Investigation of Intermediates Involved in the Photochemical Formation of Mo‐Blue Nanoring by Capillary Electrophoresis–Mass Spectrometry

Abstract Capillary electrophoresis (CE) coupled with electrospray ionization mass spectrometry (ESI‐MS) was employed to detect the intermediates involved in the photochemical formation of the Mo‐blue nanoring [Mo V 28 Mo VI 114 O 429 H 10 (H 2 O) 49 (CH 3 CO 2 ) 5 (C 2 H 5 CO 2 )] 30– ≡ Mo 142 (Ac) 5 (Pr) in the photolysis of the [Mo 7 O 24 ] 6– /CH 3 CO 2 H system at pH 3.4. The CE electropherogram indicated successful separation of the photolyte species into three migration times. The relative peak areas of the three kinds of signals were dependent on the duration of the photolysis. The signals in two of the regions could be identified to species (with additional defects due to the removal of binuclear {Mo 2 } ≡ [Mo VI 2 O 5 (H 2 O) 2 ] 2+ linkers) derived from the intermediates {Mo 37 } to {Mo 42 } and Mo‐blue nanoring Mo 142 (Ac) 5 (Pr). (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009)