Drug Chemistry Procedure Manual 1 SECTION A: Preliminary Tests Marquis Reagent ..................................................................................................... A - 1 Duquenois-Levine Reagent .................................................................................... A - 2 Cobalt Thiocyanate Reagent .................................................................................. A - 3 Ferric Chloride Reagent ......................................................................................... A - 4 Koppanyi Reagent................................................................................................... A - 5 Potassium Permanganate Reagent ...................................................................... A - 6 p-Dimethylaminobenzaldehyde Reagent (PDMAB) .............................................. A - 7 Froehde’s Reagent.................................................................................................. A - 8 Mecke’s Reagent..................................................................................................... A - 9 Silver Nitrate Reagent............................................................................................. A - 10 Zwikker Reagent...................................................................................................... A - 11 Barium Chloride Reagent ....................................................................................... A - 12 Methanolic Potassium Hydroxide Reagent .......................................................... A - 13 Secondary Amine Reagent #1................................................................................ A - 14 Secondary Amine Reagent #2................................................................................ A - 15 SECTION B: Polarized Light Microscopy Polarized Light Microscopy.................................................................................... B - 1 5% Mercuric Chloride With Optional 0.05 N Hydrochloric Acid Solution........... B - 2 Wagenaar Reagent.................................................................................................. B - 3 Drug Chemistry Procedure Manual 2 SECTION B: Polarized Light Microscopy (continued) Gold Chloride in 20% Acetic Acid With Optional 0.05 N Hydrochloric Acid Solution ........................................................................................................... B - 4 Free Acid Using 2% Sodium Hydroxide and 5% Sulfuric Acid Solutions........... B - 5 0.05 N Hydrochloric Acid........................................................................................ B - 6 Methanol ............................................................................................................... B - 7 Distilled Water ......................................................................................................... B - 8 Volatility Test Using Gold Chloride in Water With Concentrated Sodium Hydroxide Solution ................................................................................................. B - 9 Volatility Test Using Gold Chloride in Dilute Phosphoric Acid With 10% Sodium Hydroxide................................................................................................... B - 10 50% Acetic Acid and Gold Chloride in 50% Acetic Acid...................................... B - 11 Microscopic Examination of Hashish Using Chloral Hydrate ............................. B - 12 Microscopic Examination of Hashish Using Concentrated Sodium Hydroxide................................................................................................... B - 13 Microscopic Examination of Hashish Using Chloroform .................................... B - 14 Microscopic Examination of Hashish Using Petroleum Ether............................ B - 15 SECTION C: Thin-Layer Chromatography 9:1 Developing Solvent........................................................................................... C - 1 2:1 Developing Solvent........................................................................................... C - 2 4:1 Developing Solvent........................................................................................... C - 3 10:1 Developing Solvent (Ethanol) ........................................................................ C - 4 Drug Chemistry Procedure Manual 3 SECTION C: Thin-Layer Chromatography (continued) 10:1 Developing Solvent (Methanol)...................................................................... C - 5 T1 Developing Solvent ............................................................................................ C - 6 18:1 Developing Solvent......................................................................................... C - 7 S1 Developing Solvent ............................................................................................ C - 8 1:1 Developing Solvent........................................................................................... C - 9 T2 Developing Solvent ............................................................................................ C - 10 Iodoplatinate Visualizing Reagent......................................................................... C - 11 p-DMAB Visualizing Reagent ................................................................................. C - 12 Fast Blue B Visualizing Reagent............................................................................ C - 13 Sulfuric Acid Visualizing Reagent ......................................................................... C - 14 Iodine Visualizing Reagent..................................................................................... C - 15 SECTION D: Extractions and Separations Extraction of Organic Bases .................................................................................. D - 1 Extraction of Organic Acids ................................................................................... D - 2 Extraction of Volatile Organic Bases .................................................................... D - 3 Extraction of Amphoteric Compounds (including Morphine, Hydrocodone and other Alkaloids)................................................................................................ D - 4 Dry Solvent Extractions of Drugs Utilizing Hexane/Ammonia ............................ D - 5 Dry Solvent Extractions of Drugs Utilizing Chloroform/Ammonia...................... D - 6 Separation of Organic Acids and Bases by Solvent Wash.................................. D - 7 Drug Chemistry Procedure Manual 4 SECTION D: Extractions and Separations (continued) Extraction of Psilocybe Mushrooms ..................................................................... D - 8 Extraction of Anabolic Steroids from Vegetable Oils .......................................... D - 9 Separation of Cocaine Base and Benzocaine Base............................................. D - 10 Separation of Cocaine Base and Procaine Base.................................................. D - 11 Separation of Cocaine Hydrochloride and Dimethylerephthalate ...................... D - 12 Separation of Cocaine Hydrochloride and Lidocaine Hydrochloride................. D - 13 Separation of Dextropropoxyphene Napsylate and Acetaminophen ................. D - 14 Extraction of Diethylpropion from a Time-release Preparation .......................... D - 15 Extraction of Lysergic Acid Diethylamide (LSD) .................................................. D - 16 Extraction of Lysergic Acid Diethylamide (LSD) from Sugar Cubes .................. D - 17 Separation of Methamphetamine Hydrochloride and Dimethyl Sulfone ............ D - 18 Separation of Cocaine Hydrochloride and Nicotinamide .................................... D - 19 Separation of Cocaine from Procaine, Benzocaine, Dimethylterephthalate, and Nicotinamide ................................................................................................... D - 20 SECTION E: UV Spectrophotometry Shimadzu Ultraviolet Spectrophotometer UV-260 / UV-265 ................................ E - 1 SECTION F: Infrared Spectrophotometry Mattson Galaxy 2020 FTIR Spectrophotometer.................................................... F - 1 Nicolet Impact 410 FTIR Spectrophotometer........................................................ F - 2 Drug Chemistry Procedure Manual 5 SECTION G: Gas Chromatograph/Mass Spectrometer Hewlett-Packard 5890 Series II GC Interfaced to the Hewlett-Packard 5970 MSD .................................................................................... G - 1 SECTION H: Random Sampling Random Sampling of Multiple Packages or Units .......................................H - 1 .