tags
ammonium hyalcyonateammoniapotassiumguanidinepotassium thiocyanatehydrogen sulfidepotassium carbonateCarbonatecarbonammonium thiocyanateethanol

video tutorial Preparing guanidine from ammonium thiocyanate

  • Goal: synthesize guanidine via the thermal decomposition of ammonium thiocyanate.
  • Setup: 500 mL two‑neck flask with a thermometer in the side neck, drying tube, ventilation, heating mantle; moisture control and temperature monitoring are emphasized.
  • Reagent: ammonium thiocyanate (100 g), stored under plastic wrap due to hygroscopicity.
  • Reaction conditions: heat to a steady 180–190°C; observe condensation, color changes, and the release of fumes (hydrogen sulfide) requiring ventilation; products include H2S, NH3, and possibly CS2.
  • Duration and outcome: intended 20 hours at 190°C, but the run lasted 6 hours; after cooling a yellow deposit formed and the mixture was processed.
  • Workup: digest solid with hot water, then treat with 15 g potassium carbonate to form potassium thiocyanate and guanidine carbonate; soluble salts removed by ethanol, followed by evaporation and filtration.
  • Product and yield: about 3.9 g of insoluble residue suspected to contain guanidine carbonate (not pure); overall yield is poor and the process is slow and tedious; potential for alternative methods in future videos.

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