The catalysts (CoB, FeB, NiB) were synthesized by using reduction method of using sodium hydroxide stabilized sodium borohydride solution. The chemicals were used sodium hydroxide, cobalt chloride, iron chloride, nickel chloride (98 %, Merck), sodium borohydride. A known amount of 0.1 (M) cobalt chloride solution was taken in a rubber stopper closed botde at 273 to 278 K in a ice bath with stirring at 500 rpm using a magnetic stirrer and the precipitation by reduction reaction was performed by adding sodium hydroxide stabilized 0.1 (M) NaBFU solution drop wise using a syringe. The precipitated black material was washed three times with distilled water, filter, dried in desiccators and finally in oven at 393 K for 2h. The oven dried sample is denoted as CoB catalyst. Similarly, FeB and NiB catalysts were synthesized using the corresponding precursors by following the above method. The synthesized samples were characterized by using BET, XRD, FTIR, and in situ UV-vis studies. The in situ reduction reaction of cobalt chloride solution to the catalyst (CoB) using in situ UV-vis was monitored by using cuvette with rubber stopper with gradual drop wise addition of sodium borohydride solution. The hydrogen generation studies were performed by using the same apparatus using the synthesized catalysts. (CoB, FeB and NiB) and the generated hydrogen was collected by water displacement using a labeled glass tube. The details experimental set up for hydrogen collection and in situ reduction for catalyst synthesis is given in Scheme-1.
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