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National audience; A novel approach for controlling and flattening the radial distribution of the erbium ions within an aluminium enriched silica core glass as part of the modified chemical vapour deposition and solution doping techniques is presented.

By combining the capabilities of advanced sample preparation methodologies with the latest generation of secondary ion mass spectrometry instrumentation, we show that chemical information on the distribution of even dilute species in biological samples can be obtained with spatial resolutions of better than 100 nm. Here, we show the distribution of nickel and other elements in leaf tissue of the nickel hyperaccumulator plant Alyssum lesbiacum prepared by high-pressure freezing and freeze substitution.

Plant roots and microorganisms interact and compete for nutrients within the rhizosphere, which is considered one of the most biologically complex systems on Earth. Unraveling the nitrogen (N) cycle is key to understanding and managing nutrient flows in terrestrial ecosystems, yet to date it has proved impossible to analyze and image N transfer in situ within such a complex system at a scale relevant to soil-microbe-plant interactions. Linking the physical heterogeneity of soil to biological processes marks a current frontier in plant and soil sciences. Here we present a new and widely applicable approach that allows imaging of the spatial and temporal dynamics of the stable isotope 15 N assimilated within the rhizosphere. This approach allows visualization and measurement of nutrient resource capture between competing plant cells and microorganisms. For confirmation we show the correlative use of nanoscale secondary ion mass spectrometry, and transmission electron microscopy, to image differential partitioning of 15 NH 4 + between plant roots and native soil microbial communities at the submicron scale. It is shown that 15 N compounds can be detected and imaged in situ in individual microorganisms in the soil matrix and intracellularly within the root. Nanoscale secondary ion mass spectrometry has potential to allow the study of assimilatory processes at the submicron level in a wide range of applications involving plants, microorganisms, and animals.

High-resolution analysis using a Cameca NanoSIMS 50 has been used to map the oxide chemistry in intergranular cracks in stainless steels. The technique has proven ideal for this type of sample, as it is able to discern between the different oxide layers and clarify the role of minor segregants such as boron and sulphur. Results are compared with analysis of the same sample by scanning auger microscopy and its interpretation discussed. The short time required to prepare and examine multiple regions present the NanoSIMS as an optimum tool for corrosion characterization. © 2007 Elsevier B.V. All rights reserved.

Ambient inclusion trails (AIT) are enigmatic microtubular structures created by the migration of mineral crystals through a lithified substrate. The decomposition of organic material has been suggested as the driving force for the crystal migration, but has yet to be rigorously tested. AIT may hold potential as a biosignature for investigating early life on Earth if the associated organic material can be shown to be biological. This paper attempts to test the formation mechanism and biogenicity of AIT from the c . 3400 Ma Strelley Pool sandstone of Western Australia using NanoSIMS technology. In doing so, we demonstrate the unique ability of the NanoSIMS to combine sub-micron scale imaging with in situ chemical and isotopic data, thereby enhancing our ability to evaluate the biogenicity criteria for Archaean microstructures. Enrichments of a suite of major elements (C, N, P, S) and trace elements (Co, Fe, Ni, Zn), often associated with biological processes, are found within several AIT in this sandstone. C and N enrichments are most common along AIT margins, and correlate with depletions of Si, O, Ca and Mg, indicating that this material is indeed organic in nature. δ 13 C values of this carbonaceous material average −26‰. Petrographic observations show that some of the AIT occur in the centre of detrital sandstone grains where they were sealed from later fluid flow and therefore preserve primary Archaean (bio)geochemistry. In contrast, AIT found around the outer edges of sandstone grains may contain more recent organic material introduced by later fluid migration and are an unreliable biosignature. Using the petrographic and geochemical data a multi-stage model for AIT formation and subsequent diagenetic modification is proposed. The possible sources of the primary organic material are discussed and we conclude that the data are consistent with a biological origin for these AIT. An abiogenic origin is more difficult to sustain but cannot yet be completely excluded for AIT in general.

Soils are structurally heterogeneous across a wide range of spatio-temporal scales. Consequently, external environmental conditions do not have a uniform effect throughout the soil, resulting in a large diversity of micro-habitats. It has been suggested that soil function can be studied without explicit consideration of such fine detail, but recent research has indicated that the micro-scale distribution of organisms may be of importance for a mechanistic understanding of many soil functions. Current techniques still lack the adequate sensitivity and resolution for data collection at the micro-scale, and the question ‘How important are various soil processes acting at different scales for ecological function?’ is therefore challenging to answer. The nano-scale secondary ion mass spectrometer (NanoSIMS) represents the latest generation of ion microprobes, which link high-resolution microscopy with isotopic analysis. The main advantage of NanoSIMS over other secondary ion mass spectrometers is its ability to operate at high mass resolution, whilst maintaining both excellent signal transmission and spatial resolution (down to 50 nm). NanoSIMS has been used previously in studies focussing on presolar materials from meteorites, in material science, biology, geology and mineralogy. Recently, the potential of NanoSIMS as a new tool in the study of biophysical interfaces in soils has been demonstrated. This paper describes the principles of NanoSIMS and discusses the potential of this tool to contribute to the field of biogeochemistry and soil ecology. Practical considerations (sample size and preparation, simultaneous collection of isotopes, mass resolution, isobaric interference and quantification of the isotopes of interest) are discussed. Adequate sample preparation, avoiding bias due to artefacts, and identification of regions-of-interest will be critical concerns if NanoSIMS is used as a new tool in biogeochemistry and soil ecology. Finally, we review the areas of research most likely to benefit from the high spatial and high mass resolution attainable with this new approach.

In order to understand the influence of boron on the grain size and microstructure of a series of low carbon steel rods the imaging of elemental distributions of B, N and C has been undertaken using Cameca NanoSIMS 50. This instrument provides the high sensitivity, spatial and mass resolution required for the identification of small precipitates and segregation of light elements that are traditionally difficult to study by other micro-analytical techniques. However, the use of NanoSIMS to investigate metallurgical problems is complicated by matrix effects. This leads to changes in ionization yield and variable sputter rates due to the matrix composition. In order to help overcome this problem, the results from the sequential characterisation of exactly the same area of a sample using first transmission electron microscopy (TEM) and then NanoSIMS will be described. This permits the direct comparison of sensitivity and spatial resolution on precisely the same individual particles, which can help us determine the most efficient characterisation strategy. (c) 2006 Elsevier B.V. All rights reserved.

Physical wear of orthopedic implants is inevitable. CoCr alloy samples, typically used in joint reconstruction, corrode rapidly after removal of the protective oxide layer. The behavior of CoCr pellets immersed in human serum, foetal bovine serum (FBS), synovial fluid, albumin in phosphate-buffered saline (PBS), EDTA in PBS, and water were studied using X-ray Photoelectron Spectroscopy (XPS) and Time-of-Flight Secondary Ion Mass Spectroscopy (ToF-SIMS). The difference in the corrosive nature of human serum, water, albumin in PBS and synovial fluid after 5 days of immersion was highlighted by the oxide layer, which was respectively 15, 3.5, 1.5, and 1.5 nm thick. The thickness of an additional calcium phosphate deposit from human serum and synovial fluid was 40 and 2 nm, respectively. Co and Cr ions migrated from the bulk metal surface and were trapped in this deposit by the phosphate anion. This may account for the composition of wear debris from CoCr orthopedic implants, which is known to consist predominantly of hydroxy-phosphate compounds. Known components of synovial fluid including proteoglycans, pyrophosphates, phospholipids, lubricin, and superficial zone protein (SZP), have been identified as possible causes for the lack of significant calcium phosphate deposition in this environment. Circulation of these compounds around the whole implant may inhibit calcium phosphate deposition.

Calcium doping is well known to increase the grain boundary critical current, Jcgb, in polycrystalline Y1Ba 2Cu3O7-δ, (YBCO). High resolution Secondary Ion Mass Spectroscopy (nanoSIMS) analysis has been used to map the distribution of Ca+ ions in three dimensions in an YBCO grain boundary grown on a 24° SrTiO3 bicrystal. High resolution SIMS imaging has produced Ca, Sr, and Ti elemental maps at 20 nm intervals from the YBCO surface. From the variation of Ca concentration with depth a Ca grain boundary diffusion coefficient can be estimated. Moreover, localised hot spots of Ca at the YBCO grain boundary have been observed, perhaps at regions with a high dislocation density. There is also some diffusion of Sr and Ti ions from the substrate along the boundary. This is an important observation because it has been proposed that these ions are electrically active. © 2006 IOP Publishing Ltd.

During hair coloring a number of disulfide bonds in cystine are oxidized (1) to create cysteic acid, forming binding sites for metal ions such as Ca(2+ )and Cu(2+ )from tap water (2). The increased uptake of these metals can have a detrimental impact on fiber properties-for example, reducing shine and causing a poor wet and dry feel (3). In addition, the increased uptake of copper can also contribute to further fiber damage during subsequent coloring due to its ability to take part in metal-induced radical chemistry (4). It is important to know where in the fibers these metals are located in order to either effectively remove these metals or control their chemistry. Nanoscale secondary ion mass spectrometry (NanoSIMS) has been used to locate the calcium and copper within hair that has been treated with a colorant and washed multiple times in tap water containing these ions. Untreated hair is used as a baseline standard material. Images with up to 50-nm spatial resolution of the preferential locations of calcium uptake were obtained, showing a high concentration of calcium in the cuticle region of colored hair, specifically in the sulfur-rich regions (A-layer and exocuticle).

Simultaneous multi-element imaging using NanoSIMS (nano-scale secondary ion mass spectrometry), exploiting the novel combination of (195)Pt and (15)N in platinum-am(m)ine antitumour drugs, provides information on the internalisation and subcellular localisation of both metal and ligands, and allows identification of ligand exchange.