Determination of odorous compounds in water by headspace solid-phase microextraction-gas chromatography-mass spectrometry

Three major odorous compounds are 2-methylisoborneol ( 2-MIB), geosmin and beta-cyclocitral, which in water were determined by coupling headspace solid-phase microextraction ( HS-SPME) with gas chromatography-mass spectrometry (GC-MS). The operating conditions of HS-SPME, such as fibre type, salt concentration, water temperature, stirring, absorption time and desorption time were studied and discussed.The highest absorption of the odorous compounds were obtained under the following operating conditions as the addition of 30% ( m/V) NaCl, stirring at 60 degrees C for 40 min, using 65 mu m polydimethyl siloxane/divinylbenzene coated fibre. After the odorous compounds had been absorbed in the fibre under the optimal conditions of HSSPME, they were desorbed at 250 degrees C and determined by GC-MS. The limits of detection for geosmin, beta-cyclocitral and 2-MIB in water were 1. 0, 1. 3, 1. 7 ng/L, and the relative standard deviations for them were 4. 9%, 8. 4%, 6. 2%,respectively. There were good linear correlation (the calibration coefficients were all above 0. 997) for the three odorous compounds in the range of 5 similar to 1000 ng/ L. Therefore, trace levels of the odorous compounds at ng/L in water could be quantified by the simple method with satisfactory result.

Cytological and biochemical alterations in Carassius auratus hepatocytes from exposure to sediment containing dioxins and related compounds

Cytological and biochemical alterations of crucial carp (Carassius auratus) hepatocytes were characterized after exposure to sediments from a lake contaminated with dioxins and other industrial chemicals. Carp were exposed in 20 L water containing 25, 50, or 100 g of contaminated sediment for 2 and 4 weeks. Ultrastructural changes in the liver were characterized by severe enlargement of hepatocytes. Alterations in the cell. included formation of condensed and irregular cell nucleus, polynuclei, dispersed heterochromatin, enlargement of the nucleolus, and degeneration of the nucleus. Mitochondrial numbers were reduced and cristae were deformed. Myelin figures and lysosomes were increased, and sometimes cell organelles and cell matrix were totally lost after 4 weeks of exposure. The ultrastructural alterations were correlated with exposure time and sediment concentrations. Hepatosometic index was significantly increased in experimental groups at 2 and 4 weeks as compared with the control group. EROD enzyme activities were strongly induced in liver. A trend from rough endoplasmic reticulum (RER) to SER was observed. Our results suggest that the dioxin-like compounds bound by sediment were bioavailable to C. auratus and cause sublethal effects.

Analysis of organchlorine compounds in water by solid phase microextraction and gas chromatography

In this work, both,solid phase microextraction (SPME) and solid phase extraction(SPE) were used to enrich organochlorine compounds in water samples and analyzed by gas chromatography with electron capture detector. The operating conditions of SPME have been studied and different kinds of solid phase were compared. Linear alkybenzene sulfonate(LAS) was added to the samples to investigate its effect on the analysis. The results indicated that polyacrylate was better than other commercial solid phases in extraction of moderated polar organic compounds and the sensitivity of SPME was higher than SPE. LAS affect much in liquid-liquid extraction and headspace SPME; but it has little effect on SPE and direct-SPME method. The applications showed that SPME was a fast and effective method in sample preparation.

UV-sensitive P compounds: Release mechanism, seasonal fluctuation and inhibitory effects on alkaline phosphatase activity in a shallow Chinese freshwater lake (Donghu Lake)

Filtrable phosphorus compounds in a shallow Chinese freshwater lake (Donghu Lake) were fractionated by Sephadex G-25 gel-filtration chromatography. Some portions of those compounds released soluble reactive phosphorus upon irradiation with low dose ultraviolet light. Catalase and a hydroxyl radical scavenger (mannitol) markedly prevented photosensitive phosphorus release. The observed effects may be explained by the action of oxidizing reagents such as hydroxyl radicals, produced in photochemical reactions between UV irradiation and humic substances in the water. There was a strong seasonality in UV-sensitive P (UVSP) release. Michaels constants (K-m) of total alkaline phosphatase in the lake water showed a direct positive relation to UVSP. Plot of K-m against the UVSP/phosphomonoester ratio reveals a strong relationship between the two variables. These results suggest that in some situations UVSP may be a competitive inhibitor of alkaline phosphatase activity in the lake. The competitive inhibition of fractionated UVSP on alkaline phosphatase reagent (Sigma) apparently supports this hypothesis.

Rapid bioassay as indicator of potentially harmful effects for dioxin-like compounds in sample of Ya-Er Lake, China: Requirements for clean-up and comparison to chemical analysis

A rapid bioassay was established measuring the extracts of wildlife samples which were taken from Ya-Er Lake area, China. In extracts of these samples containing PCDD/Fs and PCBs, bioassay and chemically derived TCDD-equivalents (TEQs) were nearly identical. Our results indicate this bioassay is an excellent complement to chemical residue analysis and a useful tool in understanding the complex interactions of halogenated hydrocarbons. However, it must be mentioned that the proper prior clean-up method is very important for using the bioassay.

Magnetic ordering and irreversible magnetization between ZFC and FC states in RCo5Ga7 compounds

The magnetic properties of RCo5Ga7 (R = Y, Tb, Dy, Ho and Er) compounds which crystallize in the ScFe6Ga6-type structure have been studied. The compounds with R, Y, Tb, Dy, Ho and Er display behaviour similar to semiconductors. The Co transition metal sublattice is ferrimagnetic with a very low spontaneous magnetization. The ferrimagnetic ordering observed for R = Y, Tb, Dy, Ho and Er is due to the transition metal sublattice with transition temperatures at about 295 K. At low temperatures, the magnetic ordering for R Tb, Dy, Ho and Er is due to the rare-earth sublattice, which is ferromagnetic with a Curie temperature below 5 K. By fitting the linear part of the inverse magnetization, the effective magnetic moment of the R ion is found to be close to its expected theoretical value, with paramagnetic Curie temperatures below 5 K. Due to the paramagnetic nature of the R sublattice above 60 K, the ferrimagnetic ordering temperature of the Co sublattice does not vary with the type of rare-earth ion. The irreversibility of the magnetization of YCo5Ga7, as measured in zero-field cooled (ZFC) and field cooled (FC) states, is attributed to movement of domain walls. Application of a large enough applied field completes the movement of the domain wall from the low-temperature to the high-temperature one at 5 K. With a very low magnetic field 100 Oe, the difference between the ZFC and the FC shrinks. (C) 2004 Elsevier B.V. All rights reserved.

(Ga,Mn,N) compounds growth with mass-analyzed low energy dual ion beam deposition

The (Ga,Mn,N) samples were grown by the implantation of low-energy Mn ions into GaN/Al2O3 substrate at different elevated substrate temperatures with mass-analyzed low-energy dual ion beam deposition system. Auger electron spectroscopy depth profile of samples grown at different substrate temperatures indicates that the Mn ions reach deeper in samples with higher substrate temperatures. Clear X-ray diffraction peak from (Ga,Mn)N is observed in samples grown at the higher substrate temperature. It indicates that under optimized substrate temperature and annealing conditions the solid solution (Ga,Mn)N phase in samples was formed with the same lattice structure as GaN and different lattice constant. (C) 2003 Elsevier Science B.V. All rights reserved.

The PL "violet shift" of cerium dioxide on silicon

CeO2 thin film was fabricated by dual ion beam epitaxial technique. The phenomenon of PL violet shift at room temperature was observed, and the distance of shift was about 65 nm. After the analysis of crystal structure and valence in the compound were carried out by XRD and XPS technique, it was concluded that the PL shift was related with valence of cerium ion in the oxides. When the valence of cerium ion varied front tetravalence to trivalence, the PL peak position would move from blue region to violet region and the phenomenon of "violet shift" was observed.

(Ga,Mn,As) compounds grown on semi-insulating GaAs with mass-analyzed low energy dual ion beam depositionw

The (Ga,Mn,As) compounds were obtained by the implantation of Mn ions into semi-insulating GaAs substrate with mass-analyzed low energy dual ion beam deposition technique. Auger electron spectroscopy depth profile of a typical sample grown at the substrate temperature of 250degreesC showed that the Mn ions were successfully implanted into GaAs substrate with the implantation depth of 160 nm. X-ray diffraction was employed for the structural analyses of all samples. The experimental results were greatly affected by the substrate temperature. Ga5.2Mn was obtained in the sample grown at the substrate temperature of 250degreesC. Ga5.2Mn, Ga5Mn8 and Mn3Ga were obtained in the sample grown at the substrate temperature of 400degreesC. However, there is no new phase in the sample grown at the substrate temperature of 200degreesC. The sample grown at 400degreesC was annealed at 840degreesC. In this annealed sample Mn3Ga disappeared, Ga5Mn8 tended to disappear,Ga5.2Mn crystallized better and a new phase of Mn2As was generated. (C) 2002 Elsevier Science B,V. All rights reserved.

Syntheses, crystallographic and magnetic properties of Nd3Fe29-xCrx and other associated compounds

A systematic study of syntheses and magnetic properties of the Nd-3 Fe29-xCrx (x=4.5, 4.7, 5.0, and 5.5) compounds has been performed. The single-phase compounds of Nd3Fe29-xCrx can be formed in the range 4.5 less than or equal to x less than or equal to 5.5. The Curie temperature Tc, the saturation magnetization M-S at 4.2 K, the anisotropy field H-A at 4.2 K and room temperature, and the intra-sublattice exchange coupling parameter j(FeFe) at 4.2 K for the Nd3Fe29-xCrx compounds decrease with increasing Cr composition from x=4.5 to 5.5, respectively. Nitrogenation and carbonation, unlike hydrogenation, result mainly in improvements of the Curie temperature, the saturation magnetization and the anisotropy field at 4.2 K and room temperature for the Nd3Fe29-xCrx compounds compared with their parent compounds.

Photoluminescence enhancement of porous silicon by organic cyano compounds

A pronounced photoluminescence enhancement on chemically oxidized porous silicon was induced by a series of organic cyano compounds including 1,2-dicyanoethylene (CE), 1,3-dicyanobenzene (1,3-CB), 1,4-dicyanobenzene (1,4-CB), 1-cyanonaphthalene (1-CN), and 9-cyanoanthracene (9-CA). Photoluminescence enhancement effects were reversible for all compounds studies in this work. A dependence of photoluminescence enhancement on the steric effect and the electronic characteristics of these compounds and the structure of the porous silicon substrates were analyzed in terms of the photoluminescence enhancing factors. Surface chemical composition examined by Fourier transform infrared (FTIR) spectra demonstrated that the surface Si-H bonds were not changed and no new luminescent compounds were formed on porous silicon surface during adsorption of cyano compounds. A mechanism based on induced surface states acting as radiative recombination centers by cyano compounds adsorption was suggested.

A colorimetric assay for screening microcystin class compounds in aquatic systems

Secondary metabolites produced by water-blooming cyanobacteria in eutrophic waters include some potent hepatotoxins, These compounds also have tumour-promoting properties, attributable to their inhibition and activation of protein phosphatases and kinases respectively. The inhibitory effect of these toxins on protein phosphatases have been employed in a commonly used radiometric assay, involving the use of a P-32-labeled substrate, for the detection and quantitation of these compounds. This paper investigates and describes a colorimetric method in which the activity of protein phosphatase 2A is determined by measuring the rate of colour production from the release of yellow p-nitrophenol using p-nitrophenyl phosphate as the substrate. Results of this study suggest that the colorimetric protein phosphatase inhibition assay is a simple, inexpensive tool for screening substances that may have tumour-promoting characteristics in aquatic systems. The detection limit of the colorimetric method is comparable to the radiometric assay. (C) 1998 Elsevier Science Ltd. All rights reserved.

CERIUM SILICIDE FORMATION IN THIN CE SI MULTILAYER FILMS

Alternating layers of Si(200 angstrom thick) and Ce(200 angstrom thick) up to 26 layers altogether were deposited by electron evaporation under ultrahigh vacuum conditions on Si(100) substrate held at 150-degrees-C. Isothermal, rapid thermal annealing has been used to react these Ce-Si multilayer films. A variety of analytical techniques has been used to study these multilayer films after annealing, and among these are Auger electron spectroscopy, Rutherford backscattering, X-ray diffraction, and high resolution transmission electron microscopy. Intermixing of these thin Ce-Si multilayer films has occurred at temperatures as low as 150-degrees-C for 2 h, when annealed. Increasing the annealing temperature from 150 to 400-degrees-C for 1 h, CeSi2 forms gradually and the completion of reaction occurs at approximately 300-400-degrees-C. During the formation of CeSi2 from 150-400-degrees-C, there is some evidence for small grains in the selected area diffraction patterns, indicating that CeSi2 crystallites were present in some regions. However, we have no conclusive evidence for the formation of epitaxial CeSi2 layers, only polycrystals were formed when reacted in the solid phase even after rapid thermal anneal at 900-degrees-C for 10 s. The formation mechanism has also been discussed in combining the results of the La-Si system.