Large-Scale Methamphetamine Manufacture

2.4 Chemicals

The following chemicals will be used:
Laboratory grade 37% hydrochloric acid. One can try hardware store muriatic acid if it is 30% or better. It is unknown what the impurities in the cheap hardware-store stuff may do to the catalyst, but many times the only difference between laboratory grade chemicals and commercial grade stuff is the fact that the laboratory grade chemicals have been tested to make sure there's nothing strange in it. It may have come out of the same tanker car, but it was tested.
One will need 200ml of 70% nitric acid in order to make aqua regia. Jewelers can buy this in very small quantities for making aqua regia, which is required to dissolve metals like platinum and rhodium for alloying or plating. Otherwise, one can whip up a batch fairly easily. See Section 6.0 for instructions.
About 3 kg of sodium or potassium nitrate. This is our oxidizer, and it is used at a 10:1 weight ratio with ammonium chloroplatinate (which we will make). It is also used to manufacture 70% nitric acid. Sodium nitrate is preferred, but only because this writer has used it extensively. Use the powdered form as it requires less grinding and seems to work better than the beaded form often found in university labs.
About 3 kg of ammonium chloride will be used. This common salt is used for metal preparation and making chilling solutions. It should not be difficult to find. Try the drugstore or pharmacy.

2.5 Dissolution of Platinum in Aqua Regia

The first step is to dissolve the platinum, either in coin form or as spent catalyst, in aqua regia to make chloroplatinic acid. This is not as easy as may first appear. Platinum coins are especially difficult to dissolve. Left on it's own, it could take months for the platinum to completely dissolve. Heating to just below the boiling point of the acid will increase the activity of the acid many times and will let the chemist dissolve his platinum coins in 3-4 days. Spent catalyst may also be recycled, and will dissolve much more quickly than coins. This procedure must be performed inside a properly functioning fume cabinet or the fumes will kill you. See the appendix for construction details.
Place a 1000ml Pyrex beaker on the stirring hotplate. Place a 2" Teflon-coated stirbar with a center ridge inside the beaker. If one is using fresh 1oz platinum coins, gently place two of them (64g) in the beaker. There should be room for the stirbar to turn without touching the coins. Two coins is the very most one should attempt to dissolve in 800ml of aqua regia as additional platinum will not dissolve and react but will remain as unreacted particles in suspension, screwing up subsequent procedures. (If one is recycling spent platinum dioxide catalyst, wait until after the aqua regia is made and stirring, but not heating, is begun before adding the spent catalyst in small portions.) Add 200ml of 70% nitric acid. Add 600ml of laboratory grade 37% hydrochloric acid. Once the platinum and aqua regia are inside the beaker, fill a 1000ml round-bottom flask half full of cold tap water, dry the outside with a paper towel, and carefully place it on top of the beaker. Make sure there is an air-gap at the pouring lip of the beaker so no pressure builds up. This is our makeshift condenser, designed to condense and recycle the aqua regia while the platinum dissolves. Without the condenser, the aqua regia will quickly boil off without dissolving much platinum. Do not fill the 1000ml flask to more than 1/3 or ½ full or it will become top-heavy and tip over from the vibration. Begin heating while stirring, slowly raising the temperature over several hours until the first signs of boiling begin. On my stirring hotplate, an 800watt unit, the heat setting is 3.5-3.75. The solution will turn orange, and then a very deep ruby red. Do not leave the reaction unattended for more than a few minutes, and turn it off at night. When recycling spent catalyst, a small amount of contaminant may appear on the surface. Let the beaker cool until it can be handled and then filter the liquid through your 4" Buchner using filter paper, holding the coins in place with the Teflon-coated stirbar chaser. Do not use any metal, as it can contaminate the batch. A more porous grade of filter paper may be used. Pour the filtrate back into the beaker with the coins and continue the heating and stirring. It should take 3-4 days to dissolve two coins. The variables affecting dissolution speed are surface area, acid temperature, and stirring effectiveness.
One needs to mix up a saturated solution of ammonium chloride in distilled water. Pour 3000ml of distilled water into a 5000ml beaker (or a 1gal pickle jar) along with a 3" stirring bar. Place on a stirplate if available, otherwise stir using a clean spatula from the kitchen. With stirring, slowly add ammonium chloride to the water until it will not dissolve any more. Continue stirring occasionally until the solution comes up to room temperature once again, then add more ammonium chloride until no more will dissolve. Repeat one more time. When finished, the chemist should have a room temperature solution with a little undissolved ammonium chloride at the bottom.
Once the platinum is completely dissolved, remove the condenser flask and allow the remaining acid to boil off until it is all gone and there remains in the bottom of the beaker a grayish-red-black layer of ugly metallic stuff. This is chloroplatinic acid. Be aware that the fumes created when boiling off the acid will create large, very visible clouds of acid-laced fog if exhausted into cool, still air. In addition, all nearby plant life will turn brown and quickly die. If performed while a stiff breeze is blowing, this hazard is eliminated. Let the beaker cool down, add 500ml of 37% hydrochloric acid, let it react with the chloroplatinic acid, then boil off the acid almost to dryness. Do this three times to remove any trace of nitric acid, boiling off the acid to dryness on the third boil. Once cool, add small portions of ammonium chloride solution and work it with the end of a stirbar chaser. Continue adding ammonium chloride solution until all of the chloroplatinic acid has reacted and there are no solid chunks left. Decant into another clean beaker or jar as the beaker fills. A bright yellow suspension will form as the chloroplatinic acid reacts with the ammonium ion to make ammonium chloroplatinate. Do not get in a hurry. It can take over an hour for the chloroplatinic acid to completely react. Black particles or other discoloration is a sign of incomplete dissolution of the platinum. Remove the water by vacuum filtering through the 4" Buchner with Qualitative 5 filter paper using a water aspirator or vacuum pump. This also may take several hours. Remove the pasty ammonium chloroplatinate cake and break it up as finely as possible using a clean razor knife in a glass bowl or plate. It will be difficult to handle and a little sticky. At this point one must improvise a little. I use a vacuum oven purchased at a mining equipment sale (mines do a lot of inorganic chemistry) to gently vacuum dry the ammonium chloroplatinate overnight at low heat. Those without vacuum ovens should use an infrared lamp placed near the plate and be patient. Do not overheat, as ammonium chloroplatinate will decompose. Look for any brown or black discoloration as a sign of excess heat. Break up into smaller chunks as the paste dries. Dried ammonium chloroplatinate is hard, granular, and dark yellow in color.
Ammonium chloroplatinate is a convenient form in which to store catalyst, as platinum dioxide catalyst can be extremely pyrophorric (this stuff explodes!). Store in a cool, dry place and oxidize it as the need for fresh catalyst arises. If one started with 64g of platinum coins (Pt, 195g/mole, 0.328mole), one should end up with slightly less than 0.328 mole of ammonium chloroplatinate ((NH4)2PtCl6, 443.9g/mole), or about 140g. This is enough to make about 50g of useful catalyst, which translates to 150-300 moles worth of reactions, or about 40-80lb of very pure methamphetamine, depending upon how many times one is able to reuse the catalyst.