephedrine.

sit the jar with crystals in a pot with water boiling underneath and slowly add hydrochloric acid solution (1/20 diluted 37%, approximately 0.5M solution), about 18ml will be required per 18x120mg pack of pills. add it slowly with heating, the HCl solution will dissolve the freebase and convert it to the salt. as the volume of remaining crystals shrinks, slow down the addition process to ensure one does not overshoot the point of neutrality and end up with excess HCl which will end up in the air when you evaporate it down.

evaporate the solution down on the steam bath until it forms dry crystals.

while still on the heat, add about 50ml of dry acetone to the beaker, and then slowly add dry alcohol to the solution slowly until all of the crystals dissolve (methanol and isopropanol are better but 95% ethanol will work *ok*). seal the beaker with polyethylene plastic wrap, wrap in fabric and put into the freezer. 2 hours or so later it will have deposited all of the crystals.

loki · guinea pig

i thought i should also add that the particular pills that swim uses contain loratadine... this substance is virtually insoluble in water and probably, almost certainly, insoluble in the extracting brine (thus unlikely to get through the charmin filtering) and the final recrystallisation is done because this ensures the last traces of it are gone, as well as residual povidone that is likely to be in the mixture.

geezmeister · Busy Bee

The freebase crystals obtained by freezing the naptha can be further cleaned by recrystallization without returning them to the salt form. Some cooks prefer the use of the freebase form to the salt form.

The note on the presence of impurities explains the behavior of the pseudo/gakk mix when vaporizing it. The same is true of what happens to a ----/msm mixture. The unusual activity on melting altered SWIG to the presence of impurities, even though the pseudo mix vaporized cleanly on foil.

There are more numerous reports of success with this approach with the generic 120's although few reports of yields have been posted. One of the shortcomings common among posters at Wetdreams is the failure to follow through with yield information.

Regarding substituting HCl for the citric and acetic acid mix, you might recall that several have approached pill extraction with HCl presoaks or boils, and none that I recall claimed much success. The saturation of the acid with salts is critical to the success of the method. Yields seem to improve with longer times for extraction into the brine and with longer times for the naptha to simmer over the based brine. Giving the extraction some time to complete appears to be a wise approach.

loki · guinea pig

i think a lot of dreamers don't have scales, swim doesn't either, he guesstimates. he would like to amend this situation in the future however, when he gets enuf $$ together to get some nice 4 beam 1 arm balance scales with milligram accuracy.

yeah i figure that the combination of acetic acid and citric acid and nearly saturated salt solution is all neccessary. it would result in a solution with very little active water in it, due to forming H3O+ ions from the acids (citric acid in particular is very strong at doing this). i wonder whether GAA would work similarly... the end result of using 80% acetic acid would be that the alkaloid would be dissolved in the GAA but there would be very insignificant amounts of water. water definitely seems to be the bad guy in the extractions.

swim works with sulphate pills, and it turns out from a little research that pseudo sulphate is very soluble in water, *extremely* soluble in fact, but very low solubility in alcohols (which would explain swim's failures when using alcohol to extract). in the stbIII.ppp sulphate pills would work even better because they are more readily taken up into the water.

WhoMe · Wed Jul 06, 2005 7:16 pm

Hi all VE here. Hey p2e3r4f5e6c7t8 ltns dude. Thank you hAzzBEEn for preserving the original document formating in the copy. There are two important changes in the method based on feedback SWIVE has recieved so far. One, increase the amout of brine used to 100ml per box used and change the amount of naptha from 1/3 to 1/2. Second, after neutralizing the filtered brine with sodium carbonate, finish basing using an excess of NaOH BEFORE the brine nears it's boiling point which will bee higher than 100c due to the salt saturation. Make sure the brine and the naptha reach a temperature of 100c and simmer for at least 10-15 minutes beefore seperating.

-VE out

loki · guinea pig

box=48x60?

i figured that amount of naptha was probably lower than needed. wouldn't it work better to do 1/3 amounts and three passes?

is there any particular reason for ensuring the basing solution is cold.

i presume the basing must be done before the heat because if it's not basified the heat helps the polymers grab the alkaloids back when they are hot like that.

what's the rationale and can you explain what happens if it is not done this way (one pass, base before heat, etc)

WhoMe · Wed Jul 06, 2005 8:34 pm