Secondary Ion Mass Spectrometry Research Papers (original) (raw)

This paper gives an overview of recent progress in microstructure-specific hydrogen mapping techniques. The challenging nature of mapping hydrogen with high spatial resolution, i.e. at the scale of finest microstructural features, led to... more

This paper gives an overview of recent progress in microstructure-specific hydrogen mapping techniques. The challenging nature of mapping hydrogen with high spatial resolution, i.e. at the scale of finest microstructural features, led to the development of various methodologies: thermal desorption spectrometry, silver decoration, the hydrogen microprint technique, secondary ion mass spectroscopy, atom probe tomography, neutron radiography, and the scanning Kelvin probe. These techniques have different characteristics regarding spatial and temporal resolution associated with microstructure-sensitive hydrogen detection. Employing these techniques in a site-specific manner together with other microstructure probing methods enables multi-scale, quantitative, three-dimensional, high spatial, and kinetic resolution hydrogen mapping, depending on the specific multi-probe approaches used. Here, we present a brief overview of the specific characteristics of each method and the progress resulting from their combined application to the field of hydrogen embrittlement.

Trace element and Hf-Nd-Sr isotope compositions of eight rutile-bearing eclogite xenoliths from the Udachnaya kimberlite pipe in central Siberian craton were determined to further characterize their origins and the nature of their... more

Trace element and Hf-Nd-Sr isotope compositions of eight rutile-bearing eclogite xenoliths from the Udachnaya kimberlite pipe in central Siberian craton were determined to further characterize their origins and the nature of their protoliths, in particular based on data for the HFSE (Ti, Zr, Hf, Nb, Ta) and the Lu-Hf isotope system. Major element compositions of minerals and their proportions in

We present an automated method for U–Pb age dating of zircon by single collector laser ablation-magnetic sectorfield-inductively coupled plasma-mass spectrometry (LA-SF-ICP-MS). The high sensitivity of SF-ICP-MS allows routine analysis... more

We present an automated method for U–Pb age dating of zircon by single collector laser ablation-magnetic sectorfield-inductively coupled plasma-mass spectrometry (LA-SF-ICP-MS). The high sensitivity of SF-ICP-MS allows routine analysis with spot diameter of 20 to 30 μm and ablation time of 30 s, resulting in an ablation crater depth of ∼15–20 μm (∼35 to ∼65 ng of zircon). Zircon consumption is therefore limited to

Semiconductor nanoclusters embedded in thin coatings of transparent and homogeneous silica glasses are suitable materials for the development of optical devices. The optical properties of such systems are strongly dependent on the... more

Semiconductor nanoclusters embedded in thin coatings of transparent and homogeneous silica glasses are suitable materials for the development of optical devices. The optical properties of such systems are strongly dependent on the elemental composition and the morphology of the coatings as well as on the nanocluster size distribution, their mutual interactions and the interactions with the host matrix. To achieve a good control over film composition and morphology the sol–gel route was used. The sol–gel synthesis of ZnO nanocrystals embedded in silica has been faced by the study of the gel-derived binary system ZnO–SiO2. The dip-coating procedure from alcoholic solutions containing tetraethoxysilane [Si(OC2H5)4, TEOS] and zinc acetate [Zn(CH3COO)2] was adopted. Zinc oxide nanograins have been generated in silica by hydrolysis of TEOS and the zinc salt and subsequent thermal annealing of the coatings. The system evolution under thermal treatment was studied by X-ray photoelectron spectroscopy, X-ray diffraction, transmission electron microscopy, UV-Vis absorption spectroscopy and secondary-ion mass spectrometry.

This study thoroughly explores the use of time-of-flight secondary ion mass spectrometry (ToF-SIMS) for determining the deposition sequence of fingermarks and ink on a porous paper surface. Our experimental work has demonstrated that... more

This study thoroughly explores the use of time-of-flight secondary ion mass spectrometry (ToF-SIMS) for determining the deposition sequence of fingermarks and ink on a porous paper surface. Our experimental work has demonstrated that mapping selected endogenous components present in natural fingermarks enables the observation of friction ridges on a laser-printed surface, only when a fingerprint is deposited over this layer of ink. Further investigations have shown limited success on ink-jet printing and ballpoint pen inks. 51 blind tests carried out on natural, latent fingermarks on laser-printed surfaces; up to 14th depletion with samples aged for up to 421 days have resulted in a 100% success rate. Development with ninhydrin was found to affect the fingermark residue through mobilisation of ions, therefore sequencing determination was compromised; whilst iodine fuming and 1,2-indanedione developers did not. This implied that selected development methods affected success in fingermark-ink deposition order determination. These results were further corroborated through inter-laboratory validation studies. The adopted protocol and extensive series of tests have therefore demonstrated the effectiveness and limitations of ToF-SIMS in providing chronological sequencing information of fingermarks on questioned documents; successfully resolving this order of deposition query. N Attard Montalto, JJ Ojeda, A Reynolds, L Doodkorte, M de Puit, M Ismail, M Bailey, and BJ Jones Analyst, 2014,139, 4641-4653

The southern Baffin Island chert provenance project was initiated in 2007 to investigate the effects on Palaeo-Eskimo mobility and technological organization of the differential distribution of chert sources in this area of the eastern... more

The southern Baffin Island chert provenance project was initiated in 2007 to investigate the effects on Palaeo-Eskimo mobility and technological organization of the differential distribution of chert sources in this area of the eastern Arctic. Initial characterization of chert artifacts and sources by secondary ion mass spectrometry and inductively coupled plasma-mass spectrometry (ICP-MS) indicated exploitation of both local inland and exotic chert sources by Palaeo-Eskimo toolmakers. Subsequent reanalysis of chert artifacts by ICP-MS demonstrates that data acquired using these techniques cannot be directly compared. ICP-MS trace element data collected from two primary chert sources documented in 2013 showed promise for characterizing these sources. Subsequent reanalysis of source samples demonstrates that initial results were affected by contamination during sample preparation at an external laboratory and should not be used in future studies.

Gas chromatography mass spectrometry (GC-MS) was employed to determine the chemical composition of essential oil obtained from Eucalyptus globulus and Trachyspermum ammi. The essential oil obtained from leaves of Eucalyptus globulus and... more

Gas chromatography mass spectrometry (GC-MS) was employed to determine the chemical composition of essential oil obtained from Eucalyptus globulus and Trachyspermum ammi. The essential oil obtained from leaves of Eucalyptus globulus and from seeds of Trachyspermum ammi by Clevenger apparatus. Chemical composition of the essential oils of E. globulus and T. ammi was analyzed by Gas chromatography – Mass spectrometry. Four main compounds in E. globulus were identified as Eucalyptol, Methyl –salicylate, Thymol, Para- cymene. 1, 8-cineole was found to be the main compound of E. globulus essential oil. Thymol, gamma- terpinene, para- cymene, beta- pinene were the main compounds of T. ammi oil and traces amount of beta myrcene, alpha- thujne, alpha- pinene, alpha- terpinene, carvacrol compounds of T. ammi were identified by GC-MS. Thymol was the main compound of T. ammi oil. The antifungal activity of E. globulus and T. ammi oils were screened against Trichophyton mentagrophytes and Epidermatophyton floccosum by using disc diffusion and modified micro dilution method. T. ammi oil shows highest inhibition zone in comparison to E. globulus oils and references antibiotics i.e. Clotrimazole and Ketoconazole.

Abstract—Surface properties have an enormous effect on the success or failure of a biomaterial device, thus signifying the considerable importance of and the need for adequate characterization of the biomaterial surface. Microscopy... more

Abstract—Surface properties have an enormous effect on the success or failure of a biomaterial device, thus signifying the considerable importance of and the need for adequate characterization of the biomaterial surface. Microscopy techniques used in the analysis of biomaterial surfaces include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, and confocal microscopy. Spectroscopic techniques include X-ray photoelectron spectroscopy, Fourier

We investigated the hydrogen distribution and desorption behavior in an electrochemically hydrogen-charged binary NieNb model alloy to study the role of d phase in hydrogen embrittlement of alloy 718. We focus on two aspects, namely, (1)... more

We investigated the hydrogen distribution and desorption behavior in an electrochemically hydrogen-charged binary NieNb model alloy to study the role of d phase in hydrogen embrittlement of alloy 718. We focus on two aspects, namely, (1) mapping the hydrogen distribution with spatial resolution enabling the observation of the relations between desorption profiles and desorption sites; and (2) correlating these observations with mechanical testing results to reveal the degradation mechanisms. The trapping states of hydrogen in the alloy were globally analyzed by Thermal Desorption Spectroscopy (TDS). Additionally, spatially resolved hydrogen mapping was conducted using silver decoration, Scanning Kelvin Probe Force Microscopy (SKPFM) and Secondary Ion Mass Spectrometry (SIMS): The Ag decoration method revealed rapid effusion of hydrogen at room temperature from the g-matrix. The corresponding kinetics was resolved in both, space and time by the SKPFM measurements. At room temperature the hydrogen release from the g-matrix steadily decreased until about 100 h and then was taken over by the d phase from which the hydrogen was released much slower. For avoiding misinterpretation of hydrogen signals stemming from environmental effects we also charged specimens with deuterium. The deuterium distribution in the microstructure was studied by SIMS. The combined results reveal that hydrogen dissolves more preferably inside the g-matrix and is diffusible at room temperature while the d phase acts as a deeper trapping site for hydrogen. With this joint and spatially resolving approach we observed the microstructure-and time-dependent distribution and release rate of hydrogen with high spatial and temporal resolution. Correlating the obtained results with mechanical testing of the hydrogen-charged samples shows that hydrogen enhanced decohesion (HEDE) occurring at the d/matrix interfaces promotes the embrittlement.

Secondary Ion Mass Spectrometry (SIMS) analyses were carried out on type 304 austenitic stainless steel. On annealed specimen exposed to hydrogen (10 MPa, 358 K), Element Depth Profiles SIMS mode was able to describe quantitatively the... more

Secondary Ion Mass Spectrometry (SIMS) analyses were carried out on type 304 austenitic stainless steel. On annealed specimen exposed to hydrogen (10 MPa, 358 K), Element Depth Profiles SIMS mode was able to describe quantitatively the hydrogen profile content computed by the Fick's law. Based on SIMS analyses on the wake of a fatigue crack (propagation in hydrogen gas at 0.6 MPa and RT), it was possible to compute an apparent diffusivity and solubility in the crack tip region. The apparent solubility and diffusivity in the deformed regions were two times and five orders of magnitude higher than the ones on annealed material, respectively. High hydrogen content was found around the crack tip, where the plastic deformation was well developed (pronounced slip activity). The high apparent diffusivity is presumed to result from enhanced hydrogen transport induced by cyclic plastic activity at the crack tip.

The objective of this study was to investigate if the coating extent created by a mechanofusion process corresponded with observed changes in bulk powder properties. A fine lactose powder (approximate median diameter 20 μm) was dry coated... more

The objective of this study was to investigate if the coating extent created by a mechanofusion process corresponded with observed changes in bulk powder properties. A fine lactose powder (approximate median diameter 20 μm) was dry coated with magnesium stearate using from 0.1 to 5% (w/w) content. An ultra-thin coating layer of magnesium stearate was anticipated, but previous attempts to determine such thin layers on these fine particles have had limited success, with poor resolution. In this study, the surface coating was examined using the state-of-the-art XPS and ToF-SIMS systems. The powder flow was characterized by Carr index and shear cell testing. XPS was successfully applied to demonstrate variations in surface coverage, as a function of additive levels, and indicated near complete coating coverage at additive levels of 1% (w/w) and above. ToF-SIMS results supported such coating coverage assessment, and indicated coating uniformly across the fine particle surfaces. The flow ...

The loss of ductility in the high strength polycrystalline superalloy 720Li is studied in air between room temperature and 1000 C. Tensile ductility is influenced profoundly by the environment, leading to a pronounced minimum at 750 C. A... more

The loss of ductility in the high strength polycrystalline superalloy 720Li is studied in air between room temperature and 1000 C. Tensile ductility is influenced profoundly by the environment, leading to a pronounced minimum at 750 C. A relationship between tensile ductility and oxidation kinetics is identified. The physical factors responsible for the ductility dip are established using energy-dispersive X-ray spectroscopy, nanoscale secondary ion mass spectrometry and the analysis of electron back-scatter diffraction patterns. Embrittlement results from internal intergranular oxidation along the g-grain boundaries, and in particular, at incoherent interfaces of the primary g 0 precipitates with the matrix phase. These fail under local microstresses arising from the accumulation of dislocations during slip-assisted grain boundary sliding. Above 850 C, ductility is restored because the accumulation of dislo-cations at grain boundaries is no longer prevalent.

Talc mineralisation occurs as hematite–talc schist between soft hematite ore and dolomitic itabirite at Gongo Soco, Quadrilátero Ferrífero of Minas Gerais, Brazil. The hematite–talc schist and soft hematite have a prominent tectonic... more

Talc mineralisation occurs as hematite–talc schist between soft hematite ore and dolomitic itabirite at Gongo Soco, Quadrilátero Ferrífero of Minas Gerais, Brazil. The hematite–talc schist and soft hematite have a prominent tectonic foliation of tabular hematite. Tabular hematite without preferential orientation is superimposed on the tectonic foliation. The talcose schist is enriched in F and has a constant Fe/S ratio. Electron-microprobe analyses indicate trace amounts of S in different generations of hematite. The whole-rock Fe/S ratio possibly represents sulfate S from hematite-hosted fluid inclusions. Fluid inclusions in foliation-overprinting hematite and chlorite geothermometry from talcose rocks suggest, respectively, temperatures from <200°C to ~300°C. Tourmaline, a rarely observed mineral in the hematite–talc schist, belongs to the alkali group and falls in the dravite compositional field. Boron-isotope determinations of tourmaline crystals, using secondary ion mass spectrometry, vary from −20‰ to −12‰ δ11B. This compositional isotopic range and the tourmaline chemical composition suggest a meta-evaporitic origin. A non-marine evaporitic setting is the most likely source of acidic, highly oxidising fluids, which resulted in the abundant F-bearing talc and the presence of otherwise immobile Ti in hematite. Oxidising brines were channelled along shear zones and converted dolomitic itabirite into the Gongo Soco soft hematite and the talc mineralisation. The latter is envisaged as the hydrothermal wall-rock alteration of dolomitic itabirite, which gave rise to the soft hematite ore.