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1.
Poly‐aniline (PAn) film can be oxidized by contacting oxygen in an electron‐transfer reaction and its redox state, for instance the open circuit potential and the dielectric constant, is quantitatively related to oxygen concentration. This feature may contribute to an improved application of dissolved oxygen (DO) detection with the combined optical and electrochemical sensor. In this paper, PAn is used as a sensing surface to detect DO by the combination sensor composed of electrochemistry and total internal reflection imaging ellipsometry (EC‐TIRIE). Results demonstrate that both optical and electrical signals show a logarithmic correlation with DO concentration (0–20 ppm). Compared with the results obtained only with the gold surface, both the optical and electrical signals of the EC‐TIRIE sensor for DO detection are amplified with the PAn modified gold surface.  相似文献   

2.
This communication describes the determination of an essential amino acid, L ‐methionine (L ‐Met) in the presence of important interferents, ascorbic acid (AA) and uric acid (UA) at physiological pH using a glassy carbon electrode modified with an electropolymerized film of 3‐amino‐5‐mercapto‐1,2,4‐triazole (p‐AMTa). The bare glassy carbon electrode fails to show a voltammetric signal for L ‐Met in the presence of AA and UA at pH 7.2. However, the p‐AMTa electrode separates the voltammetric signals of AA, UA and L ‐Met with pronounced oxidation currents. The amperometric current of L ‐Met was increased linearly from 1.0×10?7 to 1×10?4 M and the detection limit was found to be 4.12×10?10 M (S/N=3).  相似文献   

3.
Layer‐by‐layer assemblies consisting of alternating layers of nitrilotris(methylene)triphosphonic acid (NTMP), a polyfunctional corrosion inhibitor, and zirconium(IV) were prepared on alumina. In particular, a nine‐layer (NTMP/Zr(IV))4NTMP stack could be constructed at room temperature, which showed a steady increase in film thickness throughout its growth by spectroscopic ellipsometry up to a final thickness of 1.79 ± 0.04 nm. At higher temperature (70 °C), even a two‐layer NTMP/Zr(IV) assembly could not be prepared because of etching of the alumina substrate by the heated Zr(IV) solution. XPS characterization of the layer‐by‐layer assembly showed a saw tooth pattern in the nitrogen, phosphorus, and zirconium signals, where the modest increases and decreases in these signals corresponded to the expected deposition and perhaps removal of NTMP and Zr(IV). Time‐of‐flight secondary ion mass spectrometry (ToF‐SIMS) confirmed the attachment of the NTMP molecule to the surface through PO?, PO2?, PO3?, and CN? signals. Increasing attenuation of the Al signal from the substrate after deposition of each layer was observed by both XPS and ToF‐SIMS. Essentially complete etching of the alumina by the heated Zr(IV) solution was confirmed by spectroscopic ellipsometry, XPS, and ToF‐SIMS. Atomic force microscopy revealed that all the films were smooth with Rq roughness values less than 0.5 nm. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

4.
In this article, a soluble poly[2‐methoxy‐5‐(3′‐methyl)butoxy]‐p‐phenylene vinylene (MMB‐PPV) was synthesized by dehydrochlorination reaction and the MMB‐PPV film was implanted by nitrogen ions (N+) with the ion dose and energy in the range of 3.8 × 1015 to 9.6 × 1016 ions/cm2 and 15–35 keV, respectively. The surface conductivity, optical absorption, optical band gap (Eg) of modified MMB‐PPV film were studied, and the third‐order nonlinear optical susceptibility (χ(3)) as well as its environmental stability of modified MMB‐PPV film were also measured by degenerate four‐wave mixing system. The results showed that the surface conductivity of MMB‐PPV film was up to 3.2 × 10?2 S when ion implantation was performed with the energy of 35 keV at an ion dose of 9.6 × 1016 ions/cm2, which was seven order of magnitude higher than that of the pristine film. UV‐Vis absorption spectra demonstrated that the optical absorption of MMB‐PPV film was enhanced gradually in the visible region followed by a red shift of optical absorption threshold and the Eg value was reduced from 2.12 eV to 1.59 eV with the increase of ion dose and energy. The maximum χ(3) value of 2.45 × 10?8 esu for modified MMB‐PPV film was obtained with the ion energy of 20 keV at an ion dose of 3.8 × 1016 ions/cm2, which was almost 33 times larger than that for pristine film. In comparison to the reduction of 17% in the χ(3) value of pristine MMB‐PPV film, the maximum χ(3) value of 2.45 × 10?8 esu for modified MMB‐PPV film decreased by over 5.3% when they had been exposed under the same ambient conditions for 90 days. © 2010 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48: 2072–2077, 2010  相似文献   

5.
《Electroanalysis》2002,14(24):1691-1698
Three different recently synthesized aza‐thioether crowns containing a 1,10‐phenanthroline sub‐unit (L1–L3) and a corresponding acyclic ligand (L4) were studied to characterize their abilities as silver ion ionophores in PVC‐membrane electrodes. Novel conventional silver‐selective electrodes with internal reference solution (CONISE) and coated graphite‐solid contact electrodes (SCISE) were prepared based on one of the 15‐membered crowns containing two donating S atoms and two phenanthroline‐N atoms (L1). The electrodes reveal a Nernstian behavior over wide Ag+ ion concentration ranges (1.0×10?5?1.0×10?1 M for CONISE and 5.0×10?8?4.0×10?2 M for SCISE) and very low limits of detection (8.0×10?6 M for CONISE and 3.0×10?8 M for SCISE). The potentiometric response is independent from pH of the solution in the pH range 3.0–8.0. The electrodes manifest advantages of low resistance, very fast response and, most importantly, good selectivities relative to a wide variety of other cations. The electrodes can be used for at least 2 months (for CONISE) and 4 months for (SCISE) without any appreciable divergence in potentials. The electrodes were used as an indicator electrode in the potentiometric titration of Ag+ ion and in the determination of silver in photographic emulsions and in radiographic and photographic films.  相似文献   

6.
A novel amperometric sensor based on a rigid graphite‐epoxy composite of which composition is near to the percolation is reported. The electrochemical response of the novel transducer material was evaluated in terms of reproducibility of the fabrication process and reproducibility and repeatability of the analytical signal. The signal to noise ratio was improved. atomic force microscopy (AFM) technique was used to obtain qualitatively information. Amperometric detection of chlorine in water was carried on at a set potential of ?250 mV vs. Ag/AgCl. The developed flow injection analysis (FIA) system responded linearly to chlorine concentration between 0.15 mg L?1 and 4 mg L?1with a sensitivity of ?0.20 μA L mg?1. The proposed system was applied to real samples from swimming‐pool water. No significant difference was observed regarding the standard method.  相似文献   

7.
《Electroanalysis》2003,15(9):803-811
Ru(II) tris‐bipyridine based ECL sensors were produced by embedding the complex inside silica glass thin films deposited via a sol‐gel dipping procedure on K‐glass conducing substrates. Films were prepared starting from a pre‐hydrolyzed ethanolic solution of Si(OC2H5)4 and Ru(bpy)3Cl2. Transparent, crack‐free and homogeneous reddish silica layers, having a thickness of 200±20 nm, were obtained. The films, either deposited at room temperature or thermally annealed at 100, 200 and 300 °C for 30 h, were structurally and chemically characterized. Ru(bpy)3Cl2 thermal stability was previously checked by thermogravimetric analysis (TGA). The films were investigated by X‐Ray photoelectron spectroscopy (XPS), secondary ion mass spectrometry (SIMS) and UV‐vis spectroscopy. XPS in‐depth profiles revealed a homogeneous distribution of the ruthenium complex inside the silica thin layers. SIMS data suggested that the embedded Ru(bpy)3Cl2 did not react with oxygen inside the oxygen‐rich silica matrix to give Ru‐O bonds. Electrochemical and ECL characterization of the thin film electrodes were made by means of cyclic voltammetry (CV) and controlled potential step experiments. The ECL sensor showed a diffusive redox behavior of the Ru(bpy)32+/Ru(bpy)33+ system. Light emission produced from the reaction between oxalic acid and the electrogenerated Ru(bpy)33+ was larger and stable when thermally treated electrodes were used after a suitable hydration period. The 300 °C treated sample was the best performing sensor both in terms of low complex leakage and sensitivity. Calibration plots relative to oxalic acid were obtained both in stationary and in flowing solutions in the concentration range 2×10?6?3×10?4 M. A linear behavior appeared in the former case, while in the latter a slight curvature was evident as a consequence of a finite diffusion time of the analyte inside the thin film. The signal repeatability, obtained by multiple 100 μL of 10?5 M oxalic acid injections in flowing solutions, was better than 4%. The obtained detection limit (computed as three times the standard deviation of the base‐line noise) was 10?6 M as oxalic acid.  相似文献   

8.
《Analytical letters》2012,45(4):675-682
Abstract

Enantioselective, potentiometric membrane electrodes (EPMEs) based on antibiotics are proposed for the enantioanalysis of L‐vesamicol. A carbon paste was modified with antibiotics (vancomycin, teicoplanin, and teicoplanin modified with acetonitrile), as chiral selectors. The EPMEs based on antibiotics were reliably used for enantiopurity tests of L‐vesamicol using the direct potentiometric technique. The following linear concentration ranges: 1.0×10?6–1.0×10?4, 1.0×10?6–1×10?3 and 1×10?7?1×10?2 mol/L; and detection limits: 1.1×10?7, 9.6×10?8, and 3.6×10?8 mol/L were determine for vancomycin, teicoplanin, and teicoplanin modified with acetonitrile–based EPMEs, respectively. The proposed EPMEs were applied for the enantioanalysis of L‐vesamicol in urine samples.  相似文献   

9.
《Electroanalysis》2006,18(16):1620-1626
A polyvinylchloride membrane sensor based on N,N′‐bis(salecylidene)‐1,2‐phenylenediamine (salophen) as membrane carrier was prepared and investigated as a Al3+‐selective electrode. The sensor exhibits a Nernstian response toward Al(III) over a wide concentration range (8.0×10?7–3.0×10?2 M), with a detection limit of 6.0×10?7 M. The potentiometric response of the sensor is independent of the pH of the test solution in the pH range 3.2–4.5. The electrode possesses advantages of very fast response and high selectivity for Al3+ in comparison with alkali, alkaline earth and some heavy metal ions. The sensor was used as an indicator electrode, in the potentiometric titration of aluminum ion and in determination of Al3+ contents in drug, water and waste water samples.  相似文献   

10.
A dichromate‐selective PVC‐membrane electrode based on Quinaldine Red (an acridinium derivative) is described. The electrode exhibits rapid (< 30 s) and linear response to the activity of Cr(VI) anions in the range of 5.2 × 10?6 ?1.0 × 10?1 M dichromate with the limit of detection 2.5 × 10?6 Mof Cr2O72?. The sensor is used as an indicator electrode in potentiometric determination of Cr(VI) anions and is also suitable for end‐point indication in the titrations of proper metal ions with dichromate under laboratory conditions. The proposed electrode has been applied to the direct potentiometric determination of Cr(VI) anions in water samples with satisfactory results.  相似文献   

11.
A polyvinyl chloride (PVC) membrane based Pr(III) selective electrode was constructed using 1,6,7,12‐tetramine‐2,5,8,11‐tetraoxo‐1(12),6(7)‐di(biphenyl)dodecane (TATODBDD) as a neutral carrier. The sensor exhibits a Nernstian response for Pr(III) ions, a wide concentration range of 3.9×10?7?1.0×10?1 mol/L with a detection limit of 5.0×10?8 mol/L and slope of 19.5 mV/decade. The developed sensor revealed relatively good selectivity and high sensitivity for Pr(III) ions over the other lanthanide ions. The potentiometric response of the sensor is independent in the pH range 2.9–9.5. The advantages of sensor are low resistance, very fast response time (<10 s) with good selectivity. This sensor can be used up to 6 weeks without any divergences in potential response.  相似文献   

12.
《Electroanalysis》2005,17(17):1534-1539
The construction, performance, and applications of a novel ytterbium(III) sensor based on N‐(2‐pyridyl)‐N′‐(2‐methoxyphenyl)‐thiourea (PMT), as an excellent carrier, in plasticized poly(vinyl chloride) PVC matrix, is described. The influences of membrane composition and pH on the potentiometric response of the sensor were investigated. The sensor exhibits a nice Nernstian response for Yb(III) ion over a wide concentration range of 4 decades of concentration (1.0×10?6–1.0×10?2 M), and a detection limit of 5.0×10?7 M. The response time of the electrodes is between 8 and 10 s, depending on the concentration of ytterbium(III) ions. The proposed sensor can be used for about 8 weeks without any considerable divergence in potential. The sensor revealed very good selectivity for Yb(III) in the presence of several metal ions. The best performance was observed for the membrane containing; 30% PVC, 59% o‐nitrophenyloctyl ether (NPOE) as solvent mediator, 7% PMT, and 4% sodium tetraphenyl borate (NaTPB). It was successfully applied as indicator electrodes in the potentiometric titration of Yb(III) with EDTA and for the determination of fluoride ion in two mouth wash formulations. The proposed La(III) sensor was found to work well under laboratory conditions. It was also used as an indicator electrode in titration of a 1.0×10?4 M of Yb(III) with a standard EDTA solution (1.0×10?2 M). It was also used for determination of Yb(III) ion in Xenotime .  相似文献   

13.
The effect of dissolved oxygen (DO) and agitation rate in open and closed reactors was examined for sulfur-utilizing autotrophic denitrification. The reaction rate constants were determined based on a half-order kinetic model. Declining denitrification rate constants obtained for open reactors those of 8.46, 8.03, and 2.18 for 50 mg NO3 ?-N/L, while 11.12, 9.14, and 0.12 mg1/2/L1/2?h were for 100 mg NO3 ?-N/L at agitation speeds of 0, 100, and 200 rpm. In closed reactors, the ever-increasing denitrification rates were 10.13, 22.56, and 37.03, whereas for the same nitrate concentrations and speeds the rates were 13.17, 15.63, and 26.67 mg1/2/L1/2?h. The rate constants correlated well (r 2 ?=?0.89–0.99) with a half-order kinetic model. In open reactors, high SO4 2?/N ratios (8.02–75.10) while in closed reactors comparatively low SO4 2?/N ratios (6.10–13.39) were obtained. Sulfur oxidation occurred continuously in the presence of DO, resulting in mixed cultures acclimated to sulfur and nitrate. SO4 2? was produced as an end product, which reduced alkalinity and lowered pH over time. Furthermore, DO inhibited sulfur denitrification in open reactors, while agitation in closed reactors increased the rate of denitrification.  相似文献   

14.
《Analytical letters》2012,45(8):1596-1609
Abstract

An original highly selective and sensitive PVC membrane sensor, working as a Fe(III) ion selective electrode and using 4‐amino‐6‐methyl‐3‐methylmercapto‐1,2,4‐triazin‐5‐one (AMMTO) as an ionophore, has been developed. This cetain sensor demonstrated the following performance; a linear dynamic range between 1.0×10?6 and 1.0×10?1 M with a near Nernstian slope of 19.4±0.5 mV per decade; a detection limit of 6.8×10?7 M; characteristically, the best performance was obtained with a membrane composition of 30% poly(vinyl chloride), 65.5% nitrophenyl octyl ether, 2% sodium tetraphenyl borate and 2.5% AMMTO. Furthermore, the potentiometric response of the developed electrode is independent of the solution pH in the range of 2.2–4.8. The sensor possesses the advantages of short conditioning time, fast response time (<15 s) and, especially, great selectivity towards transition and heavy metal ions and some mono, di‐ and trivalent cations. The electrode can be used for at least 9 weeks without any considerable potential divergence. It was effectively used as an indicator electrode in the potentiometric titration of Fe(III) ions with EDTA and the direct determination of Fe3+ in different water samples.  相似文献   

15.
Arsenic contamination of groundwater has long been reported in the Mushidabad district of West Bengal, India. We visited 13 arsenic‐affected families in the Makrampur village of the Beldanga block in Mushidabad during 18–21 December 2001 and collected five shallow tubewell‐water samples used general household purposes, four deep tubewell‐water samples used for drinking and cooking purposes, and 44 urine samples from those families. The arsenic concentrations in the five shallow tubewell‐water samples ranged from 18.0 to 408.4 ppb and those in the four deep tubewell‐water samples were from 5.2 to 9.6 ppb. The average arsenite (arsenic(III)), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and arsenate (arsenic(V)) in urine were 28.7 ng mg?1, 168.6 ng mg?1, 25.0 ng mg?1 and 4.6 ng mg?1 creatinine respectively. The average total arsenic was 227.0 ng mg?1 creatinine. On comparison of the ratio of (MMA + DMA) to total arsenic, the average proportion was 86.7 ± 9.2% (mean plus/minus to residual standard deviation, n = 43). The exception was data for one boy, whose proportion was 8.0%. One woman excreted the highest total arsenic, at 2890.0 ng mg?1 creatinine. When using 43 of the urine samples (the exception being the one sample obtained from the boy) there were significantly positive correlations (p < 0.01) between arsenic(III) and MMA, between arsenic(III) and DMA and between MMA and DMA. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

16.
《Analytical letters》2012,45(12):1847-1855
Abstract

Enantioselective, potentiometric membrane electrodes (EPMEs) based on immobilization of β‐, γ‐cyclodextrin (CD) or 2‐hydroxy‐3‐trimethylammoniopropyl‐β‐cyclodextrin (as chloride salt) (β‐CD‐derivative) in carbon paste have been designed. The β‐CD and β‐CD‐derivative‐based electrodes were applied in the 10?8–10?6 and 10?7–10?5 mol/L concentration ranges for the determination of L‐2‐hydroxyglutaric acid (L‐2‐HGA), whereas γ‐CD‐based electrode was applied for the determination of D‐2‐hydroxyglutaric acid (D‐2‐HGA) in the concentration range 10?6–10?4 mol/L. The β‐CD‐based EPME showed the lowest detection limit (1×10?9 mol/L). The enantioselectivity and selectivity of the proposed electrodes for the assay of L‐2‐HGA and D‐2‐HGA, respectively, were determined over D‐2‐HGA/L‐2‐HGA, creatine, and creatinine. The proposed EPMEs can be applied for the enantioanalysis of 2‐hydroxyglutaric acid in urine samples.  相似文献   

17.
《Analytical letters》2012,45(6):1075-1086
Abstract

A novel plasticized membrane sensor for Ho(III) ions based on N‐(1‐thien‐2‐ylmethylene)‐1,3‐benzothiazol‐2‐amine (TBA) as a neutral carrier was prepared. The best performance was obtained with a membrane composition of 31% PVC, 61% benzyle acetate, 2% sodium tetra phenyl borate and 6% carrier. The electrode exhibits a Nernstian response for Ho(III) ions over a particular concentration range (1.0×10?5?1.0×10?2 M) with a slope of 19.7±0.2 mV decade?1. The limit of the detection is 7.0×10?6 M. The sensor has a response time of <15 s and a useful working pH range of 4.0–9.5. The proposed sensor discriminates relatively well towards Ho(III) ions with regard to common alkali, alkaline earth, and specially lanthanide ions. It was successfully applied as an indicator electrode in a potentiometric titration of Ho(III) ions with EDTA. It was also applied in determination of fluoride ions in a mouth wash preparation. The proposed sensor was applied for the determination of Ho(III) ion concentration in binary mixtures.  相似文献   

18.
《Analytical letters》2012,45(4):683-695
Abstract

A highly selective and sensitive triiodide sensor based on a 2‐(((2‐(((E)‐1‐(2‐hydroxy phenyl) methylidine) amino) phenyl) imino) methyl) phenol with iodine (CTC) as membrane carrier was developed. The electrode revealed a Nernstian behavior over a very wide triiodide‐ion concentration range (5.0×10?8–1.0×10?2 M), and relatively low detection limit (3.0×10?8 M). The potentiometric response is independent of the pH of solution in the pH range of 3.0–10.0. The electrodes manifest advantages of low resistance, very fast response (<12 s), and most importantly, good selectivities relative to a wide variety of inorganic and organic anions, including iodide, bromide, chloride, fluoride, sulfite, sulfate, cyanide, thiocyanate, and acetate. In fact, the selectivity behavior of the proposed triiodide ion‐selective electrode shows great improvements compared to the previously reported electrodes for the triiodide ion. The proposed membrane sensor can be used for at least 6 months without any significant divergences in the potential. The electrode was successfully applied as an indicator electrode in the titration of triiodide with thiosulfate ion.  相似文献   

19.
《Analytical letters》2012,45(10):1923-1938
Abstract

In this work, for the first time, we introduce a highly selective and sensitive lutetium(III) micro‐sensor. N‐(2‐furylmethylene) pyridine‐2,6‐diamine (FPD) was used as a membrane‐active component to prepare a highly sensitive Lu(III)‐selective polymeric membrane microelectrode. Theoretical calculations for FPD, lutetium and some other metal ions were carried out and selectivity toward Lu(III) ions was confirmed. The best performance was achieved by a membrane composed of 32% PVC, 60% o‐nitrophenyloctyl ether, 4% potassium tetrakis (p‐chlorophenyl) borate (KTpClPB) and 4% FPD. The electrode exhibits a Nernstian response for Lu(III) ions over a particular concentration range (1.0×l0?11?1.0×10?6 mol l?1) with a slope of 20.5±0.2 mV decade?1. The detection limit is 3.0×10?11 mol l?1 while the sensor presents a response time of <10 s and a useful working pH range of 4.0–10.5. As a matter of fact, the proposed sensor discriminates relatively well for Lu(III) ions in compare to common alkali, alkaline earth, heavy metals and, specially, lanthanide ions. The sensor was successfully applied as an indicator electrode in a potentiometric titration of Lu(III) ions with EDTA. In addition, it was used for determination of lutetium in some soil samples where domestic devices were stored. The proposed sensor was evaluated for Lu(III) ions determination in some binary mixtures.  相似文献   

20.
《Electroanalysis》2005,17(24):2260-2265
A new Cu(II) ion‐selective PVC membrane sensor based on 6‐methyl‐4‐(1‐phenylmethylidene)amino‐3‐thioxo‐1,2,4‐triazin‐5‐one (MATTO) as an excellent sensing material was developed. The electrode exhibits a Nernstian slope of 29.2±0.4 mV per decade over a very wide concentration range between 1.0×10?1 and 1.0×10?6 M, with a detection limit of 4.8×10?7 M (30.5 ng/mL). The sensor possesses the advantages of short conditioning time, fast response time (<10 s), and especially, very good selectivity towards transition and heavy metal, and some mono, di and trivalent cations. The proposed electrode was successfully applied to the determination of copper in wastewater of copper electroplating samples and as an indicator electrode in potentiometric titration of Cu(II) ions with EDTA.  相似文献   

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