GC/multiple collector-ICPMS method for chlorine stable isotope analysis of chlorinated aliphatic hydrocarbons

Stable isotopic characterization of chlorine in chlorinated aliphatic pollution is potentially very valuable for risk assessment and monitoring remediation or natural attenuation. The approach has been underused because of the complexity of analysis and the time it takes. We have developed a new method that eliminates sample preparation. Gas chromatography produces individually eluted sample peaks for analysis. The He carrier gas is mixed with Ar and introduced directly into the torch of a multicollector ICPMS. The MC-ICPMS is run at a high mass resolution of >= 10 000 to eliminate interference of mass 37 ArH with Cl. The standardization approach is similar to that for continuous flow stable isotope analysis in which sample and reference materials are measured successively. We have measured PCE relative to a laboratory TCE standard mixed with the sample. Solvent samples of 200 nmol to 1.3 mu mol ( 24- 165 mu g of Cl) were measured. The PCE gave the same value relative to the TCE as measured by the conventional method with a precision of 0.12% ( 2 x standard error) but poorer precision for the smaller samples.

Development of orientation during electrospinning of fibres of poly(ε-caprolactone)

We explore the influence of a rotating collector on the internal structure of poly(ε-caprolactone) fibres electrospun from a solution in dichloroethane. We find that above a threshold collector speed, the mean fibre diameter reduces as the speed increases and the fibres are further extended. Small-angle and wide-angle X-ray scattering techniques show a preferred orientation of the lamellar crystals normal to the fibre axis which increases with collector speed to a maximum and then reduces. We have separated out the processes of fibre alignment on the collector and the orientation of crystals within the fibres. There are several stages to this behaviour which correspond to the situations (a) where the collector speed is slower than the fibre spinning rate, (b) the fibre is mechanically extended by the rotating collector and (c) where the deformation leads to fibre fracture. The mechanical deformation leads to a development of preferred orientation with extension which is similar to the prediction of the pseudo-affine deformation model and suggests that the deformation takes place during the spinning process after the crystals have formed.