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1.
Anal Methods ; 16(25): 4178-4186, 2024 Jun 27.
Artigo em Inglês | MEDLINE | ID: mdl-38874550

RESUMO

A novel bifunctional magnetic sorbent with mercapto and amino groups and ion imprinting (MBII) was synthesized using a one-step aqueous sol-gel process for preconcentration and determination of Cd(II) ions. MBII was employed as a microcolumn (MC) filler in a flow-through system coupled to GFAAS. The magnetic properties of the solid allowed microcolumn magnetic solid-phase extraction (MCMSPE) to be performed by simply including a single circular magnet around the MC. This assembly enabled complete attachment of the solid to the MC wall leaving a central void to facilitate higher sample flow rates without blockage or material loss. For comparison, a bifunctional magnetic solid without imprinting (MBNI) was also synthesized and evaluated. Both MBII and MBNI were characterized by FTIR, SEM, EDX, BET and magnetization measurements. The results showed the preservation of the magnetic core, its superparamagnetism and the functional groups in the solid. Batch studies revealed a maximum adsorption capacity for both materials at pH around 6 with equilibrium reached within 5 minutes. The advantages were reflected in the maximum adsorption capacity of MBII, which was found to be 2.5 times greater than that of MBNI. Both adsorbents were compared as MC fillers for dynamic preconcentration in MCMSPE systems. Under optimized conditions, MBNI showed a PCF of 125 and MBII of 250. The higher selectivity of MBII was corroborated by interfering ion studies. The analytical performance parameters for the proposed method using MBII as an adsorbent showed a detection limit of 0.05 ng L-1, a linear range of 2.0-80 ng L-1, an RSD% of 2.2 (n = 7; 20 ng L-1) and a lifetime of more than 300 preconcentration-elution cycles without loss of sensitivity or need for refilling. The method was successfully applied to the determination of trace Cd(II) in osmosis, lake and tap water with recoveries ranging from 98 to 105%. Comparison of these results with those of similar reported methods showed a considerable improvement primarily attributed to the combined effect of MBII's higher retention capacity and its magnetic properties that allowed higher sample flow rates and, thus, enhanced figures of merit.

2.
Sci Rep ; 13(1): 7971, 2023 05 17.
Artigo em Inglês | MEDLINE | ID: mdl-37198446

RESUMO

Peatlands in southern South America (Tierra del Fuego region, TdF) play a key role in the ecological dynamics of Patagonia. It is, therefore, necessary to increase our knowledge and awareness of their scientific and ecological value to ensure their conservation. This study aimed to assess the differences in the distribution and accumulation of elements in peat deposits and Sphagnum moss from the TdF. Chemical and morphological characterization of the samples was carried out using various analytical techniques, and total levels of 53 elements were determined. Furthermore, a chemometric differentiation based on the elemental content of peat and moss samples was performed. Some elements (Cs, Hf, K, Li, Mn, Na, Pb, Rb, Si, Sn, Ti and Zn) showed significantly higher contents in moss samples than in peat samples. In contrast, only Mo, S and Zr were significantly higher in peat samples than in moss samples. The results obtained highlight the ability of moss to accumulate elements and to act as a means to facilitate the entry of elements into peat samples. The valuable data obtained in this multi-methodological baseline survey can be used for more effective conservation of biodiversity and preservation of the ecosystem services of the TdF.


Assuntos
Briófitas , Sphagnopsida , Ecossistema , Sequestro de Carbono , Monitoramento Ambiental/métodos , Sphagnopsida/química , Solo , Carbono
3.
Talanta ; 253: 123898, 2023 Feb 01.
Artigo em Inglês | MEDLINE | ID: mdl-36108519

RESUMO

A method based on flow injection hydride generation atomic absorption spectrometry (FI-HGAAS) with an on-line pre-reduction of Se(VI) to Se(IV) was developed and optimized to determine phosphate-extractable Se (0.1 M phosphate buffer KH2PO4/K2HPO4 at pH 7). The extracted fraction involves water-soluble Se (i.e. the most mobile Se fraction) and exchangeable Se (i.e. sorbed onto soil component surface). Kinetic discrimination mechanisms allowed the complete removal of interferences caused by organic matter due to the formation of humic substances (HS)-Se(IV) complexes observed when batch pre-reduction processes were used. Se(IV) and Se(VI) recoveries ranged 95-105% at a fortification level of 150 µg kg-1. The pre-reduction was efficiently carried out in 20 s in a 6 M HCl medium at 100 °C. Results from phosphate-extractable fractions were comparable to those obtained by ICP-MS. Se bound to organic matter was released digesting the remaining material from the phosphate buffer extraction with 0.1 M K2S2O8. Detection and quantification limits were 15 µg kg-1 Se and 50 µg kg-1 Se, respectively, in each fraction. The methodology was applied to 10 agricultural soils from Argentina with total Se concentration levels between 130 µg kg-1 and 419 µg kg-1.


Assuntos
Selênio , Espectrofotometria Atômica , Solo , Fosfatos
4.
Anal Methods ; 14(30): 2920-2928, 2022 08 04.
Artigo em Inglês | MEDLINE | ID: mdl-35861161

RESUMO

In this paper we present the determination of ultratraces of cadmium ions in water by means of a minicolumn (MC) flow-through preconcentration system coupled with graphite furnace atomic absorption spectrometry. The core of the system is a lab-made ion imprinted magnetic organosilica nanocomposite which is employed as filler of the MC for the selective retention of the analyte. In this case superparamagnetic magnetite nanoparticles were coated with an amine-functionalized shell and ion imprinted with Cd(II) by a simple sol-gel co-condensation method. The setup was completed with the inclusion of a magnet fixed around the packed MC. This assembly - which is studied with an MII material for the first time here - allowed a homogeneous distribution of the solid on the walls of the MC, leaving a hole in the center and enabling the absence of material bleeding or obstructions to the free movement of fluids. Ion imprinted (MII) and non-imprinted (MNI) materials were studied for comparison purposes. Both were characterized and compared by DRX, FTIR, and SEM and their magnetic behavior by magnetization curves. Batch experiments showed an equilibration time of less than 10 minutes and a maximum adsorption pH of around 7 for both solids. The maximum capacity for MII was greater than that of MNI (200 mg g-1 and 30 mg g-1 respectively) and thus, the former was chosen for analytical purposes. Under MC dynamic conditions, sample and elution flow rates, volumes of the sample and eluant, and type and concentration of the most suitable eluant have been thoroughly investigated and optimized. Under the optimal experimental conditions, the MII filler showed a preconcentration factor of 200, a limit of detection of 0.64 ng L-1, a linear range of 2.5-100 ng L-1, RSD% of 1.9 (n = 6; 10 ng L-1) and a lifetime of more than 800 cycles of concentration-elution with no loss of sensitivity or need for refilling. The effect of potentially interfering ions on the percent recovery of cadmium was also studied. The proposed method was successfully applied to the determination of traces of Cd(II) in osmosis and tap water with recoveries of 98.0-101.3%. A comparison with similar methods is also provided.


Assuntos
Grafite , Nanocompostos , Cádmio/análise , Cádmio/química , Fenômenos Magnéticos , Espectrofotometria Atômica/métodos , Água
5.
Food Res Int ; 128: 108777, 2020 02.
Artigo em Inglês | MEDLINE | ID: mdl-31955751

RESUMO

The purpose of this paper is to investigate the trace metal content in edible biomonitors (i.e., mollusks) in the Beagle Channel (southern Patagonia) and to assess the human health risks associated with their consumption. Rationale: The monitoring breakdown structure (MBS) conceptual model was applied to four sampling campaigns (2005 → 2012) that collected 729 samples of Mytilus chilensis and Nacella magellanica. The composition of trace elements (Cd, Cr, Cu, Ni, Pb and Zn) in the mollusks was determined using graphite furnace (GFAAS) or flame atomic absorption spectrometry (FAAS). We compared the mean obtained values with the maximum levels (MLs) of each element established by international organizations. Then, based on semi-structured interviews, we calculated the estimated daily intake (EDI) of local residents and compared it with safety reference doses, i.e., the provisional tolerable daily intake (PTDI), provisional maximum tolerable daily intake (PMTDI), and tolerable daily intake (TDI), as well as the benchmark dose level lower confidence limit for Pb (BMDL01, a reference point (RP)/point of departure (POD). Moreover, to obtain information about the potential health risks of ingesting heavy metals (HMs) through mollusk consumption, we evaluated the target hazard quotient (THQ) and the hazard index (HI). Findings: For Cd and Pb, 65% and 40% of bivalves exceeded the MLs established by the Mercado Común del Sur (Mercosur), respectively. Except for Cd in N. magellanica (i.e., 1.20 µg/kg/bw/day), EDI values were clearly lower than the safety reference doses. For Cr, Cu, Ni, Pb and Zn, mussels were safe for consumption and did not raise concerns for public health. Likewise, THQ values were well below one for most of the studied metals, indicating that the exposed human population is assumed to be safe. Occasional high consumers of mollusks from the most contaminated sites may be at some health risk. Originality: The food production system and the environment are complex systems; this is crucial to understand when we consider ecosystems as a food source (i.e., marine ecosystems). Here we consider edible biomonitors, that are organisms that can have a dual function. They are food, and at the same time, if properly calibrated, they can act as indicators of environmental quality. This study is the first to investigate relevant essential and non-essential trace metal content in two edible mollusks from the Beagle Channel in a long-term survey (2005 → 2012). The information variety was high; approximately thirteen thousand determinations were conducted to support the risk assessment for mollusk consumption. Other aspects connected with the health risks and the uncertainty factors related to the presence of essential and non-essential minerals in edible mollusks as well as the use of the MBS are also discussed.


Assuntos
Monitoramento Ambiental/métodos , Contaminação de Alimentos , Gastrópodes/química , Metais Pesados/química , Mytilus/química , Poluentes Químicos da Água/química , Animais , Argentina , Ecossistema , Metais Pesados/metabolismo , Oceanos e Mares , Medição de Risco
6.
Ecotoxicology ; 21(4): 1112-25, 2012 May.
Artigo em Inglês | MEDLINE | ID: mdl-22350107

RESUMO

With the aim to evaluate the mollusk Nacella (P)magellanica as biomonitor of elemental pollution in seawater of the Beagle Channel, more than one hundred individuals of the gastropod were sampled, separated in viscera and muscle, and then examined with respect to the accumulation of Cd, Cr, Cu, Ni, Pb and Zn. Collection was performed in seven strategic locations along 170 km of the coastal area of the Beagle Channel (Tierra del Fuego, Argentina) in two campaigns during 2005 and 2007. Samples of surrounding seawater in the different sites were obtained and tested for the same metals as well. The accumulation capacity of Nacella (P)magellanica and thus its aptitude as biomonitor, was evaluated through the calculus of the preconcentration factors of the metals assayed. A discussion involving the comparison with other mollusks previously tested will be given. Several statistical approaches able to analyze data with environmental purposes were applied. Non parametric univariate tests such as Kruskal-Wallis and Mann-Whitney were carried out to assess the changes of the metal concentrations with time (2005 and 2007) in each location. Multivariate methods (linear discriminant analysis on PCA factors) were also applied to obtain a more reliable site classification. Johnson's probabilistic method was carried out for comparison between different geographical areas. The possibility of employing these results as heavy metals' background levels of seawater from the Beagle Channel will be debated.


Assuntos
Monitoramento Ambiental/métodos , Gastrópodes/química , Oligoelementos/análise , Poluentes Químicos da Água/análise , Animais , Argentina , Ecossistema , Metais Pesados/análise , Água do Mar
7.
Ecotoxicology ; 20(6): 1341-53, 2011 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-21544557

RESUMO

In order to test the aptitude of individuals of Mytilus chilensis as biomonitors of heavy metals pollution in seawater, several samples of this mollusk together with surrounding seawater samples were collected along 170 km of the coastal area of the Beagle Channel (Tierra del Fuego, Argentina) in 2005 and 2007. The study, performed in seven locations strategically selected, involved the determination of Cd, Cr, Cu, Ni, Pb and Zn in seawaters and mollusks by atomic absorption spectrometry (AAS) and the calculation of the respective concentration factors (CFs). Obtained data were standardized and analyzed by multivariate techniques in order to establish differences between sampling sites and periods. Obtained results will be shown and the bioaccumulation ability of M. chilensis will be evaluated by comparison with results obtained for Mytilus species in different geographical marine areas. A fully discussion on the possibility of employing the results as background levels for comparative purposes in other marine waters of the world will be provided. The possible harm derived from human consumption of these mollusks will be also assessed.


Assuntos
Metais/metabolismo , Mytilus/metabolismo , Poluentes Químicos da Água/metabolismo , Animais , Argentina , Monitoramento Ambiental , Água do Mar/química , Poluição Química da Água/estatística & dados numéricos
8.
J Hazard Mater ; 188(1-3): 311-8, 2011 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-21345585

RESUMO

A simple and robust on-line sequential injection system based on solid phase extraction (SPE) coupled to a flow injection hydride generation atomic absorption spectrometer (FI-HGAAS) with a heated quartz tube atomizer (QTA) was developed and optimized for the determination of As(III) in groundwater without any kind of sample pretreatment. The method was based on the selective retention of inorganic As(V) that was carried out by passing the filtered original sample through a cartridge containing a chloride-form strong anion exchanger. Thus the most toxic form, inorganic As(III), was determined fast and directly by AsH(3) generation using 3.5 mol L(-1) HCl as carrier solution and 0.35% (m/v) NaBH(4) in 0.025% NaOH as the reductant. Since the uptake of As(V) should be interfered by several anions of natural occurrence in waters, the effect of Cl(-), SO(4)(2-), NO(3)(-), HPO(4)(2-), HCO(3)(-) on retention was evaluated and discussed. The total soluble inorganic arsenic concentration was determined on aliquots of filtered samples acidified with concentrated HCl and pre-reduced with 5% KI-5% C(6)H(8)O(6) solution. The concentration of As(V) was calculated by difference between the total soluble inorganic arsenic and As(III) concentrations. Detection limits (LODs) of 0.5 µg L(-1) and 0.6 µg L(-1) for As(III) and inorganic total As, respectively, were obtained for a 500 µL sample volume. The obtained limits of detection allowed testing the water quality according to the national and international regulations. The analytical recovery for water samples spiked with As(III) ranged between 98% and 106%. The sampling throughput for As(III) determination was 60 samplesh(-1). The device for groundwater sampling was especially designed for the authors. Metallic components were avoided and the contact between the sample and the atmospheric oxygen was carried to a minimum. On-field arsenic species separation was performed through the employ of a serial connection of membrane filters and anion-exchange cartridges. Advantages derived from this approach were evaluated. HPLC-ICPMS was employed to study the consistency of the analytical results.


Assuntos
Arsênio/análise , Arsenicais/análise , Espectrofotometria Atômica/instrumentação , Água/análise , Desenho de Equipamento , Limite de Detecção , Extração em Fase Sólida , Espectrofotometria Atômica/métodos , Abastecimento de Água/análise
9.
Talanta ; 82(3): 923-30, 2010 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-20678647

RESUMO

Several studies involving the physicochemical interaction of three silica based hybrid mesoporous materials with metal ions of the group IB have been performed in order to employ them for preconcentration purposes in the determination of traces of Cu(II), Ag(I) and Au(III). The three solids were obtained from mesoporous silica functionalized with 3-aminopropyl (APS), 3-mercaptopropyl (MPS) and N-[2-aminoethyl]-3-aminopropyl (NN) groups, respectively. Adsorption capacities for Au, Cu and Ag were calculated using Langmuir's isotherm model and then, the optimal values for the retention of each element onto each one of the solids were found. Physicochemical data obtained under thermodynamic equilibrium and under kinetic conditions - imposed by flow through experiments - allowed the design of simple analytical methodologies where the solids were employed as fillings of microcolumns held in continuous systems coupled on-line to an atomic absorption spectrometry. In order to control the interaction between the filling and the analyte at short times (flow through conditions) and thus, its effect on the analytical signal and the presence of interferences, the initial adsorption velocities were calculated using the pseudo second order model. All these experiments allowed the comparison of the solids in terms of their analytical behaviour at the moment of facing the determination of the three elements. Under optimized conditions mainly given by the features of the filling, the analytical methodologies developed in this work showed excellent performances with limits of detection of 0.14, 0.02 and 0.025 microg L(-1) and RSD % values of 3.4, 2.7 and 3.1 for Au, Cu and Ag, respectively. A full discussion of the main findings on the interaction metal ions/fillings will be provided. The analytical results for the determination of the three metals will be also presented.


Assuntos
Técnicas de Química Analítica/métodos , Metais Pesados/análise , Dióxido de Silício/química , Adsorção , Técnicas de Química Analítica/normas , Cobre/análise , Ouro/análise , Limite de Detecção , Porosidade , Prata/análise
10.
Talanta ; 79(3): 940-6, 2009 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-19576468

RESUMO

In this work, a non-chromatographic procedure for the on-line determination of ultratraces of V(V) and V(IV) is presented. The method involves a solid phase extraction-flow injection system coupled to electrothermal atomic absorption spectrometry (SPE-FI-ETAAS). The system holds two microcolumns (MC) set in parallel and filled with lab-made mesoporous silica functionalized with 3-aminopropyltriethoxy silane (APS) and mesoporous silica MCM-41, respectively. The pre-concentration of V(V) is performed by sorption onto the first MC (C1) filled with APS at pH 3, whilst that of V(IV) is performed by sorption onto the second column (C2) filled with mesoporous silica MCM-41 at pH 5. Aqueous samples containing both analytes are loaded and, after pre-concentration (pre-concentration factor PCF=10, sorption flow rate=1 mL min(-1), sorption time=10 min), they are eluted in separate vessels with hydroxylammonium chloride (HC) 0.1 mol L(-1) in HCl 0.5 mol L(-1) (elution volume=1 mL, elution flow rate=0.5 mL min(-1)). Afterwards, both analytes are determined through ETAAS with graphite furnace. Under optimized conditions, the main analytical figures of merit for V(V) and V(IV) are, respectively: detection limits (3s): 0.5 and 0.6 microg L(-1), linear range: 2-100 microg L(-1) (both analytes), sensitivity: 0.015 and 0.013 microg(-1)L and sample throughput: 6h(-1) (both analytes). Recoveries of both species were assayed in different water samples. Validation was performed through certified reference materials for ultratraces of total vanadium in river water.

11.
Talanta ; 77(3): 1068-74, 2009 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-19064093

RESUMO

An hybrid mesoporous material synthesised in our laboratories for solid phase extraction (SPE) in flow through systems has been used for analytical purposes. The solid was obtained from mesoporous silica MCM-41 functionalized with 3-aminopropyltriethoxy silane by Sol-Gel methodology. In order to exploit the large sorption capacity of the material together with the possibility of modeling it for anions retention, a microcolumn (MC) filled with the solid was inserted in a flow system for preconcentration of Cr(VI) and its determination at ultratrace levels in natural waters. The analytical methodology involved a reverse flow injection system (rFI) holding a MC filled with the solid for the analyte extraction. Elution and colorimetric detection were carried out with 1-5 diphenylcarbazide (DPC) in sulfuric acid. DPC produced the reduction of Cr(VI) to Cr(III) together with the generation of a cationic red complex between Cr(III) and 1-5 diphenylcarbazone which was easily eluted and detected with a visible spectrophotometer. Moreover, the filling material got ready for the next sample loading remaining unspoiled for more than 300 cycles. The effect of several variables on the analytical signal as well as the influence of cationic and anionic interferences were discussed. Particular attention was given to sulfuric acid interference since it is the required media for the complex generation. Under optimal conditions, 99.8% of Cr(VI) recovery was obtained for a preconcentration time of 120s (sample and DPC flow rates=1 mL min(-1)) and an elution volume of 250 micro L. The limit of detection (3s) was found to be 0.09 microg L(-1) Cr(VI) with a relative standard deviation (n=10, 3 microg L(-1)) of 1.8. Since no Cr(III) was retained by the solid material and Cr(VI) was completely adsorbed, electrothermal atomic absorption spectrometry (ET AAS) determinations of Cr(III) were also performed by simply measuring its concentration at the end of the microcolumn after Cr(VI) retention by the mesoporous solid. Applications to the determination of Cr(VI) and Cr(III) in natural waters and the validation of the methodology were also studied.


Assuntos
Cromo/análise , Cromo/química , Colostomia/instrumentação , Colostomia/métodos , Sistemas On-Line/instrumentação , Oligoelementos/análise , Oligoelementos/química , Concentração de Íons de Hidrogênio , Íons/química , Porosidade , Propanolaminas/química , Água/análise , Água/química
12.
Am J Trop Med Hyg ; 79(5): 662-9, 2008 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-18981500

RESUMO

Multidrug-resistant Plasmodium falciparum malaria is a severe public health problem on the Thailand-Myanmar border. Many villagers buy packets of 4-5 mixed medicines ("yaa chud") from shops without medical assessment as their first-line malaria treatment. In 2000-2001 a local researcher purchased 50 yaa chud from 44 shops around Mae Sot, Thailand and Myawaddy, Myanmar (Burma), for his wife who was said to be pregnant with fever and drowsiness. The tablets/capsules were provisionally identified by appearance and active ingredients determined in a subset by using mass and atomic spectrometry. The most frequently detected active ingredients were acetaminophen (22%), chlorpheniramine (13.4%), chloroquine (12.6%), tetracycline/doxycycline (11.4%), and quinine (5.1%). Only seven bags contained potentially curative medicine for malaria. A total of 82% of the bags contained medicines contraindicated in pregnancy. Inappropriate, ineffective antimalarial drugs on the Thailand-Myanmar border are likely to increase malaria morbidity, mortality and health costs and engender the emergence and spread of antimalarial drug resistance.


Assuntos
Resistência a Medicamentos , Malária Falciparum/epidemiologia , Medicina Tradicional , Preparações Farmacêuticas/química , Cromatografia Líquida , Humanos , Malária Falciparum/tratamento farmacológico , Espectrometria de Massas , Mianmar/epidemiologia , Espectrofotometria Atômica , Tailândia/epidemiologia
13.
Chem Cent J ; 1: 14, 2007 Jun 07.
Artigo em Inglês | MEDLINE | ID: mdl-17880749

RESUMO

BACKGROUND: The characterization of three types of Marche (Italy) honeys (Acacia, Multifloral, Honeydew) was carried out on the basis of the their quality parameters (pH, sugar content, humidity) and mineral content (Na, K, Ca, Mg, Cu, Fe, and Mn). Pattern recognition methods such as principal components analysis (PCA) and linear discriminant analysis (LDA) were performed in order to classify honey samples whose botanical origins were different, and identify the most discriminant parameters. Lastly, using ANOVA and correlations for all parameters, significant differences between diverse types of honey were examined. RESULTS: Most of the samples' water content showed good maturity (98%) whilst pH values were in the range 3.50 - 4.21 confirming the good quality of the honeys analysed. Potassium was quantitatively the most relevant mineral (mean = 643 ppm), accounting for 79% of the total mineral content. The Ca, Na and Mg contents account for 14, 3 and 3% of the total mineral content respectively, while other minerals (Cu, Mn, Fe) were present at very low levels. PCA explained 75% or more of the variance with the first two PC variables. The variables with higher discrimination power according to the multivariate statistical procedure were Mg and pH. On the other hand, all samples of acacia and honeydew, and more than 90% of samples of multifloral type have been correctly classified using the LDA. ANOVA shows significant differences between diverse floral origins for all variables except sugar, moisture and Fe. CONCLUSION: In general, the analytical results obtained for the Marche honeys indicate the products' high quality. The determination of physicochemical parameters and mineral content in combination with modern statistical techniques can be a useful tool for honey classification.

14.
Talanta ; 72(3): 1054-8, 2007 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-19071724

RESUMO

A simple and sensitive HPLC post-derivatization method with colorimetric detection has been developed for the determination of N-nitroso glyphosate in samples of technical glyphosate. Separation of the analyte was accomplished using an anionic exchange resin (2.50mmx4.00mm i.d., 15mum particle size, functional group: quaternary ammonium salt) with Na(2)SO(4) 0.0075M (pH 11.5) (flow rate: 1.0mLmin(-1)) as mobile phase. After separation, the eluate was derivatized with a colorimetric reagent containing sulfanilamide 0.3% (w/v), [N-(1-naphtil)ethilendiamine] 0.03% (w/v) and HCl 4.5M in a thermostatized bath at 95 degrees C. Detection was performed at 546nm. All stages of the analytical procedure were optimized taking into account the concept of analytical minimalism: less operation times and costs; lower sample, reagents and energy consumption and minimal waste. The limit of detection (k=3) calculated for 10 blank replicates was 0.04mgL(-1) (0.8mgkg(-1)) in the solid sample which is lower than the maximum tolerable accepted by the Food and Agriculture Organization of the United Nations.

15.
Talanta ; 69(1): 199-203, 2006 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-18970554

RESUMO

The aim of this work is the study of the best conditions for thermal stabilization of tellurium in graphite furnaces under different experimental conditions, including highly concentrated nitric and hydrochloric acids solutions as those resulting of drastic dissolution procedures. The influence of different noble metals used as matrix modifiers in solution or as permanent layers on the graphite furnace will be assessed. Amongst the assayed matrix modifiers, iridium used as permanent has shown the best performance in high concentrations of mineral acids. The mass employed was 20 microg (for 1 ng of Te), with a maximal attainable pyrolysis temperature of 1400 degrees C without losses of the analyte or sensitivity (height, area and form of the atomization peak), being mo=20 pg. Some speculations on the mechanisms of thermal stabilization of tellurium in graphite furnaces will be discussed. The potentiality of ETAAS for tellurium determination in technical grade sulfur will be evaluated. Results involving characteristics mass, limit of detection and percentage of recovery of tellurium in a mineralized sulfur sample will be compared with those obtained through a working curve in absence of interferences.

16.
Analyst ; 127(7): 990-4, 2002 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-12173663

RESUMO

A novel methodology for the determination of iron at the ppb level by spectrophotometric flow injection analysis is described. The method is based on the control of the flow dissolution of the colorimetric reagent 1,10-phenanthroline. This is achieved by means of the minimization of the area of contact between the carrier and the solid reagent, thus allowing the use of the fairly soluble organic compound without affecting the reactor lifetime. The reagent is melted inside an acrylic column (3.0 x 0.5 cm id) in such a way that a hollow space is left in the center after cooling. This new design improves some aspects of the performance of the classical solid-phase reactors as no problems related to the increase in the backpressure of the system are evidenced. Furthermore, the total reagent loading of the column is increased as no inert support is needed. A comparison between the performance of this novel methodology and that of the conventional packed reactor was performed and several advantages were observed: the use of higher flow rates, an increase in the reactor lifetime and a decrease in reagent consumption. A mathematical model to fit the concentration profiles of the dissolved reagent as a function of the residence time of the sample within the column is presented. The application of this strategy to the determination of Fe(II) improves the figures of merit in comparison to those obtained with a single-line homogeneous system: the limit of detection is 2 microg Fe L(-1) (3s) and the sensitivity is similar to that of the batch procedure. Results obtained for the determination of iron in natural waters are also presented.


Assuntos
Ferro/análise , Poluentes Químicos da Água/análise , Análise de Injeção de Fluxo/métodos
17.
Buenos Aires; Universidad de Buenos Aires. Facultad de Arquitectura, Diseño y Urbanismo; 2001. 189 p. ilus, tab.
Monografia em Espanhol | LILACS-Express | BINACIS | ID: biblio-1205094

RESUMO

Trabajo desarrollado en el marco de UBACYT, proyecto que integró a las Facultades de Arquitectura, Diseño y Urbanismo, y de Ciencias Exactas y Naturales, y que reúne la información disponible sobre contaminantes del agua y del aire en el área metropolitana de Buenos Aires. Para esto, se utilizó un sistema de información geográfica (SIG) para un rápido acceso al banco de datos, a las características principales, y a su ubicación geográfica, con el objetivo de facilitar la planificación de monitoreos más sistemáticos y exhautivos

18.
Buenos Aires; UBA-FADU; 2001. 189 p.
Monografia em Espanhol | BINACIS | ID: biblio-1194724

RESUMO

Este trabajo reune la información disponble sobre contaminantes del aire y del agua en la Ciudad de Buenos Aires. Sus capitulos son: contaminacion del aire, del agua,los problemas ambientales y los sistemas de información geografica


Assuntos
Poluição da Água , Poluição do Ar , Sistemas de Informação Geográfica
19.
Buenos Aires; Universidad de Buenos Aires. Facultad de Arquitectura, Diseño y Urbanismo; 2001. 189 p. ilus:, tab. (83008).
Monografia em Espanhol | BINACIS | ID: bin-83008

RESUMO

Trabajo desarrollado en el marco de UBACYT, proyecto que integró a las Facultades de Arquitectura, Diseño y Urbanismo, y de Ciencias Exactas y Naturales, y que reúne la información disponible sobre contaminantes del agua y del aire en el área metropolitana de Buenos Aires. Para esto, se utilizó un sistema de información geográfica (SIG) para un rápido acceso al banco de datos, a las características principales, y a su ubicación geográfica, con el objetivo de facilitar la planificación de monitoreos más sistemáticos y exhautivos

20.
Buenos Aires; UBA-FADU; 2001. 189 p. (68637).
Monografia em Espanhol | BINACIS | ID: bin-68637

RESUMO

Este trabajo reune la información disponble sobre contaminantes del aire y del agua en la Ciudad de Buenos Aires. Sus capitulos son: contaminacion del aire, del agua,los problemas ambientales y los sistemas de información geografica


Assuntos
Poluição da Água , Poluição do Ar , Sistemas de Informação Geográfica
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