Introduction.
What is the Drug Ice?“Ice” is the street name for pure methamphetamine (meth). Meth is a powerful stimulant that increases dopamine and makes a person feel a rush of euphoria and high-energy levels. Since a lot of street methamphetamine is adulterated with harmful chemicals, ice is prized for being a pure form of the drug, which causes a longer high.
Are Meth and Ice the Same Thing?
Yes, Ice (also referred to as crystal meth) refers to the rock or glass-like form of methamphetamine. Both crystal meth and ice are common street names for meth. However, ice does differ from other types of meth for things like appearance, strength, duration of effects, etc.
Differences in Effects.
As a stimulant, all forms of meth can produce a ‘rush,’ which refers to feelings of euphoria and a burst of energy. However, using meth in different forms can alter the effects. For example, in its purest form, the effects can be stronger and can last longer. Using speed or base will still produce a high but may not be as quick-acting or strong. Speed is a powder form of meth that often contains other substances and is usually the least pure form of meth. Base is a damp or oily substance that is purer than speed powder and is often injected or swallowed but is not as pure as ice/crystal. In general, high purity means that the substance will produce a more intense high and for a longer period.
Yes, Ice (also referred to as crystal meth) refers to the rock or glass-like form of methamphetamine. Both crystal meth and ice are common street names for meth. However, ice does differ from other types of meth for things like appearance, strength, duration of effects, etc.
Differences in Effects.
As a stimulant, all forms of meth can produce a ‘rush,’ which refers to feelings of euphoria and a burst of energy. However, using meth in different forms can alter the effects. For example, in its purest form, the effects can be stronger and can last longer. Using speed or base will still produce a high but may not be as quick-acting or strong. Speed is a powder form of meth that often contains other substances and is usually the least pure form of meth. Base is a damp or oily substance that is purer than speed powder and is often injected or swallowed but is not as pure as ice/crystal. In general, high purity means that the substance will produce a more intense high and for a longer period.
The way #1.
A one-mole batch of P2P with 100% conversion would result in 149 g (one mole) of methamphetamine base, but the typical yield is 90-93%, resulting in 134-140 g of base. Meth base will quickly react with carbon dioxide in the air to form the carbonate, so it is advisable to crystallize the base as soon as possible. Crystallization is performed by adding 450 g (3 moles) of meth base to a 1000 ml Pyrex beaker and placing the beaker on a stirring hotplate. Carefully drop in a Teflon- coated stirring bar and begin stirring. One now adds 37% hydrochloric acid in 15 ml portions. A graduated 15 ml test-tube makes an ideal dispenser. A great deal of heat is generated as the acid reacts with the meth base and will result in boiling if added too quickly. Add 15 ml of acid at intervals of 1 minute until 19 portions (285 ml) have been added, then add acid in smaller portions and watch the color carefully. If the meth base was clean to begin with, it will turn light pink when the pH reaches 3-4. Test with pH strips (Colorphast 0-14 strips) or a meter. Stop adding acid when the pH reaches 3.
Now we must boil off the water contained in the acid, as water solvates meth very efficiently. Turn the heat on the hotplate to 4.5 while stirring continues, and place a thermometer that reaches 150 °C into the beaker on the bottom. Over the next 1.5 hours, the temperature will climb to 110 °C where boiling begins, then gradually rise as the water is boiled off. When the temperature reaches 130 °C, turn off the heat and remove the thermometer. Using a dishtowel, grip the beaker with both hands and quickly pour it into a 5000 ml plastic bucket containing 4.5 liters of acetone which has been frozen for 2 weeks. Retrieve the stir-bar with a chaser, replace the lid and return to the deep freeze for 1 week to allow complete crystallization. Clean, freshly distilled acetone will retain about 0.113 g of product the first time it is used, which is why one should recycle one's acetone. Alternatively, one can pour the hot methamphetamine hydrochloride into a 20 liters plastic bucket containing 15 liters of acetone that has been frozen for about a month (it takes a long time to pull the heat out of a large mass). The meth will crystallize the instant it hits the frozen acetone, although about 25% will remain in the acetone and must be frozen to crystallize.
Paradoxically, dirty meth crystallizes better than pure meth because the crystals quickly grow around a particle of impurity, forming nice large, hard crystals. The meth crystals are filtered out using a large Buchner, two 4000 ml filter flasks, and a high-volume vacuum aspirator. A 18 cm porcelain Buchner will hold a little over 1 lb of filtered product. Do not use Qualitative 5 filter paper for this filtration. This writer has found that the filters used in milk processing equipment are ideal for meth harvesting. A lot of money has been spent by the dairy industry over the years figuring out how to quickly filter solids out of mixed-phase solutions. These filters will allow liquids, both water and oils, to pass freely while trapping the finest solids, making them ideal for rapid filtering. The problem with the fine paper filters is that oil-water mixtures plug them up very quickly. Milk filters do not have this problem, and they are easy to find, cheap, and suspicionless. One will need to cut-to-fit, but this is a small inconvenience. A suitable high-volume filtering setup can be easily made using 5 and 20-liter buckets, a round plastic plate, and some glue. This writer was fortunate enough to discover a large Buchner being used as a planter by a nice lady in my neighborhood. Happily paying the lady for a replacement, the retrieved treasure holds over 0.9 kg of product and makes the chemist's life much easier. The point is that one can find useful equipment almost anywhere. Pure meth is more difficult to crystallize, and results in a light, flaky white product with a mild scent of marzipan (actually benzaldehyde). Empty the product into a large cake tray and let the acetone evaporate in the fume cabinet for a day or two, separating it as it dries.
Now we must boil off the water contained in the acid, as water solvates meth very efficiently. Turn the heat on the hotplate to 4.5 while stirring continues, and place a thermometer that reaches 150 °C into the beaker on the bottom. Over the next 1.5 hours, the temperature will climb to 110 °C where boiling begins, then gradually rise as the water is boiled off. When the temperature reaches 130 °C, turn off the heat and remove the thermometer. Using a dishtowel, grip the beaker with both hands and quickly pour it into a 5000 ml plastic bucket containing 4.5 liters of acetone which has been frozen for 2 weeks. Retrieve the stir-bar with a chaser, replace the lid and return to the deep freeze for 1 week to allow complete crystallization. Clean, freshly distilled acetone will retain about 0.113 g of product the first time it is used, which is why one should recycle one's acetone. Alternatively, one can pour the hot methamphetamine hydrochloride into a 20 liters plastic bucket containing 15 liters of acetone that has been frozen for about a month (it takes a long time to pull the heat out of a large mass). The meth will crystallize the instant it hits the frozen acetone, although about 25% will remain in the acetone and must be frozen to crystallize.
Paradoxically, dirty meth crystallizes better than pure meth because the crystals quickly grow around a particle of impurity, forming nice large, hard crystals. The meth crystals are filtered out using a large Buchner, two 4000 ml filter flasks, and a high-volume vacuum aspirator. A 18 cm porcelain Buchner will hold a little over 1 lb of filtered product. Do not use Qualitative 5 filter paper for this filtration. This writer has found that the filters used in milk processing equipment are ideal for meth harvesting. A lot of money has been spent by the dairy industry over the years figuring out how to quickly filter solids out of mixed-phase solutions. These filters will allow liquids, both water and oils, to pass freely while trapping the finest solids, making them ideal for rapid filtering. The problem with the fine paper filters is that oil-water mixtures plug them up very quickly. Milk filters do not have this problem, and they are easy to find, cheap, and suspicionless. One will need to cut-to-fit, but this is a small inconvenience. A suitable high-volume filtering setup can be easily made using 5 and 20-liter buckets, a round plastic plate, and some glue. This writer was fortunate enough to discover a large Buchner being used as a planter by a nice lady in my neighborhood. Happily paying the lady for a replacement, the retrieved treasure holds over 0.9 kg of product and makes the chemist's life much easier. The point is that one can find useful equipment almost anywhere. Pure meth is more difficult to crystallize, and results in a light, flaky white product with a mild scent of marzipan (actually benzaldehyde). Empty the product into a large cake tray and let the acetone evaporate in the fume cabinet for a day or two, separating it as it dries.
The way #2.
The product is about 90 ml of clear to pale yellow methamphetamine. We are ready to make his liquid methamphetamine free base into crystalline methamphetamine hydrochloride. Half of the product is put into each of two clean, dry 500 ml Erlenmeyer flasks. The chemist now has a choice to make. He can use either toluene or ethyl ether as the solvent to make the crystals in. Toluene is cheaper, and less of it is needed because it evaporates more slowly during the filtering process. Ether is more expensive, and flammable. But since it evaporates more quickly, the crystals are easier to dry off. If ether is used, it is anhydrous (contains no water). A third choice is also possible for use as a crystallization solvent. This is mineral spirits available from hardware stores in the paint department. Mineral spirits are roughly equivalent to the petroleum ether or ligroin commonly seen in chem. labs. Those brands which boast of low odor are the best choice, such as Coleman camper fuel. Before using this material, it is best to fractionally distill it, and collect the lowest boiling point half of the product. This speeds crystal drying. Since the choice of mineral spirits or naphtha eliminates ether from the supply loop, the clandestine operator may well go this route. Toluene is also a very acceptable solvent.
With the solvent of his choice, the chemist rinses the insides of the condenser, vacuum adapter and 250 ml flask to get out the methamphetamine clinging to the glass. This rinse is poured in with the product. Solvent is added to each of the Erlenmeyer flasks until the volume of liquid is 300 ml. They are mixed by swirling.
With the solvent of his choice, the chemist rinses the insides of the condenser, vacuum adapter and 250 ml flask to get out the methamphetamine clinging to the glass. This rinse is poured in with the product. Solvent is added to each of the Erlenmeyer flasks until the volume of liquid is 300 ml. They are mixed by swirling.
A source of anhydrous hydrogen chloride gas is now needed. The chemist will generate his own. The glassware is set up as in Pic.1. He will have to bend another piece of glass tubing to the shape shown. It should start out about 45 сm long. One end of it should be pushed through a one-hole stopper. A 125 ml sep. funnel is the best size. The stoppers and joints must be tight, since pressure must develop inside this flask to force the hydrogen chloride gas out through the tubing as it is generated.
Into the 1000 ml three-necked flask is placed 200 grams of table salt. Then 35% concentrated hydrochloric acid is added to this flask until it reaches the level shown in the figure. The hydrochloric acid must be of laboratory grade. Some concentrated sulfuric acid (96-98%) is put into the sep. funnel and the spigot turned, so that I ml of concentrated sulfuric acid flows into the flask. It dehydrates the hydrochloric acid and produces hydrogen chloride gas, and also goes on to make more HCl from reaction with table salt. This gas is then forced by pressure through the glass tubing.
One of the Erlenmeyer flasks containing methamphetamine in solvent is placed so that the glass tubing extends into the methamphetamine, almost reaching the bottom of the flask. Dripping in more sulfuric acid as needed keeps the flow of gas going to the methamphetamine. If the flow of gas is not maintained, the methamphetamine may solidity inside the glass tubing, plugging it up.
An even more distressing phenomenon can occur when using hardware store sulfuric acid. This material is not quite as concentrated as lab grade sulfuric acid, and the initial "push" of HCI gas in the flask can turn into a "pull". This vacuum will suck your product up the tubing and into the HCl generating flask. You can imagine how that really sucks!
When using lower grade sulfuric acid, one needs to watch carefully, or use a closely related procedure. In this procedure, the HCl generating flask is filled 1/4 full of hardware store sulfuric acid and the sep. funnel is filled with muriatic acid. By dripping the muriatic acid into the sulfuric acid, the HCI solution (muriatic) is dehydrated to dry HCI gas, and the gas is pushed out the flask and tubing. It is advisable to do a dry run first without product at risk when using hardware store acids in this procedure to avoid heartbreaking losses.
Another popular clandestine method using lower grade sulfuric acid is to put the salt in a mason jar, and punch two holes in the lid. Plastic tubing is attached to both holes. One line of tubing goes into the solution of free base meth in solvent. The other line of tubing is run to an aquarium pump or other source of air The low grade sulfuric acid is then added to the mason jar, and the air blower is started to slowly keep the fumes of dry HCI flowing into the meth free base rather than ever being sucked backwards.
Within a minute of bubbling, white crystals begin to appear in the solution. More and more of them appear as the process continues. It is an awe-inspiring sight. In a few minutes, the solution becomes as thick as watery oatmeal.
Into the 1000 ml three-necked flask is placed 200 grams of table salt. Then 35% concentrated hydrochloric acid is added to this flask until it reaches the level shown in the figure. The hydrochloric acid must be of laboratory grade. Some concentrated sulfuric acid (96-98%) is put into the sep. funnel and the spigot turned, so that I ml of concentrated sulfuric acid flows into the flask. It dehydrates the hydrochloric acid and produces hydrogen chloride gas, and also goes on to make more HCl from reaction with table salt. This gas is then forced by pressure through the glass tubing.
One of the Erlenmeyer flasks containing methamphetamine in solvent is placed so that the glass tubing extends into the methamphetamine, almost reaching the bottom of the flask. Dripping in more sulfuric acid as needed keeps the flow of gas going to the methamphetamine. If the flow of gas is not maintained, the methamphetamine may solidity inside the glass tubing, plugging it up.
An even more distressing phenomenon can occur when using hardware store sulfuric acid. This material is not quite as concentrated as lab grade sulfuric acid, and the initial "push" of HCI gas in the flask can turn into a "pull". This vacuum will suck your product up the tubing and into the HCl generating flask. You can imagine how that really sucks!
When using lower grade sulfuric acid, one needs to watch carefully, or use a closely related procedure. In this procedure, the HCl generating flask is filled 1/4 full of hardware store sulfuric acid and the sep. funnel is filled with muriatic acid. By dripping the muriatic acid into the sulfuric acid, the HCI solution (muriatic) is dehydrated to dry HCI gas, and the gas is pushed out the flask and tubing. It is advisable to do a dry run first without product at risk when using hardware store acids in this procedure to avoid heartbreaking losses.
Another popular clandestine method using lower grade sulfuric acid is to put the salt in a mason jar, and punch two holes in the lid. Plastic tubing is attached to both holes. One line of tubing goes into the solution of free base meth in solvent. The other line of tubing is run to an aquarium pump or other source of air The low grade sulfuric acid is then added to the mason jar, and the air blower is started to slowly keep the fumes of dry HCI flowing into the meth free base rather than ever being sucked backwards.
Within a minute of bubbling, white crystals begin to appear in the solution. More and more of them appear as the process continues. It is an awe-inspiring sight. In a few minutes, the solution becomes as thick as watery oatmeal.
It is now time to filter out the crystals, which is a two-man job. The flask with the crystals in it is removed from the HCl source and temporarily set aside. The three-necked flask is swirled a little to spread around the sulfuric acid, and then the other Erlenmeyer flask is subjected to a bubbling with HCl. While this flask is being bubbled, the crystals already in the other flask are filtered out.
The filtering flask and Buchner funnel are set up as shown in Pic.2. The drain stem of the Buchner funnel extends all the way through the rubber stopper, because methamphetamine has a nasty tendency to dissolve rubber stoppers. This would color the product black. A piece of filter paper covers the flat bottom of the Buchner funnel. The vacuum is turned on, and the hose attached to the vacuum nipple. Then the crystals are poured into the Buchner funnel. The solvent and the uncrystallized methamphetamine pass through the filter paper, and the crystals stay in the Buchner funnel as a solid cake. About 15 ml of solvent is poured into the Erlenmeyer flask. The top of the flask is covered with a palm, and it is shaken to suspend the crystals left clinging to the sides. This is also poured into the Buchner funnel. Finally, another 15 ml of solvent is poured over the top of the filter cake.
Now the vacuum hose is disconnected and the Buchner funnel, stopper and all, is pulled tram the filtering flask. All the filtered solvent is poured back into the Erlenmeyer flask it came from. It is returned to the HCl source for more bubbling. The Buchner funnel is put back into the top of the filtering flask. It still contains the filter cake of methamphetamine crystals. It will now be dried out a little bit. The vacuum is turned back on, the vacuum hose is attached to the filtering flask, and the top of the Buchner funnel is covered with the palm or a section of latex rubber glove. The vacuum builds and removes most of the solvent from the filter cake. This takes about 60 seconds.
The filter cake can now be dumped out onto a glass or China plate (not plastic) by tipping the Buchner funnel upside-down and tapping it gently on the plate. And so, the filtering process continues, one flask being filtered while the other one is being bubbled with HCl. Solvent is added to the Erlenmeyer flask to keep their volumes at 300 ml. Eventually, after each flask has been bubbled for about seven times, no more crystal will come out and the underground chemist is finished.
If ether was used as the solvent, the filter cakes on the plates will be nearly dry now. With a knife from the silverware drawer, the cakes are cut into eighths. They are allowed to dry out some more, than chopped up into powder. If toluene was used, this process takes longer. Heat lamps may be used to speed up this drying, but no stronger heat source.
The yield of product is about 100 grams of nearly pure product. It should be white and should not get wet,except in the most humid weather, it is suitable for any purpose. It can be cut in half and the underground chemists will still have a better product than their competition. But they will not cut it until a few days have passed, so that their options are not limited should one of the problems described in the next few paragraphs arise.
The filtering flask and Buchner funnel are set up as shown in Pic.2. The drain stem of the Buchner funnel extends all the way through the rubber stopper, because methamphetamine has a nasty tendency to dissolve rubber stoppers. This would color the product black. A piece of filter paper covers the flat bottom of the Buchner funnel. The vacuum is turned on, and the hose attached to the vacuum nipple. Then the crystals are poured into the Buchner funnel. The solvent and the uncrystallized methamphetamine pass through the filter paper, and the crystals stay in the Buchner funnel as a solid cake. About 15 ml of solvent is poured into the Erlenmeyer flask. The top of the flask is covered with a palm, and it is shaken to suspend the crystals left clinging to the sides. This is also poured into the Buchner funnel. Finally, another 15 ml of solvent is poured over the top of the filter cake.
Now the vacuum hose is disconnected and the Buchner funnel, stopper and all, is pulled tram the filtering flask. All the filtered solvent is poured back into the Erlenmeyer flask it came from. It is returned to the HCl source for more bubbling. The Buchner funnel is put back into the top of the filtering flask. It still contains the filter cake of methamphetamine crystals. It will now be dried out a little bit. The vacuum is turned back on, the vacuum hose is attached to the filtering flask, and the top of the Buchner funnel is covered with the palm or a section of latex rubber glove. The vacuum builds and removes most of the solvent from the filter cake. This takes about 60 seconds.
The filter cake can now be dumped out onto a glass or China plate (not plastic) by tipping the Buchner funnel upside-down and tapping it gently on the plate. And so, the filtering process continues, one flask being filtered while the other one is being bubbled with HCl. Solvent is added to the Erlenmeyer flask to keep their volumes at 300 ml. Eventually, after each flask has been bubbled for about seven times, no more crystal will come out and the underground chemist is finished.
If ether was used as the solvent, the filter cakes on the plates will be nearly dry now. With a knife from the silverware drawer, the cakes are cut into eighths. They are allowed to dry out some more, than chopped up into powder. If toluene was used, this process takes longer. Heat lamps may be used to speed up this drying, but no stronger heat source.
The yield of product is about 100 grams of nearly pure product. It should be white and should not get wet,except in the most humid weather, it is suitable for any purpose. It can be cut in half and the underground chemists will still have a better product than their competition. But they will not cut it until a few days have passed, so that their options are not limited should one of the problems described in the next few paragraphs arise.
Ice meth forming.
For making a crystal line yet volatile derivative of meth similar to crack rocks, one just recrystallizes the nicely small crystals one gets by bubbling dry HCI through toluene. Crank rocks similar to crack rocks are pretty simple to make also. These would be just big crystals of pure meth hydrochloride. To get such big rocks, just dissolve the meth hydrochloride into a minimum amount of alcohol. Then let the alcohol evaporate away. As it evaporates away, it will make pretty large crystals of meth hydrochloride. An alternative recrystallization solvent would be acetone containing a bit of water. This will evaporate away faster, but give more of a tell-tale smell.
Crystallization common problems and solutions.
Here are some of the common problems that arise with the crystals, and how they are dealt with. To spot these possible problems, the crystals are first left on the plate to dry out, and then transferred to glass jars or plastic baggies.
Yellow Crystals. This is caused by not properly rinsing off the crystals while in the Buchner funnel, or not using enough solvent to dissolve the methamphetamine in the Erlenmeyer flasks. To whiten them up, they are allowed to soak in some ether or toluene in a glass jar, then filtered again.
Yellow Stinky Crystals. The smell takes a few days to develop fully. They are left alone for 5 days, then soaked in ether and filtered again. The smell should not return. (The problem is caused by heating the reaction mixture above the °145 C upper limit.)
Crystals Refuse to Dry. This can especially be a problem using toluene as a solvent. It can also be a problem on very humid days. The crystals are placed in the clean, dry filtering flask, the top is stoppered and vacuum applied at full strength for 15 minutes. Warming the outside of the filtering flask with hot water while it is under vacuum speeds the process.
Crystals Melt. Here the crystals soak up water from the air and melt. This is usually caused by raising the temperature of the reaction too rapidly, or by collecting too much high boiling material during the distillation. First, they are put into the filtering flask and a vacuum applied to dry them out. They are soaked in ether or toluene and filtered. If this doesn't cure the problem, cutting the material to 50% purity should take care of it.
Crystals Are Sticky. Here the crystals seem covered by a thin layer of oily material, causing them to stick to razor blades, etc. The problem is dealt with in the same way as melting crystals.
Crystals Fail to Form. This problem occurs during the process of bubbling HCl into the methamphetamine. Instead of forming crystals, an oil settles to the bottom of the flask. This is generally caused by incomplete hydrolysis of the formyl amide. Perhaps it didn't mix with the hydrochloric acid. It is put in a flask and the solvent boiled off under a vacuum. Then 200 ml of hydrochloric acid is added, and the process is repeated, starting from the hydrolysis of the formyl amide of methamphetamine. The 35% laboratory grade of hydrochloric acid is used.
In the event of melting or sticky crystals, cutting is first tried on a small sample of the crystals to see, if that will solve the problem. If it does not, then a recrystallization must be resorted to. This i s done by dissolving the crystals in the smallest amount of warm alcohol, that will dissolve them. One hundred ninety proof grain alcohol, 95% denatured alcohol, or absolute alcohol may be used. Then 20 times that volume of ether is added. After vigorous shaking for three minutes, the crystals reappear. If not, more ether is added, followed by more shaking. After being filtered, the crystals should be in good shape.
A technique, which may be used in especially stubborn cases is to dissolve the crystals in dilute hydrochloric acid solution, extract out the oily impurities with toluene, and then isolate the methamphetamine.
This is done as follows:
For every 100 grams of crystal, 200 ml of 10% hydrochloric acid is prepared by mixing 60 ml of 35% hydrochloric acid with 140 ml of water. The crystals are dissolved in the acid solution by stirring or shaking in the sep. funnel. One hundred ml of toluene is added to the solution in the sep. funnel, which is then shaken vigorously for about 2 minutes. The lower layer is drained out into a clean beaker. It contains the methamphetamine. The toluene layer is thrown out. It contains the oil grunge, which was polluting the crystals.
The acid solution is returned to the sep. funnel and the acid neutralized by pouring in a solution of 70 grams of sodium hydroxide in 250 ml of water. After it has cooled down, the mixture is shaken for 3 minutes to make sure that all the methamphetamine hydrochloride has been converted to free base. Then 100 ml of toluene is added and the mixture shaken again. The lower water layer is drained out and thrown away. The toluene-methamphetamine solution is distilled as described earlier in this chapter. Then, as described earlier in this chapter, dry hydrogen chloride gas is bubbled through it to obtain clean crystals. (Hydrogen chloride gas must be made in a well-ventilated area; otherwise, it will get into the chemist's lungs and do real damage.)
There is an alternative method for converting amphetamine free base into the crystalline hydrochloride. It is based on the method that South American cocaine manufacturers use to tum coca paste into cocaine hydrochloride. This method does not give the really high-quality crystals that the bubble-through method gives, but its use is justified when really big batches are being handled. In this alternative procedure, the free base is dissolved in two or three volumes of acetone. Concentrated hydrochloric acid (37%) is then added to the acetone while stirring until the mixture becomes acid to litmus paper. Indicating pH paper should show a pH of 4 or lower. The hydrochloride is then precipitated from solution by slowly adding ether with stirring. It will take the addition of 10 to 20 volumes of ether to fully precipitate the hydrochloride. Toluene or mineral spirits may be substituted for the ether. Then the crystals are filtered out using a Buchner funnel as described before, and set aside to dry. The filtrate should be tested for completeness of precipitation by adding some more ether to it.
Yellow Crystals. This is caused by not properly rinsing off the crystals while in the Buchner funnel, or not using enough solvent to dissolve the methamphetamine in the Erlenmeyer flasks. To whiten them up, they are allowed to soak in some ether or toluene in a glass jar, then filtered again.
Yellow Stinky Crystals. The smell takes a few days to develop fully. They are left alone for 5 days, then soaked in ether and filtered again. The smell should not return. (The problem is caused by heating the reaction mixture above the °145 C upper limit.)
Crystals Refuse to Dry. This can especially be a problem using toluene as a solvent. It can also be a problem on very humid days. The crystals are placed in the clean, dry filtering flask, the top is stoppered and vacuum applied at full strength for 15 minutes. Warming the outside of the filtering flask with hot water while it is under vacuum speeds the process.
Crystals Melt. Here the crystals soak up water from the air and melt. This is usually caused by raising the temperature of the reaction too rapidly, or by collecting too much high boiling material during the distillation. First, they are put into the filtering flask and a vacuum applied to dry them out. They are soaked in ether or toluene and filtered. If this doesn't cure the problem, cutting the material to 50% purity should take care of it.
Crystals Are Sticky. Here the crystals seem covered by a thin layer of oily material, causing them to stick to razor blades, etc. The problem is dealt with in the same way as melting crystals.
Crystals Fail to Form. This problem occurs during the process of bubbling HCl into the methamphetamine. Instead of forming crystals, an oil settles to the bottom of the flask. This is generally caused by incomplete hydrolysis of the formyl amide. Perhaps it didn't mix with the hydrochloric acid. It is put in a flask and the solvent boiled off under a vacuum. Then 200 ml of hydrochloric acid is added, and the process is repeated, starting from the hydrolysis of the formyl amide of methamphetamine. The 35% laboratory grade of hydrochloric acid is used.
In the event of melting or sticky crystals, cutting is first tried on a small sample of the crystals to see, if that will solve the problem. If it does not, then a recrystallization must be resorted to. This i s done by dissolving the crystals in the smallest amount of warm alcohol, that will dissolve them. One hundred ninety proof grain alcohol, 95% denatured alcohol, or absolute alcohol may be used. Then 20 times that volume of ether is added. After vigorous shaking for three minutes, the crystals reappear. If not, more ether is added, followed by more shaking. After being filtered, the crystals should be in good shape.
A technique, which may be used in especially stubborn cases is to dissolve the crystals in dilute hydrochloric acid solution, extract out the oily impurities with toluene, and then isolate the methamphetamine.
This is done as follows:
For every 100 grams of crystal, 200 ml of 10% hydrochloric acid is prepared by mixing 60 ml of 35% hydrochloric acid with 140 ml of water. The crystals are dissolved in the acid solution by stirring or shaking in the sep. funnel. One hundred ml of toluene is added to the solution in the sep. funnel, which is then shaken vigorously for about 2 minutes. The lower layer is drained out into a clean beaker. It contains the methamphetamine. The toluene layer is thrown out. It contains the oil grunge, which was polluting the crystals.
The acid solution is returned to the sep. funnel and the acid neutralized by pouring in a solution of 70 grams of sodium hydroxide in 250 ml of water. After it has cooled down, the mixture is shaken for 3 minutes to make sure that all the methamphetamine hydrochloride has been converted to free base. Then 100 ml of toluene is added and the mixture shaken again. The lower water layer is drained out and thrown away. The toluene-methamphetamine solution is distilled as described earlier in this chapter. Then, as described earlier in this chapter, dry hydrogen chloride gas is bubbled through it to obtain clean crystals. (Hydrogen chloride gas must be made in a well-ventilated area; otherwise, it will get into the chemist's lungs and do real damage.)
There is an alternative method for converting amphetamine free base into the crystalline hydrochloride. It is based on the method that South American cocaine manufacturers use to tum coca paste into cocaine hydrochloride. This method does not give the really high-quality crystals that the bubble-through method gives, but its use is justified when really big batches are being handled. In this alternative procedure, the free base is dissolved in two or three volumes of acetone. Concentrated hydrochloric acid (37%) is then added to the acetone while stirring until the mixture becomes acid to litmus paper. Indicating pH paper should show a pH of 4 or lower. The hydrochloride is then precipitated from solution by slowly adding ether with stirring. It will take the addition of 10 to 20 volumes of ether to fully precipitate the hydrochloride. Toluene or mineral spirits may be substituted for the ether. Then the crystals are filtered out using a Buchner funnel as described before, and set aside to dry. The filtrate should be tested for completeness of precipitation by adding some more ether to it.
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