Hans-Jürgen Götze

DETERMINATION OF POLYCYCLIC AROMATIC HYDROCARBONS IN DIESEL SOOT BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

SummaryThe described identification and determination of polycyclic aromatic hydrocarbons (PAH) in Diesel soot is based on a class-fractionation using an open Al2O3-column and a following separation on a reversed-phase HPLC-column with post-chromatographic derivatization. The optimized analysis has been applied to the determination of PAH in soots from different engines such as locomotives and motor vehicles by variation of the fuel additives and different Diesel/water emulsions. The results obtained by locomotives show that a special Diesel/water emulsion emits a minor amount of mutagenic and cancerogenic polycyclic aromatic hydrocarbons, whereas the emission of the comparatively harmless compounds like phenanthrene and benzo(h)quinoline increases.

Flüssig-chromatographische Trennung von Lanthanoid-Komplexen mittels Ionenpaar-Chromatographie (HPLC)

SummaryThe liquid-chromatographic separation conditions of lanthanoid acetylacetonates and lanthanoid EDTA complexes were investigated by means of HPLC. An ionpair-chromatographic separation method was developed for the EDTA complexes using tetraalkylammonium salts and reversed-phase materials. The dependence of retention on the chemical nature and the concentration of the salt addition and the pH-value of the mobile phase (water/methanol) was investigated.ZusammenfassungDie flüssig-chromatographischen Trenneigenschaften von Lanthanoid-Acetylacetonat- und Lanthanoid-EDTA-Komplexen wurden mittels HPLC systematisch untersucht. Für die EDTA-Komplexe der Lanthanoide wurde auf Umkehrphasen ein ionenpaar-chromatographisches Trennverfahren unter Anwendung von Tetraalkylammoniumsalzen entwickelt. Hierbei wurde insbesondere die Abhängigkeit der Retentionseigenschaften von Art und Konzentration des Salzzusatzes und dem pH-Wert der mobilen Phase (Wasser/Methanol) ermittelt.

Determination of aldehydes and ketones in natural gas combustion in the ppb range by high-performance liquid chromatography

SummaryThe reported identification and determination of trace compounds in flue products of natural gas burning equipment is based on DNPH precolumn derivatization and followed by HPLC separation. The optimized HPLC analysis has been applied to the determination of trace amounts of aldehydes and ketones in polluted air such as lab and ambient air as well as natural gas and oil combustion products in a hospital. The results obtained in a hospital show that the oil fuel combustion process emits a considerable amount of toxic acrolein, whereas the emission of acetone is predominant in natural gas combustion.

Separation of aminoacidato ruthenium(II) complexes by ion-pair chromatography

SummaryThe chromatographic conditions for analytical separation of (η6-C6H6) ruthenium(II) complexes with amino acid and dipeptide ligands have been investigated in dependence on their molecular structure. Different chromatographic phases were tested and the efficiency parameters were determined by the reversed-phase ion-pair technique. For the enantiomeric species L-penicillaminato ruthenium(II) complexes cis- and trans-[(η6-C6H6)Ru(L-Pen)H−1]2Cl2 and the reaction byproducts a complete chromatographic separation has been obtained using sodium dodecylsulphate as an ion-pair reagent. For the purification procedure of the L-penicillaminato ruthenium(II) complexes, in order to characterize the separated pure complexes by 1H-NMR spectroscopy, a preparative separation has been carried out using the volatile trifluoroacetic acid as an ion-pair reagent.

Schwingungsspektroskopische Untersuchungen an Organostannylaminen

The formerly unknown organostannyl amines of the type R3SnNH2-(t-Bu)3SnNH2, (t-Bu)3SnND2 and (t-Bu)3Sn15NH2 were prepared in order to investigate the vibrational properties of the organometallic amines of group IVa. The Infrared and Raman spectra were recorded in the region 4000-200 cm−1 and 4000-50 cm−1, respectively. A complete vibrational assignment and normal coordinate treatment of the C3SnNH2 (ND2,15NH2) group were carried out. The results are discussed in terms of tetrahedral or planar configurations of the SnNH2 group.ZusammenfassungIm Rahmen einer Untersuchung über schwingungsspektroskopische Eigenschaften von Organometallaminen der IV. Hauptgruppe wurden die bisher unbekannten Organostannylamine des Typs R3SnNH2:(t-Bu)3SnNH2, (t-Bu)3SnND2 und (t-Bu)3Sn15NH2 dargestellt und deren IR- und Ramanspektren im Bereich von 4000-200 cm−1 bzw. 4000-50 cm−1 aufgenommen. Bei der Zuordnung der beobachteten Frequenzen lag der Schwerpunkt auf den Schwingungen der C3SnNH2-Gruppe. Zur weiteren Aufklärung der Natur der Zinn-Stickstoffbindung in Organostannylaminen wurde von den primären Stannylaminen (t-C4H9SnNH2, (t-C4H9)3SnND2 und (t-C4H9)3Sn15NH2 eine Normalkoordinatenanalyse durchgeführt. Neben der Ermittlung der Kraftkonstanten war hierbei von besonderem Interesse die Entscheidung über eine pyramidale (Punktgruppe Cs) oder planare (Punktgruppe C2V) Konfiguration der SnNH2- bzw. SnND2-Gruppe.

Liquid chromatographic and infrared studies on ethylenediamineplatinum(II) guanosine complexes

Abstract The complexes of platinum are of great interest in anticancer research and chemotherapy. The investigation of the binding properties of the different adducts formed from platinum complexes and DNA bases by liquid chromatographic separation and the spectroscopic identification of chromatographic fractions frequently requires a large amount of analytical material. It is shown that the combination of ion-pair reversed-phase chromatography and infrared spectroscopy combined with theoretical methods like molecular modelling and normal coordinate analysisi allows the separation and characterization of 7 ethylenediamineplatinum(II) (Pt(en)) guanosine complexes in Pt(en) guanosine reaction mixtures in the micro range. The classification of the monofunctional N1, N3, N7 and the bifunctional N7-N1 (two species), N7-N3, N7-N7 adducts was confirmed with the quantitative interpretation of the chromatographic peak area in dependence of the different Pt(en)/guanosine ratio and the thermodynamic stability of the adduct compounds obtained by molecular modelling calculations. Additionally it was distinguished between the N7 and N1/N3 coordination of the Pt(en) guanosine complexes by vibrational spectroscopy and normal coordinate analysis.