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This study aimed to identify and characterise indoor sources of particulate matter (PM) in domestic environments. 74 inhabited apartments located in the urban area of Gela (Sicily, Italy), close to a refinery, and in three villages of the hinterland were evaluated, in real-world conditions, for the elemental composition of PM2.5. The samples were collected simultaneously inside and outside each apartment for 48 h. In addition, two of the apartments were simultaneously studied for four weeks. The elemental composition of PM2.5 was determined by applying a chemical fractionation procedure followed by inductively-coupled plasma spectrometry analysis, with both optical emission and mass detection. The extractable, more bio-accessible fraction (ext), and the mineralised residual fraction (res) of each element were determined, thus increasing the selectivity of elements as source tracers. Indoor air in the considered apartments was affected by both outdoor pollution and specific indoor emission sources. The behaviour of each source was studied in detail, identifying a reliable tracer: Tires for soil, Asext for industrial sources, Vext for heavy oil combustion, Ce for cigarette smoking and Mo for the use of vacuum dust cleaners. Asext and Vext showed an excellent infiltration capacity, while the concentration of Tires was affected by a low infiltration capacity and by the contribution of particles re-suspension caused by the residents' movements. In the case of Ce and Mo, indoor concentrations were much higher than outdoor with a high variability among the apartments, due to the inhabitants' habits concerning cigarette smoke and use of electric appliances. To test the overall effect of the concomitant exposure to the identified sources on Wh12 M and on DDA, a WQS analysis was conducted. Cigarette smoking and heavily oil combustion driven the Wh12 M odds increase, while the DDA odds increase was mainly driven by heavily oil combustion and the use of vacuum dust cleaners.
Assuntos
Poluentes Atmosféricos , Poluição do Ar em Ambientes Fechados , Poluentes Atmosféricos/análise , Poluição do Ar em Ambientes Fechados/análise , Poeira/análise , Monitoramento Ambiental , Tamanho da Partícula , Material Particulado/análise , SicíliaRESUMO
PURPOSE: Autoimmune thyroiditis and its complications for the reproductive system are a growing problem. Selenium is a common ingredient in numerous food supplements recommended for thyroiditis and pregnancy. A fast, simple method to measure serum selenium concentration will improve knowledge of its pharmacokinetics and toxicity. AIM: To validate a useful method to measure serum selenium concentration and to study selenium absorption and accumulation in a prospective interventional study of prolonged treatment. METHODS: Thirty healthy volunteers received a single dose of L-selenomethionine one tablet (83 mcg) (Phase 1), a single dose of two tablets (Phase 2), and two tablets daily for 14 days (Phase 3). Total selenium and selenium time profiles were generated by serial sampling (T0, T3, T6, T12, and T24 hours after ingestion-Phases 1 and 2; and T0 and T24 hours-Phase 3). Selenium concentration was investigated by open-vessel acid digestion of small serum volumes followed by hydride generation atomic fluorescence spectroscopy analysis. RESULTS: There was a significant increase in serum selenium concentration (mcg/L) in all treatment phases. Significantly increased levels were reached at T3 in Phase 1 (baseline: 76.5 ± 2.47; T3: 82.8 ± 3.28) and at T6 in Phase 2 (83.8 ± 3.46). They remained significantly increased at T12 in Phase 1 and T24 in Phase 2 (79.03 ± 2.69). There was significant selenium accumulation after prolonged intake (14 days) (102.13 ± 5.61). CONCLUSIONS: Prolonged selenomethionine administration increases circulating blood selenium concentration and hydride generation atomic fluorescence spectroscopy enables its accurate quantification.
Assuntos
Suplementos Nutricionais , Selênio/sangue , Selenometionina/administração & dosagem , Adulto , Feminino , Voluntários Saudáveis , Humanos , Masculino , Estudos ProspectivosRESUMO
BACKGROUND: Exposure to single and multiple carcinogenic metals and/or semimetals represents a major environmental risk factor for public health. In particular, children are more susceptible to environmental pollutants than adults, but specific studies are still limited. The aims of the present study were: 1) to trace the exposure and co-exposure profiles to eight known or suspected carcinogenic metals and semimetals (As, Be, Cd, Co, Cr, Ni, Pb, and Sb); and: 2) to evaluate the influence of some possible interfering/confounding factors on the exposure to these elements during childhood. STUDY DESIGN: Cross-sectional study. METHODS: We recruited 159 healthy Italian children attending a primary school of the urban area of Rome, Italy. Selected metals were determined by inductively coupled plasma mass spectrometry on urinary samples collected at the end of a "typical" day (one sample for each child), while information about possible confounding/interfering factors were collected via questionnaires. RESULTS: The great part of the studied children resulted co-exposed to the monitored metals: 83.2%, 69.2%, 51.0% and 29.3% of the participants were concurrently exposed to at least two, three, four and five trace elements, respectively. Gender was the only one among the investigated variable that significantly influenced the co-exposure, with females resulting at lower risk (OR = 0.392; 95 IC = 0.156 - 0.989; p < 0.047). CONCLUSIONS: Given the importance of protecting child's health and the risks related to the exposure to carcinogenic metals, especially when they occur simultaneously, other researches in this field are strongly recommended.
Assuntos
Carcinógenos Ambientais/efeitos adversos , Exposição Ambiental/estatística & dados numéricos , Saúde da População Urbana , Criança , Estudos Transversais , Feminino , Humanos , Itália , MasculinoRESUMO
The daily concentration and chemical composition of PM2.5 was determined in indoor and outdoor 24-h samples simultaneously collected for a total of 5 weeks during a winter and a summer period in an apartment sited in Rome, Italy. The use of a specifically developed very quiet sampler (<35 dB) allowed the execution of the study while the family living in the apartment led its normal life. The indoor concentration of PM2.5 showed a small seasonal variation, while outdoor values were much higher during the winter study. Outdoor sources were found to contribute significantly to indoor PM concentration especially during the summer, when the apartment was naturally ventilated by opening the windows. During the winter the infiltration of outdoor PM components was lower and mostly regulated by the particle dimensions. Organics displayed In/Out ratios higher than unity during both periods; their indoor production increased significantly during the weekends, where the family stayed mostly at home. PM components were grouped into macrosources (soil, sea, secondary inorganics, traffic, organics). During the summer the main contributions to outdoor PM2.5 came from soil (30%), secondary inorganics (29%) and organics (22%). Organics dominated both indoor PM2.5 during the summer (60%) and outdoor and indoor PM2.5 during the winter (51% and 66%, respectively).
Assuntos
Poluentes Atmosféricos/análise , Poluição do Ar em Ambientes Fechados/análise , Monitoramento Ambiental/métodos , Habitação , Material Particulado/análise , Tamanho da Partícula , Cidade de Roma , Estações do Ano , Ventilação/métodosRESUMO
The response of Phragmites australis (Cav.) Trin. Ex. Steudel to zinc (Zn) and lead (Pb) was studied separately in two hydroponic tests, during a three weeks experiment. The effects on ecophysiology and biomass partitioning were evaluated during the metal treatments and at the recovery, and total metal content and accumulation capacity in different plant organs were assessed. Zn and Pb had different effects on the overall measured parameters, highlighting different mechanism of action. In particular, Zn concentration was higher in roots and, being a micronutrient, it was translocated into leaves, producing a reduction of assimilation rate, stomatal conductance (-71.9 and -81.3% respect to the control plant respectively), and a strong down regulation of photosystems functionality both at PSII and PSI level. Otherwise, Pb was accumulated mainly in the more lignified tissue such as rhizomes, with slightly effect on gas exchange. Chlorophyll a fluorescence highlighted that Pb inhibits the electron transfer process at the PSI donor side, without recovery after the removal of the metal stress. Despite these physiological limitations, P. australis showed a high capacity to accumulate both metals, and only slight reduction of biomass, being therefore a suitable species for phytoremediation interventions.
Assuntos
Chumbo/metabolismo , Chumbo/toxicidade , Fotossíntese/efeitos dos fármacos , Poaceae/efeitos dos fármacos , Poaceae/metabolismo , Zinco/metabolismo , Zinco/toxicidade , Biodegradação AmbientalRESUMO
The concentration of air pollutants is governed by both emission rate and atmospheric dispersion conditions. The role played by the atmospheric mixing height in determining the daily time pattern of PM components at the time resolution of 2 h was studied during 21 days of observation selected from a 2-month field campaign carried out in the urban area of Rome, Italy. Natural radioactivity was used to obtain information about the mixing properties of the lower atmosphere throughout the day and allowed the identification of advection and stability periods. PM10 composition was determined by X-ray fluorescence, ion chromatography, inductively coupled plasma-mass spectrometry and thermo-optical analysis. A satisfactory mass closure was obtained on a 2-h basis, and the time pattern of the PM10 macro-sources (soil, sea, secondary inorganics, organics, traffic exhaust) was acquired at the same time scale. After a complete quality control procedure, 27 main components and source tracers were selected for further elaboration. On this database, we identified some groups of co-varying species related to the main sources of PM. Each group showed a peculiar behaviour in relation to the mixing depth. PM components released by soil, biomass burning and traffic exhaust, and, particularly, ammonium nitrate, showed a clear dependence on the mixing properties of the lower atmosphere. Biomass burning components and organics peaked during the night hours (around midnight), following the atmospheric stabilization and increased emission rate. Traffic exhausts and non-exhausts species also peaked in the evening, but they showed a second, minor increase between 6:00 and 10:00 when the strengthening of the emission rate (morning rush hour) was counterbalanced by the dilution of the atmosphere (increasing mixing depth). In the case of ammonium nitrate, high concentrations were kept during the whole night and morning.
Assuntos
Poluentes Atmosféricos , Poluição do Ar , Poluentes Atmosféricos/análise , Poluição do Ar/análise , Monitoramento Ambiental/métodos , Material Particulado/análise , Solo , Emissões de Veículos/análiseRESUMO
The possibility of a relevant contribution of biomass burning for domestic heating to PM10 in the urban area of Rome was explored. The concentration of levoglucosan was determined for 31 months in Rome and in a nearby peri-urban area. During the cold season it reached several hundreds of ng/m3 at both sites, with a clear inverse relationship with air temperature. During the summer it remained well below 100â¯ng/m3. Although at the peri-urban station the concentration was about 50% higher than at the urban site, the two seasonal patterns show a very good agreement (R2â¯=â¯0.95), pointing at a main contribution of biomass burning in both areas. Additional information came from the comparison of the 2-h time pattern of levoglucosan and the mixing conditions of the atmosphere, evaluated by monitoring natural radioactivity. During the summer levoglucosan concentration followed the pattern of natural radioactivity, indicating a contribution from many small sources scattered on a wide area (wildfires, barbecues, agricultural fires). During the heating season the activity of a source that switched in the early afternoon and switched off before midnight was highlighted. A 2-h delay between levoglucosan time patterns at the peri-urban and the urban site suggests that biomass burning mainly occurs outside Rome and the combustion products are then transported towards the city centre. Biomass burning contribution to PM10 was estimated as 12% at the peri-urban site and 6.7% inside the city, with relevant implications for the health of the about 2.800.000 citizens living in the urban area of Rome.
Assuntos
Poluentes Atmosféricos/análise , Biomassa , Incêndios , Material Particulado/análise , Cidades , Monitoramento Ambiental , Glucose/análogos & derivados , Glucose/análise , Calefação , Itália , Cidade de Roma , Estações do Ano , Temperatura , Fatores de TempoRESUMO
We studied the size distribution of ions (Cl-, NO3-, SO4=, Na+, NH4+, K+, Mg++, Ca++) and elements (As, Ba, Cd, Co, Cs, Cu, Fe, Li, Mn, Ni, Pb, Rb, Sb, Se, Sn, Sr, Ti, Tl, V, Zn) during the winter and summer seasons of seven consecutive years (2008-2014) in an area of the Po Valley (Northern Italy) characterised by industrial, agricultural and urban settings. The study included the collection and analysis of 41 series of size-segregated samples (MOUDI sampler, 10 stages, cut sizes from 0.18 to 18⯵m). Ions were analysed by ion chromatography; elemental analysis was carried out by ICP-MS, by applying a chemical fractionation method able to increase the selectivity of PM source tracers. Our results indicate that important winter/summer variations occurred in both the concentration and size distribution of most PM components. These variations were explained in terms of variations in the strength of the prevailing sources of each component. The contribution of biomass burning for domestic heating was highlighted by the well-known tracer K+ but also by the soluble fraction of Rb, Cs and Li. Biomass burning contribution to atmospheric PM was mostly contained in the fine fraction, with a broad size-distribution from 0.18 to 1.8⯵m. This source also appreciably increased the concentration of other elements in fine PM (As, Cd, Co, Mn, Pb, Sb, Sn). A few PM components (tracers of sea-spray, brake lining and some industries) did not show marked seasonal variations in concentration and size distribution. However, during winter, for brake lining and industry tracers we observed an upward shift in the dimension of fine particles and a downward shift in the dimension of coarse particles, due to the ageing of the air masses.
Assuntos
Poluentes Atmosféricos/análise , Monitoramento Ambiental , Material Particulado/análise , Aerossóis/análise , Envelhecimento , Fracionamento Químico , Calefação , Indústrias , Íons/análise , Itália , Peso Molecular , Tamanho da Partícula , Estações do AnoRESUMO
A field study was carried out at six locations in the Lazio region (Central Italy) aimed at characterising atmospheric particulate matter (PM10 and PM2.5) from the point of view of the chemical composition and grain size distribution of the particles, the mixing properties of the atmosphere, the frequency and relevance of natural events. The combination of four different analytical techniques (ion chromatography, X-ray fluorescence and ICP for inorganic components, thermo-optical analysis for carbon compounds) yielded sound results in terms of characterisation of the air masses. During the first three months of the study (October-December 2004), many pollution events of natural (sea-salt or desert dust episodes) or anthropogenic nature were identified and characterised. More than 90% of the collected mass was identified by chemical analysis. The central role played by the mixing properties of the lower atmosphere when pollution events occurred was highlighted. The results show a major impact of primary anthropogenic pollutants on traffic stations and a homogeneous distribution of secondary pollutants over the regional area. An evaluation of the sources of PM and an identification of possible reliable tracers were obtained using a chemical fractionation procedure.
Assuntos
Poluentes Atmosféricos/análise , Poluição do Ar/análise , Cidades , Compostos Inorgânicos/análise , Material Particulado/análise , Atmosfera , Monitoramento Ambiental/métodos , Humanos , Itália , Tamanho da Partícula , Saúde da População UrbanaRESUMO
Air quality at the main station of the metro system of Rome (Termini hub) has been characterized by the point of view of particulate matter (PM) concentration and chemical composition. Indoor air in different environments (underground train platform and shopping center, metro carriages with and without air conditioning system) has been studied and compared with outdoor air at a nearby urban site. Air quality at the railway station, located outdoor at surface level, has been also considered for comparison. PM chemical characterization included ions, elemental carbon, organic carbon, macro-elements, and the bio-accessible and residual fractions of micro- and trace elements. Train platform and carriages without air conditioning resulted to be the most polluted environments, with indoor/outdoor ratio up to two orders of magnitude for many components. PM mass concentration was determined on filter membranes by the gravimetric procedure as well as from the optical particle counter (OPC) number concentration measurements. The OPC results, taken with the original calibration factor, were below 40 % of the value obtained by the gravimetric measurements. Only a chemical and morphological characterization of the collected dust could lead to a reconciliation of the results yielded by the two methods. Macro-components were used to estimate the strength of the main macro-sources. The most significant contribution is confirmed to derive from wheels, rails, and brakes abrasion; from soil re-suspension (over 50 % at the subway platform); and from organics (about 25 %). The increase in the concentration of elements was mostly due to the residual fraction, but also the bio-accessible fraction showed a remarkable enrichment, particularly in the case of Ba, Zn, Cd, and Ni.
Assuntos
Poluentes Atmosféricos/análise , Poluentes Atmosféricos/química , Monitoramento Ambiental , Material Particulado/análise , Material Particulado/química , Ferrovias , Cidade de RomaRESUMO
Formation constants of the silver(I) complexes with some amino-alcohols have been determined at 25 degrees C in 0.5 M KNO(3) by means of two independent potentiometric measurements employing glass and silver electrode. The ligands considered are: sec-butylamine, 2-amino-1-propanol, 2-amino-1-methoxy-propane, 2-amino-2-methyl-1-propanol, 2-amino-1-butanol, 2-amino-1-pentanol, 2-amino-1-hexanol, 2-amino-1,3-propanediol, 2-amino-1,3-hexandiol, 2-amino-2-methyl-1,3-propanediol and Tris(hydroxymethyl)-aminomethane. Protonation constants of the selected ligands have also been determined. Calculations were made using HYPERQUAD computer program. The influence exerted by the introduction of hydroxy groups and by the presence of alkyl residuals in the ligand structure on the formation equilibria, is discussed.
RESUMO
A study of complex formation equilibria of some beta-amino-alcohols with lead(II) and cadmium(II) ions at 25 degrees C and in 0.5 M KNO(3) is reported. The amino-alcohols considered are 2-amino-1-propanol, 2-amino-1-butanol, 2-amino-1-pentanol and 2-amino-1,3-propanediol. sec-Buthylamine and 2-amino-1-methoxy-propane have been also considered for comparison. The results are discussed in terms of ligand structure, paying attention to the number of hydroxyl groups and to the length of the alkyl residual. A weak contribution of the alcoholic oxygen in the coordination of cadmium(II) and the presence of a mixed hydroxyl species in lead(II) containing systems are hypothesized.
RESUMO
The present work deals with the optimization and validation of a method for the quantitative simultaneous ICP determination of metals in ambient air particulate matter. The attention has been focused on the thoracic fraction (PM10) and twelve different metals were chosen on the basis of their toxicity and of their possible use as chemical tracers. The microwave acidic digestion of the samples has been performed in the presence of different reagents and under different conditions and particular attention has been paid to the optimization of the whole analytical procedure and to the evaluation of accuracy and precision related to the single operative steps. The interferences due to the reagents and to the sampling supports have also been evaluated. In addition, the analytical procedure has been checked by examining the equivalence of results related to parallel sampled filters pairs.
Assuntos
Poluentes Atmosféricos/análise , Metais/análise , Respiração , Poluentes Atmosféricos/química , Poluentes Atmosféricos/toxicidade , Filtração , Humanos , Resíduos Industriais/análise , Pulmão/efeitos dos fármacos , Pulmão/patologia , Pulmão/fisiologia , Metais/química , Metais/toxicidade , Micro-Ondas , Tamanho da Partícula , Padrões de Referência , Reprodutibilidade dos Testes , Respiração/efeitos dos fármacos , UrbanizaçãoRESUMO
The seasonal variability in the mass concentration and chemical composition of atmospheric particulate matter (PM10 and PM2.5) was studied during a 2-year field study carried out between 2010 and 2012. The site of the study was the area of Ferrara (Po Valley, Northern Italy), which is characterized by frequent episodes of very stable atmospheric conditions in winter. Chemical analyses carried out during the study allowed the determination of the main components of atmospheric PM (macro-elements, ions, elemental carbon, organic matter) and a satisfactory mass closure was obtained. Accordingly, chemical components could be grouped into the main macro-sources of PM: soil, sea spray, inorganic compounds from secondary reactions, vehicular emission, organics from domestic heating, organics from secondary formation, and other sources. The more significant seasonal variations were observed for secondary inorganic species in the fine fraction of PM; these species were very sensitive to air mass age and thus to the frequency of stable atmospheric conditions. During the winter ammonium nitrate, the single species with the highest concentration, reached concentrations as high as 30 µg/m(3). The intensity of natural sources was fairly constant during the year; increases in natural aerosols were linked to medium and long-range transport episodes. The ratio of winter to summer concentrations was roughly 2 for combustion product, close to 3 for secondary inorganic species, and between 2 and 3 for organics. The winter increase of organics was due to poorer atmospheric dispersion and to the addition of the emission from domestic heating. A similar winter to summer ratio (around 3) was observed for the fine fraction of PM.
Assuntos
Poluentes Atmosféricos/análise , Poluição do Ar/estatística & dados numéricos , Monitoramento Ambiental , Material Particulado/análise , Aerossóis/análise , Poluentes Atmosféricos/química , Carbono/análise , Calefação/estatística & dados numéricos , Compostos Inorgânicos/análise , Íons/análise , Itália , Nitratos/análise , Tamanho da Partícula , Material Particulado/química , Estações do Ano , Emissões de Veículos/análiseRESUMO
Size distribution (fine and coarse fraction) and solubility distribution (extracted and residual fraction) of 20 elements (As, Ba, Be, Cd, Co, Cu, Fe, Li, Mn, Pb, Ni, Rb, S, Sb, Se, Sn, Sr, Ti, Tl, V) in atmospheric particulate matter (PM) were determined during a 5-year field study carried out in the Po Valley (peri-urban area of Ferrara, in Northern Italy). By studying the contribution of the two size fractions and the two solubility fractions to the atmospheric concentration of each element, it was possible to obtain interesting information about the variability of PM sources, to assess the role played by atmospheric stability in determining pollution episodes, and to obtain an estimate of the bio-accessible fraction. Atmospheric stability is confirmed to be one of the main causes of atmospheric pollution in this area and is to be responsible for the pronounced winter increase in both PM and elemental concentration. Long-range transport of natural and polluted air masses caused temporary increases in PM and elemental concentration, while local industrial emission seemed to play a secondary role. Regulated elements were well below their concentration limit, but many toxic elements were in the form of fine particles and soluble chemical species, more accessible to the environment, and the human body.
Assuntos
Poluentes Atmosféricos/análise , Poluição do Ar/estatística & dados numéricos , Monitoramento Ambiental , Material Particulado/análise , Oligoelementos/análise , Humanos , Indústrias/estatística & dados numéricos , Itália , Material Particulado/química , Estações do Ano , SolubilidadeRESUMO
INTRODUCTION: The copper bioaccumulation by the floating Lemna minor and by the completely submerged Ranunculus tricophyllus as a function of exposure time and copper concentration was studied, with the aim of proposing these species as environmental biosensors of the water pollution. RESULTS: The results show that both these aquatic angiosperms are good indicators of copper pollution because the copper uptake is the only function of metal concentration (water pollution). CONCLUSION: Uptake behavior is reported as a function of the time and concentration, based on the results of a 3-year study. Kinetic evaluations are proposed.
Assuntos
Cobre/metabolismo , Monitoramento Ambiental/métodos , Ranunculus/metabolismo , Poluentes Químicos da Água/metabolismo , Cobre/análise , Água/química , Poluentes Químicos da Água/análise , Qualidade da ÁguaRESUMO
It is here described the comparison of extraction efficiency of some solutions (acetate buffer, deionized water, diluted HNO(3) and EDTA) frequently adopted in literature for evaluating the elemental solubility in airborne particulate matter. This comparison was performed considering the distribution of As, Ba, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Na, Ni, Pb, S, Si, Sb, Sn, Sr, Ti, V, Zn between the extractable and mineralized residual fractions on the NIST 1648 certified material, PM(10) real samples and size-segregated samples, collected by a 13-stage impactor. The extracting solutions were evaluated by comparing extractive efficiencies and robustness towards some factors, such as acidity and concentration of complexing species, that have great environmental variability and that could be able to modify the extractive efficiency. Furthermore, extraction methods application to size-segregated samples allowed estimating the selectivity of extracting solutions towards dimensionally characterized emission sources, as dusts originated from abrasion and road dust re-suspension. On the basis of the obtained results, it was possible to define the main advantages and disadvantages resulting from the use of different extracting solutions, necessary to make possible the comparison of environmental studies carried out in different extractive conditions and to start up a proper study for harmonizing extracting procedures.
Assuntos
Elementos Químicos , Material Particulado/análise , Fracionamento Químico , Ácido Edético/química , Monitoramento Ambiental , Material Particulado/química , Solubilidade , Água/químicaRESUMO
In this paper, we describe a validation procedure for chemical fractionation analysis of elements (Al, As, Ba, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, S, Sb, Si, Sr, Ti and V) and soluble ions (Cl(-), NO(3)(-), SO(4)(2-), Na(+), NH(4)(+), Mg(2+), Ca(2+)) in suspended particulate matter (PM). The procedure applies three distinct measurement techniques (XRF, IC and ICP-OES) to the analysis of individual samples. The techniques used generate different outputs at different stages in the procedure. This makes it possible to identify the contributions of specific parameters to measurement uncertainty. On this basis, we propose a scheme for controlling the analytical quality of data from individual samples in which inter-technique comparisons is used in the same way many analytical methods use surrogates. We apply this scheme to about 310 samples of PM(10) and PM(2.5) identifying and assessing the main factors contributing to measurement uncertainty. This procedure successfully resolved a number of difficulties frequently encountered during the analysis of PM, including lack of appropriate reference materials and the low reliability of alternative techniques of quality control. The results demonstrate the critical importance of sample treatment prior to destructive analysis by IC and ICP.
Assuntos
Técnicas de Química Analítica/métodos , Íons/análise , Metais/análise , Material Particulado/análise , Controle de QualidadeRESUMO
A field study was carried out at six locations in the Lazio region (Central Italy) aimed at characterising atmospheric particulate matter (PM10 and PM2.5) from the point of view of the chemical composition and grain size distribution of the particles, the mixing properties of the atmosphere, the frequency and relevance of natural events. The combination of four different analytical techniques (ion chromatography, X-ray fluorescence and ICP for inorganic components, thermo-optical analysis for carbon compounds) yielded sound results in terms of characterisation of the air masses. During the first three months of the study (October-December 2004), many pollution events of natural (sea-salt or desert dust episodes) or anthropogenic nature were identified and characterised. More than 90% of the collected mass was identified by chemical analysis. The central role played by the mixing properties of the lower atmosphere when pollution events occurred was highlighted. The results show a major impact of primary anthropogenic pollutants on traffic stations and a homogeneous distribution of secondary pollutants over the regional area. An evaluation of the sources of PM and an identification of possible reliable tracers were obtained using a chemical fractionation procedure.
Assuntos
Poluentes Atmosféricos/química , Compostos Inorgânicos/análise , ItáliaRESUMO
The optimisation of a micro-analytical two-step sequential leaching procedure for the determination of non-volatile ions (NO(3)(-), SO(4)(2-), Cl(-), Na(+), Mg(2+), NH(4)(+) and Ca(2+)) and of 17 elements (Al, As, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, S, Se, V, Zn, Sb, Si and Ti) in two fractions-extract and residue-on the same sample of air particulate matter is described. The two-step method was tested on the SRM NIST 1648 for equivalence with two reference methods, the EMEP procedure for ions extraction and the EN 12341 standard for the elemental determination of the PM(10) and is suitable for application to small sample amounts (less than 1mg of particulate matter is needed), i.e. those collected by daily low volume filter-sampling. Performance times of the procedure were optimised to meet the target of routine application for large scale monitoring samples. A single ultrasonic-assisted extraction of air particulate matter is performed in 0.01M acetate buffer at pH 4.5, followed by IC ions analysis and ICP-OES elemental analysis of the extract and by ICP-OES elemental analysis of the mineralized residue after dissolution by microwave-assisted digestion with a HNO(3)/H(2)O(2) mixture. Using a pH buffered extracting solvent was preferred to water or diluted acid solutions to improve the reproducibility of metals extraction with respect to existing leaching methods; the influence of pH, nature and concentration of the buffer solution and extraction time on analytes concentration in the extract is discussed. Values of ions extraction and elements recoveries resulted fairly equivalent with those obtained by the reference methods. The study was also extended to some non-certified elements (Mg, S, Sb, Si and Ti) for their environmental significance. Elements recoveries were obtained as sum of the extract and residue fractions and were comparable with those obtained by direct dissolution. Standard deviations were within 10% for almost all detected ions and elements.