(a) Spectrophotometry
of the appearance (during irradiation) and
disappearance (upon addition of NiP in the dark) of photoexcited
electrons in NCNCNx at λ = 650 nm. A suspension with NCNCNx (5 mg) and
4-MBA (30 μmol) in KPi (0.02 M, pH 4.5, 3 mL) was
irradiated (AM 1.5G) for 30 min, followed by addition of NiP (50 nmol, 400 μL) or KPi (400 μL). (b) Two
photoreactors were prepared with NCNCNx (5 mg) and 4-MBA (30 μmol)
in the absence of NiP in an aqueous KPi solution
(0.02 M, pH 4.5, 3 mL) and irradiated with 1 sun irradiation (AM 1.5G,
25 °C). Both of these photoreactors were taken into the dark
after 4 h of irradiation, while NiP (50 nmol) was added
to one of them. The pair of hollow and filled symbols of the same
shape and color corresponds to H2 and aldehyde production,
respectively, under the specified reaction conditions.