Finally, the generated volatile NMM was analyzed by headspace gas chromatography. The generation of in situ CuH, complete reduction of NMMO, and the gas–liquid equilibration of NMM can be synchronously completed at 80 °C in 30 min, with a cupric ion concentration of 20 μmol, sodium hydroxide (0.8 mmol), sodium borohydride (3.0 mg), and 1.0 mL 30% ammonium hydroxide in 5.0 mL aqueous solution.