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Low temperature hysteresis loops have been measured on compositions of the spinel series Fe3-xTixO4, 0?x?1, with x=0.4, 0.5, 0.6 and 0.8. All compounds studied exhibit an anomaly of the hysteresis parameters in the temperature range 40–80 K below which a marked effect of field cooling on the hysteresis loops is observed. 相似文献
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Readman JE Grey CP Ziliox M Bull LM Samoson A 《Solid state nuclear magnetic resonance》2004,26(3-4):153-159
17O NMR studies of various cation-exchanged LTA and LSX zeolites have shown similarities between the two systems. LSX samples containing divalent cations contain resonances with similar chemical shifts to those previously assigned to ‘bare’ framework oxygen atoms in Ca-LTA and Sr-LTA. The assignments are consistent with the trends seen in the spectra of monovalent cation-containing LSX and LTA zeolites, which show an increase in the average chemical shift with increasing cationic radius. The spectrum of Li-LSX, like Na-LSX, can be assigned based on the T–O–T bond angles. Gas sorption studies on Li-LSX are used to help identify the framework oxygen atoms that form the β-cages and demonstrate the sensitivity of the 17O shifts to gas loading. 相似文献
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Amanda J. King James W. Readman 《International journal of environmental analytical chemistry》2013,93(3):211-225
Solid-phase microextraction (SPME) has been successfully used for extracting polycyclic aromatic hydrocarbons (PAHs) from porewater samples from the Mersey Estuary, UK. The majority of the PAHs in porewater samples are associated with colloids due to the high DOC concentrations. The truly dissolved PAH concentrations varied from 66 to 1050?ng?L?1 in core 2 and from 95 to 740?ng?L?1 in core 3, and were dominated by naphthalene, fluoranthene, and pyrene. Although absent in the dissolved phase, the high-molecular-mass compounds were found in the colloid-associated fraction of porewater. PAHs in sediments arose from a range of compounds with 4- and 5-ring PAHs dominating. The partitioning of PAHs between sediment and porewater shows that PAHs are enriched in the sediment phase. When the soot carbon content was considered, predictions of the partition behaviour were found to agree more closely with the observed distribution. The results reiterate the importance of evaluating the speciation of organic pollutants in both porewater and sediments in order to accurately predict their environmental fate and potential toxicity. 相似文献
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A method was developed to determine the biocide pyrithione in natural waters. The method is based on cathodic stripping voltammetry (CSV) in the presence of Triton-X-100, which is used to separate the peak from interfering thiol compounds. Optimised conditions include a Triton-X-100 concentration of 4 ppm and a pH adjusted to 9 using ammonia buffer. The adsorption potential for pyrithione was −0.10 V and the peak occurred at −0.2 to −0.3 V. Detection was by differential-pulse CSV. The detection limit in UV-digested seawater was 1.5 nM for a deposition time of 60 s. In principle, this limit of detection could be lowered by extending the adsorption time, but in practice this may not be possible due to interferences by other organic compounds (surfactants and thiol compounds) in natural waters. 相似文献
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An analytical method is described for the determination of a broad range of emerging and priority pollutants, together with sewage molecular markers in environmental waters. The step-by-step study of the GC/MS analyses focuses on the effects of experimental variables using a large volume injection (LVI) technique [a programmed temperature-vaporising (PTV) inlet], the evaluation of a clean-up step using classical and newer sorbents (i.e. Al-N, Fl, NH2, PSA, Si, CN and DIOL), and the revision of how organic matter [i.e. humic acids (HA) content] affects method performance. Reproducibility and recoveries from spiked coastal water samples at different analyte concentrations (100, 250 and 500 ng L−1) as well as with different levels of spiked humic acids (2, 10 and 20 mg L−1) are reported indicating a good performance of the extraction procedure with low levels of HA (<10 mg L−1). The presence of HA is a critical parameter during the solid-phase extraction (SPE) procedures. Of the clean-up sorbents tested, CN and DIOL proved most efficient in cleaning-up the extracts with recoveries in the range of 66-77% and 100-114%, respectively for the selected analytes. Both GC/MS and PTV-GC/MS instrumental configurations were tested using final sewage effluents, riverine, estuarine and coastal water samples. However, limited applicability of the PTV inlet is reported for environmental applications, affording only a modest improvement in chromatographic signal-to-noise ratios. 相似文献
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Enikö Kádár David M. Lowe Montserrat Solé Andrew S. Fisher Awadhesh N. Jha James W. Readman Thomas H. Hutchinson 《Analytical and bioanalytical chemistry》2010,396(2):657-666
Nano-Fe particle uptake was experimentally examined in vitro using excised gills and blood cells of the edible blue mussel
Mytilus sp. Whole gills were exposed to both Fe2O3 nanoparticles and a solution of the hydrated FeCl3 salt, for up to 12 h, and blood cells for 30 min. Equimolar Fe+3 in the nano- and the soluble form was estimated under the assumption of dense spherical particles accommodating the same
number of Fe+3 as in the dissolved salt solution, namely: 1,000 μg L−1 Fe2O3 equivalent to 100 μg L−1 FeCl3·6H2O. Putative toxic impact of nano-Fe in gill epithelia and blood cells was assessed by an array of techniques including light-
and electron microscopy, biomarkers for oxidative stress (lipid peroxidation levels), neurotoxic effects (acetylcholinesterase
activity) and cytotoxicity (neutral red retention). Total and filtered fractions (20 and 200 nm, respectively) of Fe were
analysed by ICP-OES. Our results provide evidence for the following: (1) much of both the soluble (95%) and the nano-Fe (90%)
were removed from the water column within 12 h; (2) dissolved- and nano-Fe seemed to follow different routes of uptake within
the gill epithelium; (3) both nano-Fe and soluble FeCl3 caused similar impairment of lysosomal stability in circulating blood cells; (4) lipid peroxidation in gills exposed to the
two distinct forms of Fe was increased, while acetylcholinesterase activity was unaffected. In these short-term in vitro studies,
there appears to be little difference in toxic response between exposure to the Fe salt and the nano-Fe indicating that, in
this case, the nanoparticles do not invoke special properties affecting biological function in gills. However, with the use
of nano-Fe as a food additive, clearly longer-term in vivo studies are warranted. 相似文献
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Montserrat Solé Jennifer P. Shaw Patricia E. Frickers James W. Readman Thomas H. Hutchinson 《Analytical and bioanalytical chemistry》2010,396(2):649-656
Environmental risk assessments of human pharmaceuticals and other ‘emerging contaminants’ should integrate both population-relevant
endpoints and biomarkers of potential modes of action in a range of species. Adult Mytilus galloprovincialis were exposed to the beta-adrenergic receptor blocker propranolol or to the anti-inflammatory drug acetaminophen (paracetamol),
both commonly used therapeutic drugs present in aquatic ecosystems. Mussels were exposed under semi-static conditions for
10 days to either acetaminophen (CAS number 103-90-2; mean measured concentrations 23 and 403 μg/L) or propranolol hydrochloride
(CAS number 318-98-9; mean measured propranolol concentrations 11 and 147 μg/L) at 15 ± 1 °C sea water. Feeding rate was assessed
as an indicator of general toxicity. For propranolol, the 10-day no-observed effect concentration (feeding rateNOEC) and lowest observed effect concentration (feeding rateLOEC) were 11 and 147 μg/L, respectively. For acetaminophen, feeding rate was increased at both 23 and 403 μg/L, suggesting
a 10-day feeding rateNOEC of 403 μg/L. Primarily, phase I carboxylesterase (CbE), phase II glutathione S-transferase (GST) and the anti-oxidant catalase activities were evaluated in digestive gland. Gill GST and acetylcholinesterase
(AChE) activities were also measured. Lipid peroxidation (LPO) levels were measured in both tissues to assess oxidative stress.
Some enzymatic activities in liver were also reduced after propranolol exposure whilst acetaminophen enhanced them (CbE p < 0.05). Acetaminophen exposure significantly increased hepatic LPO levels and inhibited AChE activity in gill (10-day NOEC
and LOEC of 23 and 403 μg/L, respectively), whereas propranolol (11 μg/L) enhanced gill GST. 相似文献
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Research into the analysis and monitoring of steroidal estrogens has grown significantly over the last decade, resulting in the emergence of a range of applicable techniques. In this study, three popular techniques, gas chromatography-mass spectrometry (GC-MS), gas chromatography-tandem mass spectrometry (GC-MS-MS) and liquid chromatography-tandem mass spectrometry (LC-MS-MS) for the analysis of three highly potent steroidal estrogens in the aquatic environment have been compared. It has been observed that overall, the three techniques appear comparable in generating similar estrogen concentrations for river and effluent samples. Of the three techniques, the GC-MS technique is the simplest to operate, but fails to detect the estrogens at the lower-end of environmentally relevant concentrations. The tandem MS techniques are more selective than MS, and therefore able to detect lower concentration levels of the three steroidal estrogens of interest. However, the LC-MS-MS technique is more susceptible to matrix interferences for the analysis of samples, resulting in a reduction of the signal-to-noise ratio and a subsequent reduction in reliability and stability compared to GC-MS-MS. With the GC-MS-MS technique offering increased selectivity, the lowest limits of detection, and no false positive identification, it is recommended to be the preferred analytical technique for routine analysis of estrogens in environmental water samples. 相似文献