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1.
Anal Chem ; 95(20): 8137-8144, 2023 05 23.
Artículo en Inglés | MEDLINE | ID: mdl-37167590

RESUMEN

Developing a novel strategy for the sensitive and rapid detection of pathogenic bacterial spores in field or on-site settings will be helpful in minimizing their potential threats to human health, environmental safety, and food safety. In this study, Tb3+ was combined with glutathione (GSH)-modified copper nanoclusters (CuNCs), and an aggregation-induced emission (AIE) fluorescent probe based on Tb-GSH-CuNCs was fabricated for dipicolinic acid (DPA, a pathogenic bacterial spore marker) sensing. Making use of the competitive binding of Tb3+ between GSH-CuNCs and DPA, a multicolor sensing of DPA was facilely realized without introducing fluorescent materials as the reference. Due to an "off-on" response mechanism of the AIE fluorescent probe, this multicolor response to DPA exhibited a feature of rich color gradients and highly discriminative color change, allowing a dosage-sensitive visual quantification of DPA. The DPA with a concentration even as low as 0.5 µM can still be identified by the naked eye. Moreover, together with a smartphone app, which can extract the R (red), G (green), and B (blue) values from the probe system, a portable platform can be established for sensitive DPA quantification in the range of 0.5-70 µM, showing great potential for the practical monitoring of DPA in field or on-site settings.


Asunto(s)
Colorantes Fluorescentes , Esporas Bacterianas , Humanos
2.
Anal Chem ; 91(9): 6141-6148, 2019 05 07.
Artículo en Inglés | MEDLINE | ID: mdl-30990020

RESUMEN

The excellent fluorescence property of Au nanoclusters (AuNCs) has received great attention for various chemosensing and biorelated applications, but the sample matrix is still an important problem that causes undesirable fluorescence variation. On the one hand, hydride generation (HG) is an effective strategy to separate the target analyte from the complex sample matrices, but the implementation of HG with AuNC-based fluorescent assays was not realized. On the other hand, due to the ultrasmall size of AuNCs and good catalytic performance of Au, AuNCs are also featuring intriguing catalytic applications. Herein, we proposed a new type of AuNC-based fluorescence assay for Se(IV) detection, in which hydride generation of Se(IV) was coupled with the fluorescence/catalytic dual functions of AuNCs. In a batch hydride generation mode, Se(IV) was first converted to volatile H2Se. When it spread in the headspace to contact with AuNCs supported paper, AuNC-catalyzed oxidation of H2Se by O2 to yield elemental selenium occurred, which further deposited on the surface of AuNCs to induce fluorescence quenching. The catalytic effect of AuNCs was studied in depth via both experimental and theoretical (density functional theory) investigations. Three main steps for H2Se oxidation were identified, with energy barriers in the presence of AuNCs significantly lower than those without. Benefiting from the reduced matrix interference by hydride generation and the unique catalysis/fluorescence of AuNCs, the proposed assay featured high selectivity, good sensitivity, and simplicity, with successful applications for selenium detection in real samples.

3.
Anal Chem ; 91(5): 3359-3366, 2019 03 05.
Artículo en Inglés | MEDLINE | ID: mdl-30688069

RESUMEN

A disposable, instrument-free, height readout paper-based analytical device (HR-PAD) based on a paper strip inkjet-printed with CdTe quantum dots (QDs) was developed for the sensitive speciation analysis of Ag+ and silver nanoparticles (AgNPs). When the paper strip is immersed into a sample solution, capillary action draws it through the surface and any Ag+ in the solution quenches the fluorescence of CdTe QDs via a cation exchange reaction between Ag+ and the CdTe QDs, with the height of the quenched band being proportional to the concentration of Ag+. In contrast, fluorescence quenching cannot be observed when only AgNPs are present in solution. Thus, the concentration of AgNPs can be obtained by subtracting the Ag+ content from the total silver determined by the HR-PAD after digestion with HNO3. Under optimized conditions, the methodology provides high selectivity, sensitivity, and accuracy for the detection of Ag+ or AgNPs in various samples, even at concentrations as low as 0.05 mg L-1. Precisions of 4.5% and 2.2% RSDs were achieved at concentrations of 1 mg L-1 and 7 mg L-1 of Ag+, respectively. Compared to conventional methods, this approach is inexpensive and user-friendly and eliminates the need for expensive and sophisticated detection instruments. The practicality of the method was demonstrated via the speciation analysis of AgNPs and Ag+ in river water and 12 commercial products with satisfactory results.

4.
Anal Chem ; 90(15): 9598-9605, 2018 08 07.
Artículo en Inglés | MEDLINE | ID: mdl-29983047

RESUMEN

Cataluminescence (CTL) is one of the most important sensing-transduction principles for the real-time monitoring of atmospheric pollutants. Highly sensitive CTL-based CO detection still remains a challenge because of the relatively poor reactivity of CO and the low catalytic efficiency of the catalysts. Herein, combining ultraviolet (UV)-light activation and chemical modification of the sensing element, we have successfully established a UV-assisted CTL sensor for gaseous CO based on g-C3N4 with high sensitivity, selectivity, and stability. UV irradiation can efficiently activate CO molecules and induce the generation of reactive oxygen species (ROS) for CO oxidation. Furthermore, carboxyl groups greatly facilitate the chemisorption of CO on functionalized g-C3N4 nanomaterials, thus enhancing the CTL sensitivity. The influences of experimental conditions and the possible catalytic mechanism of CO on functionalized g-C3N4 have been investigated in detail. Under the optimal experimental conditions, the proposed CTL sensor presents a detection limit (3σ) toward CO of 0.008 µg mL-1, which is much lower than the maximum allowable emission concentration of CO in atmospheric conditions (0.030 µg mL-1). The UV-CTL system is green, sensitive, stable, and low cost, and thus it possesses great potential application in gas sensing.

5.
Anal Chem ; 89(9): 5101-5106, 2017 05 02.
Artículo en Inglés | MEDLINE | ID: mdl-28382824

RESUMEN

Singlet oxygen (1O2), generated via photosensitization, has been proved to oxidize chromogenic substrates with neither H2O2 oxidation nor enzyme (horseradish peroxidase, HRP) catalysis. Of the various methods for modulation of the 1O2 generation, DNA-controlled photosensitization received great attention. Therefore, integration of the formation/deformation DNA structures with DNA-controlled photosensitization will be extremely appealing in visual biosensor developments. Here, the stable melamine-thymine complex was explored in combination with DNA-controlled photosensitization for visual detection of melamine. A T-rich single stand DNA was utilized as the recognition unit. Upon the formation of the T-M-T complex, double stand DNA was formed, which was ready for the binding of SYBR Green I and activated the photosensitization. Subsequent oxidation of TMB allowed visual detection of melamine in dairy products, with spike-recoveries ranging from 94% to 106%.


Asunto(s)
Técnicas Biosensibles/métodos , ADN de Cadena Simple/química , Compuestos Orgánicos/química , Oxígeno Singlete/química , Timina/química , Triazinas/análisis , Animales , Disparidad de Par Base , Bencidinas/química , Benzotiazoles , Compuestos Cromogénicos/química , Colorimetría/métodos , ADN de Cadena Simple/genética , Diaminas , Contaminación de Alimentos/análisis , Enlace de Hidrógeno , Luz , Leche/química , Compuestos Orgánicos/efectos de la radiación , Quinolinas
6.
Anal Chem ; 89(8): 4695-4700, 2017 04 18.
Artículo en Inglés | MEDLINE | ID: mdl-28326763

RESUMEN

Gold nanoparticles (AuNPs)-based colorimetric assays are of particular interest since molecular events can be easily read out with the color changes of AuNPs by the naked eye. However, the molecular recognitions occur almost exclusively in the liquid phase (i.e., the interaction between target analytes and AuNPs is always proceeded in the presence of the sample matrix). Since the aggregation of the unmodified AuNPs is prone to be influenced by the ionic strength of the solution, sample matrix will cause undesirable interference. Here, we proposed a new type of AuNP-based colorimetric assay, in which target analyte selenium was first converted to its hydride chemical vapor (H2Se) and then delivered into the solution of AuNPs to induce color change. Therefore, sample matrix (for example, high salinity) were eliminated, leading to excellent selectivity. With the aid of hydride generation, the proposed method offered a detection limit of 0.05 µM with UV-vis detection and 1 µM with the naked eye. Successful application of this method for selenium detection in biological and environmental samples was demonstrated.


Asunto(s)
Oro/química , Nanopartículas del Metal/química , Selenio/análisis , Colorimetría , Gases/química , Límite de Detección , Concentración Osmolar , Selenio/química , Espectrofotometría
7.
Anal Chem ; 88(1): 789-95, 2016 Jan 05.
Artículo en Inglés | MEDLINE | ID: mdl-26631425

RESUMEN

A low-cost, simple, and highly selective analytical method was developed for sensitive visual detection of selenium in human urine both outdoors and at home, by coupling hydride generation with headspace solid-phase extraction using quantum dots (QDs) immobilized on paper. The visible fluorescence from the CdTe QDs immobilized on paper was quenched by H2Se from hydride generation reaction and headspace solid-phase extraction. The potential mechanism was investigated by using X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) as well as Density Functional Theory (DFT). Potential interferences from coexisting ions, particularly Ag(+), Cu(2+), and Zn(2+), were eliminated. The selectivity was significantly increased because the selenium hydride was effectively separated from sample matrices by hydride generation. Moreover, due to the high sampling efficiency of hydride generation and headspace solid phase extraction, the sensitivity and the limit of detection (LOD) were significantly improved compared to conventional methods. A LOD of 0.1 µg L(-1) and a relative standard deviation (RSD, n = 7) of 2.4% at a concentration of 20 µg L(-1) were obtained when using a commercial spectrofluorometer as the detector. Furthermore, a visual assay based on the proposed method was developed for the detection of Se, 5 µg L(-1) of selenium in urine can be discriminated from the blank solution with the naked eye. The proposed method was validated by analysis of certified reference materials and human urine samples with satisfactory results.


Asunto(s)
Compuestos de Cadmio/química , Papel , Puntos Cuánticos , Selenio/orina , Extracción en Fase Sólida , Telurio/química , Animales , Compuestos de Cadmio/síntesis química , Cazón , Cabello/química , Humanos , Músculos/química , Teoría Cuántica
8.
Analyst ; 141(4): 1512-8, 2016 Feb 21.
Artículo en Inglés | MEDLINE | ID: mdl-26759832

RESUMEN

A new digestion method using UV-assisted Fe(0) Fenton reaction was developed for the determination of trace Cd in rice by hydride generation atomic fluorescence spectrometry. The proposed method integrated the advantages of simplicity, small dose of reagents, low cost and moderate reaction conditions, and was successfully utilized to analyze a Certified Reference Material (CRM) and real rice samples. A 1 mL mixture of the sample and reagents (0.0500 g rice powder, 0.2% (m/v) Fe(0), 0.75% (v/v) HNO3 and 18% (v/v) H2O2) was irradiated by UV-light for 50 min and then a clear solution was obtained by separating excess Fe(0) with a magnet prior to spectral analysis. The limit of detection (LOD) for Cd was found to be 0.02 mg kg(-1) and the relative standard deviation was better than 5.0% at a concentration level of 0.40 mg kg(-1). The recovery obtained by analyzing the CRM was 103% and spiked recoveries with 0.40 mg kg(-1) Cd in rice samples were 93% and 101%. The t-test proved that there is no significant difference between the certified value and the determined value of the CRM, and between the proposed method and microwave-assisted digestion coupled with inductively coupled plasma mass spectrometry (MWD-ICP-MS) at 95% confidence level.


Asunto(s)
Cadmio/análisis , Análisis de los Alimentos/métodos , Peróxido de Hidrógeno/química , Hidrógeno/química , Hierro/química , Límite de Detección , Oryza/química , Rayos Ultravioleta , Cadmio/química , Contaminación de Alimentos/análisis , Tecnología Química Verde , Procesos Fotoquímicos , Espectrometría de Fluorescencia
9.
Anal Chem ; 87(13): 6584-91, 2015 Jul 07.
Artículo en Inglés | MEDLINE | ID: mdl-26017198

RESUMEN

To evaluate the toxicity of silver nanoparticles (AgNPs) and Ag(+) and gain deep insight into the transformation of AgNPs in the environment or organisms, ultrasensitive analytical methods are needed for their speciation analysis. About 40-fold of Cd(2+) in CdTe ionic nanocrystals can be "bombarded-and-exploded" (exchanged) in less than 1 min simply by mixing the nanocrystals with Ag(+) solution at room temperature, while this cation exchange reaction did not occur when only silver nanoparticles were present. On the basis of this striking difference, an ultrasensitive method was developed for speciation analysis of Ag(+) and AgNPs in complex matrices. The released Cd(2+) was reduced to its volatile species by sodium tetrahydroborate, which was separated and swept to an inductively coupled plasma mass spectrometer (ICPMS) or an atomic fluorescence spectrometer (AFS) for the indirect but ultrasensitive detection of Ag(+). Owing to the remarkable signal amplification via the cation exchange reaction and the advantages of chemical vapor generation for sampling, the limit of detection was 0.0003 µg L(-1) for Ag(+) by ICPMS, which was improved by 100-fold compared to the conventional method. Relative standard deviations are better than 2.5% at a concentration of 0.5 µg L(-1) Ag(+) or AgNPs regardless of the detector. The proposed method retains several unique advantages, including ultrahigh sensitivity, speciation analysis, simplicity and being organic reagent-free, and has been successfully utilized for speciation analysis of Ag(+) and AgNPs in environmental water samples and paramecium cells.


Asunto(s)
Cationes , Nanopartículas del Metal , Nanopartículas , Plata/química , Límite de Detección , Temperatura
10.
Chemistry ; 21(39): 13618-24, 2015 Sep 21.
Artículo en Inglés | MEDLINE | ID: mdl-26267394

RESUMEN

A one-step, template-free method is described to synthesize porous carbons (PCs) in situ on a metal surface by using a room-temperature, atmospheric-pressure dielectric barrier discharge (DBD) plasma. This method not only features high efficiency, environmentally friendliness, and low cost and simple equipment, but also can conveniently realize large-area synthesis of PCs by only changing the design of the DBD reactor. The synthesized PCs have a regulated nestlike morphology, and thus, provide a high specific surface area and high pore volume, which result in excellent adsorption properties. Its applicability was demonstrated by using a PC-coated stainless-steel fiber as a solid-phase microextraction (SPME) fiber to preconcentrate polycyclic aromatic hydrocarbons (PAHs) prior to analysis by gas chromatography with flame ionization detection (GC-FID). The results showed that the fiber exhibited excellent enrichment factors (4.1×10(4) to 3.1×10(5)) toward all tested PAHs. Thus, the PC-based SPME-GC-FID provides low limits of detection (2 to 20 ng L(-1)), good precision (<7.8%), and good recoveries (80-115%) for ultra-sensitive determination of PAHs in real water samples. In addition, the PC-coated fiber could be stable enough for more than 500 replicate extraction cycles.

11.
Guang Pu Xue Yu Guang Pu Fen Xi ; 35(9): 2393-6, 2015 Sep.
Artículo en Zh | MEDLINE | ID: mdl-26669136

RESUMEN

Methyltin mercaptide is widely used as one of the best heat stabilizer in the polyvinylchloride (PVC) thermal processing due to its excellent stability, good transparency, high compatibility and weather resistance. The content of sulfur and tin significantly affects its quality and performance, so it is of great significance to develop an analytical method for the simultaneous determination of sulfur and tin. Inductively coupled plasma atomic emission spectrometry (ICP-OES) has been a powerful analytical tool for a myriad of complex samples owing to its advantages of the low detection limits, rapid and precise determinations over wide dynamic ranges, freedom from chemical inter-element interferences, the high sample throughput and above all, simultaneous multi-elements analysis. Microwave technique as a well-developed method for sample preparation can dramatically reduce the digestion time and the loss of volatile elements compared with the traditional open digestion. Hereby, a microwave-assisted acid digestion (MW-AAD) procedure followed by inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis was developed for the simultaneous determination of Sn and S in methyltin mercaptide. This method has the advantages of simplicity, rapidness, good accuracy, green and less use of samples. Parameters affecting the MW-AAD such as the digestion solution and digestion time were optimized by using a chemical analyzed reference sample (DX-181) to attain tin and sulfur quantitative recoveries. HNO3-HCl-HClO4 (v/v/v=9:3:1) and 10 min were the optimum digestion solution and digestion time, respectively. Under optimum conditions, the standard addition method and the standard calibration curve method were both been used to detect Sn and S in DX-181. There was no significant difference between two methods and the relative deviations to the chemical analysis values were both less than 2%. Additionally, the accuracy of the MW-AAD method was examined by analyzing three methyltin mercaptide samples (DX-181, DX-990, DX-960). The results were satisfactory with the relative deviations (<3%) and the recoveries of standard addition (99%~102%).

12.
Anal Chem ; 86(24): 12093-9, 2014 Dec 16.
Artículo en Inglés | MEDLINE | ID: mdl-25409265

RESUMEN

A simple and sensitive approach is proposed and evaluated for determination of ultratrace Zn and Cd in limited amounts of samples or tens of cells based on a novel single drop (5-20 µL) solution electrode glow discharge assisted-chemical vapor generation technique. Volatile species of Zn and Cd were immediately generated and separated from the liquid phase for transporting to atomic fluorescence or atomic mass spectrometric detectors for their determination only using hydrogen when the glow discharge was ignited between the surface of a liquid drop and the tip of a tungsten electrode. Limits of detection are better than 0.01 µg L(-1) (0.2 pg) for Cd and 0.1 µg L(-1) (2 pg) for Zn, respectively, and comparable or better than the previously reported results due to only a 20 µL sampling volume required, which makes the proposed technique convenient for the determination of Zn and Cd in limited amounts of samples or even only tens of cells. The proposed method not only retains the advantages of conventional chemical vapor generation but also provides several unique advantages, including better sensitivity, lower sample and power consumption, higher chemical vapor generation efficiencies and simpler setup, as well as greener analytical chemistry. The utility of this technique was demonstrated by the determination of ultratrace Cd and Zn in several single human hair samples, Certified Reference Materials GBW07601a (human hair powder) and paramecium cells.


Asunto(s)
Cadmio/análisis , Electrodos , Gases em Plasma , Zinc/análisis , Humanos , Límite de Detección , Espectrometría de Masas , Espectrometría de Fluorescencia
13.
Analyst ; 139(10): 2538-44, 2014 May 21.
Artículo en Inglés | MEDLINE | ID: mdl-24691520

RESUMEN

A dual-mode chemical vapor generation integrating hydride generation and photochemical vapor generation was developed for simultaneous multi-element analysis of hydride-forming and non-hydride-forming elements by atomic fluorescence spectrometry. Four elements were selected as model elements of hydride-forming (As, Cd) and non-hydride-forming (Ni, Fe) elements to validate this proposed method. Standard or sample solutions were separately pumped to mix with tetrahydroborate, and concentrated formic acid and ammonia, and then directed to a hydride generator and a photochemical reactor to realize simultaneous hydride generation and photochemical vapor generation, respectively. Optimum conditions for dual-mode chemical vapor generation were carefully investigated. Under the optimized conditions, limits of detection of 0.05, 0.008, 0.8 and 0.1 µg L(-1) were obtained for As, Cd, Fe and Ni, respectively. The precisions were 5.0, 5.5, 4.3 and 4.5% (n = 6, RSDs) for 2 µg L(-1) of As, 1 µg L(-1) of Cd, 50 µg L(-1) of Fe and 10 µg L(-1) of Ni, respectively. This method was validated for accuracy with three certified reference water samples and applied to the simultaneous determination of these elements in a tap water sample with spike recoveries in the range of 95-99%.

14.
Anal Chim Acta ; 1287: 342132, 2024 Jan 25.
Artículo en Inglés | MEDLINE | ID: mdl-38182354

RESUMEN

BACKGROUND: Recently, headspace single-drop microextraction (HS-SDME) has attracted some attention for developing sensitive and selective colorimetric assays due to its excellent capability to reduce matrix interference and enrich analytes. However, the single droplet limits direct visual observation of color change and its quantitative measurement suffers from reduced optical path length. Therefore, amplifying the detection signals in both volume and intensity is an important and challenging task for improving the sensitivity, stability, and accuracy of such colorimetric analysis. RESULTS: In this study, a "headspace-nanoenzyme" (HS-NE) strategy was proposed that successfully addressed these challenges and enabled the colorimetric and fluorescent dual-mode detection of trace Hg2+. Atomic Hg0, generated via chemical vapor generation (CVG), underwent headspace reaction with AuNPs droplet to form Au@HgNPs, thus catalyzing the oxidation of o-phenylenediamine (OPD) in the presence of H2O2. The absorbance and fluorescence intensity of oxidized OPD were proportion to the concentration of Hg2+ in the sample solution. Due to the greatly enhanced peroxidase-like activity by Au@HgNPs, the limit of detection was as low as 0.98 nM and 0.21 nM for the colorimetric and fluorescent modes, respectively. The applicability of this assay was further demonstrated with determination of Hg2+ in real environmental and biological samples. Moreover, a convenient and cost-effective paper-based sensing platform was fabricated for rapid on-site detection of Hg2+. SIGNIFICANCE AND NOVELTY: This novel HS-NE strategy combines HS-SDME and nanoenzyme-based sensing to achieve dual effects of eliminating matrix interference and amplifying the measurement signal, resulting in improved accuracy, enhanced stability, high sensitivity, and exceptional selectivity, with great potential for on-site determination of trace Hg2+.


Asunto(s)
Mercurio , Nanopartículas del Metal , Colorimetría , Oro , Peróxido de Hidrógeno , Colorantes , Peroxidasas
15.
Analyst ; 138(8): 2249-53, 2013 Apr 21.
Artículo en Inglés | MEDLINE | ID: mdl-23471437

RESUMEN

A simple and economical multi-channel optical sensor using corona discharge radical emission spectroscopy is developed and explored as an optical nose for discrimination analysis of volatile organic compounds, wines, and even isomers.

16.
Minerva Anestesiol ; 89(10): 876-883, 2023 10.
Artículo en Inglés | MEDLINE | ID: mdl-36800809

RESUMEN

BACKGROUND: Pain following open reduction and internal fixation of distal radius fracture (DRF) can be significant. This study compared the intensity of pain up to 48 hours after volar plating for DRF, associated to either an ultrasound guided distal nerve block (DNB) or surgical site infiltration (SSI). METHODS: In this prospective single blind randomized study, 72 patients scheduled for DRF surgery under 1.5% lidocaine axillary block were allocated to receive, at the end of surgery, either an ultrasound-guided median and radial nerves block with ropivacaine 0.375% (DNB) performed by the anesthesiologist or a SSI with the same drug regimen, performed by the surgeon. Primary outcome was the duration between analgesic technique (H0) and pain reappearance (Numerical Rating Scale (NRS 0-10)>3). Secondary outcomes were the quality of analgesia, the quality of sleep, the magnitude of motor blockade, and the patient satisfaction. The study was built on a statistical hypothesis of equivalence. RESULTS: Fifty-nine patients were included in the final per-protocol analysis (DNB=30, SSI=29). Time to reach NRS>3 was (in median [95%CI]) 267 min [155;727] and 164 min [120;181] respectively after DNB and SSI (difference=103 min [-22;594] - rejection of equivalence hypothesis). Pain intensity throughout the 48 hours, quality of sleep, opiate consumption, motor blockade and patient satisfaction was not significantly different between groups. CONCLUSIONS: Although DNB provides a longer analgesia than SSI, both techniques gave comparable level of pain control during the first 48 hours after surgery, without any difference in the incidence of side effects or patient satisfaction.


Asunto(s)
Analgesia , Fracturas de la Muñeca , Humanos , Dolor Postoperatorio/tratamiento farmacológico , Estudios Prospectivos , Método Simple Ciego , Analgesia/métodos , Nervio Radial , Anestésicos Locales/uso terapéutico
17.
Guang Pu Xue Yu Guang Pu Fen Xi ; 32(10): 2842-6, 2012 Oct.
Artículo en Zh | MEDLINE | ID: mdl-23285900

RESUMEN

Two types of manganese oxides, the octahedral layer structure (OL) and the octahedral molecular tunnel structure (OMS), were controllably synthesized via a facilely hydrothermal route and used to remove heavy metal ions (Pb2+, Cu2+, Ni2+ , Hg2+) in solutions. The heavy metal ion concentrations before and after adsorption were determined by atomic absorption spectroscopy (AAS) and atomic fluorescence spectroscopy (AFS) to evaluate the material adsorption performance. The competitive adsorption of the four ions (Pb2+, Cu2+, Ni2+, Hg2+) on manganese oxides was also investigated. The results showed that OMS exhibited better adsorption ability than OL and had excellent adsorption selectivity to Pb2+, with 98% adsorption efficiency in two minutes. Therefore, this can be proposed as a simple, green and efficient method for treatment of polluted water.

18.
Anal Chem ; 83(13): 5050-5, 2011 Jul 01.
Artículo en Inglés | MEDLINE | ID: mdl-21599029

RESUMEN

A novel microplasma molecular emission spectrometer based on an atmospheric pressure dielectric barrier discharge (DBD) is described and further used as a promising multichannel GC detector for halohydrocarbons. The plasma is generated in a DBD device consisting of an outer electrode (1.2 mm in diameter) and an inner electrode (1.7 mm in diameter) within a small quartz tube (3.0 mm i.d. × 5.0 mm o.d. × 50 mm), wherein analyte molecules are excited by the microplasma to generate molecular emission. Therefore, the analytes are selectively and simultaneously detected with a portable charge-coupled device (CCD) via multichannel detection of their specific emission lines. The performance of this method was evaluated by separation and detection of a model mixture of chlorinated hydrocarbons (CHCl(3) and CCl(4)), brominated hydrocarbons (CH(2)Br(2) and CH(2)BrCH(2)Br), and iodinated hydrocarbons (CH(3)I and (CH(3))(2)CHI) undergoing GC with the new detector. The completely resolved identification of the tested compounds was achieved by taking advantages of both chromatographic and spectral resolution. Under the optimized conditions with the CCD spectrometer set at 258, 292, and 342 nm channels for determination of chlorinated hydrocarbons, brominated hydrocarbons, and iodinated hydrocarbons, respectively, this detector with direct injection provided detection limits of 0.07, 0.06, 0.3, 0.04, 0.05, and 0.02 µg mL(-1) for CCl(4), CHCl(3), CH(2)Cl(2), CH(3)I, CH(3)CH(2)I, and (CH(3))(2)CHI, respectively.

19.
Anal Chem ; 83(17): 6552-8, 2011 Sep 01.
Artículo en Inglés | MEDLINE | ID: mdl-21761923

RESUMEN

In this work, a novel dual-channel sensing mode, i.e., UV-induced surface photovoltage (SPV) and photoluminescence (PL) on n-type Si/TiO(2)/Eu(3+)-doped TiO(2) (n-Si/TiO(2)/TiO(2):Eu), was demonstrated for the discrimination of 20 volatile compounds. The SPV signaling in this work employed a laboratory-constructed microvoltammeter with good analytical performances. This device also features wireless communication, portability, along with low cost and power consumption. The SPV and PL pattern of each analyte was distinct, and the hierarchical clustering analysis (HCA) result showed that these 20 volatile species were distinguishable, even for structural isomers. Linear discriminant analysis (LDA) further demonstrated the robustness of this sensor: 180 unknown samples from three groups at concentrations of 15.3, 31.7, and 79.2 mg/L were classified with accuracies of 96.7%, 95.0%, and 100%, respectively. Principal component analysis (PCA) revealed that SPV and PL channels contributed equally to the good discrimination ability due to two distinct sensing mechanisms. This dual-channel sensor was also successfully applied in the discrimination of beverage samples such as liquor, wine, and vinegar.

20.
Guang Pu Xue Yu Guang Pu Fen Xi ; 31(7): 1946-9, 2011 Jul.
Artículo en Zh | MEDLINE | ID: mdl-21942058

RESUMEN

A simple method has been developed for the determination of silver in environmental water samples using solid phase extraction with tungsten-coil electrothermal atomic absorption spectrometry. Silica gel was used as an adsorbent and packed into a syringe barrel for solid phase extraction of silver prior to its determination by using a portable tungsten-coil electrothermal atomic absorption spectrometer. Optimum conditions for adsorption and desorption of silver ion, as well as interferences from co-existing ions, were investigated. A sample pH value of 6.0, a sample loading flow rate of 4.0 mL x min(-1), and the mixture of 4% (m/v) thiourea and 2% (phi) nitrate acid with the eluent flow rate of 0.5 mL x min(-1) for desorption were selected for further studies. Under optimal conditions, a linear range of 0.20-4.00 ng x mL(-1), a limit of detection (3sigma) of 0.03 ng x mL(-1) and a preconcentration factor of 94 were achieved. The proposed method was validated by testing three environmental water samples with satisfactory results.

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