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Trace Determination (trace + determination)
Selected AbstractsTrace Determination of Chromium by Square-Wave Adsorptive Stripping Voltammetry on Bismuth Film ElectrodesELECTROANALYSIS, Issue 21 2004Eleni Chatzitheodorou Abstract This works reports the use of adsorptive stripping voltammetry (AdSV) for the trace determination of chromium on a rotating-disk bismuth-film electrode (BFE). During the reductive accumulation step, all the chromium species in the sample were reduced to Cr(III) which was complexed with cupferron and the complex was accumulated by adsorption on the surface of a preplated BFE. The stripping step was carried out by using a square-wave (SW) potential-time voltammetric signal. Electrochemical cleaning of the bismuth film was employed, enabling the same bismuth film to be used for a series of measurements in the presence of dissolved oxygen. The experimental variables as well as potential interferences were investigated and the figures of merit of the method were established. Using the selected conditions, the 3, limit of detection for chromium was 100,ng L,1 (for 120,s of preconcentration) and the relative standard deviation was 3.6% at the 2,,g L,1 level (n=8). Finally, the method was applied to the determination of chromium in real samples with satisfactory results. [source] Trace determination of arsenic species by capillary electrophoresis with direct UV detection using sensitivity enhancement by counter- or co-electroosmotic flow stacking and a high-sensitivity cellELECTROPHORESIS, Issue 12-13 2003Baoguo Sun Abstract Stacking techniques used independently and also with a high-sensitivity cell (HSC) were employed to optimise sensitivity and detection limits in the direct photometric detection of the following eight arsenic species by capillary zone electrophoresis (CZE): arsenite, arsenate, monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), 4-hydroxy-3-nitrophenylarsonic acid (Roxarsone), p -aminophenylarsonic acid (p -ASA), 4-nitrophenylarsonic acid (4-NPAA), and phenylarsonic acid (PAA) (target analytes). The stacking mechanisms, optimised stacking and separation conditions, and concentration sensitivity enhancement factors were discussed and compared for (i) normal stacking mode (NSM, sometimes also referred to as field-amplified stacking) in an uncoated fused-silica capillary in the counter-electroosmotic flow (EOF) mode, (ii) large-volume sample stacking (LVSS) with polarity switching, and (iii) the less often applied stacking method of co-EOF NSM stacking with EOF reversal using a poly(diallydimethylammonium chloride) (PDDAC)-coated capillary. The optimal injection volumes were 7.4, 60 and 17.2% of the total capillary volume, for the above three methods, respectively. LVSS with polarity switching gave the lowest limit of detection (LOD). The use of the HSC further reduced the LOD of each target analytes by a factor of 5,8 times. By combining LVSS and HSC, LODs of the target analytes could be reduced by a factor of 218,311, to 5.61, 9.15, 11.1, and 17.1 ,g/L for As(III), DMA, MMA, and As(V), respectively. The method was demonstrated to be applicable to the determination of the target analytes in tap water and lake water, with recoveries in the range of 89.4,103.3%. [source] Determination of Trace Amounts of Copper in Tap Water Samples with a Calix[4]arene Modified Carbon Paste Electrode by Differential Pulse Anodic Stripping VoltammetryELECTROANALYSIS, Issue 10 2007Çelik Canpolat Abstract A calix[4]arene modified carbon paste electrode was used for trace determination of copper. The study of the preconcentration of copper as well as the other heavy metal ions at the modified electrode, with subsequent measurement by differential pulse anodic stripping voltammetry (DPASV), indicates the efficient open-circuit accumulation of the analytes onto the electrode. Many parameters such as the composition of the paste, pH, preconcentration time and stirring rate influence the response of the measurement. The procedure was optimized for copper determination. For a 10-minute preconcentration time at pH,6.5,7.5, the detection limit (LOD) was 1.1,,g L,1. The optimized method was successfully applied to the determination of copper in tap water sample by means of standard addition procedure. The copper content of the sample was comparable with the result obtained with AAS method. [source] Trace Determination of Chromium by Square-Wave Adsorptive Stripping Voltammetry on Bismuth Film ElectrodesELECTROANALYSIS, Issue 21 2004Eleni Chatzitheodorou Abstract This works reports the use of adsorptive stripping voltammetry (AdSV) for the trace determination of chromium on a rotating-disk bismuth-film electrode (BFE). During the reductive accumulation step, all the chromium species in the sample were reduced to Cr(III) which was complexed with cupferron and the complex was accumulated by adsorption on the surface of a preplated BFE. The stripping step was carried out by using a square-wave (SW) potential-time voltammetric signal. Electrochemical cleaning of the bismuth film was employed, enabling the same bismuth film to be used for a series of measurements in the presence of dissolved oxygen. The experimental variables as well as potential interferences were investigated and the figures of merit of the method were established. Using the selected conditions, the 3, limit of detection for chromium was 100,ng L,1 (for 120,s of preconcentration) and the relative standard deviation was 3.6% at the 2,,g L,1 level (n=8). Finally, the method was applied to the determination of chromium in real samples with satisfactory results. [source] Selective Electrochemical Analysis of Various Metal Ions at an EDTA Bonded Conducting Polymer Modified ElectrodeELECTROANALYSIS, Issue 16 2004Aminur Rahman Abstract An EDTA-bonded conducting polymer modified electrode was prepared and characterized by FT-IR. The modified electrode was used for the selective electrochemical analysis of various trace metal ions such as, Cu(II), Hg(II), Pb(II), Co(II), Ni(II), Fe(II), Cd(II), and Zn(II) at the different pHs by linear sweep and square wave voltammetry. Dynamic ranges were obtained using square wave voltammetry from 0.1,,M to 10.0,,M for Co(II), Ni(II), Cd(II), Fe(II), and Zn(II) and 0.5,nM to 20,nM for Cu(II), Hg(II), and Pb(II) after 10,min of preconcentration. The detection limits were determined to be 0.1,nM, 0.3,nM, 0.4,nM, 50.0,nM, 60.0,nM, 65.0,nM, 80.0,nM, and 90.0,nM for Cu(II), Hg(II), Pb(II), Co(II), Ni(II), Cd(II), Fe(II), and Zn(II), respectively. The technique offers an excellent way for the selective trace determination of various heavy metal ions in a solution. [source] A Study of the Determination of Cu(II) by Anodic Stripping Voltammetry on a Novel Nylon/Carbon Fiber ElectrodeELECTROANALYSIS, Issue 7 2004A. Mylonakis Abstract In this work we report a new electrode material formed by injection-moulding of a conducting polymer consisting of carbon fibers in a Nylon matrix. This material is highly conductive, inexpensive, easy to mould in different shapes and requires minimal pretreatment. The electrode was tested as a mercury-free sensor for the trace determination of Cu(II) by anodic stripping voltammetry (ASV). The deposition and stripping behavior of copper on the conducting material was initially studied by cyclic voltammetry and the chemical and instrumental parameters of the determination were investigated. The electrode has been shown to be suitable for the determination of Cu(II) in the range 8,,g L,1 to 30,mg,L,1 (with deposition times ranging from 30,s to 10,min) with a relative standard deviation of 2.2% (at the 0.5,mg,L,1 level) and a limit of detection of 8,,g L,1 Cu(II) for 10,min of accumulation (at a S/N ratio of 5). The electrode was, finally, applied to the determination of copper in tap-water, pharmaceutical tablets and bovine serum with recoveries of 97.4, 94.9 and 93.4%, respectively [source] Highly sensitive determination of tetrabromobisphenol A and bisphenol A in environmental water samples by solid-phase extraction and liquid chromatography-tandem mass spectrometryJOURNAL OF SEPARATION SCIENCE, JSS, Issue 11 2010Ru-Song Zhao Abstract Using bamboo-activated charcoal as SPE adsorbent, a novel SPE method was developed for the sensitive determination of tetrabromobisphenol A and bisphenol A in environmental water samples by rapid-resolution LC-ESI-MS/MS. Important parameters influencing extraction efficiency, including type of eluent, eluent volume, sample pH, volume and flow rate, were investigated and optimized. Under the optimal extraction conditions (eluent: 8,mL methanol, pH: 7; flow rate: 4,mL/min; sample volume: 100,mL), low LODs (0.01,0.02,ng/mL), good repeatability (6.2,8.3%) and wide linearity range (0.10,10,ng/mL) were obtained. Satisfied results were achieved when the proposed method was applied to determine the two target compounds in real-world environmental water samples with spiked recoveries over the range of 80.5,119.8%. All these facts indicate that trace determination of tetrabromobisphenol A and bisphenol A in real-world environmental water samples can be realized by bamboo-activated charcoal SPE-rapid resolution-LC-ESI-MS/MS. [source] Determination of the pesticides considered as endocrine-disrupting compounds (EDCs) by solid-phase extraction followed by gas chromatography with electron capture and mass spectrometric detectionJOURNAL OF SEPARATION SCIENCE, JSS, Issue 12 2007Vasiliki I. Valsamaki Abstract An SPE method followed by GC-electron capture detection (ECD) with confirmation by MS for the trace determination of four pesticides considered as endocrine-disrupting compounds (EDCs) in natural waters and sediments has been developed. Target analytes, fenarimol, fenvalerate, pendimethalin, and vinclozolin, belong to different chemical groups and are used mainly in agriculture. In the present study, analysis employs an offline SPE step for the extraction of the target analytes from natural waters. Sonication and subsequent SPE clean-up was used for extraction and purification of the sediment samples which were finally treated with activated copper powder. The type of SPE disk, eluents as well as solution parameters including pH value, and concentrations of salts and humic substances were examined for the efficiency of the method. The recoveries of all pesticides were in relatively high levels, ranging from 75 to 97% for waters and 71 to 84% for sediment samples. Both methods were applied to real water and sediment samples and the presence of the tested compounds was investigated. [source] Validation of a quantitative assay using GC/MS for trace determination of free and conjugated estrogens in environmental water samplesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 1-2 2003Asmaa Mouatassim-Souali Abstract It has been shown that sewage effluent can discharge human hormones and pharmaceuticals, particularly estrogens and synthetic chemicals, which are able to disrupt animal and human endocrine systems into surface waters. Since many surface waters receive sewage effluent and are subsequently used to produce drinking water, it is of principal interest to assess their contamination level and thereby their possible public health and environmental impact. To date, no data concerning the occurrence of estrogens present in the French aquatic environment are available. We therefore developed and validated an analytical procedure, which allows simultaneous quantitative determination of three natural estrogens, 17,-estradiol, estriol, and estrone and one of the synthetic estrogens most widely used in contraception, ethinylestradiol, in water. Water samples are extracted using solid-phase extraction (SPE) and then separated by gas-chromatography coupled with mass spectrometric detection. Under our conditions, detection limits of estrogens reached the pg range of injected sample, i. e. less than 0.1 ng L,1. Conjugated estrogens were also investigated using the same procedure as described above but with a enzymatic hydrolysis preliminary step before extraction. The analysis of samples collected from four wastewater treatment plants and from surface water showed significant concentrations of estrogens ranging from 2 to 18 ng L,1 and from 0.5 to 3 ng L,1, respectively. Furthermore, no estrogen conjugated forms were detected in the water samples. [source] | ||||||||||