Separation of non UV-absorbing cations by capillary electrophoresis

Summary A new buffer system for the separation of cations with capillary electrophoresis using indirect UV-detection is described. p-Aminopyridine can be used in the wide pH-range between 3 and 10. High-speed separations of positively charged non-UV absorbing ions are possible. Separation of ions with similar mobilities can be achieved by the addition of complexation reagents. The separation of potassium and ammonium is possible either with the addition of crown ether or at high pH-values. Transition metals can be separated by adding 2-hydroxybutyric acid to the buffer.Dedicated to Professor Dr. Wilhelm Fresenius on the occasion of his 80th birthday     

Automatische Analyse und Simulation von NMR-Spektren

Analytical and Bioanalytical Chemistry -     

N(nPr)4[B5O6(OH)4][B(OH)3]2 and N(nBu)4[B5O6(OH)4][B(OH)3]2: Clathrates with a diamondoid arrangement of hydrogen-bonded pentaborate anions

Single-crystal X-ray structure analyses of N(nPr)₄[B₅O₆(OH)₄][B(OH)₃]₂,1, and N(nBu)₄ [B₅O₆(OH)₄][B(OH)₃]₂,2, reveal that these materials are novel clathrates, the isotypic host structures of which are three-dimensional assemblies of hydrogen-bonded [B₅O₆(OH)₄]^– ionsand B(OH)₃ molecules. The assembly of only the pentaborate anions is a distorted (i.e., along [102] elongated) fourconnected diamond-related network. The N(nPr) ₄ ⁺ and N(nBu) ₄ ⁺ ions are trapped within the complex three-dimensional channel systems of the host frameworks. Both1 and2 crystallize monoclinically with space groupP2₁/c andZ=4. The cell constants are:1:a=13.592(5),b=12.082(2),c=17.355(6) Å, =106.60(2)° (298K);2:a=13.874(3),b=12.585(1),c=17.588(4) Å, =107.04(1)° (238 K). The results obtained by both¹¹B and¹³C MAS NMR spectroscopy are discussed. Thermogravimetric studies under a flowing inert-gas atmosphere suggest that water, stemming from polycondensation of the hydrous borate species, is released from the clathrates at ca. 443 K (1) and 398 K (2) before the decomposition of the organic cations starts at ca. 603 K (1) and 603 K (2).Author for correspondence. Supplementary Data relating to this article are deposited with the British Library as supplementary publication No. SUP 82172 (82 pages).     

31P-NMR-Untersuchung an PhPH(CO)6Fe2(PPh)3Fe2(CO)6PPhH ? einem Vierkernkomplex mit einer ungewöhnlichen (PPh)3-Brücke

(CO)₆Fe₂(PhPH)₂ bildet mit PhPCl₂ den phosphidoverbrückten tetranuklearen Komplex [PhPHFe₂(CO)₆PPh]₂PPh. ³¹P{¹H}-NMR-Spektren der Titelverbindung werden als [AB]₂C-Systeme analysiert, Stereoisomere werden diskutiert. ³¹P-NMR Studies on PhPH(CO)₆Fe₂(PPh)₃Fe₂(CO)₆PPhH ? a Tetranuclear Complex with an Unusual (PPh)₃ Bridge (CO)₆Fe₂(PhPH)₂ and PhPCl₂ form [PhPHFe₂(CO)₆PPh]₂PPh, a tetranuclear complex with phosphido bridges. ³¹P{¹H}-NMR spectra are analysed as [AB]₂C systems, stereoisomers are discussed.     

HPLC of synthetic polymers characterization of polystyrenes by high performance precipitation liquid chromatography (HPPLC)

Summary The advantages and disadvantages of high performance precipitation liquid chromatography have been demonstrated for polystyrene homopolymers. Depending on the mobile phase composition at the dissolution point of the polymeric sample and surface properties of the stationary phase, elution is governed either by a solution process or by adsorption. A contribution by adsorption was noticed on silica as well as on reversed phases based on silica with a normal phase gradient of increasing polarity (heptane to dichloromethane). Elution was solely governed by solubility of the polymers on both types of stationary phase for polystyrenes with a molecular weight above 35 000 and reversed phase gradient of decreasing polarity (methanol to dichloromethane). Under these conditions an identical dependence of elution solvent composition on sample size was found as for turbidity titrations. Due to differences in the velocity of the eluent front and the polymeric sample with porous stationary phases the polymers can be eluted as colloidal solutions Non-porous stationary phases are superior in this respect because the velocities of eluent and solutes are identical.     

Simultaneous Determination of Various Classes of Pesticides Using Micellar Electrokinetic Capillary Chromatographyin Combination with Solid-Phase Extraction

The potential of micellar electrokinetic capillary chromatography (MEKC) with UV-detection for the simultaneous determination of various selected pesticides in water samples was investigated. The developed method using solid-phase extraction showed high efficiency and good resolution with detection limits in the 0.2 to 0.5 ppm range. Comparison of several SPE cartridges demonstrates their suitability for the extraction of pesticides with different hydrophobicity achieving 5000-fold enrichment. The described method involving SPE procedure and MEKC separation enables the successful determination of a wide spectrum of pesticides in water in the range of maximum residue limits (MRLs).