Thermodynamic parameters for the molecular inclusion reaction of dulcin with beta-cyclodextrin. spectrofluorimetric determination of dulcin

The inclusion of dulcin in alpha- and beta-cyclodextrin has been studied by fluorescence spectroscopy. To quantitatively describe complex formation between the beta-cyclodextrin and dulcin, an association constant of 290 M(-1) at 21 degrees was obtained. The thermodynamics associated with the complex formation between dulcin and beta-cyclodextrin in aqueous solution has been studied. The obtained value of DeltaG(0) = -13.7 kJ/mole at 21 degrees , together with DeltaH(0) = -33.6 +/- 2.3 kJ/mole and DeltaS(0) = -67.2 +/-8.3 Jmole(-1) K(-1) indicate that dulcin has a very marked tendency to associate with beta-cyclodextrin in water. The inclusion complex of dulcin in beta-cyclodextrin has been used to determine dulein in the range 0.13-5 mug/ml the method has been applied to determine dulcin in soft drinks.     

Comparison of solid phase microextraction and hollow fiber liquid phase microextraction for the determination of pesticides in aqueous samples by gas chromatography triple quadrupole tandem mass spectrometry

This work compares two miniaturised sample preparation methods, solid phase microextraction (SPME) and hollow fiber liquid phase microextraction (HF-LPME), in combination with gas chromatography coupled to tandem mass spectrometry with a triple quadrupole analyzer for the determination of 77 pesticides in drinking water. In the case of SPME, extraction temperature and time were optimized by experimental design, although other parameters, as desorption time, pH, and ionic strength, were also evaluated. The extraction and desorption solvents [octanol/dihexyl ether (75:25, v/v) and cyclohexane, respectively], as well as the extraction and desorption time, ionic strength, and pH, were studied for the HF-LPME procedure. Under the optimal conditions, recoveries (70.2–113.5% for SPME and 70.0–119.5% for HF-LPME), intra-day precision (2.1–19.4% for SPME and 4.3–22.5% for HF-LPME), inter-day precision (5.2–21.5% for SPME and 8.4–27.3% for HF-LPME), and limits of detection, between 0.1 and 28.8 ng/L for SPME and 0.2 and 47.1 ng/L for HF-LPME and overall uncertainty (9.6–25.2% for SPME and 13.3–27.5% for HF-LPME) were established for both extraction procedures. Finally, the proposed methods were successfully applied to the analysis of 41 drinking water samples, and similar results were obtained with both extraction approaches.     

Multielement analysis of green coffee and its possible use for the determination of origin

Using instrumental neutron activation analysis (INAA), graphite furnace atomic absorption spectrometry (GFAAS), flame atomic absorption spectrometry (FAAS) and combustion elemental analysis, green coffees of the Arabica species produced in crop year 1987/88 in Colombia, Costa Rica, Cuba, El Salvador, Mexico, Nicaragua, Panamá and Papua New Guinea were analysed for the elements Ba, Br, C, Ca, Co, Cr, Cu, Cs, Fe, H, K, La, Mg, Mn, N, Na, Rb, Sc, Sr and Zn. In accordance with the concentrations determined, the elements could be ranked into five groups: Sc (sub-ppb level); Br, Co, Cr, Cs and La (ppb level); Ba, Cu, Fe, Mn, Na, Rb, Sr and Zn (ppm level); Ca and Mg (%o level); and C, H, K and N (% level). On the basis of the results obtained, an attempt was made to establish the origin of the green coffee via its elemental composition. Among the investigated elements, manganese was found to be best suited as an indicator for this purpose. However, the elements C, Co, Cs, Na and Rb proved to be of interest too.     

Nonconventional C–H···Cu Interaction Between Copper Cun Clusters (n = 3–20) and Aromatic Compounds

The present study examines bonding patterns between copper Cu_n clusters (n?=?3–20) and aromatic compounds (benzene, phenol, and benzaldehyde) using a density-functional theory (DFT) approach. Hirshfeld population, natural bond orbital (NBO), molecular orbitals, and quantum theory of atoms in molecules (QTAIM) analyses suggested the formation of two types of interactions Cu–arene and C–H···Cu, in the complexation of copper clusters by an aromatic compound.

     

Neutron activation analysis of urinary stones

Human vesical, urethral and renal stones were analyzed for the trace elements Co, Cu, Mn, Zn and Mo. Statistical correlations between the elements determined were sought which would be of possible interest in further research on the initial causes of urinary stone formation in the human body. This research project was funded by a grant from the National Research Council of the Philippines. Read at the 40th Annual Convention of the Philippine Medical Association held in Manila, May 9, 1947.