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81.
James Murphy Phil Jones Steve J. Hill 《Spectrochimica Acta Part B: Atomic Spectroscopy》1996,51(14):1867-1873
A simple and accurate method has been developed for the determination of total mercury in environmental and biological samples. The method utilises an off-line microwave digestion stage followed by analysis using a flow injection system with detection by cold vapour atomic absorption spectrometry.
The method has been validated using two certified reference materials (DORM-1 dogfish and MESS-2 estuarine sediment) and the results agreed well with the certified values. A detection limit of 0.2 ng g−1 Hg was obtained and no significant interference was observed. The method was finally applied to the determination of mercury in river sediments and canned tuna fish, and gave results in the range 0.1–3.0 mg kg−1. 相似文献
82.
Stéphanie Ricol Etienne Vernaz Philippe Barboux 《Journal of Sol-Gel Science and Technology》1997,8(1-3):229-233
Gels have been synthesized in the SiO2-Na2O-ZrO2 system and calcined at various temperatures up to 700°C. They have been studied by infrared absorption spectroscopy. The position of the asymmetric stretching frequency of the SiO4 unit is used as a tracer of the homogeneity. It is shown that sodium increases the solubility of zirconium in the silica matrix as already observed in fused glasses. 相似文献
83.
Summary The aim of this investigation was to obtain qualitative and quantitative profiles of the flavonoid and biflavonoid composition
of six cypress species—Cupressus funebris L.,Cupressus sempervirens L.,Cupressus glabra L.,Cupressus arizonica L.,Cupressus goveniana L., andCupressus lusitanica L. HPLC-diode-array detection (DAD), HPLC-MS, and HPTLC were used to identify the individual compounds. A chromatographic
method was optimized for identification and quantification of the main flavonoid glycosides and biflavonoids. The flavonoids
identified and calibrated were: rutin, quercetin glucoside, quercetin rhamnoside, and kaempferol 3-O-rhamnoside. The biflavonoids identified and calibrated were: cupressuflavone, amentoflavone, robustaflavone, hinokiflavone,
methylrobustaflavone, methylamentoflavone, and dimethylcupressuflavone. 相似文献
84.
Analytical procedures for quantification of peptides in pharmaceutical research by liquid chromatography–mass spectrometry 总被引:6,自引:0,他引:6
John H Walden M Schäfer S Genz S Forssmann WG 《Analytical and bioanalytical chemistry》2004,378(4):883-897
Peptide quantification by liquid chromatography–mass spectrometry (LC–MS) combines the high resolving power of reversed-phase (RP) chromatography with the excellent selectivity and sensitivity of mass spectrometric detection. On the basis of comprehensive practical experience in the analysis of small molecules, pharmaceutical research is developing technologies for analysis of a growing number of peptidic drug candidates. This article is a detailed review of procedures based on LC–MS techniques for quantitative determination of peptides. With the focus on pharmaceutical applications several technologies for sample preparation, various aspects of peptide chromatography, important characteristics of ESI–MS, selectivity of MS-detection modes, the large variability of internal standards, and modern instrumentation are discussed. The demand for reliable, robust, sensitive, and accurate methods is discussed using numerous examples from the literature, complemented by experiments and results from our laboratory. 相似文献
85.
Tomazela DM Gozzo FC Mayer I Engelmann FM Araki K Toma HE Eberlin MN 《Journal of mass spectrometry : JMS》2004,39(10):1161-1167
Ten homologous or isomeric singly, doubly, triply and quadruply charged cationic macrocyclic complexes I-Va, bn+ (n = 1-4) formed by the coordination of [Ru(bipy)2Cl]+ to the pyridyl N-atoms of a series of meso-(phenyl)m-(meta or para-pyridyl)n-porphyrins (m + n = 4) were transferred to the gas phase and structurally characterized by electrospray ionization (ESI) mass (MS) and tandem mass (MS/MS) spectrometry. Previously known to be stable in solution and in the solid state, I-Va, bn+ are found to constitute also a new class of stable, long-lived multiply charged gas-phase ions with spatially separated charge sites. Increasing intramolecular electrostatic repulsion from Ia, b+ to IVa, b3+ facilitates in-source and tandem collision-induced dissociation (CID). However, for the quadruply charged ions Va, b4+, electrostatic repulsion is alleviated mainly by ion pairing with the CF3SO3- counterion forming the salt clusters [Va,b/CF3SO3]3+ and [Va,b/(CF3SO3)2]2+ with reduced charge states. Ion-pairing that yields [IVa,b/CF3SO3]2+ is also observed as a minor ESI process for the triply charged ions IVa, b3+. The gaseous ions I-Va, bn+ (n = 2, 3 or 4) dissociate by sequential 'charge partitioning' with the formation of two cationic fragments by the release of [Ru(bipy)2Cl]+. The meta (a) and para (b) isomers and the positional isomers II2+ and III2+ display nearly identical ESI-MS and ESI-MS/MS spectra. ESI-MS/MS of I-Va, bn+ shows that the Ru-py(P) is, intrinsically, the weakest bond since this bond breaks preferentially upon CID. 相似文献
86.
采用二硫化碳重结晶富勒烯混合物或二硫化碳二次抽提烟灰以提取高富勒烯(higherfulerenes,Cn,n>70)。产物经高效液相色谱分析,高富勒烯的含量从1%分别提高到4%和6%;经激光飞行时间质谱证明,产物中除含主要成分C60和C70以外,还含有C76、C78、C82、C84以及更高碳原子的富勒烯。 相似文献
87.
Joachim Heidberg Elisabeth Kampshoff Helmut Stein Helmut Weiss Michael Warskulat 《Mikrochimica acta》1988,94(1-6):105-108
Sample/spectrum relationships are investigated using both a low resolution rapid-scanning NIR monochromator and a Fourier transform instrument capable of high resolution and are evaluated in terms of whether or not the resolution of the instrument is sufficient for measuring the natural bandwidths corresponding to the sample. Based on the sample/spectrum relationship a criterion is developed which must be followed in order to apply either derivative spectroscopy or deconvolution to enhance the resolution of overlapped bands without generating spectral artifacts. 相似文献
88.
Based on carbon nanofibers (CNFs) as a solid phase extraction adsorbent, a microcolumn preconcentration method coupled to inductively coupled plasma mass spectrometry (ICP–MS) was developed for the determination of trace elements (Mn, Co and Ni). The effect of various experimental parameters such as pH, sample flow rate and volume, elution solution and interfering ions on the retention of the studied ions have been investigated systematically. During all the steps of the experimental process, Mn, Co and Ni could be quantitatively sorbed on the microcolumn containing CNFs in the range of pH 6.0–9.0, and then eluted completely with 0.5 mol ml− 1 HNO3. A preconcentration factor of 150-fold was obtained. The detection limits for Mn, Co and Ni were 40, 0.4 and 8.0 pg ml− 1, respectively, with relative standard deviations less than 6.0%. In order to validate the proposed method, two certified reference materials of human hair (GBW 07601) and mussel (GBW 08571), and water sample were analyzed with satisfactory results. The recoveries were between 95.0 and 114%. 相似文献
89.
H. Binder B. Kohlstrunk U. Brenn W. Schwieger G. Klose 《Colloid and polymer science》1998,276(12):1098-1109
Microcrystals of the metal silicate hydrate ilerite orient macroscopically on the surface of a ATR-crystals and thus, are
accessible for infrared linear dichroism measurements. We present first results which indicate that the alkyl chain packing
and the orientation of the polar group of dodecyltrimethylammoniumbromide (DTAB) intercalated between silicate layers can
be determined in terms of infrared order parameters. The properties of DTAB can be modulated by the relative humidity of the
surrounding atmosphere and by temperature. Upon heating DTAB undergoes a phase transition from a paraffin-like solid to a
fluid phase. The former is characterized by the orthorhombic perpendicular packing of the frozen alkyl chains with tilted
long axes. The interactions between the ionic groups of the surfactant and that of the host matrix stabilize the lamellar
arrangement of DTAB in the crystalline and in the fluid phases.
Received: 14 January 1998 Accepted: 27 July 1998 相似文献
90.
Éder Lisandro de Moraes Flores Juliano Smanioto Barin Érico Marlon de Moraes Flores Valderi Luiz Dressler 《Spectrochimica Acta Part B: Atomic Spectroscopy》2007
This work deals with the determination of fluorine by solid sampling graphite furnace molecular absorption spectrometry. The molecular absorbance of aluminum monofluoride (AlF), which is produced in the vapor phase in the presence of Al3+, is measured at 227.5 nm, a non-resonant platinum line. A conventional graphite furnace program has been used with pyrolysis and vaporization temperatures of 800 and 2300 °C, respectively. Solutions of Ba2+ and Al3+ have been used to avoid fluorine losses during the pyrolysis stage and to produce AlF in the vaporization stage, respectively. Certified coal and alumina samples were analyzed using aqueous standards for calibration. The agreement between the found concentration and the certified value, or the value obtained by another method ranged from 92 to 105%, with a relative standard deviation less than 8.5%. The limit of detection and the characteristic mass was 0.17 μg g− 1 and 205 pg, respectively. 相似文献