Claudia Brunori

Digestion methods for analysis of fly ash samples by atomic absorption spectrometry

The efficiency of different digestion methods (six microwave decomposition methods and a wet acid digestion method) in the solubilisation of six metals (Cr, Ni, Cu, Pb, Cd, Zn), for their determination in fly ashes, was compared. Five different mineral acid mixtures and two different microwave systems were tested. The study was carried out by analyzing two highly homogenised fly ash samples (from sewage sludge and city waste incineration) provided by the Joint Research Centre of Ispra. Determinations were performed by atomic absorption spectrometry and by inductively coupled plasma atomic emission spectrometry. The analytical performance of the laboratory was evaluated using the 1633a Coal Fly Ash Standard Reference Material of National Bureau of Standards (NBS SRM 1633a). Results showed that a HNO3 microwave treatment was strong enough to solubilise metals from the considered fly ashes. Moreover, microwave methods generally provided higher release than the classical aqua regia method, whereas no significant advantage was observed using a high performance microwave unit.

Evaluation of performance of time-saving extraction devices in the BCR three-step sequential extraction procedure.

Two alternative extraction methods--a routine ultrasonic bath and a microwave oven--were developed and optimized for their eventual exploitation in the three-stage sequential extraction procedure proposed by the European Standards, Measurements and Testing (S, M & T) Programme, formerly Bureau Communitaire de Reference (BCR), for the operationally defined speciation of Cd, Cr, Cu, Ni and Zn. The conventional BCR three-stage sequential extraction procedure was modified at each stage, applying ultrasonic or microwave devices in order to shorten the required 16 h of shaking in all three steps. The experimental tests and the optimization of the operating parameters were carried out on a highly homogenized estuarine sediment reference material (RM S7) prepared by the Joint Research Centre (JRC) of ISPRA. Extractable metal contents were measured by inductively coupled plasma-mass spectrometry (ICP-MS) and the results obtained in each fraction by all three methods were statistically compared for all the studied elements. The conventional and newly developed alternative extraction methods were finally compared by the analysis of BCR 601, which is certified for the three-step BCR sequential extraction procedure. According to the statistical evaluation of the results, the proposed accelerated sequential extraction methods are valid alternatives to conventional shaking, with much shorter extraction times.

Determination of Selenomethionine in Wheat Samples: Comparison of Gas Chromatography-Microwave-induced Plasma Atomic Emission Spectrometry, Gas Chromatography-Flame Photometric Detection and Gas Chromatography–Mass Spectrometry

A method is described for the selective determination of selenomethionine in wheat samples. The method is based on three steps prior to the determination: (1) hydrolysis of the proteins with tetramethylammonium hydroxide, (2) clean-up on an aluminium oxide column (acid form), (3) derivatization to convert selenomethionine into a compound suitable for GC. The derivatization reaction consists in esterification of the carboxylic acid group with propan-2-ol in 4 mol l -1 HCl medium and subsequent acylation of the amino group with heptafluorobutyric anhydride. The parameters affecting the efficiency of both reactions were optimized, as well as the esterification medium. Other esterification and acylation reagents were also tested. Three different detection techniques were evaluated using selenomethionine standard solutions: FPD, MIP-AES and MS. Electrothermal AAS was also tested, but proved to be unreliable. MS was selected as the best option.

Comparison between Different Leaching/Extraction Tests for the Evaluation of Metal Release from Fly ASH

Abstract A comparison of five different leaching/extraction tests, each characterized by different parameters such as liquid/solid ratio, pH, leachant, stirring conditions, duration time, has been performed on a highly homogenized fly ash reference material. Eight different elements (As, Cd, Cr, Cu, Ni, Pb, Se, Zn) have been considered in this study. The results show that, among all the considered experimental parameters, pH seems to have the greatest influence on metal release.

The Project for the Implementation of the Industrial Symbiosis Platform in Sicily: The Progress After the First Year of Operation

In May 2011, the Environmental Technologies Technical Unit of ENEA launched a project to build a platform of Industrial Symbiosis to be implemented in Sicilia Region. It is a 3 years project, in a framework of a larger asset to support productive development in southern Italy. This chapter summarizes the activities carried out during the 1st year of operation by the working group that participates in the initiative. The platform, whose main objective is to help in launching industrial symbiosis through a geo-referred information system support, acts as a tool in the service of business and territory and also offers a range of tools that may be of interest and use especially for SMEs. In addition to the technical aspects of the implementation of the information, tools, and website, the activities involved a first phase of consultation in Sicily with stakeholders, with particular reference to Confindustria Sicilia—with which ENEA has signed a specific Cooperation Agreement—and Sicilia Region, Regional Agency for Waste.