Determination of rare earth and concomitant elements in magnesium alloys by inductively coupled plasma optical emission spectrometry.

An Inductively Coupled Plasma Optical Emission Spectrometry method for simultaneous determination of Al, Ca, Cu, Fe, In, Mn, Ni, Si, Sr, Y, Zn, Zr and rare earth elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu) in magnesium alloys, including the new rare earth elements-alloyed magnesium, has been developed. Robust conditions have been established as nebulizer argon flow rate of 0.5mLmin(-1) and RF incident power of 1500W, in which matrix effects were significantly reduced around 10%. Three acid digestion procedures were performed at 110°C in closed PFA vessels heated in an oven, in closed TFM vessels heated in a microwave furnace, and in open polypropylene tubes with reflux caps heated in a graphite block. The three digestion procedures are suitable to put into solution the magnesium alloys samples. From the most sensitive lines, one analytical line with lack or low spectral interferences has been selected for each element. Mg, Rh and Sc have been studied as internal standards. Among them, Rh was selected as the best one by using Rh I 343.488nm and Rh II 249.078nm lines as a function of the analytical lines. The trueness and precision have been established by using the Certified Reference Material BCS 316, as well as by means of recovery studies. Quantification limits were between 0.1 and 9mgkg(-1) for Lu and Pr, respectively, in a 2gL(-1) magnesium matrix solution. The method developed has been applied to the commercial alloys AM60, AZ80, ZK30, AJ62, WE54 and AE44.

Revisiting methods for the determination of bioavailable metals in coastal sediments.

A simple methodology for the determination of bioavailability of fourteen metals in coastal sediments has been developed by simulating the conditions of digestive process of marine fishes. With this aim, a representative sediment composite sample was treated with hydrochloric acid solutions at different pH values, temperatures and contact times, in the presence and absence of Pepsin and Trypsin. The addition of Pepsin and Trypsin did not affect the extraction of most elements. As a result of the present study, the digestion with a hydrochloric acid solution at pH 1, 40°C and 12h is proposed. Adjustments of the temperature and time reaction could be made according to the specific ecosystem under study. The amount of metal extracted by other methods based on acetic acid was lower than that extracted by HCl treatment proposed.

Comparative study of digestion methods EPA 3050B (HNO3--H2O2--HCl) and ISO 11466.3 (aqua regia) for Cu, Ni and Pb contamination assessment in marine sediments.

Knowing the metal extraction capacity of a digestion method is crucial for a better environmental interpretation of metal concentrations determined in sediments. One of the main problems at the present is the lack of harmonization of information obtained by two of the most popular sediment partial digestion methods: ISO 11466.3 (aqua regia) and EPA 3050B (HNO3--H2O2--HCl). In the present work, the amount of Cu, Ni and Pb leached by using both methods was compared with the total content of those elements in marine sediments collected, as an example, from the Cienfuegos Bay, Cuba. Similar amounts of Cu were extracted by both methods; while leaching of Ni and Pb were different. Generally, the EPA method extracted more Ni than the ISO method. In contrast, Pb was extracted in a larger amount by the ISO method. Some explanations are given for the observed results. X-ray Diffraction, X-ray Fluorescence, Particle Induced X-ray Emission Spectrometry and Energy Dispersive X-ray coupled to Scanning Electron Microscopy were employed for this purpose. On the other hand, none of the methods studied extracted simultaneously the fraction of all the metals, probably provided by human activity (Theoretical Anthropogenic Fraction) in both sediments studied. The use of ISO 11466.3 or EPA 3050B is recommended since the analytical performance parameters of both, in combination with Flame Atomic Absorption Spectrometry, are adequate. For a better environmental interpretation of the analytical results, information on the extraction efficiency of the selected method for specific elements and sediments under study should also be provided, together with the determined concentrations.