Determination of cadmium in urine by platform ET-AAS independent of matrix composition

Summary The optimization of the heating conditions, absorbance profiles, the influence of different matrix composition and the effect of delivering different volumes of urine samples were examined in order to evaluate the use of simple aqueous standards for the determination of cadmium in urine samples, using atomic absorption spectrometry with electrothermal atomization and the L'vov platform. Three reference materials were analysed for cadmium by the proposed method. The results indicate that a direct and accurate determination of urine cadmium is possible by using simple aqueous calibration standards, independently of the composition of the urine matrix.     

Application of the slurry technique to biological materials: a survey of literature

Summary The literature on the application of the slurry technique to biological materials is reviewed. It is obvious from the various applications that the most frequently employed atomization method for slurry analysis in biological materials is electrothermal atomization using either graphite tube or platform atomizers. The slurry technique is particularly useful when certified reference materials are not available and when the standard addition method is to be avoided. The literature survey revealed that this technique compares favourably with other methods for the determination of trace metals in biological materials.     

Simultaneous determination of nickel,iron, and copper in margarine by inductively coupled plasma-atomic emission spectroscopy after sample emulsification

Nickel, iron, and copper were determined in margarine samples by using emulsification followed by inductively coupled plasma-atomic emission spectroscopy. Sample treatment and instrumental conditions were optimized, and the results were compared with those obtained by a pseudodigestion method in order to evaluate the compatibility of both methodologies. The optimum amount of margarine in the emulsion was 35% when the surfactant Tween 80 was added as the emulsifier. Copper was below the detection limits of both methodologies, i.e., digestion and emulsion; iron and nickel concentrations found by both methodologies were similar. The detection limits of the emulsion method were 0.002, 0.015, and 0.092 mg/kg for copper, iron, and nickel, respectively. A benefit of the emulsion method is that laborious and lengthy sample digestion procedures are avoided. In addition, accurate and precise results are obtained. Recoveries with the emulsion method ranged from 101 to 104%, with relative standard deviations of < or = 6%.     

X-ray photoelectron spectroscopy study of pyrolytically coated graphite platforms submitted to simulated electrothermal atomic absorption spectrometry conditions

The present work is part of an ongoing project aiming to a better understanding of the mechanisms of atomization on graphite furnace platforms used for electrothermal atomic absorption spectrometry (ETAAS). It reports the study of unused pyrolytic graphite coated platforms of commercial origin, as well as platforms thermally or thermo-chemically treated under simulated ETAAS analysis conditions. X-ray photoelectron spectroscopy (XPS) was employed to study the elements present at the surfaces of the platforms. New, unused platforms showed the presence of molybdenum, of unknown origin, in concentrations up to 1 at.%. Species in two different oxidations states (Mo⁶⁺ and Mo²⁺) were detected by analyzing the Mo 3d spectral region with high resolution XPS. The analysis of the C 1s region demonstrated the presence of several signals, one of these at 283.3 eV related to the presence of Mo carbide. The O 1s region showed also various peaks, including a signal that can be attributed to the presence of MoO₃. Some carbon and oxygen signals were consistent with the presence of CO and C-O- (probably C-OH) groups on the platforms surfaces. Upon thermal treatment up to 2900 °C, the intensity of the Mo signal decreased, but peaks due to Mo oxides (Mo⁶⁺ and Mo⁵⁺) and carbide (Mo²⁺) were still apparent. Thermo-chemical treatment with 3 vol.% HCl solutions and heating up to 2900 °C resulted in further diminution of the Mo signal, with complete disappearance of Mo carbide species. Depth profiling of unused platforms by Ar⁺ ion etching at increasing time periods demonstrated that, upon removal of several layers of carbonaceous material, the Mo signal disappears suggesting that this contamination is present only at the surface of the pyrolytic graphite platform.     

Evaluation of dual sample introduction systems by comparison of cyclonic spray chambers with different entrance angles for ICP-OES

The operating characteristics of a number of locally constructed inductively coupled plasma (ICP) dual sample introduction designs used for the determination of volatile and non volatile elements have been compared. Four cyclonic spray chamber arrangements with entrance angles of 0, 45, 90, and 180° were tested. The operating characteristics studied included instrumental conditions, chemical conditions for the hydride generation reaction and analytical figures of merit. Analytical performance of the nebulization systems was characterized by determination of the signal to background ratio (SBR), the limits of detection (LODs), and the precision (RSDs). In general, the results suggest that the dual system with 45° configuration was found to be the best indicator of the analytical performance of the dual pneumatic nebulizer-cyclonic chamber arrangement studied, giving the best SBR, precision (1.0–3.5%) and in most cases the lowest detection limits (0.3–24.6 ng L^{− 1}) for both, the hydride and non-hydride forming elements. Long-term reproducibility from the 45 degree-dual system was superior to those of different angles configuration (ranging from 4.2 to 5.1% for the non- and hydride forming elements respectively). The applicability of the dual system was proven by analyzing NIST 1573 Tomato Leaves with satisfactory results.     

Discontinuity wave propagation in continua with dislocations

Summary The problem of discontinuity wave propagation is treated for an elastic body with a continuous distribution of dislocations and explicit values for speeds are obtained.

---

Sommario Nell'ambito della teoria dei continui elastici con una distribuzione continua di dislocazioni viene affrontato il problema della propagazione di onde ordinarie di discontinuità e vengono dati esplicitamente i valori delle velocità.

---

---

Work done in the sphere of activity of the G.N.F.M. of Italian C.N.R.