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101.
de Toledo RA Santos MC Cavalheiro ET Mazo LH 《Analytical and bioanalytical chemistry》2005,381(6):1161-1166
This work describes an electroanalytical investigation of dopamine using cyclic voltammetry (CV) and the graphite–polyurethane composite electrode (GPU). In CV studies, well-defined redox peaks characterize the oxidation process at the GPU electrode, which is indicative of electrocatalytic effects associated with active sites on the GPU electrode surface. A new analytical methodology was developed using the GPU electrode and square wave voltammetry (SWV) in BR buffer solution (0.1 mol L–1; pH 7.4). Analytical curves were constructed under optimized conditions (f=60s–1, Ea=50 mV, EI=2 mV) and detection and quantification limits of 6.4×10–8 mol L–1 (12.1 g L–1) and 5.2×10–6 mol L–1 (0.9 mg L–1), respectively, were achieved. The precision of the method was checked by performing ten successive measurements for a 9.9×10–6 mol L–1 dopamine solution. For intra-assay and inter-assay precisions, the relative standard deviations were 1.9 and 2.3%, respectively. In order to evaluate the developed methodology, the determination of dopamine was performed with good sensitivity and selectivity, without the interference of ascorbic acid in synthetic cerebrospinal fluid, which indicates that the new methodology enables reliable analysis of dopamine. 相似文献
102.
A sensitive ion-pair liquid-liquid extraction-spectrophotometric method has been developed for the determination of copper, palladium, iron and cobalt, based on the formation of metal complexes with 1-nitroso-2-naphthol-6-sulphonic acid or 2-nitroso-1-naphthol-6-sulphonic acid as primary ligand, and zephiramine as counter-ion. The coloured metal complexes obtained over different pH ranges are easily and quantitatively extracted into dichloromethane. The method has been tested with samples containing known amounts of copper, palladium, iron and cobalt in ultrapure water. The reagents provide a sensitive spectrophotometric method for determining these metals. 相似文献
103.
Ion-imprinting concept and polysaccharide incorporated sol-gel process were applied to the preparation of a new silica-supported organic-inorganic hybrid sorbent for selective separation of Cd(II) from aqueous solution. In the prepared shell/core composite sorbent, covalently surface coating on the supporting silica gel was achieved by using a Cd(II)-imprinting sol-gel process starting from an inorganic precursor, γ-glycidoxypropyltrimethoxysiloxane (GPTMS), and a functional biopolymer, chitosan (CS). The sorbent was prepared through self-hydrolysis of GPTMS, self-condensation and co-condensation of silanol groups (Si-OH) from siloxane and silica gel surface, in combination with in situ covalent cross-linking of CS with partial amine shielded by Cd(II) complexation. Extraction of the imprinting molecules left a predetermined arrangement of ligands and tailored binding pockets for Cd(II). The prepared sorbent was characterized by using X-ray energy dispersion spectroscopy (EDX), X-ray diffraction (XRD), and scanning electron microscopy (SEM). Batch experiments were conducted to study the sorption performance by removal of Cd(II) when present singly or in binary system, an aqueous Cd(II) and Zn(II) mixture. The ion-imprinted composite sorbent offered a fast kinetics for the sorption of Cd(II) and the maximum capacity was 1.14 mmol g−1. The uptake capacity of the imprinted sorbent and the selectivity coefficient were much higher than that of the non-imprinted sorbent. The imprinted sorbent exhibited high reusability. The prepared functional sorbent was shown to be promising for the preconcentration of cadmium in environmental and biological samples. 相似文献
104.
Hydrogen peroxide in basic media is proposed as a means for dissolving whole blood samples to be analyzed by electrothermal atomization atomic absorption spectrometry, ET AAS. Approximately 2 g of the whole blood sample were directly weighed in a 150 mL volumetric flask; 3 mL of a NaOH 0.2 mol L−1 solution, two drops of 1-octanol, as an antifoaming agent, and 1 mL of 30% volume hydrogen peroxide were added to the flask to promote oxidation. The solution was then manually shaken and after approximately three minutes of shaking, a clear solution, with no apparent suspended solids or greasy layers, was obtained. Distilled-deionized water was used to complete the volume. Ten μL of the resulting solution along with 10 μL of a solution containing 5000 mg L−1 of NH4H2PO4 and 300 mg L−1 of Mg(NO3)2 as a modifier, were injected into transversely heated graphite tubes for lead determination. Both aqueous standards and standard addition calibration curves produced results not significantly different at a 95% confidence limit level. Accuracy of the measurements was assessed by analysis of the IAEA A-13 (concentration of trace and minor elements in freeze dried animal blood) standard reference material containing 0.18 mg L−1 lead on a dry basis and by means of recovery tests. Analysis of the IAEA A-13 standard produced 0.17 ± 0.02 mg L−1 lead on a dry basis; recovery tests afforded values from 95 to 105%. Ten consecutive measurements of a 5 ppb lead solution gave a characteristic mass of 47.2 pg and a (3S) detection limit of 1.77 μg L−1 Pb. Results obtained from analysis of whole blood samples of volunteer donors covered a lead concentration range between 8 and 21 μg L−1 with a mean value of 11.9 ± 4.7 μg L−1. 相似文献
105.
Low-temperature synthesis of allyl dimethylamine by selective heating under microwave irradiation used for water treatment 总被引:1,自引:0,他引:1
Low-temperature synthesis of allyl dimethylamine (ADA) by selective heating under microwave irradiation (MI) used for water treatment is investigated. The effect of MI, ultrasound irradiation (UI) and conventional heating on yield of ADA, reaction time and the flocculation efficiency of polydiallyl dimethylammunion chloride (PDADMAC) prepared form ADA were studied. The results show that by selective heating at low temperature, MI not only increases yield of ADA and reduces reaction time, but also greatly enhances the flocculation efficiency of PDADMAC. 相似文献
106.
107.
二氧化碳和氧气的快速电化学方法联合测定 总被引:4,自引:0,他引:4
根据O2和CO2在二甲亚砜(DMSO)介质中Pt电极上的伏安特性,采用微电极并结构计算机控制的电位调制技术,建立了快速联合测定CO2和O2的调制电位脉冲库仑法和调制电位脉冲电流法,取得了满意的结果。一次测量时间快达40ms。CO2检测范围0 ̄10%(体积百分比);O2检测范围不受限制。通过编程设计特定的调制电位-时间波形,可保持连续检测的长期稳定性。 相似文献
108.
Guido Kickelbick Dieter Rutzinger Thomas Gallauner 《Monatshefte für Chemie / Chemical Monthly》2002,133(8):1157-1164
Summary. Hexadentate ligands were formed by the reaction of primary dimethylaminoethyl- or methoxyethylamines with formaldehyde. The
resulting N, N′, N″-functionalized hexahydro-1,3,5-triazines contain pending amino or ether functionalities which are able to coordinate to
metals in addition to the ring nitrogen atoms. Both ligands were reacted with CuBr, and novel tricopper clusters were isolated
and characterized by X-ray structure analysis. In these compounds a ring nitrogen atom, the pending amino or ether functionality,
and two bridging bromine atoms coordinate each of the copper atoms.
Received January 22, 2002; accepted (revised) March 22, 2002 相似文献
109.
Kubo T Hosoya K Nomachi M Tanaka N Kaya K 《Analytical and bioanalytical chemistry》2005,382(7):1698-1701
A molecularly imprinted polymer was prepared using a water-soluble crosslinking agent. An ionic complex was utilized as the assembly for the template molecule and the functional monomer, and water as porogenic solvent during preparation of the imprinted polymer. The results of chromatographic evaluations for the prepared polymer suggested that the polymer had much lower hydrophobicity compared with usual octadecyl group bonded silica or the usual molecular imprinted polymer prepared from ethyleneglycol dimethacrylate, and the selective recognition ability for template molecule in the completely aqueous condition. 相似文献
110.
分散法制备的CuCl/MCM-41上C3H6选择催化还原NO反应的研究 总被引:3,自引:0,他引:3
研究了由分散法制备的两种CuCl/MCM-41催化剂上丙烯在过量氧存在下选择催化还原NO反应, 发现所制备的CuCl/AlMCM-41催化剂的反应活性明显高于CuCl/SiMCM-41. XRD, IR, TPR及ESR的研究结果表明, CuCl/AlMCM-41催化剂上的主要活性中心是与骨架铝配位的铜离子(Cu2+/Cu+). 相似文献