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91.
rico Marlon de Moraes Flores Ana Paula Fleig Saidelles Eder Lisandro de Moraes Flores Mrcia Foster Mesko Mrcio Pozzobon Pedroso Valderi Luiz Dressler Celso Figueiredo Bittencourt Adilson Ben da Costa 《Microchemical Journal》2004,77(2):113-118
An alternative device for the direct solid analysis (DSA) for copper determination by flame atomic absorption spectrometry (FAAS) is proposed. Copper was directly determined in commercial medicinal plants used as dietary supplements. The determination of copper in solid samples by DSA–FAAS was made by using a conventional air–acetylene flame. Between 0.05 and 1.5 mg of each test, sample was weighed directly into a small polyethylene vial connected to the device used for solid introduction into the flame. Test samples were introduced into the flame as a dry aerosol using a T-quartz cell set between the burner and the optical path. The T-quartz cell has a slit in the superior part by which the solid aerosol passes to the flame. A transient signal, evaluated as integrated absorbance, is produced and it is totally integrated in 2 s. Background signals always presented absorbance values less than 0.1. It was found a characteristic mass of 0.8 ng Cu and absolute limit of detection of 1.2 ng (3 s), or 1.2 μg g−1 if a sample mass of 1 mg was used. Optimized conditions for air flow rate, flame stoichiometry, and so on were established as well. No excessive grinding of the samples was needed and samples with particle of size less than 80 μm were used throughout. No statistical difference between the results from the proposed system and those obtained by sample digestion and determination by conventional FAAS was observed. With the proposed procedure, more than 50 test samples can be analyzed in 1 h and it can be easily adapted to conventional spectrometers for FAAS. 相似文献
92.
《Electroanalysis》2004,16(10):811-820
A new minicell coupling the liquid‐liquid extraction technique called permeation liquid membrane (PLM) with an integrated Ir‐based Hg‐plated microelectrode array for voltammetric detection has been developed for the speciation of heavy metals in natural waters. Lead and cadmium have been used as model compounds. The PLM consists of a carrier (0.1 M 22DD+0.1 M lauric acid) dissolved in 1 : 1 mixture of toluene/phenylhexane held in the small pores (30 nm) of a hydrophobic polypropylene membrane (Celgard 2500). One side of this membrane is in contact with a flowing source solution, containing the metal ions of interest. An acceptor or strip solution (pyrophosphate) is placed on the other side of the PLM with the microelectrode array placed at 480 μm of the PLM. The analyte is transported by the carrier from the source solution to the strip solution. The originality of the new minicell is that accumulation in the strip solution is voltammetrically followed by the integrated microelectrode array in real time, and at low concentration level, using square‐wave anodic stripping voltammetry (SWASV). In order to protect the Hg microelectrodes from the adsorption of the hydrophobic carrier, the microelectrodes are embedded in a thin gel layer (280 μm) of 1.5% LGL agarose gel containing 10% of hydrophobic silica particles C18. The choice of optimum conditions is discussed in details in this article. Due to the very small effective strip volume of the new cell (less than 1 μL), high enrichment factor can be obtained (e.g., 330 for Pb) after 2 hours of accumulation. No deaeration of the solutions is required for SWASV measurements. Detection limits under these conditions are 2 pM and 75 pM for Pb and Cd, respectively, using a voltammetric deposition time of 5 min. In addition, no fouling effects were observed with natural water samples. 相似文献
93.
94.
Measurement of labile Cu in soil using stable isotope dilution and isotope ratio analysis by ICP-MS 总被引:1,自引:0,他引:1
Isotope dilution is a useful technique to measure the labile metal pool, which is the amount of metal in soil in rapid equilibrium (<7 days) with the soil solution. This is normally performed by equilibrating soil with a metal isotope, and sampling the labile metal pool by using an extraction (E value), or by growing plants (L value). For Cu, this procedure is problematic for E values, and impossible for L values, due to the short half-life of the 64Cu radioisotope (12.4 h), which makes access and handling very difficult. We therefore developed a technique using enriched 65Cu stable isotope and measurement of 63Cu/65Cu ratios by quadrupole inductively coupled plasma mass spectrometry (ICP-MS) to measure labile pools of Cu in soils using E value techniques. Mass spectral interferences in detection of 63Cu/65Cu ratios in soil extracts were found to be minimal. Isotope ratios determined by quadrupole ICP-MS compared well to those determined by high-resolution (magnetic sector) ICP-MS. E values determined using the stable isotope technique compared well to those determined using the radioisotope for both uncontaminated and Cu-contaminated soils. 相似文献
95.
报道了35例食道癌患者血清铜/锌比值及血清硒水平,结果发现食道癌患者血清铜/锌比值增加,血清硒水平下降,具有显著性差异(P〈0.001);同时提示随着食道癌分期增加,铜/锌比值进一步增加,血硒水平进一步下降,但无统计学差异。上述结果对临床诊断及观察病情变化有一定意义。 相似文献
96.
Yellow-orange single crystals of CuSbF6, were prepared by reacting Cu wire (∼10 mmol) with SbF5 (∼3 mmol) in liquid anhydrous hydrogen fluoride (aHF) and by reduction of Cu(SbF6)2 with Cu metal in aHF. CuSbF6 crystallizes rhombohedral at 296 K with the LiSbF6 structure type, with a = 530.4(4) pm, c = 1453(1) pm and Z = 3, space group R (no. 148). The structure is dominated by isolated layers of regular [SbF6]− octahedra and Cu+ cations.An attempt to prepare CuF by reaction between CuSbF6 and CsF in aHF at ∼190 K failed. Instead of CuF, a mixture of Cu and CuF2 was obtained. 相似文献
97.
一种低磁矩、大功率复合稀土石榴石铁氧体的工艺和性能研究 总被引:4,自引:0,他引:4
为满足低场区几百兆赫的超大功率器件的性能要求,以钇铁石榴石铁氧体为基础,制备了一种低磁矩复合稀土石榴石铁氧体YGd CaVInIG,研究了少量Mn3+替代Fe3+和预烧温度、烧结温度对铁氧体性能和结构的影响。实验表明,以少量Mn3+替代Fe3+可以提高铁氧体电阻率,降低磁损耗和介电损耗。Mn3+掺入量以x为0.04~0.06比较合适,铁氧体最佳予烧温度为1050℃,最佳烧结温度1350~1380℃,保温5h,氧气中烧结,其性能为:4πMs=500±10%kA·m-1,ΔH=5.25~5.55kA·m-1,TC>180℃,tgδe≤0.5×10-5,这种材料适合微波低频段器件性能要求。X射线衍射分析指出,掺Mn3+的YGdCaVInIG铁氧体相变完全,呈单相复合石榴石铁氧体,空间群为I230,点阵常数1.25057~1.25101nm,单胞分子数n为7.75~7.80。 相似文献
98.
An extraction‐spectrophotometric method for the determination of trace amounts of copper and cobalt based on their extraction into n‐pentanol with 0. carboxyphenylhydrazoethylacetoacetate (O.CPHEAA) was per formed. Copper was extracted from pH 6.0 – 8.0 and ionic strength 0.5 M – KCl. The maximum absorption of the extracted Cu(II) ‐ O.CPHEAA complex (1:1 & 1:2 species) occurs at 415 nm. The proposed method succeeded in as saying a concentration of 3–63 μg per 10 mL of n‐pentanol (? = 1.25 × 104L mol?1 cm?1). The method failed to ex tract cobalt ion into various organic sol vents over a pH range of 2–11. The suggested method is highly selective and sensitive according to a wide scheme of interference studied. Copper in some plant samples was accurately estimated using the suggested method. The obtained results and the results of the AAS method were consistent. The reproducibility test shows a relative standard deviation of 1%. Sandell sensitivity for A = 0.001 is 5 × 10?3 μg cm?2. 相似文献
99.
The effects of M3O3 (M = Al, Sc etc.) in Cu-ZnO-M2O3 catalysts on methanol synthesis at low pressure were studied with ESR, XPS and TPR spectroscopy. The results of ESR showed that the generation of monovalent cationic defects was because the valence state and electronic charge on the ZnO lattice lost their balance as M3+ doped into ZnO. The induced effect by Sc3+ is stronger than that by Al3+. The results of XPS and TPR indicated that the amount and stabilization of Cu+ on the surface of reduced copper-based catalyst and its catalytic activity were affected by the monovalent cationic defects on the surface of ZnO. 相似文献
100.
A. Venkataraman 《Journal of Thermal Analysis and Calorimetry》1996,46(1):219-224
Thermal techniques viz., TG/DTA/DSC methods have been employed in understanding the formation and decomposition of hydrogen ferrite phase (H-F) as a metastable intermediate in the conversion of -Fe2O3·xH2O, to -Fe2O3. Magnetic hysteresis measurements carried out at liquid N2 and at room temperature for the vacancy ordered -Fe2O3 and its H-F phase also supplement these studies.The author thanks prof. M.R. Udpa, IIT, Madras for supplying TG/DTA data on Stanton Redcroft Instrument and to the Head, Department of Chemistry, S.P. University, Vallabh Vidyanagar for providing the facilities. 相似文献