Your browser doesn't support javascript.
loading
Show: 20 | 50 | 100
Results 1 - 20 de 25
Filter
Add more filters










Publication year range
1.
Nanoscale ; 16(17): 8650-8660, 2024 May 02.
Article in English | MEDLINE | ID: mdl-38618947

ABSTRACT

Driven by their excellent conductivity and redox properties, metal tellurides (MTes) are increasingly capturing the spotlight across various fields. These properties position MTes as favorable materials for next-generation electrochemical devices. Herein, we introduce a novel, self-sustained approach to creating a yolk-shelled electrode material. Our process begins with a metal-organic framework, specifically a CoFe-layered double hydroxide-zeolitic imidazolate framework67 (ZIF67) yolk-shelled structure (CFLDH-ZIF67). This structure is synthesized in a single step and transformed into CuCoLDH nanocages. The resulting CuCoFeLDH-CuCoLDH yolk-shelled microrods (CCFLDH-CCLDHYSMRs) are formed through an ion-exchange reaction. These are then converted into CuCoFeTe-CuCoTe yolk-shelled microrods (CCFT-CCTYSMRs) by a tellurization reaction. Benefiting from their structural and compositional advantages, the CCFT-CCTYSMR electrode demonstrates superior performance. It exhibits a fabulous capacity of 1512 C g-1 and maintains an impressive 84.45% capacity retention at 45 A g-1. Additionally, it shows a remarkable capacity retention of 91.86% after 10 000 cycles. A significant achievement of this research is the development of an activated carbon (AC)||CCFT-CCTYSMR hybrid supercapacitor. This supercapacitor achieves a good energy density (Eden) of 63.46 W h kg-1 at a power density (Pden) of 803.80 W kg-1 and retains 88.95% of its capacity after 10 000 cycles. These results highlight the potential of telluride-based materials in advanced energy storage applications, marking a step forward in the development of high-energy, long-life hybrid supercapacitors.

2.
Nanoscale ; 15(26): 11115-11130, 2023 Jul 06.
Article in English | MEDLINE | ID: mdl-37337891

ABSTRACT

Transition metal phosphides (TMPs) demonstrate excellent potential for supercapacitor electrode materials owing to their good theoretical capacity and great electrical conductivity. The electrochemical features of the electrode materials based on monometallic or bimetallic phosphides are not desirable or satisfactory due to their low rate performance, unfavorable energy density, and short durability. One practical solution to overcome the above problems is to bring in heteroatoms to the structure of the bimetallic materials to create trimetallic phosphides. In this work, brand-new MnNiCoP yolk-shell spheres assembled with nanosheets are synthesized in a facile self-templated way using greatly uniform co-glycerate spheres as sacrificial templates, followed by a phosphorization process. Because of the existence of plenty of oxidation-reduction active sites, great surface area (SA) with mesoporous pathways, high electrical conductivity, and synergistic effect of Mn, Ni, and Co atoms, the fabricated MnNiCoP@NiF electrode demonstrates a considerably increased electrochemical efficiency compared with the bimetallic phosphide MnCoP@NiF electrode. Noticeably, the MnNiCoP@NiF electrode exhibits a great specific capacity of 291.24 mA h g-1 at an applied current density of 1 Ag-1, 80% capacity retention at an applied current density of 20 Ag-1, and 91.3% capacity retention after 14 000 cycles. In addition, a hybrid supercapacitor device with a brand-new positive electrode (MnNiCoP@NiF) and an appropriate negative electrode (AC@NiF) demonstrates an energy density of 57.03 W h kg-1 with a power density of 799.98 W kg-1, plus superb cyclability with 88.41% of the primary capacitance after 14 000 cycles.

3.
Nanoscale ; 15(6): 2806-2819, 2023 Feb 09.
Article in English | MEDLINE | ID: mdl-36683464

ABSTRACT

Owing to their metalloid characteristics with high electrical conductivity, transition metal phosphides (TMPs) have attracted considerable research attention as prospective cathodes for hybrid supercapacitors. Unfortunately, they usually exhibit low rate performance as well as poor longevity, which does not meet the demands of hybrid supercapacitors. The nanocomposite constructed from reduced graphene oxide (rGO) and TMPs with a highly porous nature can effectively overcome the above-mentioned issues, greatly widening their utilization. In this work, we fabricated nanosheet-assembled hollow copper-nickel phosphide spheres (NH-CNPSs) by the controllable phosphatizing of copper-nickel-ethylene glycol (CN-EG) precursors. Then, porous NH-CNPSs were embedded in rGO texture (NH-CNPS-rGO) to form a unique porous nanoarchitecture. The obtained NH-CNPS-rGO has several advantages benefiting as the cathode electrode, such as (i) the hollow structure as well as porous nanosheets are conducive to fast electrolyte diffusion, (ii) the electrical conductivity of NH-CNPS is further enhanced when coupled with the rGO texture, hence promoting electron transfer in the whole structure, (iii) wrapping NH-CNPSs within the rGO texture endows the nanocomposite with much better structural stability, resulting in longer durability of the electrode, And (iv) the porous structures generated in the nanocomposite provide a perfect space for reducing the mass transfer resistance and accessing the electrolyte, thereby boosting the reaction kinetics. The tests demonstrated that the optimal NH-CNPS-rGO electrode revealed a capacity of up to 1075 C g-1, a superior rate capacity, and exceptional longevity of 94.7%. Moreover, a hybrid supercapacitor (NH-CNPS-rGO‖AC) equipped with the NH-CNPS-rGO-cathode electrode and activated carbon (AC)-anode electrode represented a satisfactory energy density of 64 W h kg-1 at 801 W kg-1 and amazing longevity (91.8% retention after 13 000 cycles), which endorses the promising potential of NH-CNPS-rGO for high-efficiency supercapacitors. This research showcases an appropriate method to engineer hollow TMP-rGO nanocomposites as effective materials for supercapacitors.

4.
Dalton Trans ; 51(35): 13405-13418, 2022 Sep 13.
Article in English | MEDLINE | ID: mdl-35993111

ABSTRACT

Design and fabrication of impressive and novel electrode materials for energy storage devices, especially supercapacitors, are of great importance. Herein, bimetallic CoSe2/FeSe2 hollow nanocuboid nanostructures derived from Co/Fe-Prussian Blue analogues (denoted as CoSe2/FeSe2 HNCs) are successfully designed and fabricated as a remarkable positive electrode material for high-performance supercapacitors. The bimetallic CoSe2/FeSe2 HNC nanostructures can have increased active sites and short electron-ion diffusion pathways. Bimetallic CoSe2/FeSe2 HNCs@NiF as a positive electrode showed efficient supercapacitive properties with a great specific capacity of 332.75 mA h g-1 (1197.90 C g-1) at 1 A g-1, retaining 80.61% of its initial capacity at 20 A g-1, considerable longevity (91.47% of its initial capacity after 10 000 cycles) and an excellent coulombic efficiency of 98.49%. Also, the designed and fabricated CoSe2/FeSe2 HNCs@NiF||AC@NiF hybrid supercapacitor device using bimetallic CoSe2/FeSe2 HNCs@NiF (positive electrode) and activated carbon@NiF (AC, negative electrode) exhibited an efficient energy density of 63.62 W h kg-1 and a superior durability of 91.14% after 10 000 cycles.

5.
Dalton Trans ; 50(35): 12168-12178, 2021 Sep 14.
Article in English | MEDLINE | ID: mdl-34519748

ABSTRACT

The development of durable, beneficial, and highly active non-precious metal-based electrocatalysts for hydrogen generation is a vital concern. This study proposes an effective strategy for the construction of Fe doped CoP nanosheet arrays wrapped by graphene (F0.25CP-G) on nickel foam as an efficient electrocatalyst for the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER). In this design, the final catalyst possesses a combination of the high conductivity of graphene, great surface porosity, and the intrinsic electrocatalytic activity of the F0.25CP-G which results in high-performance electrocatalytic activity toward the HER and OER. Therefore, the as-synthesized F0.25CP-G catalyst can achieve overpotentials of 66 mV and 230 mV for the HER and OER, respectively, in KOH at 10 mA cm-2. Furthermore, a practical electrolyzer (F0.25CP-G||F0.25CP-G) exhibits a current density of 10 mA cm-2 at 1.60 V along with good durability for 24 h.

6.
Dalton Trans ; 50(24): 8372-8384, 2021 Jun 22.
Article in English | MEDLINE | ID: mdl-34037022

ABSTRACT

Metal-organic framework (MOF) derived nanoarchitectures have special features, such as high surface area (SA), abundant active sites, exclusive porous networks, and remarkable supercapacitive performance when compared to traditional nanoarchitectures. Herein, we propose a viable strategy for the synthesis of hollow manganese nickel selenide spheres comprising nanosheets supported on the nickel foam (denoted as MNSe@NF) from the MOF. The MNSe nanostructures can demonstrate enriched active sites, and shorten the ion-electron diffusion pathways. When the MNSe@NF electrode is used as a cathode electrode for a hybrid supercapacitor, the electrode reflected impressive supercapacitive properties with a high capacity of 325.6 mA h g-1 (1172.16 C g-1) at 2 A g-1, an exceptional rate performance of 86.6% at 60 A g-1, and remarkable longevity (3.2% capacity decline after 15 000 cycles). Also, the assembled MNSe@NF∥AC@NF hybrid supercapacitors employing activated carbon on the nickel foam (AC@NF, anode electrode) and MNSe@NF (cathode electrode) revealed an impressive energy density of 66.1 W h kg-1 at 858.45 W kg-1 and an excellent durability of 94.1% after 15 000 cycles.

7.
Nanoscale ; 13(5): 2931-2945, 2021 Feb 11.
Article in English | MEDLINE | ID: mdl-33503101

ABSTRACT

Thanks to the attractive structural characteristics and unique physicochemical properties, mixed metal selenides (MMSes) can be considered as encouraging electrode materials for energy storage devices. Herein, a straightforward and efficient approach is used to construct multi-shelled nickel-manganese selenide hollow spheres (MSNMSeHSs) as cathode and double-shell nickel-iron selenide hollow spheres (DSNFSeHSs) as anode electrode materials by tuning shell numbers for supercapacitors. The as-designed MSNMSeHS electrode can deliver a splendid capacity of ∼339.2 mA h g-1/1221.1 C g-1, impressive rate performances of 78.8%, and considerable longevity of 95.7%. The considerable performance is also observed for the DSNFSeHS electrode with a capacity of 258.4 mA h g-1/930.25 C g-1, rate performance of 75.5%, and longevity of 90.9%. An efficient asymmetric apparatus (MSNMSeHS||DSNFSeHS) fabricated by these two electrodes depicts the excellent electrochemical features (energy density of ≈112.6 W h kg-1 at 900.8 W kg-1) with desirable longevity of ≈94.4%.

8.
Dalton Trans ; 49(29): 10028-10041, 2020 Aug 07.
Article in English | MEDLINE | ID: mdl-32643715

ABSTRACT

Porous structures have attracted considerable attention as promising electrode designs for supercapacitor applications. Herein, we introduce a procedure towards the construction of nanoporous CuCoNi-P nanotube arrays (CCNP-NAs) by a metal-organic framework and hierarchical CoFe2Se4 nanosheet arrays (CFS-NAs) through a hydrothermal strategy, followed by selenization for the flexible asymmetric device. Due to the unique design of the electrode materials, the CCNP-NA and CFS-NA electrodes show exceptional specific capacities of ∼406.73 and 248.2 mA h g-1 at 2 A g-1, reasonable rate capabilities of 84.2 and 71.2% at 50 A g-1, and remarkable durability of 98.9% and 95.1%, respectively. Remarkably, an advanced flexible device was constructed using the CCNP-NA positive electrode and CFS-NA negative electrode. Our flexible device demonstrates tremendous energy density (∼153.5 W h kg-1 at 852.8 W kg-1), super-high durability of 96.2%, and considerable flexibility under bending conditions. This work proposes insight into the rational construction of porous nanostructures for next-generation electronic devices.

9.
Talanta ; 217: 121025, 2020 Sep 01.
Article in English | MEDLINE | ID: mdl-32498910

ABSTRACT

Agarose gel as a green membrane has been proposed for use in electromembrane extraction of five hypothalamic-related peptides without an ionic carrier. Octreotide, goserelin, triptorelin, cetrorelix, and somatostatin were extracted from 5.0 mL of sample solution (adjusted to pH 5.0) into a microvolume acceptor solution (HCl, 100 mM) under the applied voltage of 30 V in 15 min. The pH of the agarose gel 3.0% (w/v) was adjusted to 4.0 to facilitate the movement of peptides through the membrane. Quantification was performed using an HPLC-UV system on a C18 column. Quantification and detection limits were found to be in the range of 15.0-20.0 ng mL-1 and 4.5-6.0 ng mL-1, respectively. Dynamic linear ranges were found to be in the range of 15.0-1000 ng mL-1 (R2 > 0.995) and recoveries were in the range of 62.3-77.6%. The optimized method was applied to spiked human plasma samples. The method showed relative recoveries in the range of 44.8-66.0%. Finally, the proposed method was compared with and shown to have higher recoveries than, the conventional electromembrane extraction method for the peptides under study.


Subject(s)
Gonadotropin-Releasing Hormone/analogs & derivatives , Goserelin/blood , Octreotide/blood , Peptides/chemistry , Somatostatin/blood , Triptorelin Pamoate/blood , Electrochemical Techniques , Gels/chemistry , Gonadotropin-Releasing Hormone/blood , Gonadotropin-Releasing Hormone/chemistry , Goserelin/chemistry , Healthy Volunteers , Humans , Octreotide/chemistry , Somatostatin/chemistry , Triptorelin Pamoate/chemistry
10.
Nanoscale ; 12(23): 12476-12489, 2020 Jun 21.
Article in English | MEDLINE | ID: mdl-32495793

ABSTRACT

The practical exploration of electrode materials with complex hollow structures is of considerable significance in energy storage applications. Mixed-metal selenides (MMSs) with favorable architectures emerge as new electrode materials for supercapacitor (SC) applications owing to their excellent conductivity. Herein, a facile and effective metal-organic framework (MOF)-derived strategy is introduced to encapsulate multi-shelled zinc-cobalt-selenide hollow nanosphere positive and yolk-double shell cobalt-iron-selenide hollow nanosphere negative electrode materials with controlled shell numbers in a graphene network (denoted as G/MSZCS-HS and G/YDSCFS-HS, respectively) for SC applications. Due to the considerable electrical conductivity and unique structures of both electrodes, the G/MSZCS-HS positive and G/YDSCFS-HS negative electrodes exhibit remarkable capacities (∼376.75 mA h g-1 and 293.1 mA h g-1, respectively, at 2 A g-1), superior rate performances (83.4% and 74%, respectively), and an excellent cyclability (96.8% and 92.9%, respectively). Furthermore, an asymmetric device (G/MSZCS-HS//G/YDSCFS-HS) has been fabricated with the ability to deliver an exceptional energy density (126.3 W h kg-1 at 902.15 W kg-1), high robustness of 91.7%, and a reasonable capacity of 140.3 mA h g-1.

11.
Dalton Trans ; 49(10): 3353-3364, 2020 Mar 14.
Article in English | MEDLINE | ID: mdl-32107505

ABSTRACT

Owing to the increased requirement for efficient energy storage systems (ESs), investigating favorable electrodes with porous nanoarchitecture for supercapacitors (SCs) is vital. Nonetheless, the development of these kinds of electrodes to obtain high energy density remains a difficult task. Low specific capacitances of positive (cathode) and negative (anode) electrode materials are a serious obstacle that limits the performance of asymmetric SCs (ASCs). Herein, we proposed the preparation of yolk-shell Cu-Co-P hollow nanospheres (Y-CCP HN) as a positive electrode using a metal-organic framework (MOF) and CuFeS2 nanosheet (CFS NS) arrays as a negative electrode via a low-cost and simple hydrothermal route for ASCs. The Y-CCP HN and CFS NS electrodes exhibited significant specific capacitances (∼2043.3 F g-1 (340.55 mA h g-1) and 654.3 F g-1 (218.1 mA h g-1), respectively), considerable rate performances (∼77.55% and 63.2%, respectively, even at 24 A g-1), and exceptional durability (96.7% and 95.3% after 8000 cycles, respectively). Most notably, the Y-CCP HN//CFS device delivers a wonderful energy density of 158.4 W h kg-1 at a power density of 900.3 W kg-1, a notable specific capacitance of 352.1 F g-1 (176.05 mA h g-1), and excellent cyclability (96.1% after 8000 cycles). This exploration demonstrates a good strategy for the construction of other metal phosphides and sulfides with porous nature, emphasizing considerable prospects for next-generation ESs.

12.
Nanoscale ; 12(3): 1643-1656, 2020 Jan 23.
Article in English | MEDLINE | ID: mdl-31872846

ABSTRACT

To construct a supercapacitor (SC) with considerable performance, synthesis of an electrode material with a highly porous structure is necessary. Herein, an efficient metal-organic framework (MOF)-derived procedure is offered to construct a graphene wrapped multi-shelled NiGa2O4 hollow sphere (GW-MSNGOHS) positive electrode material and a graphene-wrapped yolk-shell NiFe2O4 hollow sphere (GW-YS-NFOHS) negative electrode material with a highly porous nature in SCs. The GW-MSNGOHS and GW-YS-NFOHS electrodes exhibit excellent capacities (∼411.25 mA h g-1 and 254.25 mA h g-1, respectively, at 1 A g-1), reasonable rate performances (75.85%, and 62.7%, respectively), and outstanding cyclability (98.9% and 90.9%, respectively). Benefiting from the reasonably engineered negative and positive electrodes, the fabricated asymmetric device (GW-MSNGOHS//GW-YS-NFOHS) can show an excellent energy density (ED) of 118.97 W h kg-1 at a power density (PD) of 1702 W kg-1, an exceptional robustness of 92.1%, and an excellent capacity (Cs) of 140.2 mA g-1.

13.
J Sep Sci ; 42(19): 3126-3133, 2019 Oct.
Article in English | MEDLINE | ID: mdl-31347772

ABSTRACT

Herein, electromembrane extraction was combined with ultraviolet spectrophotometry using a customized manifold for preconcentration and simultaneous determination of morphine, codeine, and papaverine in water and human urine samples. Absorption spectra of the extracts were recorded inside the lumen of the hollow fiber using two fiber optics connected to a miniature spectrophotometer. Partial least squares regression was applied to resolve the overlapped spectra of the analytes. Performance of the model was validated by an independent test set. Central composite design was applied to optimize the extraction parameters. The optimized extraction conditions are as follows; supporting liquid membrane: 2-nitrophenyl octyl ether containing 15% v/v bis(2-ethylhexyl) phosphate, applied voltage: 80 V, donor pH: 3.0, acceptor pH: 1.0, extraction time: 20 min. Finally, the optimized extraction method was validated for determination of the mentioned alkaloids in human urine samples. The method showed good linearity (R2  > 0.995) for all of the mentioned alkaloids. The limits of detection for morphine, codeine, and papaverine in diluted human urine were found to be 0.6, 1.1, and 0.6 ng/mL, respectively with acceptable relative standard deviations. Enrichment factors of 104, 108, and 102 were achieved for morphine, codeine, and papaverine, respectively.


Subject(s)
Codeine/analysis , Morphine/analysis , Papaverine/analysis , Water Pollutants, Chemical/chemistry , Electrochemical Techniques , Humans , Spectrophotometry, Ultraviolet
14.
Dalton Trans ; 48(13): 4274-4282, 2019 Mar 26.
Article in English | MEDLINE | ID: mdl-30855631

ABSTRACT

Herein, we proposed a desirable strategy for the synthesis of graphene-wrapped NiCo2Se4 microspheres (positive electrode) and petal-like iron disulfide (FeS2) (negative electrode) on nickel foam substrates. The positive electrode represents a substantial specific capacitance of 2112.30 F g-1 and excellent durability (6.8% loss after 5000 cycles). Furthermore, the negative electrode reflects good electrochemical performance with a specific capacitance of 321.30 F g-1 and a satisfactory rate capability of 47% capacitance retention. Considering the notable properties of the electrodes, a flexible asymmetric all-solid-state device based on graphene-wrapped NiCo2Se4 microspheres (positive electrode) and petal-like iron disulfide (negative electrode) was assembled. Our flexible device exhibits the high specific capacitance of 221.30 F g-1, the significant energy density of 78.68 W h kg-1 and excellent flexibility.

15.
Electrophoresis ; 40(7): 1074-1081, 2019 04.
Article in English | MEDLINE | ID: mdl-30653693

ABSTRACT

An electromembrane extraction followed by HPLC-UV technique was developed and validated for quantification of leuprolide and triptorelin in rabbit plasma. The influencing parameters on the extraction efficiency were optimized using experimental design methodology. The optimized conditions were found to be; supported liquid membrane: a mixture of 1-octanol and 2-ethyl hexanol (1:1) containing 10% v/v di(2-ethylhexyl) phosphate, applied voltage: 5 V, extraction time: 5 min, pH of the donor phase: 4.5 and pH of the acceptor phase: 1.0. The optimized method was validated for linearity, intraday and interday precision, and accuracy in rabbit plasma. The range of quantification for both peptides was 0.5-1000 ng/mL with regression coefficients higher than 0.994. Relative recoveries of leuprolide and triptorelin were found to be 80.3 and 75.5%, respectively. Limits of quantification and detection for both peptides were found to be 0.5 and 0.15 ng/mL, respectively. The validated method was successfully applied to pharmacokinetic study of the 1-month depot formulations of each peptide after subcutaneous administration to rabbits.


Subject(s)
Leuprolide/blood , Triptorelin Pamoate/blood , 1-Octanol/chemistry , Administration, Cutaneous , Animals , Chromatography, High Pressure Liquid , Drug Liberation , Hexanols/chemistry , Hydrogen-Ion Concentration , Limit of Detection , Lipids/chemistry , Membranes, Artificial , Organophosphates/chemistry , Rabbits , Ultraviolet Rays
16.
Anal Chim Acta ; 935: 151-60, 2016 Sep 07.
Article in English | MEDLINE | ID: mdl-27543024

ABSTRACT

In this work, a new solid-phase microextraction fiber was prepared based on nitrogen-doped graphene (N-doped G). Moreover, a new strategy was proposed to solve problems dealt in direct coating of N-doped G. For this purpose, first, Graphene oxide (GO) was coated on Pt wire by electrophoretic deposition method. Then, chemical reduction of coated GO to N-doped G was accomplished by hydrazine and NH3. The prepared fiber showed good mechanical and thermal stabilities. The obtained fiber was used in two different modes (conventional headspace solid-phase microextraction and cold-fiber headspace solid-phase microextraction (CF-HS-SPME)). Both modes were optimized and applied for the extraction of benzene and xylenes from different aqueous samples. All effective parameters including extraction time, salt content, stirring rate, and desorption time were optimized. The optimized CF-HS-SPME combined with GC-FID showed good limit of detections (LODs) (0.3-2.3 µg/L), limit of quantifications (LOQs) (1.0-7.0 µg/L) and linear ranges (1.0-5000 µg/L). The developed method was applied for the analysis of benzene and xylenes in rainwater and some wastewater samples.

17.
Electrophoresis ; 37(2): 339-46, 2016 Jan.
Article in English | MEDLINE | ID: mdl-26462723

ABSTRACT

Electromembrane extraction (EME) of model analytes was carried out using a virtually rotating supported liquid membrane (SLM). The virtual (nonmechanical) rotating of the SLM was achieved using a novel electrode assembly including a central electrode immersed inside the lumen of the SLM and five counter electrodes surrounding the SLM. A particular electronic circuit was designed to distribute the potential among five counter electrodes in a rotating pattern. The effect of the experimental parameters on the recovery of the extraction was investigated for verapamil (VPL), trimipramine (TRP), and clomipramine (CLP) as the model analytes and 2-ethyl hexanol as the SLM solvent. The results showed that the recovery of the extraction is a function of the angular velocity of the virtual rotation. The best results were obtained at an angular velocity of 1.83 RadS(-1) (or a rotation frequency of 0.29 Hz).The optimization of the parameters gave higher recoveries up to 50% greater than those of a conventional EME method. The rotating also allowed the extraction to be carried out at shorter time (15 min) and lower voltage (200 V) with respect to the conventional extraction. The model analytes were successfully extracted from wastewater and human urine samples with recoveries ranging from 38 to 85%. The RSD of the determinations was in the range of 12.6 to 14.8%.


Subject(s)
Chemical Fractionation/instrumentation , Clomipramine/isolation & purification , Electrochemical Techniques/instrumentation , Membranes, Artificial , Trimipramine/isolation & purification , Verapamil/isolation & purification , Anti-Arrhythmia Agents/isolation & purification , Anti-Arrhythmia Agents/urine , Antidepressive Agents, Tricyclic/isolation & purification , Antidepressive Agents, Tricyclic/urine , Clomipramine/urine , Electrodes , Equipment Design , Humans , Limit of Detection , Rotation , Trimipramine/urine , Urinalysis/instrumentation , Verapamil/urine , Wastewater/analysis , Water Pollutants, Chemical/isolation & purification , Water Pollutants, Chemical/urine , Water Purification/instrumentation
18.
Anal Chim Acta ; 891: 151-9, 2015 Sep 03.
Article in English | MEDLINE | ID: mdl-26388374

ABSTRACT

The distribution of electric field vectors was first calculated for electromembrane extraction (EME) systems in classical and cylindrical electrode geometries. The results showed that supported liquid membrane (SLM) has a general field amplifying effect due to its lower dielectric constant in comparison with aqueous donor/acceptor solutions. The calculated norms of the electric field vector showed that a DC voltage of 50 V can create huge electric field strengths up to 64 kV m(-1) and 111 kV m(-1) in classical and cylindrical geometries respectively. In both cases, the electric field strength reached its peak value on the inner wall of the SLM. In the case of classical geometry, the field strength was a function of the polar position of the SLM whereas the field strength in cylindrical geometry was angularly uniform. In order to investigate the effect of the electrode geometry on the performance of real EME systems, the analysis was carried out in three different geometries including classical, helical and cylindrical arrangements using naproxen and sodium diclofenac as the model analytes. Despite higher field strength and extended cross sectional area, the helical and cylindrical geometries gave lower recoveries with respect to the classical EME. The observed decline of the signal was proved to be against the relations governing migration and diffusion processes, which means that a third driving force is involved in EME. The third driving force is the interaction between the radially inhomogeneous electric field and the analyte in its neutral form.

19.
Mater Sci Eng C Mater Biol Appl ; 48: 213-9, 2015 Mar.
Article in English | MEDLINE | ID: mdl-25579916

ABSTRACT

We are introducing mercapto-mesoporous carbon modified carbon paste electrode (mercapto-MP-C-CPE) as a new sensor for trace determination of omeprazole (OM) in biological samples. The synthesized modifier was characterized by thermogravimetry analysis (TGA), differential thermal analysis (DTA), transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FT-IR), X-ray diffraction (XRD), elemental analysis (CHN) and N2 adsorption surface area measurement (BET). The electrochemical response characteristic of the modified-CPE toward OM was investigated by cyclic and differential pulse voltammetry (CV and DPV). The proposed sensor displayed a good electrooxidation response to the OM, its linear range is 0.25nM to 25µM with a detection limit of 0.04nM under the optimized conditions. The prepared modified electrode shows several advantages such as high sensitivity, long-time stability, wide linear range, ease of preparation and regeneration of the electrode surface by simple polishing and excellent reproducibility.


Subject(s)
Carbon/chemistry , Electrochemical Techniques/instrumentation , Electrochemical Techniques/methods , Electrodes , Omeprazole/analysis , Humans , Limit of Detection , Microscopy, Electron, Transmission , Omeprazole/blood , Omeprazole/urine , Porosity , Reproducibility of Results , Spectroscopy, Fourier Transform Infrared , Thermogravimetry , X-Ray Diffraction
20.
Ultrason Sonochem ; 22: 382-90, 2015 Jan.
Article in English | MEDLINE | ID: mdl-24997048

ABSTRACT

A new lead complex, [Pb(Q)2] (1) (Q=quinoline-2-carboxylic acid), was prepared via conventional electrochemical method in a fast and facile process and fully characterized by (1)H and (13)C NMR, IR, UV spectroscopies and elemental analysis. The nano-structures of same compound were successfully prepared at 25, 48 and 60°C by a facile and environment-friendly sonoelectrochemical route. The new nano-structure particles were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analysis. Thermal stability of single-crystal and nano-size samples of the prepared compound was studied by thermogravimetric and differential thermal analysis. The effect of sonoelectrochemical temperature on particle size has been investigated, and possible explanations offered. The photoluminescence properties of the nano-structured and crystalline bulk of the prepared complex at room temperature in the solid state have been investigated in detail. The results indicate that the size of the complex particles has an important effect on the optical properties of it. The prepared complexes, as bulk and as nano-particles, were utilized as a precursor for preparation of PbO nanoparticles by direct thermal decomposition at 600°C in air. The nano-structures of PbO were characterized by scanning electron microscopy, X-ray powder diffraction and IR spectroscopy.

SELECTION OF CITATIONS
SEARCH DETAIL
...