in water
by decompn. of concd. aq. soln. of sulfite with aq. H3PO4; draying over CaCl2 and P4O10;
参考文献
Gmelin Handbook: S: SVol.4a/b, 1.1.11, page 46 - 48
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Feher, F.
in: G. Brauer, Handbuch der Praeparativen Anorganischen Chemie, 3rd Ed., Vol. 1, Stuttgart, 1975, pp. 360/1
KOH in methanol
byproducts: H2; condensing solvent onto Mo-complex (-196°C), warming to 20°C, addn. of excess H3PO4, stirring for 18 h, addn. of excess 40percent KOH; distn. into dild. H2SO4, colorimetry of NH3, volumetry of free and totalN2 (after reaction with NaOBr);
参考文献
Chatt, Joseph; Pearman, Alan J.; Richards, Raymond L.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1977 , p. 1852 - 1860
KOH in methanol
condensing solvent onto W-complex (-196°C), warming to 20°C, addn. of excess H3PO4, stirring for 48 h (N2-atmosphere), solvent removal (vac.), addn. of excess 40percent KOH; distn. into dild. H2SO4; colorimetry of NH3, N2H4; volumetry of total N2(after reaction with NaOBr);
参考文献
Chatt, Joseph; Pearman, Alan J.; Richards, Raymond L.
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1977 , p. 1852 - 1860