Sorption experiments in batch mode with Chelex-100 resin have been carried out for the determination of total Ag, labile and inert fractions in seawater from Ria de Vigo (NE Atlantic ocean) by inductively coupled plasma-mass spectrometry (ICP-MS). The method allows an accurate determination of the total Ag thus avoiding the effect of the saline matrix when direct determination by ICP-MS is performed. Similarly, the distribution patterns of Ag among species with different lability can be established in seawater as a function of pH. Species distribution and total Ag contents have been obtained in CRM CASS-4 (near shore seawater) and four coastal seawater samples. While the free silver ion concentration accounts for a significant fraction at low pH, the labile inorganic fraction is most important at natural pH (%8) in non-polluted seawater. The inert and labile organic fractions were the most relevant in polluted coastal seawater. Complexation mechanisms of silver were also investigated from the sorption curves of silver on Chelex-100 according to the Gibbs-Donnan model. Two complexes were formed, AgL and AgL 2 with the following intrinsic complexation constants log b ð1npÞ ¼ À2:11 and À 10.02, respectively. The formation of the complex AgL predominates up to pH 4 but is negligible due to chloride ions effect, while the complex AgL 2 predominates from pH 4.
Depth concentration profiles of 26 elements, i.e. trace elements (As, Ba, Cd, Co, Cr, Cu, Hg, Ni, Pb, Rb, Sr, V and Zn), lithophiles (Si, Al, Fe, Mn, Na, K, Mg, Ca and Ti) and nutrients (C, P, N, S) have been established in a sediment core collected at the Respomuso Lake (Pyrenees, Spain). This high altitude lake of glacier origin was transformed into reservoir in the fifties of last century. Correlations among the depth profiles of the above elements were established. HCl-extractable elements, which are better related to bioavailability, followed the profiles of total contents. Principal component analysis was applied to establish the binding behaviour of trace elements in the sediment matrix and, in turn, to search for their anthropogenic or natural sources. It was seen that Cu, Ni, Pb, Sr and Zn clustered together, and with exception of Sr, they were not clearly associated with any major component of the sediment. Their depth profiles correlate well with each other, hence indicating their presence as a result of atmospheric pollution. Redox-sensitive elements such as Fe and Mn follow a similar trend along the vertical profile. Depth profiles of As an Co correlate well with those of Fe and Mn. Principal component analysis showed that As, Co, Fe and Mn clustered together, which confirms the close association of As and Co with Fe-Mn oxyhydroxides. As concentrations in many strata exceed the ERM value, and therefore, significant biological effects are expected. Dissolution of minerals such as pyrite, chalcopyrite and galena taking part in the mineralogy of this area accounts for the As concentration found. Ba, Cr, Rb and V were associated with the sediment matrix (aluminosilicates), hence showing low mobility.
A speciation method based on Chelex-100 titration in combination with electrothermal-atomic absorption spectrometry has been developed to study the distribution of Pb among different fractions in coastal seawater. The method allows an accurate determination of total Pb, thereby avoiding the effect of the saline matrix. Additionally, the distribution patterns of Pb among species with different lability can be established in seawater as a function of pH. Four Pb fractions have been obtained in a model seawater and two seawater samples from Ria de Vigo (NE Atlantic ocean), i.e. free Pb ion, inorganic Pb fraction, organic Pb fraction and inert Pb fraction. The inert and labile organic Pb fractions dominate at natural pH (%8).Complexation mechanisms of Pb were investigated from the sorption curves of lead on Chelex-100 according to the Gibbs -Donnan model. Three complexes were formed, PbL, PbL 2 and PbðHLÞ 2 with the following intrinsic complexation constants log b ð1npÞ ¼ À3:25, À 10.10 and À 1.98, respectively. The formation of the complex PbL is negligible in all range of pH studied, while the complex PbðHLÞ 2 predominates up to pH 4 and PbL 2 from pH 4.
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