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1.
Single-wall carbon nano-tubes were used to modify the surface of a glassy carbon electrode (GC) and applied in the determination
of folic acid with voltammetry. The experiments demonstrated that the presence of a carbon nano-tube film on the electrode
greatly increased the reduction peak current of folic acid. Cyclic voltammetry (CV) and linear sweep voltammetry (LSV) were
used in a comparative investigation of the electrochemical reduction of folic acid with the film electrode. Effects of pH
on the peak current and the peak potential were studied in the pH range of 4.0–8.0 with Britton-Robinson buffer solution.
The reduction peak current was found to be linearly related to folic acid concentration over the range of 1 × 10−8 to 1 × 10−4 mol L−1 with a detection limit of 1 × 10−9 mol L−1 after 5 min accumulation. The film electrode provides an efficient way for eliminating interferences from some inorganic
and organic species in the solution. The high sensitivity, selectivity and stability of the film electrode demonstrate its
practical application from a simple and rapid determination of folic acid in tablets. 相似文献
2.
Determination of nitrobenzene by differential pulse voltammetry and its application in wastewater analysis 总被引:1,自引:0,他引:1
A new method for the determination of nitrobenzene (NB) by differential pulse voltammetry (DPV) based on an adsorptive stripping
technique was developed. Cyclic voltammetry (CV) was used in a comparative investigation into the electrochemical reduction
of NB at a glassy carbon electrode (GCE). With this electrode, the sharp peak of NB appeared at −0.71 V (vs. Ag/AgCl). The
experimental parameters were optimized. Studies on the effect of pH on the peak height and peak potential were carried out
over the pH range ca. 9.0–11.5 with sodium carbonate/sodium hydrogen carbonate buffer solution. A solution of pH 9.9 was chosen
as analytical medium. Cathodic peak currents were found to be linearly related to the concentration of NB over the range ca.
12.3–1.23 × 104 μg L−1 with relative standard deviations of ca. 3.26–6.75%. The detection limit of NB in water was 5.42 μg L−1. The interference of organic and inorganic species on the voltammetric response was also studied. The proposed method was
applied to the determination of NB in wastewater samples with an average recovery of ca. 95.9–102.4%. 相似文献
3.
Design of a field flow system for the on-line spectrophotometric determination of phosphate, nitrite and nitrate in natural water and wastewater 总被引:1,自引:0,他引:1
Ioannis A. Tsoulfanidis George Z. Tsogas Dimosthenis L. Giokas Athanasios G. Vlessidis 《Mikrochimica acta》2008,160(4):461-469
This study describes the design and optimisation of a field flow system for the in-situ collection and on-line determination
of phosphate, nitrate and nitrite by flow injection analysis-spectrophotometry. The method is based on the initial determination
of phosphate as its phosphoantimonylmolybdenum blue complex which is then oxidized on-line by nitrite and the decrease in
absorbance is monitored at 880 nm. Nitrate is determined as the difference between total and initial nitrite content in a
separate flow after reduction to nitrite in a cadmium reductive column. The calibration curves were linear in the range 0–2.00 mg L−1 P-phosphate, 0–10.00 mg L−1 nitrite and 0–7.00 mg L−1 nitrate with correlation coefficients of 0.9979, 0.9993 and 0.9995, respectively. The detection limits, calculated as 3S/N,
were 0.15 mg L−1 for P-phosphate, 0.17 mg L−1 for nitrite and 0.09 mg L−1 for nitrate. The reproducibility was below 3.0% (n = 7). Method validation in the analysis of natural water and wastewater samples revealed that it can efficiently be applied
to the determination of the target analytes, with recoveries in the range of 92–108%.
Correspondence: Athanasios G. Vlessidis, Laboratory of Analytical Chemistry, Department of Chemistry, University of Ioannina,
Ioannina 45110, Greece 相似文献
4.
A 3-amino-5-mercapto-1,2,4-triazole (TA) self-assembled monolayer-modified gold electrode (TA SAM/Au) is characterized by
X-ray photoelectron spectroscopy, A.C. impedance, cyclic voltammetry, chronoamperometry and chronocoulometry. The TA SAM/Au
exhibited good promotion of the electrochemical oxidation of dopamine. Some electrochemical parameters of dopamine such as
electron transfer number, exchange current density, standard heterogeneous rate constant, diffusion coefficient, etc., were
measured by different electrochemical methods. The peak currents of dopamine were linearly dependent on its concentration
in the range of 1.5 × 10−6–1.0 × 10−4 mol L−1, with a detection limit of 5.0 × 10−7 mol L−1. The oxidative peak potentials of dopamine and ascorbic acid were well separated at about 190 ± 10 mV in pH 2.0 BR buffers
at TA SAM/Au, the oxidation peak current increases approximately linearly with increasing concentration of both dopamine and
ascorbic acid in the concentration range of 9.98 × 10−6–4.54 × 10−4 mol L−1. It can be used for simultaneous determination of dopamine and ascorbic acid. 相似文献
5.
A novel L-cysteine film modified electrode has been fabricated by means of an electrochemical oxidation procedure, and it
was successfully applied to the electrochemical determination of acetaminophen. This method utilizes the electrooxidation
of amines to their analogous cation radicals to form a chemically stable covalent linkage between the nitrogen atom of the
amine and edge plane sites at the glassy carbon electrode surface. The electrochemical behaviour of acetaminophen at the film
electrode was investigated in 0.1 mol L−1 phosphate buffer (pH 6.20). It was found that the redox peak current of acetaminophen was enhanced greatly on the film electrode.
Linearity between the oxidation peak current and the acetaminophen concentration was obtained in the range of 1.0 × 10−4–2.0 × 10−7 mol L−1 with a detection limit of 5.0 × 10−8 mol L−1. For seven parallel detections of 1.0 × 10−5 mol L−1 acetaminophen, the relative standard deviation (RSD) was 1.46%, suggesting that the film electrode has excellent reproducibility.
Application to the determination of acetaminophen in drug tablets and human urine demonstrated that the film electrode has
good stability and high sensitivity. 相似文献
6.
Jun Yue Bai Liang Wang Hong Jing Wang Peng Fei Huang Yu Qing Zhao Sheng Di Fan 《Mikrochimica acta》2006,156(3-4):321-326
The electrochemical behavior of epinephrine (EP) at a mercaptoacetic acid (MAA) self-assembled monolayer modified gold electrode
was studied. The MAA/Au electrode is demonstrated to promote the electrochemical response of epinephrine by cyclic voltammetry.
The possible reaction mechanism is also discussed. The diffusion coefficient D of EP is 6.85 × 10−6 cm2 s−1. In 0.1 mol L−1 phosphate buffer (pH 7.20), a sensitive oxidation peak was observed at 0.177 V, and the peak current is proportional to the
concentration of EP in the range of 1.0 × 10−5–2.0 × 10−4 mol L−1 and 1.0 × 10−7–1.0 × 10−6 mol L−1. The detection limit is 5 × 10−8 mol L−1. The modified electrode is highly stable and can be applied to the determination of EP in practical injection samples. The
method is simple, quick, sensitive and accurate. 相似文献
7.
Jorge L. Guzmán Mar Leticia López Martínez Pedro L. López de Alba Jesús E. Castrejón Durán Víctor Cerdà Martín 《Mikrochimica acta》2006,153(3-4):139-144
1-Naphthylamine (NPA) is one of the main degradation products of pesticides derived from naphthalene, and a well-known bladder
carcinogen in men. The Griess assay is used for NPA determination because of its high sensitivity and selectivity. The azo
dye 4-(sulphophenylazo)-1-naphthylamine is formed, which shows a peak maximum at 540 nm. After optimizing multisyringe flow
injection analysis (MSFIA) parameters, the analytical characteristics of the method were obtained, with a working linear range
of 0.5 to 14 mg L−1, according to the equation A = 0.0738±0.0019 [NPA] + 0.0028 ± 0.0042, r = 0.9997. Values for RSD (%) and Erel (%) were calculated for the concentration levels of 0.5, 6 and 12 mg L−1; values obtained were 1.1, 0.4 and 0.3% for RSD and 0.8, 0.3 and 0.2% for Erel, respectively. LD was 0.01 mg L−1 and LQ was 0.04 mg L−1 NPA. The MSFIA procedure for the determination of NPA was applied to different water samples (well water, tap water, seawater,
and wastewater from the EDAR-1, Palma de Mallorca water treatment plant), with satisfactory results and a throughput of 90
samples per hour. 相似文献
8.
Soledad García Concepción Sánchez-Pedreño Isabel Albero Concepción García 《Mikrochimica acta》2001,136(1-2):67-71
Two flow injection (FI) spectrophotometric methods are proposed for the determination of diclofenac (DCF) or mefenamic acid
(MF) in bulk samples and pharmaceuticals. Both methods are based on the reaction of DCF or MF with potassium ferricyanide
in a sodium hydroxide medium. The absorbance of the orange products obtained is measured at 455 nm for DCF and 465 nm for
MF. The corresponding calibration graphs are linear over the range 0.20–20.0 mg L−1 for DCF and 1.00–100 mg L−1 for MF, while the limits of detection were 0.05 and 0.18 mg L−1, respectively.
Received March 27, 2000. Revision November 15, 2000. 相似文献
9.
Dimitrios V. Stergiou Spyros C. Karkabounas Panayotis G. Veltsistas Nicholaos P. Evmiridis Athanasios G. Vlessidis 《Mikrochimica acta》2007,158(1-2):59-64
A kinetic-potentiometric method is described for the quantitative assay of formaldehyde (HCHO) in pharmaceutical and industrial
preparations. It is based on the reaction of HCHO with (ethylenediamine)-Cu(II)-sulfate [Cu(CH2NH2)2(H2O)2] · SO4. The changes in potential, resulting from the release of the Cu(II) cations, are monitored with a Cu(II)-ion selective electrode.
The calibration curve for the HCHO is linear in the concentration range 50–250 mg L−1, with a limit of detection of 8.5 mg L−1. The method shows very good reproducibility with an RSD of 2.6% for successive injections (n = 5) of 150 mg L−1 HCHO primary solution, while it is interference free. The method was successfully tested in various industrial and pharmaceutical
preparations. 相似文献
10.
The fabrication and electrochemical characteristics of a penicillamine (PCA) self-assembled monolayer modified gold electrode
were investigated. The electrode can enhance the electrochemical response of uric acid (UA), and the electrochemical reaction
of UA on the PCA electrode has been studied by cyclic voltammetry and differential pulse voltammetry. Some electrochemical
parameters, such as diffusion coefficient, standard rate constant, electron transfer coefficient and proton transfer number
have been determined for the electrochemical behavior on the PCA self-assembled monolayer electrode. The electrode reaction
of UA is an irreversible process, which is controlled by the diffusion of UA with two electrons and two protons transfer at
the PCA/Au electrode. In phosphate buffer (pH 5.0), the peak current is proportional to the concentration of UA in the range
of 6.0 × 10−5–7.0 × 10−4 mol L−1 and 2.0 × 10−5–7.0 × 10−4 mol L−1 for the cyclic voltammetry and differential pulse voltammetry methods with the detection limits of 5.0 × 10−6 and 3.0 × 10−6 mol L−1, respectively. The method can be applied to determine UA concentration in real samples. 相似文献
11.
A sensitive adsorptive anodic stripping procedure for the determination of trace zirconium at a carbon paste electrode (CPE)
has been developed. The method is based on adsorptive accumulation of the Zr(IV)-alizarin red S(ARS) complex onto the surface
of the CPE, followed by oxidation of adsorbed species. The optimal experimental conditions include the use of 0.10 mol · L−1 ammonium acetate buffer (pH 4.3), ARS, an accumulation potential of 0.20 V (versus SCE), an accumulation time of 2 min, a
scan rate of 200 mV · s−1 and a second-order derivative linear scan mode. The oxidation peak for the complex appears at 0.69 V. The peak current is
proportional to the concentration of Zr(IV) over the range of 1.0 × 10−9–2.0 × 10−7 mol · L−1, and the detection limit is 3 × 10−10 mol · L−1 for a 2 min adsorption time. The relative standard deviations (n = 8) for 5.0 × 10−8 and 5.0 × 10−9 mol · L−1 Zr(IV) are 3.3 and 4.8%, respectively. The proposed method was applied to the determination of zirconium in ore samples with
satisfactory results. 相似文献
12.
Jeff E. Prest Sara J. Baldock Peter R. Fielden Nicholas J. Goddard Bernard J. Treves Brown 《Mikrochimica acta》2005,151(3-4):223-230
A new method allowing the simultaneous determination of arsenic(V), selenium(IV) and selenium(VI) using miniaturised isotachophoresis
has been developed. The method uses 0.02 M nitric acid buffered to pH 5.5 with histidine as the leading electrolyte. Using
a miniaturised poly(methyl methacrylate) chip device with an integrated conductivity detector, separations of model samples
and an industrial process stream sample were achieved. Limits of detection were calculated to be 0.85 mg L−1 for arsenic(V), 0.95 mg L−1 for selenium(IV) and 1.0 mg L−1 for selenium(VI). A method for the analysis of arsenic(III), using a glycolic acid based leading electrolyte to eliminate
carbonate interference is also presented. 相似文献
13.
The redox characteristics of the drug domperidone at a glassy-carbon electrode (GCE) in aqueous media were critically investigated
by differential-pulse voltammetry (DPV) and cyclic voltammetry (CV). In Britton–Robinson (BR) buffer of pH 2.6–10.3, an irreversible
and diffusion-controlled oxidation wave was developed. The dependence of the CV response of the developed anodic peak on the
sweep rate (ν) and on depolizer concentration was typical of an electrode-coupled chemical reaction mechanism (EC) in which an irreversible
first-order reaction is interposed between the charges. The values of the electron-transfer coefficient (α) involved in the rate-determining step calculated from the linear plots of E
p,a against ln (ν) in the pH range investigated were in the range 0.64 ± 0.05 confirming the irreversible nature of the oxidation peak. In
BR buffer of pH 7.6–8.4, a well defined oxidation wave was developed and the plot of peak current height of the DPV against
domperidone concentration at this peak potential was linear in the range 5.20 × 10−6 to 2.40 × 10−5 mol L−1 with lower limits of detection (LOD) and quantitation (LOQ) of 6.1 × 10−7 and 9.1 × 10−7 mol L−1, respectively. A relative standard deviation of 2.39% (n = 5) was obtained for 8.5 × 10−6 mol L−1 of the drug. These DPV procedures were successfully used for analysis of domperidone in the pure form (98.2 ± 3.1%), dosage
form (98.35 ± 2.9%), and in tap (97.0 ± 3.6%) and wastewater (95.0 ± 2.9%) samples. The method was validated by comparison
with standard titrimetric and HPLC methods. Acceptable error of less than 3.3 % was also achieved.
Figure In aqueous media at pH 7.6- 8.4, the DPV and cyclic voltammetry of the drug domperidone (I) at GCE showed an irreversible
and diffusion controlled oxidation wave. The values of the electron transfer coefficient (α) involved in the rate determining
step were found in the range 0.64± 0.05 confirming the irreversible nature of the peak. The analysis of the drug in pure form
and in wastewater samples was successfully achieved 相似文献
14.
A simple and selective method using ammonium pyrrolidinedithiocarbamate modified activated carbon (APDC-AC) as solid phase
extractant has been developed for speciation of As(III) in water samples. At pH 1.8–3.0, As(III) could be adsorbed quantitatively
by APDC-AC, and then eluted completely with 2.0 mL of 0.1 mol L−1 HNO3, while As(V) could almost not be retained at pH 1–7. Effects of acidity, sample flow rate, concentration of elution solution
and interfering ions on the recovery of As(III) have been systematically investigated. Under the optimal conditions, the adsorption
capacity of APDC-AC for As(III) is 7.3 mg g−1. The detection limit (3σ) of As(III) is 0.05 ng mL−1 for graphite furnace atomic absorption spectrometry (GFAAS) with enrichment factor of 50, and the relative standard deviation
(RSD) is 4.1% (n = 9, C = 5 ng mL−1). The method has been applied to the determination of trace As(III) in water, and the recoveries of As(III) are 100 ± 10%.
Correspondence: Yiwei Wu, Department of Chemistry and Environmental Engineering, Hubei Normal University, Huangshi 435002,
P.R. China 相似文献
15.
Citric acid was thermochemically esterified onto defatted cotton fibre to produce a carboxyl cotton chelator (CCC), which
had been used for extraction of copper prior to its determination by flame atomic absorption spectrometry. The extraction
of copper has been studied under both batch and column methods. Quantitative extraction of copper was achieved in the pH range
4–7. The time needed to extract each sample was less than 30 min by the batch method. The copper extraction capacity of CCC
was found to be 22.7 mg g−1 at optimal pH value. The elution was quantitative with 1 mol L−1 hydrochloric acid. The feasible flow rate of copper-containing solution for quantitative extraction onto the column packed
with CCC was 0.5–4.0 mL min−1, whereas for elution it was less than 1.5 mL min−1. A 100-fold extraction factor could be achieved under the optimal column conditions. The tolerance limits for common metal
ions on the extraction of copper and the time of column reuse were investigated. The proposed method has been successfully
applied for extraction and determination of copper in industrial wastewater and natural water samples. 相似文献
16.
CeO2 nanoparticles approximately 12 nm in size were synthesized and subsequently characterized by XRD, TEM and UV-vis spectroscopy.
Then, a gold electrode modified with CeO2 nanoparticles was constructed and characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV).
The modified electrode demonstrated strong catalytic effects with high stability towards electrochemical oxidation of rutin.
The anodic peak currents (measured by differential pulse voltammetry) increased linearly with the concentration of rutin in
the range of 5.0 × 10−7–5.0 × 10−4 mol · L−1. The detection limit (S/N = 3) was 2.0 × 10−7 mol · L−1. The relative standard deviation (RSD) of 8 successive scans was 3.7% for 5.0 × 10−6 mol · L−1 rutin. The method showed excellent sensitivity and stability, and the determination of rutin in tablets was satisfactory. 相似文献
17.
Erdal Kendüzler Özcan Yalçınkaya Sıtkı Baytak Ali Rehber Türker 《Mikrochimica acta》2008,160(4):389-395
The preconcentration of chromium(III) by solid phase extraction and its determination from aqueous solutions by flame atomic
absorption spectrometry (FAAS) is investigated by applying an experimental design. The optimization of the preconcentration
variables such as pH of the sample solution, flow rate of the sample solution and concentration of elution solution was carried
out using 23 full factorial design. The most important parameter affecting the preconcentration of chromium is the concentration of eluent.
In the established experimental conditions, chromium can be determined with a relative standard deviation of 2.0% (N = 7) for a chromium concentration of 100 μg L−1. The detection limit for chromium was 1 μg L−1 (N = 20). The adsorption capacity of Amberlyst 36 is found to be 90.9 mg g−1 for chromium. Effect of other ions on the procedure was also evaluated. The method was validated by the analysis of certified
reference materials (tea leaves GBW 07605 and fish tissue IAEA-407). The method was applied to the determination of chromium
in waste water, dam water, carrot, parsley and lettuce.
Correspondence: Ali Rehber Türker, Department of Chemistry, Faculty of Science and Arts, Gazi University, TR-06500 Ankara,
Turkey 相似文献
18.
A new adsorbent is proposed for the solid-phase extraction of phenol and 1-naphthol from polluted water. The adsorbent (TX-SiO2) is an organosilica composite made from a bifunctional immobilized layer comprising a major fraction (91%) of hydrophilic
diol groups and minor fraction (9%) of the amphiphilic long-chain nonionic surfactant Triton X-100 (polyoxyethylated isooctylphenol)
(TX). Under static conditions phenol was quantitatively extracted onto TX-SiO2 in the form of a 4-nitrophenylazophenolate ion associate with cetyltrimethylammonium bromide. The capacity of TX-SiO2 for phenol is 2.4 mg g−1 with distribution coefficients up to 3.4 × 104 mL g−1; corresponding data for 1-naphthol are 1.5 mg g−1 and 3 × 103 mL g−1. The distribution coefficient does not change significantly for solution volumes of 0.025–0.5 L and adsorbent mass less than
0.03 g; 1–90 μg analyte can be easily eluted by 1–3 mL acetonitrile with an overall recovery of 98.2% and 78.3% for phenol
and 1-naphthol, respectively. Linear correlation between acetonitrile solution absorbance (A
540) and phenol concentration (C) in water was found according to the equation A
540 = (6 ± 1) × 10−2 + (0.9 ± 0.1)C (μmol L−1) with a detection range from 1 × 10−8 mol L−1 (0.9 μL g−1) to 2 × 10−7 mol L−1 (19 μL g−1), a limit of quantification of 1 μL g−1 (preconcentration factor 125), correlation coefficient of 0.936, and relative standard deviation of 2.5%. A solid-phase colorimetric
method was developed for quantitative determination of 1-naphthol on adsorbent phase using scanner technology and RGB numerical
analysis. The detection limit of 1-naphthol with this method is 6 μL g−1 while the quantification limit is 20 μL g−1. A test system was developed for naked eye monitoring of 1-naphthol impurities in water. The proposed test kit allows one
to observe changes in the adsorbent color when 1-naphthol concentration in water is 0.08–3.2 mL g−1. 相似文献
19.
A novel electrochemical sensor for methyl parathion based on silicate– cetyltrimethylammonium bromide nanocomposite film has
been fabricated by electro-assisted deposition onto glassy carbon electrode in one-step via an electrochemical modulation
of pH at the electrode/solution interface to promote controlled gelification of tetraethylorthosilicate sol, and was characterized
with scanning electron microscopy, X-ray diffraction, and electrochemical impedance spectroscopy. The electrochemical sensing
of methyl parathion on the film-modified electrode was investigated applying cyclic voltammetry and square wave voltammetry.
Compared to the unmodified electrode, the shapes of the redox peaks were improved and the peak currents significantly increased.
Experimental parameters such as deposition time, pH value, and accumulation conditions have been optimized. A linear relationship
between the peak current and methyl parathion concentration was obtained in the range from 1.0 × 10−7 to 1.0 × 10−4 mol L−1 with a detection limit of 1.04 × 10 −8 mol L−1 (S/N = 3) after accumulation at 0 V for 120 s. The film electrode shows great promise for determination of methyl parathion in
real samples.
相似文献
20.
Qiong He Tian Gan Dongyun Zheng ShengShui Hu 《Journal of Solid State Electrochemistry》2010,14(6):1057-1064
Simple and sensitive electrochemical method for the determination of nitrite, based on a nano-alumina-modified glassy carbon
electrode (GCE), is described. Nitrite yields a well-defined oxidation peak whose potential is 0.74 V at the nano-alumina-coated
GCE in 0.1 mol L−1 phosphate buffer (pH 5.0). Compared with bare GCE, the nano-alumina-modified GCE has evident catalytic effect towards the
oxidation of nitrite, and its peak current can be significantly enhanced. Some of the experimental parameters were optimized
for the determination of nitrite. The oxidation peak current was proportional to nitrite concentration in the range of 5.0 × 10−8–1.1 × 10−3 mol L−1, and a detection limit of 1.0 × 10−8 mol L−1 was obtained. This method has been successfully used to the determination of nitrite in sausage sample. Furthermore, results
obtained by the method have been compared with spectrophotometric method. 相似文献