The following is a SWIW's best procedure yet on generic 120's and is a collaboration of other procedures. It is in no way, (for you nit-pickers), claimed to be new, or all encompassing. This has been run on sets of 5 boxes of 20ct and yields around 8.25-9.15 grams pseudo hcl salt.
This is an edited post.Abstract of procedure:
a) Extract uncrushed pills with 99% ISO
b) Reduce ISO volume
c) Base solution, and then disarm GACK
d) Collect freebase in naphtha
e) Dry naphtha
f) Drive off ISO & filter off GACK
g) Precipitate pseudo salt rinse, dry
h) Dissolve pseudo and suction filter
i) Re-Crystallize pseudo from H2O in naphtha/acetone in microwave
j) Suction filter and rinse Pseudo with acetone
Standard Procedure:
a) Extraction:
1. Place pills in a beaker or jar uncrusded.
2. To the pills, add approximately 6 oz 99% ISO for every 100 pills (120mg ea.).
3. Allow pills to soak about 15 minutes, swirling occasionally.
4. Now heat the pills and ISO in the microwave using 30-second bursts. Do not heat to a steady boil. Stir pills intermittently when heating.
5. Decant into filter funnel with a cotton topped Charmin plug.
6. Next, apply reduced pressure and collect ISO. Do not let the filter run completely dry.
7. With the second addition of ISO to the pill mass in the jar, no soak time is required. Add 6 oz more ISO, as above only this time after heating, pour the pill mass into the filter with the ISO and suction filter. Again, do not let the pill mass and filter completely dry.
8. On the third addition of ISO, pour 3 oz ISO into the jar. Swirl around to wash residual pill mass from the sides of the jar. Heat the ISO to a boil then pour in filter funnel. This time let the vacuum pull the pill mass dry.
9. Finally, heat another 3 oz of ISO to a boil and pour over the pill mass with the vacuum still applied.
10. Combine the filtered portions and re-filter all through a clean cotton topped Charmin plug.
b) ISO Volume Reduction:
* Please see Notes and Comments first.
1. Place the ISO from above in a shallow dish. (Corelle by Corning has proven to be forgiving of extreme temperature changes.)
2. Heat the solution with rotation in the microwave with venting. Every so often, the microwave is stopped, and the door opened. (Hold your breath and step away from the microwave to breath.) Carefully and slowly, a fork is submerged into the hot ISO. This will cause a wild boiling of the ISO. If it appears the ISO will boil over remove the fork. Keep the ISO just at that point between wildly boiling and boiling over. When placing the fork in the ISO no longer causes this reaction, the fork can be drug around in the dish to reinitiate the wild boiling. When the addition of fork agitation yields no more wild boiling the microwave is turned back on.
3. As the volume reduces, the solution takes on a yellow tint. Continue until the volume is around 3 oz unless skinning can be noted. Be cautious of bumping and popping when using a microwave.
c) Base & Disarm:
1. The reduced ISO solution is now transferred to a coffee carafe. Any crystals formed in the corning dish may be scraped and added along with the ISO solution.
2. NaOH is added to form a paste.
3. Add ISO until the solution has a soupy consistency.
4. Next, add about 7 oz naphtha or until ½ inch sits above the ISO solution.
5. Heat in the microwave on high. Every minute or so with gloved hands the carafe is swirled around. The lower ISO solution will turn milky and then appear similar to a lava lamp. Blobs bounce around in the naphtha and eventually appear to curdle, then turn to a powder layer on the bottom. The naphtha layer will turn a milky color. During this process, an excess of NaOH can be seen on the bottom. A condenser of your choice is used. This process was performed with a funnel in the mouth, (condenser), of the carafe successfully.
6. When the lower layer appears to be powder, it is heated for an additional minute then removed from the microwave.
d) Collect freebase in naphtha:
1. The naphtha layer is then decanted into a filter funnel with a Charmin plug and vacuum filtered. Be careful not to pour the water layer.
2. 7 oz naphtha and more NaOH are added and swirled.
3. Then 1 oz H2O is added in small portions. Careful that the solution does not boil over, and swirl in between each addition.
4. Then, return the solution to the microwave and heat until the bottom layer boils for about 30-45 seconds. If the lower layer does not boil quickly then there may not be enough ISO to aid the boiling process. The lower layer may superheat and bump hard breaking the flask and causing a mess. A dash of ISO can be added before the above heating to help prevent this.
5. The naphtha layer is then decanted into a filter funnel with a Charmin plug. Be careful not to pour the water layer.
6. An additional 7 oz portion of naphtha is added to the carafe, as well as more NaOH and the mixture is swirled.
7. With the empty funnel (condenser) in place, the carafe is returned to the microwave and heated until the lower layer boils again for 30-45 seconds.
8. Again, naphtha layer is decanted and suction filtered.
9. Repeat this one more time if desired then set the water layer aside.
e) Dry Naphtha:
1. Combine the naphtha portions in the now clean carafe.
2. Pour about ¾ cup of salt into the carafe and swirl around.
3. Now decant the naphtha into a clean filter funnel with a new Charmin plug. Take care not to pour out salt layer.
4. Clean out carafe and put naphtha back in carafe.
5. Repeat steps 2-4.
f) Drive off ISO & filter off GACK:
1. Place naphtha solution in a clean carafe.
2. Heat to boil in microwave. If it refuses to heat or boil, try adding a bit more ISO or switch to a boiling water bath.
3. When a boil is reached, the carafe is removed from the microwave and poured out into a large baking dish.
4. Use a hairdryer to blow air onto the naphtha solution. The air stream should make a slight depression on the surface of the naphtha and follow a rotational pattern just inside the lip of the dish. First hot air followed by cool. Take care as the naphtha can easily be forced out of the dish. If splashing occurs, set hairdryer to a lower setting or move drier further away. The solution will begin to cloud. Two different crystals may be seen here. Small needle looking pseudo and GACK resembling disintegrating toilet tissue or small clumps of crushed ice.
5. If there exists and abundance of pseudo needles mixed with the GACK then reheat the solution in the carafe and allow to cool in the carafe. The GACK will precipitate out first and may be filtered off then using a fresh Charmin plug, and reduced pressure. Otherwise just filter off the GACK by reduced pressure filtration through a Charmin plug.
6. Repeat these steps 2 times, unless you are sure the GACK is not precipitating out and pseudo is being filtered instead.
g) Precipitate pseudo salt rinse, dry:
1. Transfer the naphtha and freebase crystals (if any) to a clean dry glass bottle. Allow room for the addition of acetone.
2. Pour salt into a glass.
3. To that salt, add hlc 32% solution approximately 12 drops for every1/2 cup of salt. Mix well.
4. To the salt/hcl, add acetone until the level is just above the salt level. Mix well.
5. Decant this solution through a cotton-plugged funnel with more salt into another glass.
6. Add the above filtered solution in with the naphtha solution 6 drops at a time and swirl.
7. When the naphtha solution takes on a pearl essence look add dry acetone in small portions, cap, and shake the bottle.
8. Release pressure and allow pseudo to precipitate a minute.
9. Collect the pseudo by suction filtration in a clean funnel with a cotton plug. Do not pack the cotton to tight or filtration will slow and the acetone will pull moisture from the air. Rinse each collection well with acetone immediately and add the resulting solution to the naphtha mother. Place pseudo filter cake on a dish.
10. Repeat 6-9 until no more pseudo comes out.
11. Dry the pseudo out a bit by spreading out on a dish.
h) Dissolve pseudo and suction filter.
1. Place the pseudo into a clean filter funnel with a cotton topped Charmin plug.
2. The funnel is placed in a vacuum filtration flask and ready for filtering.
3. With suction turned off, add room-temp DH2O approximately 1oz for every 10 grams of pseudo. Mix around a bit then apply suction. When filter appears to be dry, pour in an additional splash, 2-3 ml, DH2O. This is an approximation here, you want just enough water to dissolve the pseudo. Prewetting the filter adds to much water, hence the splash to follow. Save this filter as it may contain some of your pseudo.
i) Re-Crystallize pseudo from H2O in naphtha/acetone in microwave:
1. Pour the filtrate solution into a shallow corning dish. It should form a sparse layer
across the bottom of the dish. If it completely covers the bottom of the dish then a
larger dish is required. Place the lid to the dish in a manner that leaves 4 small
openings at each corner by turning the lid a bit from its intended placement.
2. Cycle the microwave in 15 to 30 second intervals. Remove the dish between each cycle. Remove the lid carefully so as not to drip water back into the dish. At the first sign of skinning pour in fresh naphtha and swirl around until it forms a layer over the pseudo water.
3. Wipe the lid dry and replace the dish in the microwave this time with lid in the intended secure position.
4. Cycle the microwave. With each cycle you should here crackling. These cycles should be 7-12 seconds each. Anymore and it will most likely bump. (no harm done with the lid on)
5. Remove the dish with each cycling.
6. Carefully remove the lid and look in the dish. The lid should be hot and will aid in the H20 removal if placed on the counter inverted. (Inside facing up).
7. Crystals should be seen forming/floating around.
8. Continue the cycling until the crackling has stopped or the crystals are now bubbling like foam rather than forming the flat crystals as before. At this point acetone is splashed in. Just enough to make things sizzle. Replace the lid and cycle again. Naphtha should be present still in the same volume as before. If the addition of acetone appears to boil away the naphtha, then more naphtha should be added.
j) Suction filter and rinse Pseudo with acetone:
1. Cycle one last time then remove from microwave and splash again with acetone. Swirl it around and more crystals should crash out. Now flood the dish with acetone. Swirl around and quickly filter by suction filtration using a single cotton ball placed in the funnel. Rinse with acetone. Rinse well to remove the naphtha. When rinsing with acetone always keep a stead pool of acetone above the filter cake. If the level of acetone drops down and air is drawn through the filter cake followed by additional rinsing, then a reduced yield will result from the condensation of moisture on the cold filter cake. Do not re-rinse a drying filter cake unless it is completely dry and at room temp.
Notes and Comments:
1. A cotton topped Charmin plug is a Charmin plug with a cotton ball on top. The cotton is not packed tight.
2. When filtering the ISO/Pill solution, hot alcohol will boil wildly during filtration. To keep this at a minimum, turn down the suction when the filtered stream begins to bubble rather then flow. Turn the vacuum down until a steady stream can be seen again. Also, removing the filtrate in-between each ISO addition assists in keeping this under control. Always keep collected portions separate as a safety precaution in case of filter failure.
3. When drying out the ISO/Pill filtrate, reducing the volume in a closed distillation setup would be best. Alternately, one could use a steam bath with a fan blowing across the setup. Never heat flammable substances with or around an open coil heat element. When boiling away 15 oz of ISO in 7 minutes you are inviting trouble. If this procedure is performed without adequate venting of the microwave, fumes will accumulate and asphyxiation may occur. Not venting in an apartment allows the smell to travel to your neighbors. Venting outside though a window in broad daylight is not suggested, and if you are on the first floor venting to the roof the smell will probably be noticed by the upstairs neighbors. Neutralizing aerosol sprays do assist in covering the smell, however it increases the possibility of asphyxiation. The above steps are for those insistent on rushing the evaporation process, and have been performed on occasion on the top floor apartment with venting to the roof. An assistant was present outside to alert of outside fume detection. Anyone who has suffered overexposure to ISO fumes will tell you it is an unpleasant experience.
4. ISO solutions reduced with a slower process have been noted to yield slightly higher. Boiling away all the ISO and rinsing with acetone is not suggested, and has been noted to reduce yields.
5. When boiling naphtha in the microwave ISO may need to be added in small portions to get it to heat.
6. If the naphtha collections in the dish cool down to room temperature or cooler and have not precipitated anything then reheating and repeating the cooling is required. If nothing results, test a small portion by drying it out completely. If freebase crystals are then seen, you should reduce the volume of naphtha until crystals precipitate then continue to the next step of adding the acetone/hcl.
7. When precipitating with acetone/hcl and the precipitate appears to be disappearing and a small collection of water appears at the bottom then this must be transferred to the microwave and dried out, CAREFULL of hard BUMPING. Alternately one could do a titration here with varying results but still recover dirty pseudo.
8. Precipitating with the acetone/hcl seems to work best with Iodized salt that has an ati-caking additive of the sulfate variety. However, the smell produced is awful.
9. One may opt to gas out the pseudo here, however that has not been tested. Maybe gassing and then adding dry acetone and filtering would sidestep the water thing.
10. When rinsing the pseudo while filtering keep a pool of acetone above the filter cake. If at anytime, the acetone is sucked away and the filter cake is aloud to pull air through it, do not pour more acetone over it unless the pseudo-cake is completely dry, and at room temperature. Otherwise, the condensation attracted will allow some pseudo to wash away.
11. This procedure currently works on generic 120’s.
