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1.
    
ICP-MS is used as an element selective detector for chromium species in aquatic samples using a coupled columm system consisting of a cation guard column and an anion column. The effects of large concentrations of disturbing ions, like NO3, Cl, CO32– and SO42–, are discussed and the comparison with the use of different chromium isotopes for data acquisition is given. Quite low concentrations such as 100 mg/l of CO32–, 10 mg/l Cl and even 5 mg/l SO42– can cause an overestimation of chromium if not properly resolved1995 / Accepted: 24 October 1995  相似文献   

2.
This study describes the development of an analytical methodology based on the use of microchip electrophoresis (ME) devices integrated with capacitively coupled contactless conductivity detection (C4D) for the separation and detection of inorganic anions in post‐blast explosive residues. The best separation condition was achieved using a running buffer composed of 35 mmol/L lactic acid, 10 mmol/L histidine and 0.070 mmol/L cetyl(trimethyl ammonium) bromide. For C4D measurements, the highest sensitivity was obtained applying a 700 kHz sinusoidal wave with excitation voltage of 20 Vpp. The separation of Cl?, NO3?, NO2?, SO42?, ClO4? and ClO3? was performed within ca. 150 s with baseline resolution and efficiencies between 4.4 × 104 and 1.7 × 105 plates/m. The found limits of detection ranged between 2.5 and 9.5 μmol/L. Last, real samples of post‐blast explosive residues were analyzed on the ME‐C4D devices obtaining successfully the determination of Cl?, NO3? and SO42?. The achieved concentration values varied between 12.8–72.5 mg/L for Cl?, 1.7–293.1 mg/L for NO3? and 1.3–201.3 mg/L for SO42?. The data obtained using ME‐C4D devices were in good agreement with the concentrations found by ion chromatography. The approach reported herein has provided short analysis time, instrumental simplicity, good analytical performance and low cost. Furthermore, the ME‐C4D devices emerge as a powerful and portable analytical platform for on‐site analysis demonstrating to be a promising tool for the crime scene investigation.  相似文献   

3.
Anion sensor properties of N‐alkyl‐substituted 1,4′‐diazaflavonium bromides in methanol–water were evaluated by UV–vis spectrometry. Pronounced changes were observed in the absorption spectra of all compounds for only OH?, CO32?, and CN? among F?, Cl?, Br?, I?, OH?, CO32?, NO3?, PO43?, CN?, SO42?, HSO4?, HCO3?, SCN?, NO2?, and P2O72? ions. Two new absorption bands at 385 and 685 nm accompanying the distinct color change for OH?, CO32?, and CN? ions were observed in case of all compounds. The color changes were from pink to blue for CO32? and OH? ions and from pink to purple for CN? ion. Thanks to the distinct color change, the compounds can be used as selective colorimetric anion sensors. Linear changes of absorbance of N‐heptyl‐substituted compound at 385 nm as a function of the ion concentration were used to determine CN? ion in water samples. Detection and quantification limits of the proposed method were 0.94 and 2.82 mg/L, respectively.  相似文献   

4.
The cloud point (CP) of triblock-copolymer L31 aqueous solution was determined with salting-out salts (Na2SO4/Na2CO3/NaF/NaCl/NaBr). The results show that all these salts can decrease the CP of L31 aqueous solution and form aqueous two-phase system (ATPS). With increasing concentrations of Na2SO4 and Na2CO3, an obvious phase inversion could be observed and phase inversion points were found. This was mainly due to the change in density, the salt-rich phase shifted from the top phase to the bottom phase. Meanwhile, the liquid-liquid equilibrium (LLE) data for L31-Na2SO4/Na2CO3/NaF/NaCl/NaBr ATPSs were measured at 288.15 K. The salt ability to decrease the CP and to induce the phase separation is as follows: Na2SO4?>?Na2CO3, NaF?>?NaCl?>?NaBr. Finally, the order of anions that reduced the CP and caused phase separation was obtained as follows: SO42? >CO32?, F??>?Cl??>?Br?.  相似文献   

5.
Abstract

The use of ion-exchange chromatography with an IonPac AS 14 column, 3.5 mM Na2CO3/1.0 mM NaHCO3 eluent and suppressed conductivity detection provides a simple, cost-effective, fast, accurate, and highly sensitive method for the determination of F?, Cl?, NO2 ?, Br?, NO3 ?, PO4 2?, SO4 2?, and C2O4 2? at low μ/L levels in environmental samples. Data on sensitivity, selectivity, accuracy, and % relative standard deviation are described. The method is suitable for many environmental applications including atmospheric aerosols (exposed on cellulose, glass fiber, and quartz filters), rainwater, cloud water, potable- and non-potable waters, and carbonated waters. Dominant components of the aerosol were SO4 2?, NO3 ?, and Cl?. Rainwater, on the other hand, has relatively very low concentrations of these three species. The wide-spread concentration range for Cl? in variety of water samples and the high concentrations for SO4 2? in drinking water are striking. Determination of the anionic composition of carbonated waters revealed a considerable variation of the individual anions.  相似文献   

6.
Gliding arc discharge process was used for the treatment of methyl violet wastewater. First, the intermediate products were studied by gas chromatography coupled with mass spectrometry and Fourier transform infrared spectrometry, and ultraviolet–visible spectrometer. Second, the effects of inorganic anions including chloride (Cl?), carbonate (CO3 2?), sulfate (SO4 2?), phosphate (PO4 3?), nitrate (NO3 ?) on the degradation efficiency of methyl violet were examined. The research results indicated that hydroxyl radicals attacked carbon atom that situated in the center of dye molecule, and the conjugating structure of methyl violet was destroyed, and dye was degraded and decolored, so a possible degradation pathway was proposed by the analysis of intermediate products detected. The methyl violet degradation rate decreased with increasing anions concentrations, and their order of sequence according to the inhibition reaction was CO3 2? > Cl? > SO4 2? > NO3 ?.  相似文献   

7.
We present the development of a method for the simultaneous determination of inorganic nitrogen species in oxidized (NO2, NO3) and reduced (NH4+) forms using ion chromatography with diode‐array detection (205, 208, and 425 nm, respectively). The oxidized forms were determined directly after the separation in the anion exchanger, while the reduced form was determined in the column hold‐up time after derivatization with the Nessler reagent. The use of an appropriate modifier (Seignette reagent) and mobile phase (NaCl) enabled the determination of inorganic nitrogen species in highly salinated environmental samples (water, sediments). Moreover, low detection limits were obtained of 0.04 mg/L for NH4+ and 0.006 and 0.005 mg/L for NO2 and NO3, respectively. The analysis of environmental samples indicated NH4+ contents of up to 1161 ± 47 mg/kg and NO3 of up to 148 ± 6 mg/kg for sediment samples, as well as the NH4+ concentrations of up to 0.98 ± 0.10 mg/L, NO2 of up to 24 ± 1 mg/L and NO3 of up to 20 ± 1 mg/L for water samples.  相似文献   

8.
A new ion chromatography method is described for the simultaneous determination of Cl, NO3 and SO42−, using a selected eluent 1.3-mM sodium gluconate/1.3-mM borax (pH 8.5). The extraction methods of Cl, NO3, SO42− in vegetables are studied. The determination limits of Cl, NO3, SO42− are 0.17 μg/ml, 0.63 μg/ml and 0.81 μg/ml. The linear ranges are 060 μg/ml, 090 μg/ml and 090 μg/ml. The relative S.D. are <2.5%. The mean recoveries of Cl, NO3, SO42− in vegetables range from 97.0 to 104%.  相似文献   

9.
《Analytical letters》2012,45(5):890-901
Abstract

A highly selective polyvinyl chloride (PVC) membrane electrode, based on N,N′‐(aminoethyl)ethylenediamide bis(2‐benzoideneimine) binuclear copper(II) complex [Cu(II)‐AEBB] as neutral carrier, was prepared for thiocyanate (SCN?) determination, which displays an anti‐Hofmeister selectivity sequence for a series of anions in the following order: SCN?>ClO4 ?>Sal? > I?>NO3 ?>Br?> Cl?>NO2 ?>SO3 2?>F?>H2PO4 ?>SO4 2?. The electrode exhibited near‐Nernst response for SCN? with a slope of –59.0 mV/decade over a wide concentration range (8.5×10?7~6.8×10?1 mol/L) with a detection limit of –5.0×10?7 mol/L in pH 5.0 phosphate buffer solution at 25°C. Alternating current (AC) impedance and equivalent circuits were used to investigate the thiocyanate response mechanism of the membrane doped with [Cu(II)‐AEBB].  相似文献   

10.
Dioctylarsinic acid, HDOAA, in chloroform (0.1 M) extracts thulium(III), dysprosium(III) and samarium(III) from their aqueous solutions in the pH ranges 1–6.5, 2–7 and 4–8, respectively, with extraction coefficients of approximately 0.1 for the lowest and 10 for the highest pH. The extractability increased with increasing ionic strength for each ion and decreased in the order ClO4- > NO3- > Cl- > SO42- > acetate for solutions of the same molarity. pH-Dependence curves had slopes ranging from 1.05 to 1.87. The reagent-dependence studies gave curves with slopes between 3.60 and 5.30. The general formula [MXn(DOAA)m(HDOAA)p(H2O)q] (X = Cl-. NO3-, SO42-/2, ClO4-, acetate, OH-; n+m=3, m+p=4 or 5, q?0)is suggested for the extracted species.  相似文献   

11.
An efficient fluorescence probe, 4‐methyl‐2,6‐bis((thiophen‐2‐ylmethylimino)methyl)phenol (DFPTMA) and its SCN? adduct has been synthesized and characterized by different spectroscopic techniques like 1H NMR,13C NMR, QTOF‐MS ES+, UV‐Vis and FTIR spectroscopy. Single crystal X‐ray structure of DFPTMA is reported. In presence of SCN?, DFPTMA exhibits significant fluorescence enhancement (λEx, 455 nm, λEm, 504 nm) in aqueous methanol (water‐methanol, 1:4, V/V, 0.1 mol/L HEPES buffer, pH 7.4). Common bio‐relevant anions viz. CH3COO?, NO2?, NO3?, Cl?, Br?, I?, SO42?, HSO4?, N3?, HAsO42?, Cr2O72?, H2PO4?, ClO4?, NCO?, CN?, CO32?, F?, PO43?, S2?, HS? do not interfere in the recognition of SCN?. Lowest detection limit for SCN? is 0.88 µmol/L with response time <5 min. The SCN? assisted enhancement in emission intensity may be attributed to the formation of H‐bond which enhances the rigidity of the molecular assembly.  相似文献   

12.
It was demonstrated that Cl, SO4 2-, NO3 -, N3 -, ClO3 , and ClO4 ions can be simultaneously and selectively determined by capillary electrophoresis using 2,4-ionene as a capillary modifier. The effect of n-butanol additives to the buffer electrolyte on the migration times of ions was shown. The optimum buffer electrolyte contained 0.5 mM Na2CrO4, 0.05% 2,4-ionene, 10%n-butanol, and 7% methanol. It was shown that azide can be identified in wash solutions obtained at the place of lead azide explosion. The detection limit for azide was 1–3 mg/L.  相似文献   

13.
The inability to separate fluoride, phosphate and sulfate by electrostatic ion chromatography (EIC) was overcome by using an ODS silica column coated with mixed zwitterionic-cationic surfactants as the stationary phase. The best results were obtained using the zwitterionic surfactant, 3-(N,N-dimethylmyristylammonium)-propanesulfonate (C19H41NO3S), and the cationic surfactant, myristyltrimethylammonium, CH3(CH2)13N+(CH3)3, in a 10:1 molar ratio in the column coating solution. With a dilute solution of sodium tetraborate as the eluent the model analyte anions were completely separated in the following elution order: F, HPO4 2–, SO4 2–, Cl, NO2 , Br, NO3 . The very early elution of phosphate and sulfate is most unusual and is unique to this system. Detection limits better than 1.1 × 10–4 mM and linear calibration plots up to 7.0 mM were obtained with a suppressed conductivity system.  相似文献   

14.
A new series of tris(2‐aminoethyl)amine (tren)‐based L ‐alanine amino acid backboned tripodal hexaamide receptors (L1–L5) with various attached moieties based on electron‐withdrawing fluoro groups and lipophilicity have been synthesized and characterized. Detailed binding studies of L1–L5 with different anions, such as halides (F?, Cl?, Br?, and I?) and oxyanions (AcO?, BzO? (Bz=benzoyl), NO3?, H2PO4?, and HSO4?), have been carried out by isothermal titration calorimetric (ITC) experiments in acetonitrile/dimethylsulfoxide (99.5:0.5 v/v) at 298 K. ITC titration experiments have clearly shown that receptors L1–L4 invariably form 1:1 complexes with Cl?, AcO?, BzO?, and HSO4?, whereas L5 forms a 1:1 complex only with AcO?. In the case of Br?, I?, and NO3?, no appreciable heat change is observed owing to weak interactions between these anions and receptors; this is further confirmed by 1H NMR spectroscopy. The ITC binding studies of F? and H2PO4? do not fit well for a 1:1 binding model. Furthermore, ITC binding studies also revealed slightly higher selectivity of this series of receptors towards AcO? over Cl?, BzO?, and HSO4?. Solid‐state structural evidence for the recognition of Cl? by this new category of receptor was confirmed by single‐crystal X‐ray structural analysis of the complex of tetrabutylammonium chloride (TBACl) and L1. Single‐crystal X‐ray diffraction clearly showed that the pentafluorophenyl‐functionalized amide receptor (L1) encapsulated Cl? in its cavity by hydrogen bonds from amides, and the cavity of L1 was capped with a TBA cation through hydrogen bonding and ion‐pair interactions to form a capped‐cleft orientation. To understand the role of the cationic counterpart in solution‐state Cl? binding processes with this series of receptors (L1–L4), a detailed Cl? binding study was carried out with three different tetraalkylammonium (Me4N+, Et4N+, and Bu4N+) salts of Cl?. The binding affinities of these receptors with different tetralkylammonium salts of Cl? gave binding constants with the TBA cation in the following order: butyl>ethyl>methyl. This study further supports the role of the TBA countercation in ion‐pair recognition by this series of receptors.  相似文献   

15.
A series of CuII metallo‐assemblies showing anion‐directed structural variations, including five metallocages [(Gn?)?{Cu2(Hdpma)4}](8?n)+(A?)8?n (Gn?=NO3?, ClO4?, SiF62?, BF4?, SO42?; A?=NO3?, ClO4?, BF4?, CH3SO4?; Hdpma=bis(3‐pyridylmethyl)ammonium cation), a complex double salt, namely, (H3dpma)4(CuCl4)5Cl2, and a coordination chain, namely, [Cu2(dpma)(OAc)4], are reported. The influence of the anion can be explained by its coordinating ability, the affinity of which for the CuII center interferes significantly with metallocage formation, and its shape, which offers host–guest recognition ability to engage in weak metal–anion coordination and hydrogen bonding to the organic ligand, which are responsible for metallocage templation. EPR studies of these metallocages in the powder phase at room temperature and 77 K showed a trend of the g values (g||>2.10>g>2.00) indicating a ‐based ground state with square‐pyramidal geometry for the CuII centers. The magnetism of these metallocages can be interpreted as the result of a combination of relatively small magnetic coupling integrals and a substantial contribution of temperature‐independent paramagnetism (TIP). The weak magnetic interaction is corroborated by the results of DFT calculations and the EPR spectra. Availability of the low‐lying state for spin population was confirmed by a magnetization study, which revealed a magnetic moment approaching 2, which would explain the presence of the larger TIP term.  相似文献   

16.
Three Cu(II) complexes constructed from 4-(2-pyridyl)-1H-1,2,3-triazole (L), namely, [CuL2Cl2]·H2O, [CuL2(CH3OH)(NO3)]NO3 and [CuL2(H2O)]SO4, have been synthesized and characterized. X-ray crystal structure analyses revealed that [CuL2Cl2]·H2O and [CuL2(CH3OH)(NO3)]NO3 have octahedral geometries, whilst [CuL2(H2O)]SO4 adopts a square-pyramidal coordination geometry. In all three complexes, the Cu(II) atoms are chelated by two L ligands in the basal plane, whilst the apical positions are occupied by Cl?, NO3?, CH3OH or H2O. The bandgaps between the HOMO and LUMO were estimated by cyclic voltammetry (CV) and diffuse reflectance spectroscopy (DRS) to be 3.43, 3.12, and 3.74 eV, respectively. Theoretical calculations on each structure gave similar results to the experiments. Frontier molecular orbital analyses showed that the higher electron density on the apical ligand, the lower the bandgap.  相似文献   

17.
The effect the salting-out agent anion nature has on the temperature and concentration intervals of the existence of the separation area is established by analyzing the phase diagrams of pseudoternary KCl (KBr, KI, KNO3, K2SO4, K4P2O7)–potassium bis(alkyl polyoxyethylene)phosphate (oxyphos B)–water systems. It is concluded that the anionic salting-out capability is reduced in the order P2O74-> SO42-> Cl? > Br?> NO74-> SO3-> I?. The thermodynamic parameters of phase separation used to interpret the results are calculated. The observed pattern of a change in the salting-out ability of the investigated salts relative to aqueous solutions of the surfactants is in good agreement with the lyotropic (Hofmeister) series.  相似文献   

18.
In this study, trimetal Mg/Ce/Mn oxide-modified diatomaceous earth (DE) was synthesized at optimal conditions. Comparison of the SEM images and the results of EDX analyses of the raw and the modified DE confirmed the surface modification of the raw DE with the trimetal oxide. Groundwater fluoride removal capacity of the sorbent was evaluated by batch method at various defluoridation conditions. At a sorbent dosage of 0.6 g/100 mL (contact time: 60 min, mixing speed of 200 rpm and temperature: 297 K), the fluoride removal was >93% for solutions containing initial fluoride concentration of 10–60 mg/L. Sorbent’s optimum fluoride uptake capacity was 12.63 mg/g at the initial fluoride concentration of 100 mg/L. Fluoride removal was >91% for solutions with initial pH range of ∼4–11 (initial fluoride concentration: 9 mg/L, sorbent dosage: 0.6 g/100 mL). Appraisal of the effect of co-existing anions on fluoride removal showed that CO32− would reduce the amount of fluoride removed from solution, while other anions such as PO43−, NO3 and SO42− had no observable effect. K2SO4 solution was found to be most suitable for regeneration of spent Mg/Ce/Mn oxide-modified DE compared to Na2CO3 and NaOH. The mechanism of fluoride removal at pH > 5.45 (pHpzc = 5.45) occurred by exchange of hydroxyl groups on surface of sorbent with fluoride ions from solution. Sorption data fitted better to Langmuir isotherm and pseudo-second-order model. External diffusion was observed to be the sorption rate limiting factor.  相似文献   

19.
Reaction of a imidazole phenol ligand 4‐(imidazlo‐1‐yl)phenol (L) with 3d metal salts afforded four complexes, namely, [Ni(L)6] · (NO3)2 ( 1 ), [Cu(L)4(H2O)] · (NO3)2 · (H2O)5 ( 2 ), [Zn(L)4(H2O)] · (NO3)2 · (H2O) ( 3 ), and [Ag2(L)4] · SO4 ( 4 ). All complexes are composed of monomeric units with diverse coordination arrangements and corresponding anions. All the hydroxyl groups of monomeric cations are used as hydrogen‐bond donors to form O–H ··· O hydrogen bonds. However, the coordination habit of different metal ions produces various supramolecular structures. The NiII atom shows octahedral arrangement in 1 , featuring a 3D twofold inclined interpenetrated network through O–H ··· O hydrogen bond and π–π stacking interaction. The CuII atom of 2 displays square pyramidal environment. The O–H ··· O hydrogen bond from the [Cu(L)4(H2O)]2+ cation and lattice water molecule as well as π–π stacking produce one‐dimensional open channels. NO3 ions and lattice water molecules are located in the channels. 3 is a 3D supramolecular network, in which ZnII has a trigonal bipyramid arrangement. Two different rings intertwined with each other are observed. The AgI in 4 has linear and triangular coordination arrangements. The mononuclear units are assembled into a 1D chain by hydrogen bonding interaction from coordination units and SO42– anions.  相似文献   

20.
For the isocratic ion chromatography (IC) separation of low-molecular-mass organic acids and inorganic anions three different anion-exchange columns were studied: IonPac AS14 (9 μm particle size), Allsep A-2 (7 μm particle size), and IC SI-50 4E (5 μm particle size). A complete baseline separation for all analyzed anions (i.e., F, acetate, formate, Cl, NO2, Br, NO3, HPO42− and SO42−) in one analytical cycle of shorter than 17 min was achieved on the IC SI-50 4E column, using an eluent mixture of 3.2 mM Na2CO3 and 1.0 mM NaHCO3 with a flow rate of 1.0 mL min−1. On the IonPac AS14 column, it was possible to separate acetate from inorganic anions in one run (i.e., less than 9 min), but not formate, under the following conditions: 3.5 mM Na2CO3 plus 1.0 mM NaHCO3 with a flow rate of 1.2 mL min−1. Therefore, it was necessary to adapt a second run with a 2.0 mM Na2B4O7 solution as an eluent under a flow rate of 0.8 mL min−1 for the separation of organic ions, which considerably enlarged the analysis time. For the Allsep A-2 column, using an eluent mixture of 1.2 mM Na2CO3 plus 1.5 mM NaHCO3 with a flow rate of 1.6 mL min−1, it was possible to separate almost all anions in one run within 25 min, except the fluoride-acetate critical pair. A Certified Multianion Standard Solution PRIMUS for IC was used for the validation of the analytical methods. The lowest RSDs (less than 1%) and the best LODs (0.02, 0.2, 0.16, 0.11, 0.06, 0.05, 0.04, 0.14 and 0.09 mg L−1 for F, Ac, For, Cl, NO2, Br, NO3, HPO42− and SO42−, respectively) were achieved using the IC SI-50 4E column. This column was applied for the separation of concerned ions in environmental precipitation samples such as snow, hail and rainwater.  相似文献   

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