Different chemical modifiers for use with electrothermal atomic absorption spectrometry (ET AAS) were investigated in relation
to determining the selenium in human urine samples. The samples were diluted in a solution containing 1% v/v HNO3 and 0.02% m/v cetyltrimethylammonium chloride (CTAC). Studying the modifiers showed that the use of either Ru or Ir as the
permanent modifier gave low sensitivity to Se and the peak shape was very noisy, while Zr or Rh gave no peak at all. The same
occurred when Zr was used in solution. For mixtures of permanent modifiers, Ir plus Rh or Zr plus Rh gave very low sensitivity,
Zr plus Rh with co-injection of Ir in solution was also not efficient, Zr plus Rh in solution gave good sensitivity, but the
best results were obtained with a mixture of Zr and Rh as the permanent modifier and co-injection of Rh in solution. Using
this last modifier, the following dilutions with the HNO3 and CTAC were studied: 1:1, 1:2, 1:3 and 1:4. The best dilution was 1:1, which promoted good sensitivity and a more defined
peak shape and made it possible to correct for the background using a deuterium arc lamp. Under these conditions, a characteristic
mass of 26±0.2 pg was obtained for Se in aqueous solution. Six certified urine samples were analyzed using matrix matching
calibration and the measured concentrations were in agreement with the certified values, according to a t-test at the 95%
confidence level. Recovery tests were carried out and the recoveries were in the range 100–103%, with relative standard deviation
better than 9%. The limit of detection (LOD, 3 sd, n=10) was 3.0 μg L−1 in the sample. The treated graphite tube could be used for at least 600 atomization cycles without significant alteration
of the analytical signal. 相似文献
A system has been developed for online preconcentration and determination of Cd using thermospray flame furnace atomic absorption
spectrometry (TS-FF-AAS). It is based on the solid-phase extraction of Cd in an Amberlite XAD-2 minicolumn loaded with 2-(2-thiazolylazo)-5-dimethylaminophenol
(TAM), and the metal ion is eluted with 1 mol L−1 hydrochloridric acid, followed by its determination. The online system allows determining Cd with a detection limit of 8.0 ng L−1 and a quantification limit of 25.0 ng L−1. The precision (repeatability), calculated as the relative standard deviation (% RSD) in sample solutions containing 0.5
and 3.0 μg L−1 of Cd, was 6.1 and 4.5%, respectively. The preconcentration factor obtained was 24. The system’s accuracy was confirmed by
analyzing the following certified reference materials (CRMs): Rice flour NIES 10b, Apple leaves NIST 1515 and Orchard leaves
NBS 1571. This procedure was applied to the determination of Cd in cabbage and powdered guarana samples. 相似文献
Themain goal of ourwork is to showthat there exists a class of 2×2 Riemann problems for which the solution comprises a singlewave group for an open set of initial conditions. This wave group comprises a 1-rarefaction joined to a 2-rarefaction, not by an intermediate state, but by a doubly characteristic shock, 1-left and 2-right characteristic. In order to ensure that perturbations of initial conditions do not destroy the adjacency of the waves, local transversality between a composite curve foliation and a rarefaction curve foliation is necessary. 相似文献
As part of an ongoing program directed toward the preparation of antraciclinones1 and aryl substituted lapachones2, which are important anticancer and antibiotic3 agents, we became interested in a efficient synthesis of substituted 1,4-naphthoquinones, such as juglone (3). This compound has received some attention due its activity as an allelophatic compound4. An extensive analysis of the literature procedures indicated that several methods are available starting from 1,5-dihydroxynaphthalene (1). All the procedures explored the oxidation of carbon four of the naphthyl ring by several known reagents, such as, chromium trioxide-piridine5, thallium trinitrate5, chromic acid6, peracetic acid7, dichromate8, iron (III) chloride9 and mercuric oxide10. None of the several known methods for the preparation of (3) proceeded in satisfactory yield (except for the thallium trinitrate method which gave 642 yield) and most of them gave a mixture of 1,2 and 1,4-naphthoquinone. 相似文献
In this study, we describe for the first time the application of an internal standard method to compensate for random errors associated with the injection procedure in batch injection analysis (BIA) systems with multiple pulse amperometric detection. A sequence of potential pulses was selected in such a way that the internal standard (IS) compound was detected individually at one potential pulse and both the IS and analyte, were detected at another potential pulse. The current ratio (IIS+analyte/IIS) was used in the construction of the calibration curve and then to compensate for random errors. The use of disposable syringes or manual pipettes in BIA systems increases the robustness of the method and dispenses with skilled operators. 相似文献
Abstract Structures of the thermotropic mesophases of lead(II) decanoate are reassigned following optical and X-ray diffraction studies. These results, and those of D.S.C., Raman and 207Pb N.M.R. spectroscopy, indicate formation of a lower temperature mesophase involving mainly increased lateral disorder, and a higher temperature Lα (smectic A) phase resulting from chain disordering and decreased lead-carboxylate interaction. Comparison of experimental thermodynamic data for the phase transitions with theoretical data in the literature indicates that the entropy change for the lower to higher mesophase transition is dominated by the increase in chain disorder. 相似文献
Afterglows of mixed gas of N2 and H2(0–2.5%) flowing microwave discharges in a 5 mm diameter tube connected to a 5 L reactor via a tube of 1.8 cm diameter and 50 cm long, have been studied using optical emission spectroscopy. The obtained results at the entrance of the afterglow tube of 1.8 cm diameter: Short time afterglow (SA), (10–3 s) and inside the 5 L reactor: Long time afterglow (LA), (10–2 s) were then compared. It was found that, in N2 at 2 Torr, 0.5 slpm, the active specie density ratios had a constant value of 10–2 for N/N2, but decreased respectively from 10–3 to 10–4 for N2 (X,v?>?13)/N2 and from 10–6 to 10–8 for N+2 /N2. By directly connecting the discharge tube inside the 5 L reactor, the density increases by 10 for N2 (X,v?>?13) and by 102 for N2+ by changing the afterglow from LA(10?2 s) to a SA(10–3 s). Moreover and by adding 1% of H2 to N2, the N/N2 and H/H2 ratios had constant values of 1% and 0.2% respectively. The SA(10–3 s) appeared to be more efficient for surface treatments than the LA (10–2 s).