From quality inspection to quality assurance

Summary Systematic quality assurance, e.g. in accordance with the provisions of ISO 9000, requires not only the targeted use of quality as a management tool, but also a revised attitude to operational procedures. Although sophisticated checking of the final results of a procedure (e.g. results of analyses, sales products, reports) meets the legal requirements and often also the customers' requirements, this misses the chance of being able to influence the quality of a final result at the earliest possible stage. It is then only possible subsequently to take the uneconomic decision as to whether the result of the work is useable or must be discarded or the object reworked. Within quality assurance, all operations are to be considered as processes with the aim of arriving at a statistically controlled process. The advantages of statistical process control are explained by way of examples from analytical procedures and production. The status of internal audits is explained as it interrelates with process control.     

Construction of multiporphyrin arrays using ruthenium and rhodium coordination to phosphines

The synthesis of linear multiporphyrin arrays with mono- and bisphosphine-substituted porphyrins as ligand donors and ruthenium(II) or rhodium(III) porphyrins as ligand acceptors is described. With appropriate amounts of the building blocks mixed, linear dimeric and trimeric arrays have been synthesized and analyzed by (1)H NMR and (31)P NMR spectroscopy. The Ru/Rh acceptor porphyrins can be located either at the periphery or in the center of the array. Likewise, the monophosphine porphyrins can be positioned at the periphery, thus allowing a high degree of freedom in the overall composition of the arrays. This way, both donor and acceptor porphyrins can act as chain extenders or terminators. One of the trimeric complexes with two nickel and one ruthenium porphyrin has also been analyzed by X-ray crystallography. Attempts have also been made to synthesize higher order arrays by mixing appropriate amounts of the porphyrins; however, from the NMR data it cannot be concluded if monodisperse five, seven, or nine porphyrin arrays are present or if the solutions are composed of a statistical mixture of smaller and larger arrays.     

Assignment of the 5,6-Double-Bond Configuration in Iloprost and Isoiloprost from 13C-NMR Shifts Determined by 2D Methods

The configurations of the 5,6-double bond in the carbacyclins iloprost ( 3 ; (E)) and isoiloprost ( 4 ; (Z)) are based on a complete assignment of the ¹³C and ¹H resonances determined by 1D and 2D ¹³C-NMR and ¹H-NMR methods.     

Adducts of Rh2[MTPA]4 with some phosphine chalcogenides: nature of binding and ligand exchange

Adducts of four phosphine chalcogenides with the chiral dirhodium complex ([Rh-Rh]) were investigated by variable-temperature 1H and 31P NMR spectroscopy in order to compare their properties as axial ligands. Whereas the selenide (1) and the sulfide (2) are strong ligands with electrostatic attraction and, in addition, a significant orbital (HOMO-LUMO) interaction, the phosphine oxide compounds (P=O) bind primarily via electrostatic attraction and are relatively weak donors. Moreover, the overall bond strength in these adducts depends on steric congestion around the P=O group.