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211.
Depleted uranium (DU) is a by-product of the uranium enrichment process for nuclear fuel. According to the Commission Decision 2002/657/EC, a confirmatory method for the quantification of DU in freeze-dried fish was developed by isotope ratio dynamic reaction cell inductively coupled plasma-mass spectrometry (IR-DRC-ICP-MS). A preliminary study was performed to determine the following parameters: instrumental detection limit (IDL), isotopic ratio measurement limit (IRML), percentage of DU (P(DU)) in presence of natural uranium (NU) and limit of quantification (LoQ(DU)). The analyses were carried out by means of IR-DRC-ICP-MS. Ammonia was the reaction gas used for the dynamic reaction cell. In addition, a sector field inductively coupled plasma mass spectrometer (SF-ICP-MS) was employed to calculate the within-laboratory reproducibility. For the confirmatory method the following parameters were determined: (a) trueness; (b) precision; (c) critical concentrations alpha and beta (CC(alpha), CC(beta)); (d) specificity; (e) stability. Trueness was assessed by using the recovery tests. The recovery and within-laboratory reproducibility were determined by fortifying the blank digested solution of dogfish tissue: six aliquots were fortified at 1, 1.5 and 2 times the LOQ(DU) with 25.0, 37.5 and 50.0 ng L(-1) or 4.16, 6.24, 8.32 microg kg(-1) with a recovery of -8.2, +9.5 and +9.6%, respectively and a within-laboratory reproducibility (three analytical run) of 15.5, 8.0 and 11.0%, respectively. The results for the decision limit and the detection capability were: CC(alpha) = 11.69 ng L(-1) and CC(beta) = 19.8 ng L(-1). The digested solutions resulted to be stable during testing time (60 days) and the method can be considered highly specific as well. 相似文献
212.
《合成通讯》2013,43(10):1863-1870
Abstract An efficient and high‐yielding one‐pot synthesis of 1,2,4‐oxadiazoles from carboxylic acids and amidoximes is described. Activation of the carboxylic acid using hydroxybenzotriazole (HOBt) and EDC/HCl followed by reaction with an amidoxime generates an oxime ester. Without isolation, the oxime ester is dehydrated to give the oxadiazole ring. 相似文献
213.
Reverse iodine transfer polymerisation (RITP) is a living radical polymerisation technique that has shown to be feasible in synthesising segmented styrene-acrylate copolymers. Polymers synthesised via RITP are typically only described regarding their bulk properties using nuclear magnetic resonance spectroscopy and size exclusion chromatography. To fully understand the complex composition of the polymerisation products and the RITP reaction mechanism, however, it is necessary to use a combination of advanced analytical methods. In the present RITP procedure, polystyrene was synthesised first and then used as a macroinitiator to synthesise polystyrene-block-poly(n-butyl acrylate) (PS-b-PBA) block copolymers. For the first time, these PS-b-PBA block copolymers were analysed by a combination of SEC, in situ1H NMR and HPLC. 1H NMR was used to determine the copolymer composition and the end group functionality of the samples, while SEC and HPLC were used to confirm the formation of block copolymers. Detailed information on the living character of the RITP process was obtained. 相似文献
214.
Preparation of a monolith functionalized with zinc oxide nanoparticles and its application in the enrichment of fluoroquinolone antibiotics 下载免费PDF全文
Dan Liu Jiutong Ma Yan Jin Xiqian Li Xiao Zhou Qiong Jia Weihong Zhou 《Journal of separation science》2015,38(1):134-140
This study describes the enrichment ability of ZnO‐modified methacrylic acid‐co‐ethylene dimethacrylate polymer monoliths as stationary phases for the simultaneous determination of antibiotics (ofloxacin, ciprofloxacin, enoxacin, and pefloxacin) combined with high‐performance liquid chromatography. The prepared monolith was characterized by scanning electron microscopy, X‐ray photoelectron spectroscopy, Fourier‐transformed infrared spectroscopy, and thermogravimetric analysis. The polymer monolith microextraction method has been applied to the enrichment of fluoroquinolone antibiotics and satisfactory results were obtained in the analysis of water samples. Compared with the conventional methacrylic acid based monolith, the developed monolith exhibited a higher enrichment capacity because of the introduction of zinc oxide into the preparation process. 相似文献
215.
Ekaterina P. Nesterenko Pavel N. Nesterenko Damian Connolly Flavie Lacroix Brett Paull 《Journal of chromatography. A》2010,1217(14):2138-2146
A new method for the fixation of polymethacrylate monoliths within titanium tubing of up to 0.8 mm I.D. for use as a chromatographic column under elevated temperatures and pressures is described. The preparation of butyl methacrylate–ethylene dimethacrylate-based monolithic stationary phases with desired porous structures was achieved within titanium tubing with pre-oxidised internal walls. The oxidised titanium surface was subsequently silanised with 3-trimethoxysilylpropyl methacrylate resulting in tight bonding of butyl methacrylate porous monolith to the internal walls, providing stationary phase stability at column temperatures up to 110 °C and at operating column pressure drops of >28 MPa. The titanium housed monoliths exhibited a uniform and dense porous structure, which provided peak efficiencies of up to 59,000 theoretical plates per meter when evaluated for the separation of small molecules in reversed-phase mode, under optimal conditions (achieved at 15 μL/min and temperature of 110 °C for naphthalene with a retention factor, k = 0.58). The developed column was applied to the reversed-phase isocratic separation of a text mixture of pesticides. 相似文献
216.
用HPLC测定具有改善睡眠等特定功能的保健药品“梦通宁”中的褪黑激素,并结合紫外光谱来鉴定样品中的褪黑激素。以Novapak C18柱为分离柱,V(甲醇):V(0.05mol/L的Na2HPO4)=30:70作流动相,检测波长为230nm,用外标法进行定量分析,方法回收率98,11%,检出限为0.5mg/L。 相似文献
217.
The bifunctional metalloligand bis(carboxyethylgermanium)sesquioxide, (HOOCCH2CH2Ge)2O3, was employed in the systematic high‐throughput (HT) investigation of the system Zn2+/(HOOCCH2CH2Ge)2O3/H2O/C4H9OH. Two new metal‐organogermanates Zn[(OOCCH2CH2Ge)2O3] ( 1 ) and Zn2(O3GeCH2CH2COO) ( 2 ) were discovered that show two new structural motifs for this class of compounds. Whereas in compound 1 a formal intercalation in the structure of (HOOCCH2CH2Ge)2O3 is observed, 2 exhibits a new layered structure composed of CGeO3 and ZnO4 unit linked by μ3‐oxygen atoms. Both connectivity modes lead to dense three‐dimensional framework structures. 相似文献
218.
J. -L. Fortier P. -A. Leduc P. Picker J. E. Desnoyers 《Journal of solution chemistry》1973,2(5):467-475
The enthalpies of dilution of NaCl, Me4NBr, andn-Bu4NBr were measured in water at 25°C with a new flow microcalorimeter. The data were analyzed with a polynomial equation, and the derived relative apparent molal enthalpies L are in good agreement with literature values. Provided care is taken that mixing is complete, flow calorimeters are as reliable and much less time-consuming than cell-type instruments for enthalpies of dilution measurements. 相似文献
219.
In the product of carbon made from tar oil by plasma pyrogenation, some nanowires, whose diameter is 9~20 nm and whose length is 300 nm were found. The result of X-ray Energy Dispersed Spectrum (EDS) indicated that it is a new compound K2Ti8O15, which has never been reported before. Compared with the corresponding stoichiometry compound K2Ti8O15, it is a non-stoichiometry compound in which two oxygen atoms are absent. It is due to the fact that the intensive deoxidization occured in the experimental process and the valence of titalium is alterable. Its microstructure in detail by high revolution electromicroscopy (HREM) and X-ray diffraction were studied. 相似文献
220.
J. M. Bayona J. Grimalt J. Albaigs W. Walker B. W. de Lappe R. W. Risebrough 《Journal of separation science》1983,6(11):605-611
Analyses of hydrocarbon fractions from different areas of the marine environment are described to illustrate the possibilities and limitations of high resolution gas chromatography (HRGC) in the analysis of environmental samples. Examples are given of dissolved, particulate, and sedimentary hydrocarbons and organochlorine compounds; the importance of an adequate sampling of the marine environment is stressed. HR chromatographic profiles obtained in two columns of low and high polarity (SE-52 and PEG 20M) permit the sources and transport pathways of both natural and anthropogenic hydrocarbons to be traced. Analysis of tissues of marine mammals, which metabolize or excrete many of the biogenic and petrogenic hydrocarbons present in other areas of the marine environment, may provide an opportunity to obtain relatively clean profiles of many anthropogenic compounds of interest. The plotting of mass chromatograms from data compiled by COM-GC-MS remains the most appropriate method for the conclusive indentification of these compounds. 相似文献