Carmen Pons

The use of anion-exchange disks in an optrode coupled to a multi-syringe flow-injection system for the determination and speciation analysis of iron in natural water samples

A combination of multi-syringe flow-injection analysis (MSFIA) technique with an optical fibre reflectance sensor for the determination of iron in water samples has been developed in this work. Anion-exchange solid phase extraction (SPE) disks have been used as solid phase. Ammonium thiocyanate has been chosen as chromogenic reagent for Fe(III). The complex Fe[SCN](6)(3-) is retained onto the SPE disk and spectrophotometrically detected at 480nm. The complex is eluted with 0.25moll(-1) hydrochloric acid in 75% ethanol. Total iron can be determined by oxidising Fe(II) to Fe(III) with hydrogen peroxide. A mass calibration was run within the range of 0.4-37.5ng. The detection limit (3s(b)/S) was 0.4ng. The repeatability (RSD), calculated from 9 replicates using 0.5ml injections of a 25microgl(-1) concentration, was 3.6%. The repeatability between five anion-exchange disks was 5.4%. An injection throughput of 7 injections per hour for a sampling volume of 1ml has been achieved. The applicability of the proposed methodology in natural water samples has been proved. The properties of anion-exchange and chelating SPE disks have been studied and compared.

Historical Mortars from the Fortified Upper Town of Eivissa (Balearic Islands, Spain)

Samples of mortars and stone of Portal de ses Taules from the Renaissance city walls of Eivissa (16th century) were characterized using thermal analysis— thermogravimetry and derivative thermogravimetry (DTG)—x-ray diffractometry, and scanning electron microscopy. The granulometric fraction of particle size <63 μm was selected as representative of the binder, while the fraction 0.5–1 mm was taken as representative of the aggregate in order to characterize mortar samples. The results show that local materials were used. Lime was the main component of most of the samples tested. Thermal analysis revealed the hydraulic nature of the lime mortars. High amounts of sodium chloride were found in the samples analysed.