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Time-of-flight Secondary Ion Mass Spectrometry (time-of-flight + secondary_ion_mass_spectrometry)

Distribution by Scientific Domains

Chemistry	40%
Polymers and Materials Science	27%
Medical Sciences	9%

Selected Abstracts

THE APPLICATION OF TIME-OF-FLIGHT SECONDARY ION MASS SPECTROMETRY (ToF-SIMS) TO THE CHARACTERIZATION OF OPAQUE ANCIENT GLASSES*

ARCHAEOMETRY, Issue 6 2009
F. J. M. RUTTEN
Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has been used, for the first time, for the characterization of opaque ancient glasses. Isotope-specific chemical imaging with sub-micron resolution enabled the separate analysis of opacifiying inclusions and the surrounding glass matrix. Phase identification has been demonstrated and quantification of the matrix composition has been investigated by use of Corning Glass Standard B as a model. Trace element detection limits are typically in the range 0.5,5.0 ppm atomic,in favourable cases down to 0.01 ppm. For the analysis of inclusions in particular, this has the potential to provide new information of use in establishing provenance and trade routes by ,fingerprinting' as well as the investigation of manufacturing techniques, as demonstrated by comparisons between glasses and with EDX data from the same samples. [source]

Effects of chemical composition and thermal stability of finishes on the compatibility between glass fiber and high melting temperature thermoplastics

POLYMER COMPOSITES, Issue 2 2000
P. Gao
Experimental studies were made on the surface characteristics of glass fibers with two different finishes. The effects of the chemical composition and thermal stability of the finishes on the compatibility between glass fibers and high melting temperature thermoplastics were investigated. Thermogravimetric Analysis (TGA) was used to characterize the composition of surface finishes and their thermal stability. The chemical composition of surface finishes was investigated using a combination of X-ray photoelectron spectroscopy (XPS) and Time-of-Flight secondary ion mass spectrometry (ToF SIMS). Static contact angle measurements were performed at room temperature to characterize the interfacial tension between the glass fibers and thermoplastics. The study provides a fundamental understanding on some important compatibility issues between thermoplastic resins and glass fiber related to composite fabrication and application. [source]

Bottom-Up Engineering of Subnanometer Copper Diffusion Barriers Using NH2 -Derived Self-Assembled Monolayers

ADVANCED FUNCTIONAL MATERIALS, Issue 7 2010
Arantxa Maestre Caro
Abstract A 3-aminopropyltrimethoxysilane-derived self-assembled monolayer (NH2SAM) is investigated as a barrier against copper diffusion for application in back-end-of-line (BEOL) technology. The essential characteristics studied include thermal stability to BEOL processing, inhibition of copper diffusion, and adhesion to both the underlying SiO2 dielectric substrate and the Cu over-layer. Time-of-flight secondary ion mass spectrometry and X-ray spectroscopy (XPS) analysis reveal that the copper over-layer closes at 1,2-nm thickness, comparable with the 1.3-nm closure of state-of-the-art Ta/TaN Cu diffusion barriers. That the NH2SAM remains intact upon Cu deposition and subsequent annealing is unambiguously revealed by energy-filtered transmission electron microscopy supported by XPS. The SAM forms a well-defined carbon-rich interface with the Cu over-layer and electron energy loss spectroscopy shows no evidence of Cu penetration into the SAM. Interestingly, the adhesion of the Cu/NH2SAM/SiO2 system increases with annealing temperature up to 7.2,J m,2 at 400,°C, comparable to Ta/TaN (7.5,J m,2 at room temperature). The corresponding fracture analysis shows that when failure does occur it is located at the Cu/SAM interface. Overall, these results demonstrate that NH2SAM is a suitable candidate for subnanometer-scale diffusion barrier application in a selective coating for copper advanced interconnects. [source]

Affinity-Based Protein Surface Pattern Formation by Ligand Self-Selection from Mixed Protein Solutions

ADVANCED FUNCTIONAL MATERIALS, Issue 19 2009
Manish Dubey
Abstract Photolithographically prepared surface patterns of two affinity ligands (biotin and chloroalkane) specific for two proteins (streptavidin and HaloTag, respectively) are used to spontaneously form high-fidelity surface patterns of the two proteins from their mixed solution. High affinity protein-surface self-selection onto patterned ligands on surfaces exhibiting low non-specific adsorption rapidly yields the patterned protein surfaces. Fluorescence images after protein immobilization show high specificity of the target proteins to their respective surface patterned ligands. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) imaging further supports the chemical specificity of streptavidin and HaloTag for their surface patterned ligands from mixed protein solutions. However, ToF-SIMS did detect some non-specific adsorption of bovine serum albumin, a masking protein present in excess in the adsorbing solutions, on the patterned surfaces. Protein amino acid composition, surface coverage, density, and orientation are important parameters that determine the relative ToF-SIMS fragmentation pattern yields. ToF-SIMS amino acid-derived ion fragment yields summed to produce surface images can reliably determine which patterned surface regions contain bound proteins, but do not readily discriminate between different co-planar protein regions. Principal component analysis (PCA) of these ToF-SIMS data, however, improves discrimination of ions specific to each protein, facilitating surface protein pattern identification and image contrast. [source]

Time-of-flight secondary ion mass spectrometry analysis of the application of a cationic conditioner to ,clean' hair

INTERNATIONAL JOURNAL OF COSMETIC SCIENCE, Issue 5 2004
A. Harvey
In this study the applicability of the surface-sensitive Time-of-flight secondary ion mass spectrometry (ToF-SIMS) technique to hair analysis and associated aqueous processing is evaluated. ToF-SIMS analysis of ,as received' human hair indicates the presence of silicones, anionic surfactants, and cationic conditioners, from previous treatments, on the fiber surface. Cleaning of the hair with SLS or SLES results in adsorption of the surfactants onto the fiber surface. In particular, the more non-polar surfactant components have greater substantivity for the fiber surface, as indicated by the relative increase in their ToF-SIMS intensity. Application of the Incroquat Behenyl 18-MEA conditioner to both ,virgin' and bleached hair results in the adsorption of the cationic C18, C20, C22, and C21 surfactant components onto the hair surface. The ToF-SIMS data indicate higher levels of conditioner on the bleached hair relative to the undamaged hair. [source]

Investigation of the postcure reaction and surface energy of epoxy resins using time-of-flight secondary ion mass spectrometry and contact-angle measurements

JOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2009
Firas Awaja
Abstract Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was used to investigate correlations between the molecular changes and postcuring reaction on the surface of a diglycidyl ether of bisphenol A and diglycidyl ether of bisphenol F based epoxy resin cured with two different amine-based hardeners. The aim of this work was to present a proof of concept that ToF-SIMS has the ability to provide information regarding the reaction steps, path, and mechanism for organic reactions in general and for epoxy resin curing and postcuring reactions in particular. Contact-angle measurements were taken for the cured and postcured epoxy resins to correlate changes in the surface energy with the molecular structure of the surface. Principal components analysis (PCA) of the ToF-SIMS positive spectra explained the variance in the molecular information, which was related to the resin curing and postcuring reactions with different hardeners and to the surface energy values. The first principal component captured information related to the chemical phenomena of the curing reaction path, branching, and network density based on changes in the relative ion density of the aliphatic hydrocarbon and the C7H7O+ positive ions. The second principal component captured information related to the difference in the surface energy, which was correlated to the difference in the relative intensity of the CxHyNz+ ions of the samples. PCA of the negative spectra provided insight into the extent of consumption of the hardener molecules in the curing and postcuring reactions of both systems based on the relative ion intensity of the nitrogen-containing negative ions and showed molecular correlations with the sample surface energy. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009 [source]

In situ thermo-TOF-SIMS study of thermal decomposition of zinc acetate dihydrate

JOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 10 2004
Anil Vithal Ghule
Abstract Time-of-flight secondary ion mass spectrometry (TOF-SIMS) was used for an in situ thermal decomposition study of Zn(CH3COO)2·2H2O forming ZnO nanoparticles. TOF-SIMS spectra were recorded at regular temperature intervals of 25 °C in positive and negative detection modes in a dynamic thermal process. Controlled heating (5 °C min,1) of Zn(CH3COO)2·2H2O was also carried out using thermogravimetric analysis (TGA) in an oxygen atmosphere (20 ml min,1). Nearly spherical ZnO nanoparticles with no agglomeration and a narrow size distribution (diameter ,50 nm) were observed, which were characterized using scanning electron microscopy, transmission electron microscopy and x-ray diffraction. In situ thermo-TOF-SIMS was used to monitor the 64Zn+ and 66Zn+ ion abundances as a function of temperature, which showed a similar profile to that observed for weight loss in TGA during decomposition. Based on the experimental results, a possible decomposition mechanism for the formation of ZnO is proposed. Copyright © 2004 John Wiley & Sons, Ltd. [source]

Luminescent properties of PP and LDPE films and rods doped with the Eu(III)-La(III) complex

POLYMERS FOR ADVANCED TECHNOLOGIES, Issue 1 2006
Roman Pogreb
Abstract The work is devoted to luminescent properties of trivalent lanthanide complexes dispersed in thermoplastic host matrices. Polyethylene films and polypropylene-rods, both doped with these complexes, were manufactured using an extrusion technique. Two kinds of dopants were used: Eu(III)-thenoyltrifluoroacetone-1,10-phenanthroline complex (1) and Eu(III)-La(III)-1,10-phenanthroline complex (2). Absorption, excitation, emission spectra and lifetime of luminescence were studied. The impact of the polymer matrix on the emission spectra was investigated. Emission spectra of the films were studied at room and helium temperatures. Time-of-flight secondary ion mass spectrometry (TOF-SIMS) surface mapping showed that in the Eu(III)-La(III) complex europium forms islands (clusters) with a dimension of 1,µm, whereas lanthanum was dispersed more uniformly in the polymer matrix. Dependence of emission intensity on the excitation was determined. Copyright © 2006 John Wiley & Sons, Ltd. [source]

Identification of human calculi with time-of-flight secondary ion mass spectrometry

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 2 2010
C. Amjad A. Ghumman
Time-of-flight secondary ion mass spectrometry was used to study four human calculi and to compare the results with those from twelve commercially available urinary calculi minerals including three organic compounds (L-cystine, uric acid and sodium urate). Phase identification of calcium phosphate compounds was carried out by considering the relative ion abundances of [Ca2O]+ and [CaPO2]+. Deprotonated [M,H], and protonated [M+H]+ uric acid were detected and used for component recognition in pure uric acid and in the mixed samples of struvite, calcium oxalate and uric acid. Iodine related to the medical history of a patient was also detected. Copyright © 2009 John Wiley & Sons, Ltd. [source]

THE APPLICATION OF TIME-OF-FLIGHT SECONDARY ION MASS SPECTROMETRY (ToF-SIMS) TO THE CHARACTERIZATION OF OPAQUE ANCIENT GLASSES*

Analysis of hopanes and steranes in single oil-bearing fluid inclusions using time-of-flight secondary ion mass spectrometry (ToF-SIMS)

GEOBIOLOGY, Issue 1 2010
S. SILJESTRÖM
Steranes and hopanes are organic biomarkers used as indicators for the first appearance of eukaryotes and cyanobacteria on Earth. Oil-bearing fluid inclusions may provide a contamination-free source of Precambrian biomarkers, as the oil has been secluded from the environment since the formation of the inclusion. However, analysis of biomarkers in single oil-bearing fluid inclusions, which is often necessary due to the presence of different generations of inclusions, has not been possible due to the small size of most inclusions. Here, we have used time-of-flight secondary ion mass spectrometry (ToF-SIMS) to monitor in real time the opening of individual inclusions trapped in hydrothermal veins of fluorite and calcite and containing oil from Ordovician source rocks. Opening of the inclusions was performed by using a focused C60+ ion beam and the in situ content was precisely analysed for C27,C29 steranes and C29,C32 hopanes using Bi3+ as primary ions. The capacity to unambiguously detect these biomarkers in the picoliter amount of crude oil from a single, normal-sized (15,30 ,m in diameter) inclusion makes the approach promising in the search of organic biomarkers for life's early evolution on Earth. [source]

Investigation of the postcure reaction and surface energy of epoxy resins using time-of-flight secondary ion mass spectrometry and contact-angle measurements

Animal urine as painting materials in African rock art revealed by cluster ToF-SIMS mass spectrometry imaging

JOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 8 2010
Vincent Mazel
Abstract The rock art site at the village of Songo in Mali is a very important Dogon ritual place where, since the end of the nineteenth century until today, takes place the ceremony of circumcision. During these ceremonies, paintings are performed on the walls of the shelter with mainly three colors: red, black and white. Ethnological literature mentions the use of animal urine of different species such as birds, lizards or snakes as a white pigment. Urine of these animals is mainly composed of uric acid or urate salts. In this article, time-of-flight secondary ion mass spectrometry (ToF-SIMS) is used to compare uric acid, snake urine and a sample of a white pigment of a Dogon painting coming from the rock art site of Songo. ToF-SIMS measurements in both positive and negative ion modes on reference compounds and snake urine proved useful for the study of uric acid and urate salts. This method enables to identify unambiguously these compounds owing to the detection in negative ion mode of the ion corresponding to the deprotonated molecule ([M , H], at m/z 167.01) and its fragment ions. Moreover, the mass spectra obtained in positive ion mode permit to differentiate uric acid and urate salts on the basis of specific ions. Applying this method to the Dogon white pigments sample, we show that the sample is entirely composed of uric acid. This proves for the first time, that animal urine was used as a pigment by the Dogon. The presence of uric acid instead of urate salts as normally expected in animal urine could be explained by the preparation of the pigment for its application on the stone. Copyright © 2010 John Wiley & Sons, Ltd. [source]

Characterization of dilute species within CVD-grown silicon nanowires doped using trimethylboron: protected lift-out specimen preparation for atom probe tomography

JOURNAL OF MICROSCOPY, Issue 2 2010
T. J. PROSA
Summary Three-dimensional quantitative compositional analysis of nanowires is a challenge for standard techniques such as secondary ion mass spectrometry because of specimen size and geometry considerations; however, it is precisely the size and geometry of nanowires that makes them attractive candidates for analysis via atom probe tomography. The resulting boron composition of various trimethylboron vapour,liquid,solid grown silicon nanowires were measured both with time-of-flight secondary ion mass spectrometry and pulsed-laser atom probe tomography. Both characterization techniques yielded similar results for relative composition. Specialized specimen preparation for pulsed-laser atom probe tomography was utilized and is described in detail whereby individual silicon nanowires are first protected, then lifted out, trimmed, and finally wet etched to remove the protective layer for subsequent three-dimensional analysis. [source]

Identification of human calculi with time-of-flight secondary ion mass spectrometry

Structural analysis of secondary ions by post-source decay in time-of-flight secondary ion mass spectrometry

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 4 2006
David Touboul
Tandem mass spectrometry measurements have been achieved using time-of-flight secondary ion mass spectrometry (TOF-SIMS) and a post source decay (PSD)-like method. The performance of the method has been demonstrated on model molecules with well-known fragmentation pathways. Several lipids have been fragmented including the phosphocholine ion, phosphatidylcholines, cholesterol and vitamin E. Pure samples were analyzed, and the results compared with those obtained with the same compounds on a quadrupole-TOF hybrid mass spectrometer. Then, the structures of some lipids which are currently observed in the TOF-SIMS imaging of mammalian tissue sections were verified. Copyright © 2006 John Wiley & Sons, Ltd. [source]

Effect of water treatment on analyte and matrix ion yields in matrix-assisted time-of-flight secondary ion mass spectrometry: the case of insulin in and on hydroxycinnamic acid

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 21 2002
Wilfried Szymczak
A systematic study was performed to identify the origin of surprisingly high analyte-to-matrix yield ratios recently observed in time-of-flight secondary ion mass spectrometry (TOF-SIMS) analysis of oligo- and polypeptides mixed in matrices of ,-cyano-4-hydroxycinnamic acid (4HCCA). Several sets of samples of porcine insulin in 4HCCA (1:3100 molar) were prepared from liquid solutions by a nebuliser technique, with more than one order of magnitude variation in sprayed material (substrate silicon). Following different periods of storage in air and/or vacuum as well as exposure to high-purity water, TOF-SIMS analysis was performed under oblique impact of 22 keV SF5+. Treatment with water involved either deposition of a droplet covering the whole sample for times between 1 and 20,min or spraying with water in droplet equivalent quantities. The analyte and matrix molecules were detected as protonated molecules (insulin also in doubly protonated form). Even the as-prepared samples usually showed insulin-to-4HCCA yield ratios exceeding the molar ratio of the mixed material. Upon ageing in vacuum the matrix ion yields remained constant but the analyte yields decreased, partly due to break-up of intrachain disulfide bonds. Water treatment resulted in a pronounced decrease in the 4HCCA yield, typically by a factor of five, in parallel with an increase of the insulin yield, by up to a factor of four. Evidence is provided that these changes occur concurrently with a partial dissolution of 4HCCA at the sample surface. The enhanced insulin yield was not correlated with the Na+ yield. The typically 20-fold increase in the insulin-to-4HCCA yield ratio, generated by water exposure of the samples, provides the explanation for the high yield ratios observed previously with water-treated samples. Spraying with water or repeated exposure to water droplets caused a pronounced degradation of the insulin parent yields in combination with an increasing appearance of signals due to the B- and A-chains of insulin. To clarify the issue of surface segregation, a few samples were prepared by spraying acetone-diluted solutions of insulin on previously deposited layers of 4HCCA. Whereas the insulin yields from as-prepared samples were rather low, the yields observed after water treatment were comparable with those observed with samples of insulin in 4HCCA. The results suggest that a large amount of insulin is present at the surface of samples prepared from liquid mixtures of insulin in 4HCCA. With both methods of sample preparation, however, high secondary ion yields of insulin were only obtained after exposure of the samples to water. The chemical changes responsible for this beneficial effect still need to be identified. Copyright © 2002 John Wiley & Sons, Ltd. [source]

CHANGES IN THE METAL CONTENT OF HUMAN HAIR DURING DIAGENESIS FROM 500 YEARS, EXPOSURE TO GLACIAL AND AQUEOUS ENVIRONMENTS

ARCHAEOMETRY, Issue 3 2010
I. M. KEMPSON
Scanning electron microscopy, inductively coupled plasma mass spectroscopy and time-of-flight secondary ion mass spectrometry have been used to examine the extent and possible mechanisms by which the metal content of human hair is altered by exposure to aqueous environments. The results, using both modern hair and samples from 500-year-old hair associated with glacier-entombed remains, show that the metal content has been altered sufficiently so that the interpretation of the metal signature in terms of diet or disease is problematic. While endogenous information is difficult to glean from these data, interesting observations have been made of possible early stages of mineral authigenic deposition. The chemistry of the outer hair surface was found to be consistent with deposition of Fe and Al silicates, as well as other mineral phases. The ancient hair was analysed at the root region and included a comparison of the internal versus external composition to assist in identifying the diagenetic processes. [source]

Magnetically Separable Gold Catalyst for the Aerobic Oxidation of Amines

CHEMCATCHEM, Issue 1 2009
Linda Aschwanden
Abstract A magnetically separable, recyclable gold catalyst consisting of gold nanoparticles supported on intimately mixed superparamagnetic ceria/iron oxide has been prepared by simple addition of the preformed mixed oxide support and the gold precursor, Au(OAc)3, to the reaction mixture of the aerobic oxidation of amines. The catalyst was characterized by means of X-ray diffraction (XRD), N2 adsorption, superconducting quantum-interference device (SQUID) measurements, time-of-flight secondary ion mass spectrometry (TOF-SIMS), scanning transmission electron microscopy (STEM), and scanning electron microscopy with an energy-dispersive X-ray spectrometer (SEM-EDAX). Catalytic tests with various amines showed high selectivity to the corresponding imines (87,100,%), and good separation efficiency and recyclability of the catalyst. [source]