International and National Journals
M. L. Bonardi, E. Rizzio, M. Gallorini, F. Groppi, H. S. Mainardi
Improved radiochemical separation of no-carrier-added vanadium-48 from proton irradiated titanium target
Journal of Radioanalalytical and Nuclear Chemistry, Vol. 263 No. 1, pp. 23-28, 2005.
A novel radiochemical separation for 48V radiotracer in no-carrier-added (NCA) form, via proton irradiation on Ti targets of natural isotopic composition has been developed. Metallic Ti targets irradiated with 21 MeV proton beam energy was submitted to a selective radiochemical separation consisting of an alkaline fusion-precipitation step, followed by column Chelex-100 chromatographic purification. Very high specific activity 48V, at levels of hundreds MBq.µg-1 was prepared. Chemical analysis of radiotracer was carried out by ET-AAS and INAA. The decontamination factor from Ti target was 5 · 105, with an overall radiochemical yield for 48V larger than 90%. The NCA 48V has used for labeling a range of chemical forms of V(III, IV, V) and applied in the study of metabolic behavior of different chemical forms in in-vivo and in-vitro experiments on rats and cell cultures.
D. Bagatti, M. C. Cantone, A. Giussani, S. Ridone, C. Birattari, M. L. Bonardi, F. Groppi, A. Martinotti, S. Morzenti, M. Gallorini, E. Rizzio
Analytical and radioanalytical quality control of purity and stability of radiopharmaceutical compound [186g Re] Re-HEDP for bone metastases pain palliation
Journal of Radioanalalytical and Nuclear Chemistry, Vol. 263, no. 2, pp. 515-520, 2005.
The nuclear properties of 186gRe make it a useful agent for radionuclide therapy and imaging. The coordination compound [186gRe]Re-HEDP has proved to be a successful bone seeking agent for palliation of metastatic bonepain. Chemical, radiochemical and radionuclidic purity of commercial radiopharmaceutical [186gRe]Re-HEDP have been checked by means by γ- and β- spectrometries, INAA and paper radiochromatography. The results indicate a good radionuclidic purity, with levels of contamination from the short-lived 188Re well below the required specifications. After injection of the radiopharmaceutical, the radiochemical measurements conducted in vivo, on biological matrices, blood, plasma and urine, have shown that, entering the systemic circulation, 186gRe dissociates from the bis-phosphonate complex as hydrosoluble [186gRe]ReO4-, and the two chemical species follow different biokinetics.
L. Bergamaschi, E. Rizzio, G. Giaveri , L. Giordani , A. Profumo, M. Gallorini
INAA for the determination of trace elements and evaluation of their enrichment factors in lichens of high altitude areas
Journal of Radioanalalytical and Nuclear Chemistry, Vol. 263, no. 3, pp 721-724, 2005.
Trace element (TE) characterization and analysis in epiphytic lichens collected in different areas of the Himalayas (Nepal) and of the Alps (Italy) is presented. The results give information for the assessment of TE distribution present in the two different areas. The evaluation of the enrichment factors may provide information for many elements about their association to long-distance atmospheric transport phenomena. To this purpose, samples of superficial soils, collected in the same areas of those of the lichens, have also been analyzed. Most of the trace elements were determined by instrumental neutron activation analysis (INAA), while lead and cadmium measurements were carried out with electrothermal atomic absorption spectroscopy (ET-AAS).
G. Giaveri, L. Bergamaschi, E. Rizzio, G. Verza, G. Zambelli, A. Brandone, A. Profumo, R. Baudo, G. Tartari, M. Gallorini
INAA at the top of the world: elemental characterization and analysis of airborne particulate matter collected in the Himalayas at 5,100 m high
Journal of Radioanalalytical and Nuclear Chemistry, Vol. 263, no. 3, pp. 725-732, 2005.
In 1990, following an agreement with the Royal Nepal Academy of Science, the Italian National Research Council (CNR) installed a scientific laboratory (Pyramid) at 5050 m (s.l.) in the Himalayan region. Among the environmental related researches, the task project RATEAP (Remote Areas Trace Elements Atmospheric Pollution), started in 2001, aims at obtaining information about the chemical composition of the high altitude airborne particulate matter. During the period of March-April 2002 series of samplings have been carried out by pump aspiration. Samples of total suspended particles (TSP) as well as of the particles size fraction PM10 and PM 2.5 have been collected and submitted to INAA for the determination of more than 30 elements present, at nanogram levels, in few micrograms of air dust. Data quality assurance has been performed by the analysis of different NIST SRMs and, in particular, the SRM 2783 Air particulate on Filter Media.
L. Zecca, F. A. Zucca, M. Toscani, F. Adorni, G. Giaveri, E. Rizzio, M. Gallorini
Iron, copper and their proteins in Substantia Nigra of human brain during aging
Journal of Radioanalalytical and Nuclear Chemistry, 263, no. 3, pp. 733-737, 2005.
Scarce information is available on the content of metals and their molecules in the human brain. Iron, copper and other metals are involved in neurodegenerative disorders like Parkinson' s Disease (PD), however, their behavior in physiological conditions is poorly understood. In this study we have measured iron, copper and their major proteins (ferritins and ceruloplasmin) in substantia nigra (SN) of normal subjects at different ages, since this is the main target region of PD. An increasing trend for iron and copper concentration was found in aging. Ferritins were also increasing in aging while ceruloplasmin did not vary. These data show that the accumulation of these metals requires an increased expression of storage molecules to prevent toxic effects of iron and copper.
L. Giordani, E. Rizzio, A. Brandone
Neutron activation analysis in forensic investigations: trace elements characterization of cigarettes
Journal of Radioanalytical and Nuclear Chemistry, Vol. 263, no. 3, pp. 739-744, 2005.
Police investigations of the Italian Ministry of Treasury Police involving the illicit sale of tobacco lead to the confiscation of large quantities of smuggled cigarettes. Thousands of tons of cigarettes of different manufacturers are sequestrated yearly in many regions of Italy and different criminal organizations have been identified as unlawful importers. In order to verify whether the recovered smuggled lots of cigarettes come from the official manufacturers, or they have produced illicitly, usually chemical analysis are carried out. By the determination of trace elements content, specific information can be obtained by comparing different brands of cigarettes and different batches of tobacco. In this work, samples of tobacco of cigarettes manufactured by the Italian State Monopoly, taken as "reference samples", have been compared with those of illicit origin. Elements such as Co, Br, Cr and Sc have been found to be useful for the selective characterization. The results, submitted to statistical elaboration, provided important information on the origin of smuggled cigarettes.
L. Bergamaschi, E. Rizzio, A. Profumo, M. Gallorini
Determination of trace elements by INAA in urban air particulate matter and transplanted lichens
Journal of Radioanalytical and Nuclear Chemistry, Vol. 263, no. 3, pp. 745-750, 2005.
In 1990, following an agreement with the Royal Nepal Academy of Science, the Italian National Research Council (CNR) installed a scientific laboratory (Pyramid) at 5050 m (s.l.) in the Himalayan region. Among the environmental related researches, the task project RATEAP (Remote Areas Trace Elements Atmospheric Pollution), started in 2001, aims at obtaining information about the chemical composition of the high altitude airborne particulate matter. During the period of March-April 2002 series of samplings have been carried out by pump aspiration. Samples of total suspended particles (TSP) as well as of the particles size fraction PM10 and PM 2.5 have been collected and submitted to INAA for the determination of more than 30 elements present, at nanogram levels, in few micrograms of air dust. Data quality assurance has been performed by the analysis of different NIST SRMs and, in particular, the SRM 2783 Air particulate on Filter Media.
P. Calza, V. Maurino, C. Minero, E. Pelizzetti, M. Sega, M. Vincenti
Photoinduced halophenol formation in the presence of iron(III) species or cadmium sulfide
Journal of Photochemistry and Photobiology A: Chemistry, ed: Elsevier, 170, 2005, pp. 61-67.
Phenol photo-induced decomposition has been investigated in the presence of iron(III) oxide or iron(III) ions at different pH, paying particular attention to the evolution of intermediates. The addition of halides causes a modest decrease in phenol degradation rate and starts additional transformation pathways. Chloride induces the formation of chlorinated compounds (2- and 4-chlorophenol), whose concentrations are strongly dependent on pH. Analogously, bromide ions lead to the formation of bromophenols. Similar investigations have been performed by adopting cadmium sulfide as a photocatalyst, whose valence band edge potential (VB..) allows the oxidation of bromide but not chloride. The addition of chloride does not lead to chlorophenols, while bromide causes the formation of bromophenols, thus confirming the possibility of obtaining selective abiotic halogenation of phenol.
P. Fisicaro, E. Ferrara, E. Prenesti, S. Berto
Role of the activity coefficient in the dissemination of pH: comparison of primary (Harned cell) and secondary (glass electrode) measurements on phosphate buffer considering activity and concentration scales
Analytical and Bioanalytical Chemistry, Vol. 383, no. 2, pp. 341-348, 2005.
Despite recent efforts devoted to assessing both the theoretical rationale and the experimental strategy for assignment of primary pH values, these have not yet been accomplished satisfactorily. Traceability and comparability of pH values are achieved only within the constraints of internationally accepted conventions and predefined conditions that cannot account for all possible situations when pH measurements is measured. For this paper, primary (Harned cell) measurements (traceable to the SI system) of the pH of a phosphate buffer have been considered and the results have been compared with secondary (glass electrode) measurements obtained considering either the activity (paH) or concentration scale (pcH) of the hydrogen ions. It is shown that fitting and comparable paH and pcH results are attainable if evaluation of the activity coefficient γi is performed using better estimates of the ionic strength, according to an enhanced application of the Debye-Hückel theory.
E. Ferrara
Earth science, soil chemistry and archaeology
American Journal of Archaeology, Vol. 109, no. 1, pp. 87-90, 2005.
Soil science, chemistry, and geology naturally combine in archaeology to study landscape, environment, the history of sites belonging to previous civilizations, to supply evidence for household and rural activities, or to retrieve fabrication and provenance of artefacts made of earth resources (e.g. chert and obsidian blades, gemstones, earthenware, and even glass and metallic objects).
A. Profumo, D. Merli, M. Pesavento
Voltammetric determination of inorganic As(III) and total inorganic As in natural waters
Analytica Chimica Acta, 539, pp, 245-250, 2005.
The paper describes a voltammetric method for the determination of As(III) and total inorganic As at ppb and sub ppb level using cathodic stripping voltammetry. This method is based on the formation of a copper-arsenic intermetallic at HDME during the preconcentration step. Sodium dithionite is used for the reduction of As(V) to As(III). As(III) is then determined in HBr supporting electrolyte. Compared to the procedures described in previous literature, the determination of total inorganic arsenic in such conditions needs shorter deposition times and less amount of copper. Moreover, better linear response; current versus concentration and peaks repeatability are obtained. In the described working conditions LOQ for As(III) and As(V) are 0.010 and 0.020 ppb respectively, for a deposition time of 300 s. Standard deviation for I ppb arsenic concentration (n = 7) is 5%. The method was applied to thermal, spring and sea waters and accuracy was verified by a recovery test on spiked samples. Total arsenic concentrations are in good agreement with those obtained in ICP-OES-HG.
G. E. Kostakis, L. Casella, N. Hadjiliasdis, E. Monzani, N. Kourkoumelis, J. C. Plakatouras
Interpenetrated networks form a novel nanometer-sized pseudopeptidic ligand, brinding water, and transition metal ions with cds topology
Chemical Communications, Royal Society of Chemistry, pp. 3859-3861, 2005.
The combination of a new pseudopeptidic ligand, transition metal ions, and bridging water molecules results in the formation of [M(µ-TBG)(µ-H2O)(H2O)(2)]· 2H(2)O (M: Cu, Co and H(2)TBG: terephthaloylbisglycine); both compounds show rare two-fold interpenetrated three-dimensional cds-nets and reversible loss of coordinated and lattice water molecules.
M. Plassa
Metrologia e chimica: una scoperta reciproca
Tutto Misure, anno VII, n. 01, pp. 27-29, 2005.
Nel presente articolo dapprima sono delineate l'evoluzione del rapporto tra la metrologia e la chimica e le implicazioni che ne derivano. Sono poi citate le principali fonti da cui tradizionalmente il mondo della chimica ha attinto i suoi riferimenti metrologici. Quindi sono descritte le difficoltà che hanno caratterizzato l'incontro tra la metrologia e la chimica. Infine sono elencati gli effetti sortiti da tale incontro e si richiama l'attenzione sulle peculiarità della grandezza "quantità di sostanza" e dell'analisi chimica.
Conference Proceedings
M. P. Sassi, E. Malgeri
Frequency referred spectroscopy as a tool for accurate gas analysis
Proceedings of the XII International Metrology Congress 2005, Lyon (France), June 2005.
F. Alasia, E. Amico di Meane, A. Capelli, M. Plassa, M. Sega
Realizzazione di miscele gassose primarie all'IMGC-CNR
Atti del Congresso Metrologia e Qualità, pp. 66-68, Torino, febbraio 2005.
For the Istituto di Metrologia "G. Colonnetti" the realization of primary reference gas mixtures is a relevant goal both from an institutional viewpoint for developing a national system for the traceability of gas analysis measurements and the establishment of national standards of amount of substance, and for the analytical equipments calibration. This paper describes the facility for preparing primary gaseous mixtures by the gravimetric method which was projected and realized entirely at the Mass section of IMGC. In addition it deals also with the first realization with the gravimetric method of two gas mixtures of CO2 at the concentration of about 250 µmol/mol in N2. Their concentration was determined by analysis with non-dispersive infrared photometry and the expanded uncertainty with k=2 on the composition was estimated to be 1%. A stability study on these mixtures is going on and until now they seem to be very stable.
E. Ferrara, P. Fisicaro
Le caratteristiche dei sistemi di misura in chimica
Atti del Congresso Metrologia e Qualità, pp. 82-87, Torino, febbraio 2005.
Applicare per trasposizione i concetti e le procedure della metrologia tradizionale alla chimica, considerando le analisi in questo campo analoghe a tutte le altre operazioni di misura, può portare a semplificazioni e sottovalutazioni azzardate. Numerose considerazioni e precisazioni sono invece opportune sulle specificità delle operazioni di misura in chimica.
E. Ferrara, P. Fisicaro
Sviluppo di un sistema di riferimento per la misura di pH in soluzioni acquose
Atti del Congresso Metrologia e Qualità, pp. 88-92, Torino, febbraio 2005.
Il pH è l'unità di misura che indica l'acidità o la basicità di una soluzione ad una determinata temperatura. La misura di pH riveste un ruolo di grande importanza nella chimica analitica e, in generale, in tutte quelle applicazioni che coinvolgono il controllo di parametri ed equilibri in soluzione acquosa.
E. Amico di Meane, A. Carotenuto, M. Dell'Isola, G. Ficco, M. Sega, A. Viola
Problematiche di misura e taratura nelle misure di energia termica e chimica
Atti del Congresso Metrologia e Qualità, pp. 97-103, Torino, febbraio 2005.
Energy measurement is doubtless among the most complex ones in metrology for both the present impossibility in carrying out direct measurements and its several forms which deal with mechanical, thermical, electrical and chemical metrology. This needs different measurement instruments and knowledge in various fields. In this paper the authors start with reminding measurement methods for the different forms of chemical and thermical energy and their flows then they analyse the main problems in measuring thermical and chemical energy with special reference to the uncertainty evaluation and to the determination of a proper metrological traceability chain. Finally the problem of energy measurement in the co-generation plants is discussed. An important additional development of the work carried out could regard an experimental analysis of the concerned plants and their metrological performances.
A. Alagna, E. Amico di Meane, A. Carotenuto, M. Dell'Isola, M. Sega, B. Viglietti
Valutazione dell'incertezza di misura secondo la Norma EN ISO 14956 per l'accreditamento di un laboratorio mobile per l'analisi di emissioni gassose
Atti del Congresso Metrologia e Qualità, pp. 427-432, Torino, febbraio 2005.
The mobile laboratory of Snam Rete Gas has been used since 1990 in order to measure gas pollutants in the emissions of the combustion processes deriving from turbines, gas engines, boilers and vaporizers, by means of O2, CO, NOx, NO, CO2 and SO2 analysers. In the present work the first results from the characterization study of the mobile laboratory are showed. This study which began in 2002, regards mainly the evaluation of the metrological performances of each analyser of the considered laboratory. Each analyser was calibrated with traceable gas mixtures in its measurement fields. The calibration uncertainty was estimated according to EN ISO 14956 standard. Its value is about 0,2% of the span concentration of each component. For the accreditation of the laboratory according to UNI CEI EN ISO/IEC 17025 standard, a field characterization of the analysers is needed and is going on.
Technical Reports
E. Amico di Meane, M. Sega
Caratterizzazione di un analizzatore NDIR di CO ABB modello URAS 14
Rapporto Tecnico IMGC n. P267, pp. 1-11, 2005.
The paper describes the tests carried out in order to characterize an NDIR analyser for the determination of carbon monoxide (CO) at emission level and comments the achieved results. A series of tests to highlight the behaviour and the main characteristics of such analyser was chosen according to the experience developed by the Gas Analysis group. At the beginning the measurement procedure is described showing the safety measures followed for the analysis of a toxic gas such CO and CO containing mixtures. The characterization shows that the instrument response is neither affected by the changes in the atmospheric pressure, within the considered variation, nor by the flow of the input gas, in the range between 20 and 70 L/h, it is linear, has a satisfactory repetability, does not show interference problems by CO2 and C3H8 in the concentrations of the automotive emissions, the zero signal is stable. The calibration uncertainty can be decreased by increasing the number of the concentration levels and/or using mixtures with a smaller composition uncertainty.
F. Rolle, E. Amico di Meane, M. Sega
Caratterizzazione di un analizzatore NDIR di CO2ABB modello URAS 14 a livello delle emissioni
Rapporto Tecnico IMGC n. P268, pp. 1-14, 2005.
The paper describes the tests carried out in order to characterize an NDIR analyser for the determination of carbon dioxide (CO2) at emission level and comments the achieved results. A series of tests to highlight the behaviour and the main characteristics of such analyser was chosen according to the experience developed by the Gas Analysis group. At the beginning the measurement procedure is described. The characterization shows that the instrument response is neither affected by the changes in the atmospheric pressure, within the considered variation, nor by the flow of the input gas, in the range between 20 and 50 L/h, it is linear, has a satisfactory repetability, does not show interference problems by CO2 and C3H8 in the concentrations of the automotive emissions, the zero signal is stable. The calibration uncertainty can be decreased by using mixtures with a smaller composition uncertainty as in the first calibration carried out or adopting a smaller concentration range as it was observed by comparing the second and the third calibration.
E. Amico di Meane
Materiali di riferimento: alcune delle principali tematiche affrontate dalla letteratura negli ultimi anni
Rapporto Tecnico IMGC n. P270, revisione della prima edizione del 1999, pp. 1-17, 2005.
In the last few years there has been a growing interest towards traceability in the chemical measurement field and, consequently, for reference materials. In the chemical measurements the metrological approach is not always well defined and the debate is still open about topics such as calibration, sampling, uncertainty, validation of the measurement method. Reference materials play an important role to achieve traceability in chemical measurement and they are used for example in the international comparisons. This paper is based on guides, work documents, and review papers. It does not aim to cover the whole literature on this subject but it presents a brief survey of the main questions that have been faced about reference materials since 1992 until 1999 and that nevertheless are still matter of discussion. The several references are reported in chronological order. In this updated version, the previous paper was revised and additional references were added.
L. Revel, V. Ciaiolo
Sensore per la determinazione di concentrazione di ammoniaca nel processo di nitrurazione
Rapporto Tecnico IMGC n. 142, dicembre 2005.