0000000000276120
AUTHOR
S. Meseguer-lloret
Chemiluminescent method for detection of eutrophication sources by estimation of organic amino nitrogen and ammonium in water.
An automatic method has been developed for the estimation of organic amino nitrogen (CH2-NH) and ammonium in water samples. We propose a continuous flow system in which nitrogen compounds react with hypochlorite reagent to produce chloramines. Subsequently, the mixture is mixed with luminol, generating a chemiluminescence signal. The signal emission at 425 nm, registered as a function of time, decreases as nitrogen concentration increases, due to the decrease on hypochlorite concentration. A large number of nitrogen compounds have been assayed and their sensitivities compared, in milligrams per liter nitrogen. The ammonium calibration graph, expressed as N, can be used for most of the assay…
FI automatic method for the determination of copper(II) based on coproporphyrin I-Cu(II)/TCPO/H(2)O(2) chemiluminescence reaction for the screening of waters.
Abstract In this paper, an automatic method for the screening of water samples containing Cu(II) was proposed, based on peryoxalate chemiluminescence reaction using coproporphyrin I as fluorophor compound to provide selectivity and a simple flow injection (FI) chemiluminescence detector (CLD). FI system conditions were chosen in order to distinguish samples over or under legislation limit established (50 μg l−1) with high reliability. The detection limit found was 9 μg l−1 and the linear dynamic range was 15–125 μg l−1 of Cu(II). Repeatibility and reproducibility studies gave good precision and accuracy with recovery near 100%. Under these conditions, the method resulted selective and only …
Magnetic molecularly imprinted polymer for the simultaneous selective extraction of phenoxy acid herbicides from environmental water samples
[EN] A selective magnetic molecularly imprinted polymer (MMIP) was synthetized with 4-chloro-2-methylphenoxyacetic acid as template and 4-vinylpiridine as monomer in presence of vinylized magnetite nanoparticles. Scanning electron microscopy, nitrogen adsorption-desorption isotherms, Fourier transform infrared spectrometry and vibrating sample magnetometry were applied to characterize the resulting material. The synthesized MMIP was applied as sorbent in magnetic molecularly imprinted solid-phase extraction (MMISPE) for selective extraction of a mixture of the five herbicides 4-chloro-2-methylphenoxyacetic acid (MCPA), 4-(4-chloro-2-methylphenoxy)butyric acid (MCPB), mecoprop (MCPP), fenoxa…
Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography
[EN] In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch®), or mixtures of H2O2 and H2SO4, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification…
Preparation of monolithic polymer-magnetite nanoparticle composites into poly(ethylene-co-tetrafluoroethylene) tubes for uses in micro-bore HPLC separation and extraction of phosphorylated compounds
[EN] This paper describes the fabrication of a novel microbore monolithic column modified with magnetite nanoparticles (MNPs) prepared in a poly(ethylene-co-tetrafluoroethylene) (EFTE) tubing, and its application as stationary phase for the chromatographic separation of phosphorylated compounds. In order to obtain the composite column, a two-step procedure was performed. The formation of a glycidyl methacrylate-based monolith inside the activated ETFE tube was firstly carried out. Then, two incorporation approaches of MNPs in monoliths were investigated. The generic polymer was modified with 3-aminopropyltrimethoxysilane (APTMS) to be subsequently attached to MNP surfaces. Alternatively, AP…
Influence of water sample storage protocols in chemiluminescence detection of trace elements.
This paper shows the influence of different sample storage protocols, on the chemiluminescence signal of some metal ions. The storage protocols studied were: acid addition (HCl or HNO(3)) and no reagent addition to filtered and refrigerated (T=4 degrees C) samples. Light emission was produced for the chemiluminescence reaction between luminol and hydrogen peroxide in buffer carbonate conditions (pH 10.8) catalysed by Cr(III), Co(II) and Cu(II). Batch and/or flow modes in different conditions were tested. Fe(II), Fe(III), Ni(II) and Mn(II) did not give chemiluminescence in the studied conditions. A parallel study of sensitivity and selectivity was performed. Then the presence or absence of t…
Selective determination of ammonium in water based on HPLC and chemiluminescence detection
Abstract A selective and sensitive method has been developed for liquid chromatographic determination of ammonium in water samples. The analyte is derivatized with Dansyl Chloride prior to injection into HPLC. Optimal solution derivatization conditions have been established. The dansyl derivative is separated with the aid of a chromatographic column and post-column mixed with peroxyoxalate (TCPO) and H 2 O 2 in order to perform chemiluminescence detection. The detection limit achieved is 8 μg/L and linear response from 0.027 to 0.750 mg/L of ammonium was obtained. Ammonium ion was determined within 2.4 min under optimum chromatographic conditions. The method is fast, and near 10 derivatized…
A microscale Kjeldahl nitrogen determination for environmental waters.
A microscale Kjeldahl system has been designed which has been homemade reduced. The digestor unit of a macroKjeldahl system and a modified glassware microdistillation unit have been used. The optimal conditions for digestion and distillation have been established for ammonium and methylamine as model compound of organic amino nitrogen. The optimised procedure has been applied to the determination of Kjeldahl nitrogen in water samples. Recoveries near 100% and good precision have been achieved. This procedure combines nitrogen miniaturized system and the use of a selective ion electrode for ammonia detection. The analysis time was reduced 4.8 times and the analysis cost 6.6 times compared wi…
Polymer-based materials modified with magnetite nanoparticles for enrichment of phospholipids
[EN] A polymeric material modified with magnetic nanoparticles (MNPs) has been synthesized and evaluated as sorbent both for solid-phase extraction (SPE) and dispersive magnetic solid-phase extraction (MSPE) of phospholipids (PLs) in human milk samples. The synthesized sorbent was characterized by scanning electron microscopy and its iron content was also determined. Several experimental variables that affect the extraction performance (e.g. loading solvent, breakthrough volume and loading capacity) were investigated and a comparison between conventional SPE and MSPE modalities was done. The proposed method was satisfactorily applied to the analysis of PLs in human milk fat extracts in diff…
Photografted fluoropolymers as novel chromatographic supports for polymeric monolithic stationary phases
[EN] In this study, porous polymer monoliths were in situ synthesized in fluoropolymers tubing to prepare microbore HPLC columns. To ensure the formation of robust homogeneous polymer monoliths in these housing supports, the inner surface of fluoropolymer tubing was modified in a two-step photografting process. Raman spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the inner poly(ethylene-co-tetrafluoroethylene) (ETFE) wall and the subsequent attachment of a monolith onto the wall. Poly(glycidyl methacrylate-co-divinylbenzene), poly(butyl methacrylate-co-ethyleneglycol dimethacrylate) and poly(styrene-co-divinylbenzene) monoliths were in situ synt…
A guide for selecting the most appropriate method for ammonium determination in water analysis
Abstract We have critically evaluated the main parameters involved in determining ammonium in water samples, in order to select the most suitable method appropriate to the requirements of the analysis. We compared several methods: reference (ion-selective electrodes, Nessler and indophenol); Roth’s modified; based on luminol reaction; and, based on peroxioxalate reaction.