Absolute methanol meoh

The hydrated fluorides M²⁺Fe₂³⁺F₈(H₂O)₂ (M²⁺ = Co, Ni) was obtained by solvothermal reaction using a MARS-5 Microwave Digestion System (CEM Corp.) from starting reactants of chloride precursors (Alfa Aesar), 9.45 mL of absolute methanol ‘MeOH’ (233 mmol, 24.7 mol L^–1, 99.8%, Sigma Aldrich) and 0.55 mL hydrofluoric acid solution (15 mmol, 27.6 mol L^–1, Riedel De Haen). A constant concentration [M^II] + [Fe^III] = 0.1 mol L^–1, a ratio [Fe^III]/[M^II] = 2 and a constant volume of liquid (HF and MeOH) were fixed. The M^II/Fe^III/HF/MeOH ratio is 1/2/44/699. The mixtures are placed in Teflon autoclaves and heated at 160 °C for 30 min with stirring. After cooling, the solid products are filtered, washed with 2 mL of ethanol and dried in a furnace under air.
CoFe₂F₈(H₂O)₂ and NiFe₂F₈(H₂O)₂ were put in a furnace at 320 °C and 340 °C, respectively, during 1 h (heating/cooling rate of 2 °C min^–1) giving the amorphous oxyfluorides with M²⁺M₂³⁺F_8–2xO_x formulations.

All chemicals were of analytical grade and used without previous purification. Crude bentonite (Sigma-Aldrich, Oakville, Canada), sodium chloride (NaCl) (ACP chemicals, Montreal, Canada), copper acetate (Cu(CH₃COO)₂) (Fisher chemicals, Ottawa, Canada), silver nitrate (AgNO₃) (Fisher chemicals), sodium borohydride 98% (NaBH₄) (Acros organics, Ottawa, Canada), copper nitrate (Cu(NO₃)₂) (Anachemia VWR company, Montreal, Canada), Boltorn™ H20 (Perstorp, Malmo, Sweden), absolute methanol (MeOH) (Sigma-Aldrich), and toluene (Sigma-Aldrich) were used. All the experiments were performed in distilled water. Cellulose tissue (gauze) denoted as CT was purchased from PJC, Canada.
Sodium-montmorillonite (NaMt) was prepared by combined ion-exchange and the purification of crude bentonite (Aldrich) in an aqueous NaCl solution using an effective procedure fully described elsewhere.^{30,31 (link)} NaMt (200 mg) was immersed in a methanol/water mixture containing 200 mg of the Boltorn™ H20 polyol dendrimer (41.2 : 58.8 v/v ratio) under continuous stirring for 1 h at 40–60 °C, resulting in H20–NaMt organoclay, which was dried overnight in a freeze-drying device. Similarly, the impregnation of a CT patch of 1 × 0.5 mm² surface in 20 mL of an aqueous solution of 0.01 mol L⁻¹ Boltorn™ H20 at room temperature (RT) for 1 h resulted in dendrimer dispersion into a H20–CT composite.