Gas-chromatographische Analyse von dl-Milchs?ure-L?sungen

Zusammenfassung Wäßrige und organische Lösungen (Äther, Benzol, Chloroform, Pentan) von Milchsäure wurden gas-chromatographisch untersucht. Dabei wurden neben dem Peak der monomeren Verbindung noch 4 weitere Peaks von Kondensationsprodukten gefunden. Der Anteil der einzelnen Komponenten am Gesamtgehalt war je nach Konzentration der untersuchten Lösung und Art des Lösungsmittels verschieden (Tabelle).

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Gas-chromatographic analysis of solutions of dl-lactic acid

Aqueous and organic solutions (ether, benzene, chloroform, pentane) of lactic acid have been submitted to gas chromatography. Besides of the peak of the monomeric compound four other peaks have been detected corresponding to condensation products. The percentage of the different components depended on the concentration of the solutions and the kind of solvent.

     

Evaluation of graphitized glass capillary columns

The performance of graphitized glass capillary columns obtained by precoating the inner glass walls with graphitized carbon black has been evaluated. It has been shown that according to the amount of stationary phase coated such columns can operate in gas–liquid-solid chromatography and in gas–liquid chromatography so that tailor-made columns for specific separations can be prepared. The versatility of these columns is shown in the separation of various mixtures (terpenes, pesticides, isomeric species and others) of analytical importance.     

Separation of polychlorinated biphenyls from chlorinated pesticides using aminopropyl bonded-phase cartridge and determination by GC-ECD

Summary Gas chromatography of polychlorinated biphenyls and chlorinated pesticides in water samples is carried out after adsorption from a 25–500 mL sample, on a cartridge containing 100 mg aminopropyl-bonded porous silica. The clean-up step in which the PCBs and chlorinated pesticides are separated in different eluates is achieved by passing 25 mL of 40% aqueous methanol through the NH₂ Sep-Pak cartridge. The PCBs are desorbed with 500 μL ethylacetate, which is concentrated and analysis by GC-ECD. The average recovery, at 1 ppb is >97% with a standard deviation <2. The limits of detection are 0.1 ng μL⁻¹ and 5 pg μL⁻¹ respectively for Cl₃-PCB and Cl₈-PCB congeners. In the separation of PCBs from the chlorinated pesticides tested in this work, only the Aldrin is adsorbed for 60% with the PCBs by the NH₂ Sep-Pak cartridge. The method described is rapid, simple and reproducible.     

Exceptionally Inert Lanthanide(III) PARACEST MRI Contrast Agents Based on an 18‐Membered Macrocyclic Platform

We report a macrocyclic ligand based on a 3,6,10,13‐tetraaza‐1,8(2,6)‐dipyridinacyclotetradecaphane platform containing four hydroxyethyl pendant arms (L¹) that forms extraordinary inert complexes with Ln³⁺ ions. The [EuL¹]³⁺ complex does not undergo dissociation in 1 M HCl over a period of months at room temperature. Furthermore, high concentrations of phosphate and Zn²⁺ ions at room temperature do not provoke metal‐complex dissociation. The X‐ray crystal structures of six Ln³⁺ complexes reveal ten coordination of the ligand to the metal ions through the six nitrogen atoms of the macrocycle and the four oxygen atoms of the hydroxyethyl pendant arms. The analysis of the Yb³⁺‐ and Pr³⁺‐induced paramagnetic ¹H NMR shifts show that the solid‐state structures are retained in aqueous solution. The intensity of the ¹H NMR signal of bulk water can be modulated by saturation of the signals of the hydroxy protons of Pr³⁺, Eu³⁺, and Yb³⁺ complexes following chemical‐exchange saturation transfer (CEST). The ability of these complexes to provide large CEST effects at 25 and 37 °C and pH 7.4 was confirmed by using CEST magnetic resonance imaging experiments.     

Sequential solid-phase extraction with cyanopropyl bonded-phase cartridges for trace enrichment of PCBs and chlorinated pesticides from water samples

Summary Gas chromatography of polychlorinated biphenyls and chlorinated pesticides in water samples has been performed after adsorption from a 50–250 mL sample on to a cartridge containing 100 mg cyanopropyl-bonded porous silica. The PCBs are desorbed with 500 μL ethyl acetate, which is concentrated and analysed by gas chromatography with electron-capture detection (GC-ECD). The average recovery of 1 ppb PCB congeners at from distilled water and from Marta river water is ≥95% (standard deviation ≤2.5). The average recovery of 20 ppb Aroclor 1260 from Marta river water was ≥91% (standard deviation ≤3.5). In the separation of the PCBs from the chlorinated pesticides only aldrin, heptachlor and 4,4′-DDD are adsorbed with the PCBs by the CN Sep-Pak cartridge. The method proposed is rapid, simple and reproducible.     

First evidence of pep solar neutrinos by direct detection in Borexino

We observed, for the first time, solar neutrinos in the 1.0-1.5 MeV energy range. We determined the rate of pep solar neutrino interactions in Borexino to be 3.1±0.6{stat}±0.3{syst} counts/(day·100 ton). Assuming the pep neutrino flux predicted by the standard solar model, we obtained a constraint on the CNO solar neutrino interaction rate of <7.9 counts/(day·100 ton) (95% C.L.). The absence of the solar neutrino signal is disfavored at 99.97% C.L., while the absence of the pep signal is disfavored at 98% C.L. The necessary sensitivity was achieved by adopting data analysis techniques for the rejection of cosmogenic {11}C, the dominant background in the 1-2 MeV region. Assuming the Mikheyev-Smirnov-Wolfenstein large mixing angle solution to solar neutrino oscillations, these values correspond to solar neutrino fluxes of (1.6±0.3)×10{8} cm{-2}?s^{-1} and <7.7×10{8} cm{-2}?s{-1} (95% C.L.), respectively, in agreement with both the high and low metallicity standard solar models. These results represent the first direct evidence of the pep neutrino signal and the strongest constraint of the CNO solar neutrino flux to date.     

Improved gas-chromatographic columns of liquid crystals supported on glass beads for analysis of polycyclic aromatic hydrocarbons

Summary Glass microbead columns withN, N-bis-(p-butoxybenzilidene) , -bi-p-toluidine (BBBT) a high-temperature smectic-nematic liquid crystalline stationary phase have been prepared. The best efficiency was obtained with BBBT from 0.025% w/w (ca. 1800 theoretical plates m^–1) to 0.1% w/w (ca. 2100 theoretical plates m^–1). Capacity ratios and separation efficiencies of columns packed with glass microbeads treated and untreated with a surfaceactive agent were studied as a function of analysis time. A separation of five methylchrysene isomers is shown.