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1.
Hong Yu  Hongjing Ai  Qian Chen 《Chromatographia》2009,70(7-8):1017-1022
Ion-interaction chromatography with direct conductivity detection has been used for analysis of nitrate and nitrite. Chromatographic separation was performed on a monolithic silica-based C18 column dynamically modified with tetrabutylammonium (TBA+). Using the optimized mobile phase, containing 2.0 mmol L?1 TBA+ and 0.8 mmol L?1 citrate (pH 6.0), delivered at a flow rate of 6.0 mL min?1, separation of five anions (chloride, nitrite, bromide, nitrate, and sulfate) was achieved in only 40 s at a column temperature of 30 °C. The detection limits for nitrate and nitrite were 0.74 and 0.92 mg L?1, respectively. The relative standard deviation (RSD, n = 5) of the retention times of nitrate and nitrite was 0.1% and RSD of chromatographic peak areas were 0.4 and 0.2%, respectively. The method was successfully used for analysis of the anions in groundwater. Recovery of nitrate and nitrite was 99.1 and 105%, respectively.  相似文献   

2.
Nitrate ions were used as the oxidant in the cathode chamber of a microbial fuel cell (MFC) to generate electricity from organic compounds with simultaneous nitrate removal. The MFC using nitrate as oxidant could generate a voltage of 111 mV (1,000 Ω) with a plain carbon cathode. The maximum power density achieved was 7.2 mW m−2 with a 470 Ω resistor. Nitrate was reduced from an initial concentration of 49 to 25 mg (NO3−N) L−1 during 42-day operation. The daily removal rate was 0.57 mg (NO3–N) L−1 day−1 with a voltage generation of 96 mV. In the presence of Pt catalyst dispersed on cathode, the cell voltage was significantly increased up to 450 mV and the power density was 117.7 mW m−2, which was 16 times higher than the value without Pt catalyst. Significant nitrate removal was also observed with a daily removal rate of 2 mg (NO3–N) L−1 day−1, which was 3.5 times higher compared with the operation without catalyst. Nitrate was reduced to nitrite and ammonia in the liquid phase at a ratio of 0.6% and 51.8% of the total nitrate amount. These results suggest that nitrate can be successfully used as an oxidant for power generation without aeration and also nitrate removal from water in MFC. However, control of the process would be needed to reduce nitrate to only nitrogen gas, and avoid further reduction to ammonia.  相似文献   

3.
An activated carbon from Coconut (Cocos nucifera) shells was prepared by physical activation with carbon dioxide and water vapor. The activated carbon obtained has a surface area of 1058 m2 g?1 and such a high micropore volume of 0.49 cm3 g?1. This carbon was studied for the removal of lead from water. Sorption studies were performed at 30 °C, at different pH and adsorbent doses, in batch mode. Lead precipitation was observed on the surface of the activated carbon. Maximum adsorption occurred at pH 9 for an adsorbent dose of 2 g L?1. Kinetic studies, at the initial concentration of 150 mg L?1 of lead, pH 5 and an adsorbent dose of 1 g L?1, yielded an equilibrium time of 50 h for this activated carbon. The kinetic data were modeled with the pseudo first order, the pseudo second order and the Bangham models. The pseudo second order model fitted the data well. The sorption rate constant (7 × 10?4 mol?1 Kg s?1) and the maximum amount of lead adsorbed (0.23 mol kg?1) are quite good compared to the data found in literature. Sorption equilibrium studies were conducted in a concentration range of lead from 0 to 150 mg L?1. In an aqueous lead solution with an initial concentration of 30 mg L?1, at pH 5, adsorbent dose 1 g L?1, activated Coconut shell carbon removed at equilibrium 100 % of the heavy metal. The equilibrium data were modeled with the Langmuir and Freundlich equations, of which the former gave the best fit. The Langmuir constants Qmax eq (0.23 mol kg?1) and KL (487667 L mol?1) are in good agreement with literature. XPS studies identified adsorbed species as lead carbonates and/or lead oxalates and precipitates as lead oxide and/or lead hydroxide on the activated carbon surface. The Coconut shell activated carbon is a very efficient carbon due to its high surface area, to the presence of many micropores on its surface and to the presence surface groups like hydroxyls promoting adsorption in the porous system and lead crystal precipitation on the activated carbon surface.  相似文献   

4.
A sensitive flow-injection method for the chemiluminescent determination of ultra-low concentration of nitrate in water is presented. Nitrate is on-line photolytically converted to peroxynitrite by absorption of UV light inside of 60 mm long quartz capillary (i.d. 530 µm, o.d. 720 µm). Peroxynitrite is subsequently determined by the chemiluminescent reaction with luminol. The detection limit of nitrate is 7 × 10?10 M (S/N = 3). The linear range of the method is 2 × 10?9–1 × 10?5 M nitrate. The interference of nitrite is eliminated by its conversion to nitrogen after mixing of sample with a solution of sulfamidic acid. Other common anions do not interfere. The interference of cations is eliminated by passing the sample through a cation-exchange column. The FIA procedure allows analysing of 15 samples per hour. The method was applied to the determination of nitrate in various real water samples. The results are in good agreement with a reference ion chromatographic method.  相似文献   

5.
Hongzhe Tian 《Chromatographia》2011,73(5-6):457-462
A method for determination of chlormequat (CCC) residue in fruits by liquid chromatography?Ctandem mass spectrometry (LC?CMS?CMS) was developed. Residue of CCC was extracted from samples with methanol?Cwater (v/v, 1:1) containing 1.0% acetic acid, cleaned up by strong cationic exchange (SCX) cartridge, and then determined by LC?CMS?CMS. The method showed good linearity over the concentration range 0.002?C5.0 mg kg?1 with correlation coefficient above 0.997. The limit of detection (LOD) and limit of quantitation (LOQ) for CCC were 5 × 10?4 mg kg?1 (S/N = 3) and 0.002 mg kg?1 (S/N = 10), respectively. Recoveries for CCC at three spiked levels (0.025, 0.050, and 0.20 mg kg?1) were in the range 80?C102%. Estimation of measurement uncertainty was calculated for CCC at the level of 0.025 mg kg?1 in fruits. The results demonstrated that the uncertainty of recovery was the main contribution to the combined standard uncertainty. The relative combined standard uncertainties associated with the method ranged from 11 to 13%, depending on the sample matrices.  相似文献   

6.

Novel instrumental set up is developed for surface tension (γ, N m?1), viscosity (η, N s m?2)) and dipole moment (μ/Debye) measurements. A new instrument is economic, viable and pollution free in use, the γ, η and μ from viscosities (η, N s m?2) and surface tension (γ, N m?1) for 0.005 to 0.125 g% polystyrene at an interval of 0.0005 g% in benzene are measured at 288.15, 293.15, and 298.15 Kelvin temperatures. The γ, η, and μ are reported stronger frictional and cohesive forces due to stronger interactions of polystyrene with benzene. The survismeter is highly accurate and mechanically operated for pulling up liquid from reservoir bulb B1 to operational bulbs B2, B3, and B4. Densities are higher than those of benzene and also infer stronger polystyrene–benzene interactions, and hydrodynamic volume (HV) calculated with intrinsic viscosity [η] is noted in 293.15 (HV) >298.15 (HV) >288.15 (HV) order with higher values at 293.15 K. Surface tension (γ) values are slightly higher than of benzene and fall in a range of 33.47 to 33.35 N m?1.  相似文献   

7.
A novel and simple coating method was developed by coating bovine serum albumin (BSA) onto the inner surface of a fused-silica capillary, to avoid the adsorption of analytes during CE. The advantage presented here was that the coating process is more simple, fast, stable, and reproducible. The coated capillary avoided the adsorption of analytes onto the inner surface of a fused-silica capillary and might be a promising candidate for separation of complex biological samples with further development. Meanwhile, the efficiencies of the coated capillary were evaluated by EOF, chromatographic peak shape, and theoretical plate number (N m?1) of RNase A. The optimal coating conditions were obtained from the results. The pH value of coating buffer PB was 4.2, the standing time was 12 h at 4 °C, and the coating concentration of BSA was 1.5 mg mL?1. The stability of the coating on the inner wall of the capillary and the reproducibility of the coated capillaries were good. The theoretical plate number values of RNase A were over 1.3 × 105 (N m?1) in the coated capillary. After successive electrophoresis for 48 h using the coated capillary, the RSD values of EOF and the theoretical plate number were 4.14 % and 9.14 %, respectively. In addition, the RSD values of EOF and the theoretical plate number (N m?1) in the coated capillaries were 13.19 % and 8.96 %, respectively. Finally, the coated capillary was successfully applied to separate the mixture of four basic proteins (RNase A, lysozyme, trypsin and myoglobin).  相似文献   

8.
Clays and specially bentonite are widely used as natural adsorbents for wastewater treatment and as a barrier in landfills to prevent the contamination of subsoil and groundwater by leachates containing radioactive materials. The adsorption of four radionuclides, 134Cs(I), 90Sr(II), 133Ba(II) and 152Eu(III) by an Egyptian bentonite (Bent) and its modified Na+ form (Na-Bent) collected from a deposit within Alexandria governorate was investigated as a function of different parameters. The batch equilibrium technique was used and the kinetic results showed that the equilibrium was mostly reached within 10 min and the kinetic data fit well to the pseudo-second order model. The Langmuir model fits well the experimental data of all metals adsorption on Bent and Na-Bent except for adsorption of 133Ba on Bent, while 152Eu adsorption on Na-Bent fits better to the Freundlich model rather than to the Langmuir. Both Bent and Na-Bent fit well to the D-R model with adsorption energy of E > 8 kJ mol?1 that means that the adsorption reaction is expected to be controlled by both cation exchange and surface complexation reactions. At lower concentrations, the values of distribution coefficient (K d), follow the order of 152Eu > 90Sr > 134Cs > 133Ba for Bent and Na-Bent. The K d of 152Eu is higher than that of 134Cs in Bent up to 150 mg L?1. This order changes at higher concentration where the K d of 134Cs becomes higher than 152Eu after 150 mg L?1 for Bent and after 200 mg L?1 for Na-Bent. Na-Bent is preferred than Bent for the uptake of 90Sr and 134Cs especially at high concentration.  相似文献   

9.
In this study, we investigated the impact of nitrate dose on toluene degradation by Pseudomonas putida to elucidate the upper limit of nitrate concentration and whether an optimum ratio of nitrate to toluene concentration exists. Batch microcosm studies were conducted in order to monitor toluene degradation for various ratios (2–20) of nitrate to toluene with nitrate concentrations ranging from 0 to 700 mg?L?1 for a given toluene concentration of 50 and 25 mg?L?1 during 4-day (short term) and 14-day (long term) incubation time, respectively. The short-term study revealed that nitrate concentration of 500 mg?L?1 was toxic to bacteria and the optimum concentration was 300 mg?L?1 yielding the highest toluene degradation rate (0.083 mg?L?1?h?1). In the batch study of long term, toluene degradation was limited to 6 days after which the nitrate at 50 mg?L?1 was depleted, indicating that nitrate was a necessary electron acceptor. For both batch studies, an optimum ratio of 6 was found yielding the highest toluene degradation rate. This indicates that an appropriate nitrate dose is essential for efficient degradation of toluene when bioremediation of groundwater contaminated with toluene is under consideration.  相似文献   

10.
In this study, the removal of nitrate using ZnO, MgO, and CeO2 nanoparticles (NPs) modified by humic acid from water was tested. Nanoparticles were modified by humic acid using the microwave-assisted technique and then modified ZnO (Zn–H), modified MgO (Mg–H), and modified CeO2 (Ce–H) were characterized through SEM, EDX, FTIR, and XRD analysis. Several important parameters influencing the removal of nitrate such as contact time, pH, adsorbent dosage and temperature were explored systematically by batch experiments. Isotherm studies were set up with the following optimum conditions: pH?=?5, adsorbent concentration of 1 g L?1, 180 min and 25 °C. The results revealed that the adsorption were best fitted to pseudo-second order and simple Elovich kinetics models. Langmuir, Freundlich and linear adsorption models were fitted to describe adsorption isotherms and constants. The isotherm analysis indicated that the adsorption data can be represented by both Freundlich and linear isotherm models. The maximum adsorption capacity (qm) was obtained at 55.1, 74.2 and 75.8 mg g?1 for Zn–H, Ce–H, and Mg–H, respectively. The thermodynamic parameters such as free energy, enthalpy and entropy of adsorption were obtained. From the thermodynamic parameters, it is suggested that the adsorption of nitrate on modified NPs (MNPs) followed the exothermic and spontaneous processes. The obtained results showed that the MNPs were efficient adsorbents for removing nitrate from aqueous media.  相似文献   

11.
《Analytical letters》2012,45(7):948-957
Abstract

A rapid, microwave-based extraction method was employed to oxidize all forms of nitrogen to nitrate in environmental samples using persulfate. The digest was then analyzed spectrophotometrically after an offline reduction of nitrate to nitrite using a cadmium reductor column was completed. The precision of the method was tested at the 0.5 mg l?1 level and was 5.2% (N = 10). The detection limit based on S/N = 3 was calculated to be 0.15 mg l?1. The method was thoroughly validated by comparison of analytical techniques and intralaboratory comparison studies.  相似文献   

12.
The removal of Th4+ ions from aqueous solutions was investigated using single-layer graphene oxide (GO) as a sorbent which was prepared by the modified Hummers’ method through batch adsorption experiments at room temperature. Structural characterizations of the sorbent were also investigated. The influences of the pH value of solution, contact time, sorbent dose, ionic strength, the initial metal ion concentration and temperature on the adsorption of Th4+ were also investigated. These results indicated that the adsorption of Th4+ was dependent on the pH and independent on the ionic strength. The sorbent provided significant Th4+ removal (>98.7 %) at pH 3.0 and the adsorption equilibrium was achieved after only 10 min. The Langmuir adsorption isotherm fit the absorption profile very closely, and indicated that a maximum adsorption capacity of 1.77 mmol g?1 of GO (411 mg g?1) after 2 h. The thermodynamic parameters showed that this adsorption process was endothermic and spontaneous. Moreover, the desorption level of Th4+ from GO, by using 0.1 mol L?1 H2SO4 as a stripping agent, was 84.2 ± 1.2 %, and that of 0.5 mol L?1 HNO3 as a stripping agent, was 79.8 ± 3.0 %.  相似文献   

13.
The anaerobic treatment of raw vinasse in a combined system consisting in two methanogenic reactors, up-flow anaerobic sludge blanket (UASB) + anaerobic packed bed reactors (APBR), was evaluated. The organic loading rate (OLR) was varied, and the best condition for the combined system was 12.5 kg COD m?3day?1 with averages of 0.289 m3 CH4 kg COD r?1for the UASB reactor and 4.4 kg COD m?3day?1 with 0.207 m3 CH4 kg COD r?1 for APBR. The OLR played a major role in the emission of H2S conducting to relatively stable quality of biogas emitted from the APBR, with H2S concentrations <10 mg L?1. The importance of the sulphate to COD ratio was demonstrated as a result of the low biogas quality recorded at the lowest ratio. It was possible to develop a proper anaerobic digestion of raw vinasse through the combined system with COD removal efficiency of 86.7% and higher CH4 and a lower H2S content in biogas.  相似文献   

14.
This study investigated the feasibility to produce biohydrogen of a mechanically stirred anaerobic sequencing batch biofilm reactor (AnSBBR) treating sucrose-based synthetic wastewater. The bioreactor performance (30 °C) was evaluated as to the combined effect of fill time (2, 1.5, and 1 h), cycle length (4, 3, and 2 h), influent concentration (3,500 and 5,250 mg chemical oxygen demand (COD)?L?1) and applied volumetric organic load (AVOLCT from 9.0 to 27.0 g COD L?1 d?1). AVOLs were varied according to influent concentration and cycle length (t C). The results showed that increasing AVOLCT resulted in a decrease in sucrose removal from 99 to 86 % and in improvement of molar yield per removed load (MYRLS.n) from 1.02 mol H2?mol carbohydrate?1 at AVOLCT of 9.0 g COD L?1 d?1 to maximum value of 1.48 mol H2?mol carbohydrate?1, at AVOLCT of 18.0 g COD L?1 d?1, with subsequent decrease. Increasing AVOLCT improved the daily molar productivity of hydrogen (MPr) from 15.28 to 49.22 mol H2?m?3 d?1. The highest daily specific molar productivity of hydrogen (SMPr) obtained was 8.71 mol H2?kg TVS?1 d?1 at an AVOLCT of 18.0 g COD L?1 d?1. Decreasing t C from 4 to 3 h decreased sucrose removal, increased MPr, and improved SMPr. Increasing influent concentration decreased sucrose removal only at t C of 2 h, improved MYRLS,n and MPr at all t C, and also improved SMPr at t C of 4 and 3 h. Feeding strategy had a significant effect on biohydrogen production; increasing fill time improved sucrose removal, MPr, SMPr, and MYRLS,n for all investigated AVOLCT. At all operational conditions, the main intermediate metabolic was acetic acid followed by ethanol, butyric, and propionic acids. Increasing fill time resulted in a decrease in ethanol concentration.  相似文献   

15.
A method for determining carbonyl emissions from motor vehicles was developed in which exhaust gases from test vehicles running on a dynamometer are directly collected in 6-L Teflon bags and then introduced into pentafluorophenyl hydrazine -coated adsorbent tubes for derivatisation and subsequent analysis of generated derivatives by GC/MS. Twenty gasoline and LPG light-duty vehicles were sampled at a vehicle inspection station in Guangzhou, China, by running test vehicles over a transient testing cycle and analysed for carbonyls. Results show that the method can achieve a detection limit of 8–28 ng m?3 for individual carbonyls with a relative standard deviation of 14.5%. Twenty-four carbonyls were identified in the gasoline vehicle exhaust gases and their total concentration was 19.2 mg m?3. For the LPG vehicles, 20 carbonyls were found in the exhaust gases with a total concentration of 4.71 mg m?3. Based on the results, carbonyl emission factors for the gasoline and LPG vehicles were estimated to be 25.0 and 7.36 mg km?1, respectively.  相似文献   

16.
《Analytical letters》2012,45(11):1952-1964
The distributions of cadmium and lead in marine sediments, surrounding soil, stones, and atmospheric particulate matter were determined at different locations in Split, Croatia. The determination of cadmium and lead was performed by flame atomic absorption spectrometry whereas atmospheric particulate matter samples were analyzed by inductively coupled plasma–optical emission spectrometry. Cadmium concentrations in the stones and soil were between 0.2 to 0.6 µg g?1 and 0.2 to 0.9 µg g?1. The concentration in the atmospheric particulate matter were <0.2 µg m?2 d?1(detection limit) to 1.4 µg m?2 d?1. Lead concentrations in marine sediments, stones, soil, and atmospheric particulate matter ranged from 31.2 to 144.4 µg g?1, 9.3 to 29.4 µg g?1, 11.3 to 66.1 µg g?1, and 0.5 to 241.4 µg m?2 d?1, respectively. The relationship between determined parameters was established using principal component analysis and the results are in agreement with the assumption that anthropogenic sources play important roles for lead and cadmium distribution.  相似文献   

17.
In this study we present quantitative elemental analysis techniques like energy dispersive X-ray fluorescence analysis and instrumental neutron activation analysis to assess the impact of industrial discharge on environment. Two cases are discussed, i.e., (a) enrichment of zinc levels in the soil (1080 ± 76 mg kg?1) and zinc uptake ranging between 628 and 40 mg kg?1 in edible plants and cereals grown in agricultural fields near an active zinc smelter, Rajasthan; (b) depth-wise distribution of Cr, Pb and other metals in the sediment core samples from Sundarban wetland, West Bengal, indicating waste discharge from tanneries and other industries.  相似文献   

18.
As the addition of low concentrations of oxygen can favor the initial degradation of benzene, toluene, ethylbenzene, and xylenes (BTEX) compounds, this work verified the applicability of the microaerobic technology to enhance BTEX removal in an anaerobic bioreactor supplemented with high and low co-substrate (ethanol) concentrations. Additionally, structural alterations on the bioreactor microbiota were assessed throughout the experiment. The bioreactor was fed with a synthetic BTEX-contaminated water (~ 3 mg L?1 of each compound) and operated at a hydraulic retention time of 48 h. The addition of low concentrations of oxygen (1.0 mL min?1 of atmospheric air at 27 °C and 1 atm) assured high removal efficiencies (> 80%) for all compounds under microaerobic conditions. In fact, the applicability of this technology showed to be viable to enhance BTEX removal from contaminated waters, especially concerning benzene (with a 30% removal increase), which is a very recalcitrant compound under anaerobic conditions. However, high concentrations of ethanol adversely affected BTEX removal, especially benzene, under anaerobic and microaerobic conditions. Finally, although bacterial community richness decreased at low concentrations of ethanol, in general, the bioreactor microbiota could deal with the different operational conditions and preserved its functionality during the whole experiment.  相似文献   

19.
A yolk–shell-structured sphere composed of a superparamagnetic Fe3O4 core and a carbon shell (Fe3O4@HCS) was etched from Fe3O4@SiO2@carbon by NaOH, which was synthesized through the layer-by-layer coating of Fe3O4. This yolk–shell composite has a shell thickness of ca. 27 nm and a high specific surface area of 213.2 m2 g?1. Its performance for the magnetic removal of tetracycline hydrochloride from water was systematically examined. A high equilibrium adsorption capacity of ca. 49.0 mg g?1 was determined. Moreover, the adsorbent can be regenerated within 10 min through a photo-Fenton reaction. A stable adsorption capacity of 44.3 mg g?1 with a fluctuation <10% is preserved after 5 consecutive adsorption–degradation cycles, demonstrating its promising application potential in the decontamination of sewage water polluted by antibiotics.  相似文献   

20.
The objective of this study was to develop a simple, efficient and reliable method for routine quantitative analysis for Psoralea corylifolia L. An ultra performance liquid chromatography with DAD detector system was employed for simultaneous quantification of ten compounds. The chromatographic analysis was performed by UPLC with C18 column and gradient elution of 0.05% formic acid aqueous solution and acetonitrile in 16 min. All calibration curves were linear (R 2 ≥ 0.9990) over the tested ranges. The LOD and LOQ were lower to 13.07 and 39.22 ng mL?1 with 2 μL of injection volume, respectively. The intra- and inter-day precisions as determined from sample solutions were below 4.1 and 4.2%. The average recoveries were ranged from 94.2 to 108.8% with RSDs ≤ 4.6%. This validated method was applied for the analysis of ten analytes in P. corylifolia L. from different origins. The variation of the content of ten compounds was remarkable among the tested samples: psoralenoside increased from 7.42 to 17.04 mg g?1, isopsoralenoside from 6.05 to 14.34 mg g?1, psoralen from 2.37 to 3.90 mg g?1, isopsoralen from 2.53 to 3.65 mg g?1, neobavaisoflavone from 1.59 to 2.96 mg g?1, bavachin from 1.02 to 2.35 mg g?1, psoralidin from 0.45 to 1.91 mg g?1, isobavachalcone from 1.33 to 4.71 mg g?1, corylifol A from 1.02 to 2.40 mg g?1 and bakuchiol from 28.10 to 63.89 mg g?1.  相似文献   

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