We report on the structural design and characterization of a series of neutral heteroleptic iridium(III) complexes equipped with 2-phenylpyridine, 2-(naphthalen-1-yl)pyridine, and 1-phenylisoquinoline as cyclometalating ligands. To gradually increase the unsymmetrical architecture of the heteroleptic iridium(III) complexes, they have been furnished with 2,2,6,6-tetramethylheptane-3,5-dione, 1-(9H-carbazol-9-yl)-5,5-dimethylhexane-2,4-dione, and 1-[3,6-bis(4-hexylphenyl)-9H-carbazol-9-yl]-5,5-dimethylhexane-2,4-dione as ancillary ligands. The photophysical and electrochemical properties of these asymmetric Ir III complexes have been investi-
Recently we introduced atmospheric pressure laser ionization (APLI) as a complementary ionization method for coupling LC-MS systems (HPLC and CEC), allowing ionization of nonpolar aromatic compounds via near-resonant two-photon excitation. In this paper, we demonstrate that APLI with the same source enclosure as for LC coupling is also suited for hyphenation of GC with atmospheric-pressure ionization mass spectrometry. This technique permits the qualitative and quantitative determination of aromatic compounds in an ultralow concentration range, as we show here with polycyclic aromatic hydrocarbons (PAHs), alkylated PAHs, and hetero-PAHs as examples. The outstanding sensitivity is demonstrated for chrysene, with a detection limit of 22 amol. Polar functional groups reduce the sensitivity, but after methylation or silylation, the analytes can also be determined very sensitively in complex matrixes, as is shown with 1-hydroxypyrene in urine.
Over the past decade, multimode ion sources operating at atmospheric pressure (i.e., more than one ionization method is operative in the ion source enclosure) have received considerable interest. Simultaneous operation of different ionization methods targeting different compound classes within one analysis run has several advantages, including enhanced sample throughput and thus significant laboratory cost reductions. Potential drawbacks are enhanced ion suppression and other undesirable effects of the simultaneous operation of ionization methods. In this contribution we present an alternative approach-the development and characterization of a widely applicable, multipurpose ion source operating at atmospheric pressure. The optimized source geometry allows rapid changing from LC-API methods (ESI, APCI, APLI) to GC-API methods (APCI, APLI, DA-APLI) along with the appropriate coupling of chromatographic equipment required. In addition, true multimode operation of the source is demonstrated for LC-ESI/APLI and LC-APCI/APLI.
The efficient synthesis of novel beta-diketonates equipped with functional carbazolyl moieties and their subsequent transformations in 5-hexyl-thienyl substituted carbazole derivatives is presented by utilizing an effective Stille cross-coupling reaction. The introduced beta-diketonates served as ancillary ligands for novel heteroleptic red- and green-emitting Ir(III) complexes, when combined with 2-(naphthalen-1-yl)pyridine and 2-phenylpyridine as cyclometalating ligands. These novel Ir(III) complexes revealed color-tunability and a very good thermal stability until at least 207 degrees C. In polystyrene blends, the heteroleptic Ir(III) complexes revealed remarkable quantum yields up to 36% and suitably short phosphorescence lifetimes ranging from 1 to 4 micros. In the case of the orange-red Ir(III) emitter, equipped with 2-(naphthalen-1-yl)pyridine cyclometallating ligands, a luminous efficiency as high as 7.7 cd/A at 7.4 V was achieved. All fabricated diodes exhibited in addition favorable color stability.
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