Abstract: FT-IR spectroscopy and impedance measurements of tin dioxide sensor materials at working temperatures up to 450 °C in atmospheres with varying O2/N2 ratio are used as an in situ probe to study the interactions at the surface of the semiconducting oxide. Every diminution in the oxygen content above the sample induces a broad IR absorption band (X-band) between 2300700 cm−1 with a few small peaks in the 1400850 cm−1 region of the spectrum superimposed on it. The X-band results from the enchanced electron concentration in the bulk of the tin dioxide domain. The fine structure is due to the absorption of several kinds of surface oxygen species associated vibration modes. The porous tin dioxide consists of domains were the outward shell is depleted of electrons by the formation of adsorbed O− species on oxygen surface sites, SO(O− species. In our proposed model for the impedance data this gives rise to a parallel RpCp circuit for the domain boundary characteristics and to an Rs parameter for the intradomain resistance. The evolution of these IR and impedance spectroscopic effects with temperature and oxygen content is used to set up, to confirm and refine a physicochemical operation model of tin dioxide gas sensor. This model consists of a sensitizing reaction sequence in the presence of oxygen and a gas-detection reaction sequence when a reducing gas is present. Based on this model, the principal disadvantages of this type of gas sensor become clear. Every factor that influences the concentration of SO(O−) species, causes a conductance modification. If we can control and direct the nature, the number and the arrangement of the tin dioxide domains, a directed development and improvement of the sensor characteristics is possible.

Abstract: Differential-pulse anodic stripping voltammetry is applied to determine cadmium, lead and copper in rain water acidified with nitric acid to pH 1.5, and zinc after partial neutralization to pH 4.5. Subsequently, cobalt and nickel are measured in the adsorptive mode after formation of their dimethylglyoximates. The effects of pH on the stripping peaks for Zn, Cd, Pb and Cu and of chloride on the stripping peak of copper are reported. Good agreement is found with d.p.s.v. determinations in hydrochloric acid medium and with a.a.s. measurements in most cases. Excellent accuracy is demonstrated; the average relative standard deviation per measurement appears to be between 12 and 22% for the overall analytical procedure for concentrations of 0.1550 μgl−1 of the various metals in the samples.

Abstract: The relative merits of eight procedures for preconcentrations of trace metal ions from natural water samples and synthetic solutions are evaluated. Spikes (100 μg l−1 ) of Mn, Co, Zn, Eu, Cs and Ba and the corresponding radioactive tracers were added to batches of drinking water, estuarine water, sea water, ground water, twice-distilled water and ahumic material solution. After equilibration for 25 months, the following techniques were applied: passage through columns of Dowex Al chelating resin and ofsilylated silica gel, filtration through laminate membrane filters and chelating diethylenetriamine cellulose filters, precipitation with sodium diethyldithiocarbamate and l-(2-pyridylazo)-2-naphthol, extraction with ammonium pyrrolidinedithiocarbamate, and chelation by 8-quinolinol (oxine) followed by adsorption on activated carbon. The quantitative characteristics of these techniques and the influence of the water matrix effects are discussed, as well as the applicability for x-ray fluorescence analysis.

Abstract: A fast (10 min) non-destructive determination of copper in. steel and cast iron by 14-MeV neutron activation analysis is described. The 0.511-MeV annihilation radiation of62Cu (T1/2=9.8 min), induced by the reaction63Cu(n,2n)62Cu, is counted by two opposing NaI(Tl) detectors operating in coincidence. An oxygen flux monitor is used to normalise the irradiations. For high phosphorus contents, two measurements are made and the 9-min activity contribution is calculated. As the iron content of the samples is known, the use of pure iron samples allows correction for53Fe activity from the reaction54Fe(n,2n)53Fe(T1/2= 8.9 min). When the phosphorus and silicon activities are low, the procedure of counting and computing can be greatly simplified. Nuclear interferences of most common alloying and impurity elements were investigated.The precision is 23% for steels containing above 1% Cu, andCa. 10% for 0.1%Cu.

Abstract: Differential-pulse stripping voltammetry is applied to measure zinc, cadmium, lead and copper by anodic stripping and selenium(IV) by cathodic stripping in rain water at pH 2; subsequently, at pH 9,1, manganese is measured by anodic stripping on the same portion, and cobalt and nickel are measured in the adsorptive mode after formation of their dimethylglyoximates. The instrumental parameters are optimized. The linear ranges, mutual interferences and detection limits are studied. Excellent accuracy is demonstrated; the standard deviation is around 15% at 2.550 μg l−1 levels. The method is shown to be applicable for rain water.