 "3 Steps" made easier than it already was.
All right, here is a slightly re-vamped version of Wicked_Rain's post "Here it all is- 3 steps". Very little actual content was changed. Just re-formatted a bit to make for easier reference, and a few minor notes and clarifications here and there on points that may be a bit confusing to a newbie (ie, the difference in amounts of H2O2 used in iodine extraction from 2% or 7%). If anyone needs clarification on any point, or any veteran dreamer finds a flaw... please let me know. Hope it helps... EM
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Section I- Preparing Reagents
A. Red Phosphorous
Materials
Equipment
1. Matchbooks - 1000
2. Scissors, Hobby Knife, or Razor Blade
3. Glass Jar w/Lid (1 qt)
4. Glass Bowl
5. Flexible Plastic Tubing
or other siphoning apparatus
6. Tongs
7. Heat Safe Beaker or Glass Jar
8. Hot Plate
Solvents
1. Acetone (100%)
2. Muriatic Acid (HCl)
3. Distilled Water (DH2O)
Process
1. Cut strike pads from matchbook covers taking special care to leave none of the colored cardboard on the sides of the strike pad. The dyes present will present problems
later. There will be some cardboard on the back of the strike pads, but that is acceptable as it should be undyed.
Safety Note: Caution should be used in this step as you are dealing with obviously flammable materials. No smoking and be careful to handle only one book at a time so as not to inadvertently strike the matches from one pack on the strike pad of another.
2. Place all 1000 strike pads in a quart sized jar and fill with acetone to approximately 3 inches above the pads. Cover and let it sit for 1 hour.
3. Shake vigorously and allow to settle (approx. 30 mins.)
4. You should now see a layer of red sediment at the bottom of the jar. Siphon acetone to approximately 1/4 above sediment. Refill to previous level with fresh acetone and repeat process. Generally 2-3 cycles of this process is sufficient.
5. Before siphoning on the final cycle, remove strike pads with tongs. Be sure to gently swish the tongs around a little to shake off any RP still clinging to the pads. Add another 1-2 inches of fresh acetone, shake vigorously and allow to settle.
6. You should now have about 1/4 of reddish-brown sediment at the bottom of the jar. Siphon off acetone and add approx. 1 cup of Distilled Water. Shake vigorously, allow to settle, siphon and repeat 4-5 times.
7. After removing as much of the excess water as possible, transfer the remaining
sediment into a glass bowl and allow to dry. The process may expedited by applying low heat from a source such as a hair dryer.
8. Take dried RP and place in Heat Safe Beaker or Jar. Add Muriatic Acid to 2 above the level of RP. Place on hot plate and bring to a boil for 20 minutes. This will burn off any impurities left in the RP.
Safety Note: This step should be performed outdoors as the fumes from Muriatic
Acid are strong and potentially harmful.
9. Allow it to cool and rinse thoroughly with 1/2 gallon of DH2O.
10. Allow to dry thoroughly.
B. Iodine
Materials
Equipment
1. (2) Large Glass Containers
2. Bedsheet
3. Paper Towels
4. Coffee Filters
Solvents
1. Tincture of Iodine 7%
2. Muriatic Acid
3. Hydrogen Peroxide 3% (H2O2)
4. Distilled Water (DH2O)
5. Dried Epsom Salts
Process
1. Put 1 liter of Iodine Tincture into a large glass jar. Carefully stir in 25mL of Muriatic Acid. Let stand 15 minutes.
2. Add 500mL of Distilled Water and stir in 1 Liter of 3% Hydrogen Peroxide. Agitate
well and let sit in a dark environment for at least 4 hours.
Note: This is the proper proportion for 7% tincture of iodine. If you are using 2% tincture you must adjust the amount of peroxide used accordingly (ie. Use 1/3 liter peroxide for 1 liter of 2% tincture). If not, you will over-oxidize and shred the iodine crystals so much they will be unusable.
3. At this point, you should see iodine crystals formed at the bottom of the jar. Decant the liquid into another jar. Do not discard this 2nd jar. Add 125mL of Peroxide
and allow to sit in a dark area until the next day. Well come back to this later.
4. Rinse the crystals in the first jar by adding Distilled Water and swirling vigorously. Decant water into waste container and repeat 5-6 times.
5. Filter remaining water through a section of the bedsheet. While the crystals are in the fabric, squeeze, squeeze, and squeeze some more to remove as much water as possible.
6. Place dried Epsom salts into the bottom of a glass container. Fold a paper towel and place it on top of the Epsom salts. Wrap iodine crystals in 2 fresh coffee filters and set them on top of the paper towel. Let sit for 4 hours and change the coffee filters. Wait 8 hours and change filters again. Keep changing to filters until crystals are completely dry.
7. The next day go back to that 2nd jar you put away. You should see more crystals in the jar, usually 10-20% of the original yield. Repeat steps 4-6.
C. Pseudoephedrine
Extraction Technique: Straight to Bee--The New Cure
A Universal Pill Extraction Technique
- Purpose -
SWIVE has only been doing free base reactions so his goal was to create a fast, clean method for producing psuedo free base from an ever changing array of pills. He believes this technique will accomplish just that. No pre washing, no soaking, no red removal. It's not a water less A/B in fact, it's just the B and thats why he calls it "Straight to Bee". It is totally OTC and uses activated carbon as a cleaning aide while exploiting the lazy characteristics of VM&P naptha. This method was written to be easily scalable. Average yield is 60% of very clean free base.
- Definitions -
In this write up SWIVE will use the phrase "for every box of pills used"
This stands for every box of 48 x 60mg, or 96 x 30mg, or 20 x 120mg.
In addition SWIVE will use the phrase "for every gram of total pill mass"
This stands for the total weight of the pills before grinding.
- Materials -
One beaker or other heat proof glassware
(approximately 100ml for every box of pills used)
One erlenmeyer flask or other heat proof glassware
(approximately 100ml for every box of pills used)
One graduated cylinder 100-200ml or other liquid measuring device in ml
One pyrex pie plate (2 if more than 5 boxes are used)
Two 5" glass funnels or plastic fuel funnels
One 5" wire mesh kitchen strainer (dollar store type)
One 5ml baby medicine dropper
Charmin bath tissue (reg no scent)
Glass stirring rod or bamboo skewers
Clean coffee grinder
Hot plate
Small fan
Small scale weighing in grams
Safety glasses, latex gloves
Activated carbon, research grade (pets fart store)
Corn starch (supermarket)
Dry acetone - CH3COCH3 (dried with baked sodium carbonate)
Sodium carbonate - Na2CO3 (washing soda)
Sodium chloride - NaCl (salt)
Sodium hydroxide - NaOH (lye)
VM&P naptha - no substitutions (paint store)
(Do Not use colemans, pet ether, lighter fluid, etc.)
- Optional Materials -
Gassing setup if HCL salt is desired outcome
One Inflatable Lab Assistant
Six pack of Guinness
- Abstract of Procedure -
Combine Pills with activated carbon, NaCl, NaOH and Na2CO3.
Grind to a fine powder and sift through strainer.
Stir in acetone.
Add trace amount of water.
Mix until paste.
Add corn starch.
Mix until consistency of damp potting soil.
Dry completely.
Add naptha.
Heat to boiling while stirring.
Filter thru Charmin filter.
Repeat two times
Freeze filtrate.
Filter out crystals.
Convert to salt form if desired.
- Standard Procedure -
01) Weigh pills and record total weight.
02) Place pills into a clean coffee grinder.
03) For every box of pills used add:
- 2 grams of washing soda
- 2 grams of salt
- 4 grams of activated carbon
- 4 grams sodium hydroxide
What if it all won't fit in the coffee grinder? Process about 3 - 4 boxes at a time.
Why am I adding salt? To attract water and to act as an abrasive to aid in grinding.
Why am I adding washing soda? To act as a buffering agent.
After grinding the mixture becomes hot and doesn't sift well? Carbon sold for aquarium filtration may contain excess moisture. The moisture content will be apparent when the carbon is ground. Moist carbon will tend to cake on the side of the grinder, and will feel moist. If the carbon is moist, dry it before use by heating in an oven or microwave. Take precautions handling the heated carbon to avoid burns. Allow the carbon to cool before grinding or combining with other ingredients. Store any unused dried carbon in an air tight container.
04) Grind the mixture to a fine powder. Its important that we grind the mixture as fine and uniformly as possible, about the consistency of coarse flour.
05) Sift the mixture into the beaker using a wire mesh strainer placed inside a large funnel to minimize dusting. When grinding and sifting be careful with vents, fans and open windows so your pseudo doesn't blow away as dust. You also dont want to inhale NaOH or carbon dust. Let the dust settle in the coffee grinder before opening the lid.
06) For every gram of total pill mass add:
- 1.5ml dry acetone
This measurement will get you in the ball park. We want the mixture to be a liquid at this point, not a paste. Add more acetone in small increments as the mixture will go from stiff to fluid very quickly. Acetone used for this purpose should be dried before use, as the moisture content of acetone can vary over such a wide range that the only way to obtain consistent results it to dry the acetone before use.
07) For every box of pills used add while stirring:
- 3 drops DH2O (use the baby medicine dropper)
Why are we using dry acetone and then adding water? Since the amount of moisture present is critical for proper basing, and the water content of non-dried acetone is widely variable, the only way to accurately control the moisture available for basing is to dry the acetone first, then add a measured amount of water.
08) Stir with a glass rod for about 3 to 4 minutes. The mixture will slowly thicken to a wet paste.
09)For every box of pills used add:
- 1.0 gram corn starch
10) Stir for a few minutes. The mixture will become very stiff and the consistency of damp potting soil, with no signs of visible liquid. Add more cornstarch in very small increments if nessesary.
Why the cornstarch? The cornstarch is a great absorbent and helps to dry our mixture fast. When drying the cornstarch will keep our mixture from turning into hard little rocks and when powdered again keeps the mixture free flowing. It also will help absorb waxy gak when we extract our free base.
11) Spread out the mixture on the pie plate(s) and let dry completely. It will dry fast because the carbon has increased the surface area of our mixture.
12) When completely dry sift the mixture back into the beaker using the wire mesh strainer placed inside a large funnel.
13) For every box of pills used add: [blue]
- 35ml Naptha
14) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a few minutes.
Isn't boiling naptha dangerous? Boiling any flammable solvent is an extremely dangerous practice. Solvents should not be heated over an open flame or on any apparatus that is capable of producing a spark. This includes defective or damaged electric hot plates. Adequate ventilation is required. This should not be done in a closed environment due to risk of explosion and/or fire and due to health concerns regarding inhalation of solvent fumes. The constant use of a fan positioned to blow across the solvent will disburse the vapor, reduce the risk of fire and explosion.
15) While waiting, make a charmin filter. Take 4 plys of charmin and fold three times to make a square. Fold that over once and then once again to make a quarter square. Completely wet the square with some clean naptha using the medicine dropper and place the pad into the bottom of funnel across the neck. The Charmin should not be "packed" or "compressed". Gently mold the edges around the contour of the funnel bottom. Wet it again with naptha and place this filter-funnel into the erlenmeyer flask.
16) Slowly decant the naptha into the funnel in small amounts and allow it to filter through the Charmin into the flask. Don't pour in more than can pass through the charmin in more or less real time. If you make a big puddle it may start to crystalize in the funnel clogging the filter. The filtered naptha should be crystal clear. Free base crystals will start to form in the filtrate. Set the flask aside.
17)[blue] For every box of pills used add:[blue]
- 20ml Naptha
18) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate and set aside to let the solids settle out for a minute.
19) Slowly decant the naptha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask combining filtrates. Don't pour in more than can pass through the charmin in more or less real time. Do not replace the charmin, continue to re-use the same pad.
20)[blue] For every box of pills used add:
- 10ml Naptha
21) Mix well. Then place the beaker on the hot plate set to med high heat. With constant gentle stirring, heat the mixture until boiling. Turn heat off and continue to stir for 1 minute. Remove from hot plate.
22)Slowly decant the naptha into the same filter-funnel in small amounts and allow it to filter through the Charmin into the flask combining filtrates. Then empty the entire contents of the beaker into the filter funnel and let drain.
23) While draining boil a small amount of naptha about 5 ml for every box of pills used. When all the liquid appears to have drained through, pour the boiling naptha over the filter cake and let it drain again. Then take a large spoon and press down on top of filter cake squeezing any remaining naptha into the flask.
Should I do a forth pull? You can try but tests have shown its usually not enough gain to justify the effort. Only do additional pulls if the end result is less than 45%
24) Place the erlenmeyer flask with the combined filtrate on the hot plate set to med high. Heat to boiling or until all crystals have re-dissolved. Pour the hot filtrate into clean pie plate(s).
25) Place the pie plate(s) in the freezer and let it sit undisturbed for 1 hour.
26) Remove the pie plate(s) from the freezer and pour off the used naptha filtering out free base crystals using a coffee filter. Let the collected free base crystals dry. Some crystals may adhere to the pie plate. Let them dry before removing.
27) WARNING: The remaining naptha does contain some additional pseudoephedrine free base. The pseudo available by titrating this naptha is known to contain contaminants, particularly polyethylene glycol. If you wish to titrate or gas to obtain this pseudo, you should be aware that it will require further cleaning by multiple recrystalizations. If you combine this pseudo with the freebase crystals in a reaction and have not cleaned them thoroughly by recrystalizations, you will contamination the reaction, your product will be contaminated, and your yield will suffer substantially.
28) If the HCL salt is the desired outcome, redissolve the free base crystals in fresh non polar solvent and gas or titrate. Do Not gas the original Naptha. If you gas the original naptha you will pick up unwanted contaminants. You may alternatively move the free base crystals into a small quantity of dH2O and add HCl drop wise with stirring until the free base crystals all dissolve. Evaporate over low heat until this alligators over, then flash with dry acetone. Filter the acetone and pseudoehphedrine HCL though a coffee filter, rinse with acetone, allow to dry.
- Calculating Yield -
When calculating your yield remember to adjust for free base.
Psuedo HCl is about 202gr per mole and psuedo free base is about 166gr per mole.
So 166 divided by 202 is a ratio of 0.82 So potential yield from 1 box of 120's
would be 20 x 120 x 0.82 = 1.9 grams free base vs 2.4 grams for psuedo HCL.
- Advantages and Disadvantages -
The technique should be, for the near future, virtually universal. It should successfully extract most pseudoephedrine pills. The materials are easily available and draw less attention than xylene and tolulene purchases. Yields should range in the sixty percent range. The pseudoephedrine so obtained will be very clean--characteristic of A/B extractions of pseudoephedrine. The main disadvantage is heating a flamable solvent.
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2003-10-05, 09:16
