Determination of tungsten and tin ions after preconcentration by flotation

A highly sensitive and selective combined method of flotation followed by spectrophotometry/d.c. polarography for the determination of tungsten and tin ions in acid and alkaline waste waters and hydrometallurgical solutions is presented here. Both kinds of ions are coprecipitated in the analyte solution with zirconium hydroxide after addition of ZrOCl₂ solution and ammonia. Afterwards, the collector precipitate is separated from the aqueous phase and preconcentrated by flotation for which sodium oleate and a frother are added. The precipitate is dissolved in a small amount of acid, with the organic reagents being destroyed by oxidation. The enrichment factor of the proposed technique is 100, with variations possible. Recovery is 94% for tungsten and 99% for tin. Spectrophotometry of the thiocyanate complex and d.c. polarography are applied as determination techniques for tungsten and tin, respectively. Detection limits attainable by this technique are 6 ng · ml^–1 for tungsten and 5 ng · ml^–1 for tin for the initial sample.     

Acid-base and surface energy characterization of grafted polyethylene using inverse gas chromatography

For a specific design of interfaces, i.e. in composites and blends, it is essential to know the surface thermodynamics of the components. Polyethylene grafted with maleic anhydride and maleic anhydride-styrene mixtures, respectively, was the component of interest of our investigations. Inverse gas chromatography (IGC) at infinite dilution was shown to be an appropriate method to evaluate the dispersive and acid-base surface characteristics although there is an influence of bulk absorption and morphology when performing IGC above the glass transition temperature of the polymer.     

A concept of a scanning positron microscope

The concept of a scanning positron microscope which is under construction in München and Trento will be shown. A beam with a variable energy from 1 to 30 keV and a spot diameter of 1 m, which can be scanned over an area of (0.6×0.6) mm², is formed after a double stage stochastic cooling of the positrons emitted from a radioactive source. Additionally, the beam will be pulsed to have a well-defined time base for positron lifetime measurements. The design of the microscope is dominated by special demands of positron physics. Therefore, the microscope contains electron optical elements which are well known but rarely used. These are the through the lens reflection remoderator and the optical column with a magnetic side gap lens as probe forming lens.     

Semi-automated hollow-fibre membrane extraction,a novel enrichment technique for the determination of biologically active compounds in water samples

An automated hollow fibre membrane extraction technique was developed for the GC-MS determination of pharmaceutical and endocrine disrupting compounds in water samples. Enrichment was carried out inside a porous polypropylene hollow fibre membrane, which separated the aqueous and organic phases and regulated the transfer of analytes. n-Octanol placed inside the hollow fibre was used as the acceptor solution. A water-solvent ratio of about 300:1 was used to concentrate the analytes. After 1 hour's extraction of the water sample under magnetic stirring, 1 microl of the n-octanol phase was automatically injected from the hollow fibre into the GC-MS. Development work included examining the influence of different sample matrices, volumes, extraction times and extraction solvents. The detection limits, linearity and standard deviations of the method were determined using drugs such as ibuprofen, phenazone and carbamazepine as well as the endocrine disrupting compounds. technical nonylphenols, bisphenol A, 17alpha-ethinylestradiol and tonalide by way of example.     

Quantification of cyclophosphamide and its metabolites in urine using liquid chromatography/tandem mass spectrometry

A reliable and easy to use liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed for the simultaneous quantification of urinary concentrations of cyclophosphamide (CP) and its main metabolites excreted in urine, i.e. N-dechloroethylcyclophosphamide (DCL-CP), 4-ketocyclophosphamide (4KetoCP), and carboxyphosphamide (CarboxyCP). Sample preparation consisted of dilution of urine with an aqueous solution of the internal standard D(4)-CP and methanol, and centrifugation. LC/MS/MS detection was performed using a triple-quadrupole mass spectrometer working in selected reaction monitoring mode. All analytes were quantified in a single run within 11.5 min. The limits of detection were 5 ng/mL for CP and 4KetoCP, 1 ng/mL for DCL-CP, and 30 ng/mL for CarboxyCP. Quantification ranges were adjusted to the expected concentrations in 24-h urine collections of patients treated with a polychemotherapy regimen (3-175 microg/mL for CP, 0.5-27 microg/mL for 4KetoCP and 0.17-9 microg/mL for CarboxyCP and DCL-CP, respectively). The method was validated according to international guidelines of the ICH and the FDA.     

Das Hexamethyl-trisila-tetraphospha-nortricyclen,P4(Sime2)3

Hexamethyl-trisila-tetraphospha-nortricyclene, P₄ Sime₂₃ Reaction of white phosphorus with Na/K alloy and subsequent treatment with me₂SiCl₂ (me = CH₃) yields crystalline P₄(Sime₂)₃ (m. p. 159–160°C) along with polymeric silylphosphanes. The structure is derived from ³¹P-n.m.r.and mass spectra and turns out to be analogous to P₄S₃.     

Characterization of maleic acid/anhydride copolymer films by low-rate dynamic liquid-fluid contact angle measurements using axisymmetric drop shape analysis

Thin films of alternating maleic acid/anhydride copolymers (poly(octadecene-alt-maleic acid/anhydride), POMA; poly(propene-alt-maleic acid/anhydride), PPMA; poly(styrene-alt-maleic acid/anhydride), PSMA) were studied to unravel the influence of the comonomer characteristics in the backbone on the surface-energetic properties of the copolymer films in the dry state and in contact with aqueous solutions. Water contact angle measurements revealed a graduation of the wettability of the dry hydrolyzed and annealed copolymer films that was dependent on the comonomer unit. It ranged from moderately hydrophilic (PPMA, annealed gamma(sv) = 39.9 mJ/m2) to very hydrophobic (POMA, annealed, gamma(sv) = 18.4 mJ/m2) surfaces. Liquid-fluid contact angle measurements using captive air bubbles were performed in different aqueous media (pure water, phosphate-buffered saline, and 10(-)(3) M KCl of two different pH values (pH = 3 and pH = 10) to study the copolymer films in their hydrated states relevant for biointerfacial phenomena. It was found that the graduation of the wettability of the copolymer films in the dry state is overall maintained upon immersion in aqueous solutions. The dependence of the wettability on the pH value of the aqueous medium could be related to the (de)protonation of the carboxylic groups.     

Regularity of ghosts in tensor tomography

We study on a compact Riemannian manifold with boundary the ray transform I which integrates symmetric tensor fields over geodesics. A tensor field is said to be a nontrivial ghost if it is in the kernel of I and is L²-orthogonal to all potential fields. We prove that a nontrivial ghost is smooth in the case of a simple metric. This implies that the wave front set of the solenoidal part of a field f can be recovered from the ray transform If. We give an explicit procedure for recovering the wave front set.     

On the structure of glassy polymers. IV. Small-angle x-ray scattering from rigid polyvinyl chloride

The small-angle x-ray scattering (SAXS) from quenched and annealed rigid polyvinyl chloride (PVC) has been measured using a Bonse–Hart system. After correcting for absorption, background, and beam divergence, the scattering has been placed on an absolute basis using a standard silica suspension as a reference. The scattering from annealed (6 days at 75°C) and unannealed PVC was identical within experimental error, varying with scattering angle in a manner similar to the SAXS from other amorphous polymers. The intensity decreases rapidly with increasing scattering angle over the ranges from 20 sec to 20 min. Beyond 20 min the intensity is fairly constant, decreasing only slightly with increasing angle. At the largest angles of measurement (in the range of 120 min), the measured intensity is close to the value calculated for thermal density fluctuations frozen-in at the glass transition. The angular variation of intensity is well described by the scattering from heterogeneities of various sizes and concentrations superimposed on the scattering from thermal density fluctuations. These heterogeneities range in radius from 50 to 4500 Å and, assuming the crystalline excess density, the total concentration of heterogeneities is less than 0.5%. The mean-square fluctuation in density, determined from the measured intensity invariant, is also consistent with such a distribution of heterogeneities. The present SAXS results on rigid PVC are inconsistent with the presence of nodular features as representative of the bulk polymer. Rather, it is suggested that they are associated with surface effects. It is further suggested that previously indicated volume fractions of crystallinity in rigid PVC (generally in the range of 5–12%) are incorrect, and that the model of a three-dimensional network of crystallites used to explain the rheological behavior of this material should be re-examined.