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11.
A method has been developed for the determination of 23 elements in marine plankton in which inductively coupled plasma (ICP) source mass spectrometry (MS) was used to quantify the elements in the solution after digestion in a mixture of hydrofluoric and nitric acids in sealed PTFE vessels in a microwave field. The procedure was validated by the analysis of a standard reference soil (SRM 2709 San Joaquin Soil) and a standard reference fresh water plankton (CRM 414). The method was applied to the analysis of several marine plankton samples grown under controlled conditions including several whose growth media had been enriched with selenium. Matrix induced signal suppressions and instrumental drift were corrected by internal standardization. The suitabilities of germanium, indium, rhodium, scandium and yttrium as internal standard elements were evaluated. Neither scandium nor yttrium could be used due to the presence of these elements in the samples, germanium was used for the determination of As, Co, Cu, Fe, Ni, Se, Si and Zn, indium was used for Al, Ba, Ca, Eu, Sr, and Tl, and rhodium was used for Cd, Cr, Hg, Mg, Pb, Sb, Sn, and V. For Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Si, Sr, V, and Zn internal standardization did not completely compensate for the suppressive effect of the heavier elements and the solutions were diluted. However, for As, Ba, Cd, Co, Eu, Hg, Pb, Sb, Se, Sn and T1, it was possible to obtain accurate results despite the 35-40% suppression in the signals. Isobaric overlap was only a problem in the cases of 42Ca and 78Se; 44Ca and 77Se, respectively, were used. Memory effects were only observed with Hg for which a nitric acid-sodium chloride solution was the most effective wash-out solution. The marine plankton samples were able to tolerate a higher concentration of Hg as the selenium concentration increased.  相似文献   
12.
Four new Hofmann–3-phenylpropylamine (3PPA) type complexes with chemical formulae M(3PPA)2Ni(CN)4 (M = Ni, Co, Cd, and Pd) have been prepared and their vibrational spectra are reported in the region of 4000–60 cm−1. The vibrational bands arising from 3PPA ligand molecule, the polymeric sheet and metal–ligand bands of the compounds are assigned. The thermal behaviour of these complexes is also provided using the DTA and TGA along with the magnetic susceptibility data. The results indicate that the monodentate 3PPA ligand molecule bonds to the metal atom of |M–Ni(CN)4| polymeric layers and hence the compounds are similar in structure to Hofmann-type complexes.  相似文献   
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Arslan Z 《Talanta》2005,65(5):1326-1334
A method is developed for determination of trace elements, including Ag, As, Cd, Co, Cr, Cu, Mn, Ni, Se, Tl and Zn, in fish otoliths by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). Hydrofluoric acid was used to precipitate calcium resulting from acid dissolution of otolith calcium carbonate. Initial acidity of the sample solution influenced the precipitation efficiency of calcium fluoride. Up to 99.5% of Ca was precipitated in solutions that contained less than 2% (v/v) HNO3. Recoveries of the elements obtained from spiked artificial otolith solutions were between 90 and 103%. Stabilization of the elements within the ETV cell was achieved with 0.3 μg Pd/0.2 μg Rh chemical modifier that also afforded optimum sensitivity for multielement determination. The method was validated by the analysis of a fish otolith reference material (CRM) of emperor snapper, and then applied to the determination of the trace elements in otoliths of several fish species captured in Raritan Bay, New Jersey. Results indicated that fish physiology and biological processes could influence the levels of Cu, Mn, Se and Zn in the otoliths of fish inhabiting a similar aqueous environment. Otolith concentrations of Cr and Ni did not show any significant differences among different species. Concentrations for Ag, As, Cd, Co and Tl were also not significantly different, but were very low indicating low affinity of otolith calcium carbonate to these elements.  相似文献   
14.
New bis(NHC)-Pd complexes were synthesized and characterized by elemental analysis, 1H NMR, 13C NMR, and IR spectroscopy. The reaction of Pd(OAc)2 and bis(benzimidazolium) salts in DMSO gave the monomeric palladium complex in which the N-heterocyclic carbene was bound to the metal centre. The crystal and molecular structure of the cis-dibromo{1,1′-di[2,3,4,5,6-pentamethylbenzyl]-3,3′-butylenedibenzimidazol-2,2′-diylidene}-palladium(II) complex was determined by single-crystal X-ray diffraction. The activity of the Pd(II) complexes in the direct arylation of benzothiazole with arylbromides was investigated. A preliminary catalytic study showed that these bis(NHC)-Pd complexes were highly active in the direct arylation of benzothiazole with arylbromides.  相似文献   
15.
A slurry sampling method has been developed for the determination of Pb in marine plankton by ETAAS using a freshwater plankton certified reference material (CRM 414). Slurries were prepared in 1–3% m/v range with 1% v/v HNO3 by ultrasonic agitation for 5 min. The effects of several chemical modifiers, including Ir(NO3)2, Mg(NO3)2, Pd(NO3)2, Pd(NO3)2 + Mg(NO3)2, and Mg(NO3)2 + NH4H2PO4, were investigated for the stabilization of Pb during thermal pretreatment. Lead in slurries was effectively stabilized up to 1000 °C with Ir, Pd and Pd + Mg modifiers among which Pd + Mg provided the best results with complete atomization at 1850 °C. Firings in the presence of Ir were, problematic due to ash formation inside the atomizer. Water, dilute HNO3 and HF were examined as suspension medium. Dilute HNO3 (1–2% v/v) proved to be advantageous over water as it afforded extraction of Pb from plankton almost quantitatively in 5 min agitation. Hydrofluoric acid was the least suitable medium. Increasing HF concentration up to 5% v/v resulted in inaccuracy and substantial background absorption. Fast-heating furnace method provided comparable accuracy and precision to that of conventional-heating in slurries of CRM 414. Detection limits and characteristic masses were, respectively, 0.49 μg L− 1 and 32 pg for the conventional method and 0.62 μg L− 1 and 37 pg for the fast-heating method. However, fast-heating approach suffered from distorted peaks at high temperatures and incomplete pyrolysis of matrix at lower temperatures. Analysis of marine plankton samples for Pb was performed by using the conventional furnace program. The results showed a high correlation with those obtained by solution ICP-MS. Differences were statistically insignificant within 95% confidence interval.  相似文献   
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Here we present a detailed study of mixed dislocations in GaN, in which the complexities of the atomic arrangement in the cores have been imaged directly for the first time using an aberration corrected scanning transmission electron microscope. In addition to being present as a full-core structure, the mixed dislocation is observed to dissociate into partial dislocations separated by a stacking fault only a few unit cells in length. The generation of this stacking fault appears to be impurity driven and its presence is consistent with theoretical predictions for dislocation dissociation in materials with hexagonal crystal symmetry.  相似文献   
20.
Electrochemical behavior of resazurin on HMDE in Britton-Robinson (B-R) buffers (pH 2.0–10.0) was studied using the square-wave voltammetry (SWV), square-wave adsorptive stripping voltammetry (SWAdSV), and cyclic voltammetry (CV) techniques. The voltammogram of resazurin in B-R buffer at pH < 4.0 exhibited two cathodic reduction peaks. The voltammetric peaks were obtained at −0.144 V (reversible) and −1.250 V (irreversible) at pH 3.2, and correspond to the reduction of resorufin to dihydroresorufin and to the catalytic hydrogen wave, respectively. At pH > 4.0, a new irreversible cathodic reduction peak, assigned to the protonation of N-oxide on the phenoxazin ring, was observed. Electrochemical parameters (I p/E p, I p/v, I p/pH, I p/t acc) of the compound were determined. From the voltammetric data, electrochemical reduction mechanisms for all peaks have been suggested. Maximum peak current for the reversible peak was obtained at pH 4.1. A linear relationship between the current and concentration was determined, and also the lowest detection limit was found as 3.25 × 10−8 mol L−1 and 1.98 × 10−10 mol L−1 for SWV and SWAdSV, respectively.  相似文献   
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