A D Warren

Investigation of colloidal graphite as a matrix for matrix-assisted laser desorption/ionisation mass spectrometry of low molecular weight analytes.

The analysis of low molecular weight compounds by matrix-assisted laser desorption/ionisation mass spectrometry is problematic due to the interference and suppression of analyte ionisation by the matrices typically employed - which are themselves low molecular weight compounds. The application of colloidal graphite is demonstrated here as an easy to use matrix that can promote the ionisation of a wide range of analytes including low molecular weight organic compounds, complex natural products and inorganic complexes. Analyte ionisation with colloidal graphite is compared with traditional organic matrices along with various other sources of graphite (e.g. graphite rods and charcoal pencils). Factors such as ease of application, spectra reproducibility, spot longevity, spot-to-spot reproducibility and spot homogeneity (through single spot imaging) are explored. For some analytes, considerable matrix suppression effects are observed resulting in spectra completely devoid of matrix ions. We also report the observation of radical molecular ions [M(-●) ] in the negative ion mode, particularly with some aromatic analytes. Copyright

The Role of Prior Fabrication and in Service Thermal Ageing on the Creep Life of AISI Type 316 Stainless Steel Components

A significant factor that influences the creep life of AISI Type 316H austenitic stainless steel components such as headers, and tubes is the initial microstructure. These components typically have a comparable specified composition but different thermo-mechanical fabrication histories. The variations in composition within the nominal range result in initial microstructures which become increasingly divergent during ageing. In this paper we explore effect of these contributions on the long term service aged microstructure and discuss the resulting impact on the overall creep life of these components. The microstructure of specific regions has been characterised with a range of techniques, including high resolution transmission electron microscopy imaging and chemical analyses undertaken using a JEOL ARM instrument operating at 200 KeV fitted with an energy dispersive spectrometer. This provides a unique identification of the service aged precipitates and the distribution of alloying and impurity elements. The results are discussed with respect to the initiation of creep cavities and the associated creep damage accumulation in the context of lifetime assessment of these AISI Type 316H austenitic stainless steel boiler components.

The Role of Post Service Heat Treatment on the Contributions of Creep Deformation and Fracture to Service Life of AISI Type 316H Steel Components

Creep cavitation is a life limiting factor in stainless steel high temperature plant. However, regenerative heat treatments offer the potential of sintering creep cavities and thus extending a component’s time to failure. This is countered by thermal aging effects which can lead to precipitate formation and an increased creep rate. This study investigates these behaviours in a AISI Type 316H austenitic stainless steel.

Methodologies for the airbrush application of MALDI matrices

There is still a need to develop reliable and robust matrix deposition methods for matrix-assisted laser desorption/ionisation mass spectrometry that are applicable to a range of matrices, solvents and analyte types. This paper presents a robust methodology for the airbrush application of matrices along with the implications of varying the set-up and airbrush parameters. A small number of organic analytes and metal salts are analysed in both positive and negative ion modes to exemplify this methodology. In the analyses with the airbrush deposited matrices, performance was enhanced when compared to standard pipette deposition with the need for a search for sweat spots greatly diminished due to the increase homogeneity of the matrix surface and resultant analyte spots. As expected, the graphite matrices were shown to specifically outperform the organic matrices in negative ion mode.

The Significance of Thermo-Mechanical Fabrication on Long Term Creep Life of Type 316H Austenitic Stainless Steel Components

The UK’s Advanced Gas Cooled Reactor (AGR) nuclear power generating plant operates at temperatures up to 550 °C, where creep life is important. We consider Type 316H austenitic stainless steel headers and tubes with thermo-mechanical fabrication histories that result in significantly different initial microstructures. The heat affected zone of weldments, in these thick section headers and thin walled boiler tubes, have been found to be susceptible to creep damage leading to cracking during service. In this work we explore these differences in the long term service aged microstructure and the link to overall creep life of these components. To achieve this, samples containing weldments have been removed from plant after extended periods of service. Specifically parent and HAZ regions have been examined to determine the types of precipitates arising from the long term ageing. In particular, thin foils have been examined in a JEOL ARM transmission electron microscope operating at 200KeV fitted with an Oxford Instruments energy dispersive spectrometer to allow comparison between high resolution images and chemical composition. The thin foils were removed from predetermined locations using gallium ion milling and finally thinned using a low ion current to minimise ion damage. Differences between the distributions and types of precipitates are considered in the context of the initial microstructure arising from the thermo-mechanical history on the loss of creep strength and initiation of creep cavities at grain boundaries. The impact on overall service life is addressed.