Luminol Chemiluminescence with Heteropoly Acids and its Application to the Determination of Arsenate,Germanate, Phosphate and Silicate by Ion Chromatography

A flow-injection chemiluminescence (CL) method has been proposed for sensitive determination of arsenate, germanate, phosphate and silicate, after separation by ion chromatography (IC). The post-column detection system involved formation of heteropoly acid in a H₂SO₄ medium before the CL reaction with luminol in an NaOH medium. For separation, heteropoly acid formation and the CL detection reaction, pH requirements were not compatible. When present as a heteropoly acid complex with molybdenum(VI), ger- manium(IV) and silicon(IV) caused CL emission from oxidation of luminol, and such a CL oxidation of luminol was observed analogously for arsenic(V) and phosphorus(V) but with the addition of metavanadate ion to the acid solution of molybdate. Good sensitivity for the three analytes arsenic(V), ger- manium(IV) and phosphorus(V) could be given by a single set of reagent conditions, chosen carefully. Another set was suitable for determining phosphorus(V) and silicon(IV). The minimum detectable concentrations of arsenic(V), germanium(IV), phosphorus(V) and silicon(IV) were 10, 50, 1 and 10 μg l⁻¹, respectively. Linear calibrations for arsenic(V), germanium(IV), phosphorus(V) and silicon(IV) were established over the respective concentration ranges of 10–1000, 50–25000, 1–1000 and 50–1 μg l⁻¹. The proposed IC–CL method was successfully applied to analyses of a seaweed reference material, rice wine and water samples.     

Thermal degradation of poly-p-oxybenzoate under vacuum

The thermal degradation of poly-p-oxybenzoate in vacuo as function of temperature has been studied. The energy of activation of the process up to about 30% volatile formation is 59.6 kcal/mole. The degradation is preceded by induction periods, which have been shown to be due to poor heat conductivity of the polymer powder. CO, CO₂, phenol, and an unknown compound of molecular weight larger than 200 are the main degradation products found by chromatographic analysis. Infrared spectra of the original polymer, the polymer residue after degradation and of a degradation product solid at room temperature are presented. The possible reactions taking place have been indicated. The heat stability of the polymer in vacuo lies between those of polytetra-fluoroethylene and polyethylene.     

Scattering of muonic hydrogen atoms

Our measurement compares the energy dependence of the scattering cross-sections of muonic deuterium and tritium on hydrogen molecules for collisions in the energy range 0.1–45 eV. A time-of-flight method was used to measure the scattering cross-section as a function of the muonic atom beam energy and shows clearly the Ramsauer–Townsend effect. The results are compared with theoretical calculations by using Monte Carlo simulations. The molecular pdμ and ptμ formation creates background processes. We measure the formation rates in solid hydrogen by detecting the 5.5 MeV (pdμ) and 19.8 MeV (ptμ) γ-rays emitted during the subsequent nuclear fusion processes. This revised version was published online in August 2006 with corrections to the Cover Date.     

New effects in low energy scattering of pµ atoms

Strong solid state effects in low energy scattering of pμ atoms in solid hydrogen are reported and analyzed. Such effects have been observed in TRIUMF experiment E742 where muons are stopped in thin frozen (3 K) layers of hydrogen. Emission of low energy pμ atoms from the hydrogen layer into adjacent vacuum was much higher than expected, based on calculations which ignored the solid nature of hydrogen. Monte Carlo simulations, performed using the scattering cross-sections with solid state effects taken into account, show the important role of the coherent elastic Bragg scattering in the diffusion of pμ atoms. For pμ energies lower than the Bragg cut-off limit (∼2 meV) the total scattering cross-section falls by several orders of magnitude, the hydrogen target becomes transparent and the emission of cold pμ atoms takes place. This revised version was published online in August 2006 with corrections to the Cover Date.