Surface, electrical and mechanical modifications of PMMA after implantation with laser produced iron plasma ions

NASA Astrophysics Data System (ADS)

Ahmed, Qazi Salman; Bashir, Shazia; Jalil, Sohail Abdul; Shabbir, Muhammad Kaif; Mahmood, Khaliq; Akram, Mahreen; Khalid, Ayesha; Yaseen, Nazish; Arshad, Atiqa

2016-07-01

Laser Produced Plasma (LPP) was employed as an ion source for the modifications in surface, electrical and mechanical properties of poly methyl (methacrylate) PMMA. For this purpose Nd:YAG laser (532 nm, 6 ns, 10 Hz) at a fluence of 12.7 J/cm2 was employed to generate Fe plasma. The fluence and energy measurements of laser produced Fe plasma ions were carried out by employing Thomson Parabola Technique in the presence of magnetic field strength of 0.5 T, using CR-39 as Solid State Nuclear Track Detector (SSNTD). It has been observed that ion fluence ejecting from ablated plasma was maximum at an angle of 5° with respect to the normal to the Fe target surface. PMMA substrates were irradiated with Fe ions of constant energy of 0.85 MeV at various ion fluences ranging from 3.8 × 106 ions/cm2 to 1.8 × 108 ions/cm2 controlled by varying laser pulses from 3000 to 7000. Optical microscope and Scanning Electron Microscope (SEM) were utilized for the analysis of surface features of irradiated PMMA. Results depicted the formation of chain scission, crosslinking, dendrites and star like structures. To explore the electrical behavior, four probe method was employed. The electrical conductivity of ion irradiated PMMA was increased with increasing ion fluence. The surface hardness was measured by shore D hardness tester and results showed the monotonous increment in surface hardness with increasing ion fluence. The increasing trend of surface hardness and electrical conductivity with increasing Fe ion fluence has been well correlated with the surface morphology of ion implanted PMMA. The temperature rise of PMMA surface due to Fe ion irradiation is evaluated analytically and comes out to be in the range of 1.72 × 104 to 1.82 × 104 K. The values of total Linear Energy Transfer (LET) or stopping power of 0.8 MeV Fe ions in PMMA is 61.8 eV/Å and their range is 1.34 μm evaluated by SRIM simulation.

Development of electrochemical sensor for the determination of palladium ions (Pd2+) using flexible screen printed un-modified carbon electrode.

PubMed

Velmurugan, Murugan; Thirumalraj, Balamurugan; Chen, Shen-Ming; Al-Hemaid, Fahad M A; Ajmal Ali, M; Elshikh, Mohamed S

2017-01-01

To date, the development of different modified electrodes have received much attention in electrochemistry. The modified electrodes have some drawbacks such as high cost, difficult to handle and not eco friendly. Hence, we report an electrochemical sensor for the determination of palladium ions (Pd 2+ ) using an un-modified screen printed carbon electrode has been developed for the first time, which are characterized and studied via scanning electron microscope and cyclic voltammetry. Prior to determination of Pd 2+ ions, the operational conditions of un-modified SPCE was optimized using cyclic voltammetry and showed excellent electro-analytical behavior towards the determination of Pd 2+ ions. Electrochemical determination of Pd 2+ ions reveal that the un-modified electrode showed lower detection limit of 1.32μM with a linear ranging from 3 to 133.35μM towards the Pd 2+ ions concentration via differential pulse voltammetry. The developed sensor also applied to the successfully determination of trace level Pd 2+ ions in spiked water samples. In addition, the advantage of this type of electrode is simple, disposable and cost effective in electrochemical sensors. Copyright © 2016 Elsevier Inc. All rights reserved.

The effect of ion plated silver and sliding friction on tensile stress-induced cracking in aluminum oxide

NASA Technical Reports Server (NTRS)

Sliney, Harold E.; Spalvins, Talivaldis

1991-01-01

A Hertzian analysis of the effect of sliding friction on contact stresses in alumina is used to predict the critical load for crack generation. The results for uncoated alumina and alumina coated with ion plated silver are compared. Friction coefficient inputs to the analysis are determined experimentally with a scratch test instrument employing an 0.2 mm radius diamond stylus. A series of scratches were made at constant load increments on coated and uncoated flat alumina surfaces. Critical loads for cracking are detected by microscopic examination of cross sections of scratches made at various loads and friction coefficients. Acoustic emission (AE) and friction trends were also evaluated as experimental techniques for determining critical loads for cracking. Analytical predictions correlate well with micrographic evidence and with the lowest load at which AE is detected in multiple scratch tests. Friction/load trends are not good indicators of early crack formation. Lubrication with silver films reduced friction and thereby increased the critical load for crack initiation in agreement with analytical predictions.

The effect of ion-plated silver and sliding friction on tensile stress-induced cracking in aluminum oxide

NASA Technical Reports Server (NTRS)

Sliney, Harold E.; Spalvins, Talivaldis

1993-01-01

A Hertzian analysis of the effect of sliding friction on contact stresses in alumina is used to predict the critical load for crack generation. The results for uncoated alumina and alumina coated with ion plated silver are compared. Friction coefficient inputs to the analysis are determined experimentally with a scratch test instrument employing an 0.2 mm radius diamond stylus. A series of scratches were made at constant load increments on coated and uncoated flat alumina surfaces. Critical loads for cracking are detected by microscopic examination of cross sections of scratches made at various loads and friction coefficients. Acoustic emission (AE) and friction trends were also evaluated as experimental techniques for determining critical loads for cracking. Analytical predictions correlate well with micrographic evidence and with the lowest load at which AE is detected in multiple scratch tests. Friction/load trends are not good indicators of early crack formation. Lubrication with silver films reduced friction and thereby increased the critical load for crack initiation in agreement with analytical predictions.

Laboratory Instruments Available to Support Space Station Researchers at Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Panda, Binayak; Gorti, Sridhar

2013-01-01

A number of research instruments are available at NASA's Marshall Space Flight Center (MSFC) to support ISS researchers and their investigations. These modern analytical tools yield valuable and sometimes new informative resulting from sample characterization. Instruments include modern scanning electron microscopes equipped with field emission guns providing analytical capabilities that include angstron-level image resolution of dry, wet and biological samples. These microscopes are also equipped with silicon drift X-ray detectors (SDD) for fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations in crystalline alloys. Sample chambers admit large samples, provide variable pressures for wet samples, and quantitative analysis software to determine phase relations. Advances in solid-state electronics have also facilitated improvements for surface chemical analysis that are successfully employed to analyze metallic materials and alloys, ceramics, slags, and organic polymers. Another analytical capability at MSFC is a mganetic sector Secondary Ion Mass Spectroscopy (SIMS) that quantitatively determines and maps light elements such as hydrogen, lithium, and boron along with their isotopes, identifies and quantifies very low level impurities even at parts per billion (ppb) levels. Still other methods available at MSFC include X-ray photo-electron spectroscopy (XPS) that can determine oxidation states of elements as well as identify polymers and measure film thicknesses on coated materials, Scanning Auger electron spectroscopy (SAM) which combines surface sensitivity, spatial lateral resolution (approximately 20 nm), and depth profiling capabilities to describe elemental compositions in near surface regions and even the chemical state of analyzed atoms. Conventional Transmission Electron Microscope (TEM) for observing internal microstructures at very high magnifications and the Electron Probe Micro-analyzer (EPMA) for very precise microanalysis are available as needed by the researcher. Space Station researchers are invited to work with MSFC in analyzing their samples using these techniques.

Microscopical and functional aspects of calcium-transport and deposition in terrestrial isopods.

PubMed

Ziegler, Andreas; Fabritius, Helge; Hagedorn, Monica

2005-01-01

Terrestrial isopods (Crustacea) are excellent model organisms to study epithelial calcium-transport and the regulation of biomineralization processes. They molt frequently and resorb cuticular CaCO(3) before the molt to prevent excessive loss of Ca(2+) ions when the old cuticle is shed. The resorbed mineral is stored in CaCO(3) deposits within the ecdysial gap of the first four anterior sternites. After the molt, the deposits are quickly resorbed to mineralise the posterior part of the new cuticle. The deposits contain numerous small spherules composed of an organic matrix and amorphous CaCO(3), which has a high solubility and, therefore, facilitates quick mobilization of Ca(2+) and HCO(3)(-) ions. During the formation and resorption of the deposits large amounts of Ca(2+), HCO(3)(-) and H(+) are transported across the anterior sternal epithelial cells. Within the last years, various light and electron microscopical techniques have been used to characterize the CaCO(3) deposits and the cellular mechanisms involved in biomineralization. The work on the CaCO(3) deposits includes studies on the ultrastructure of the deposits, the sequence of events during deposit formation and dissolution, and the mineral composition of the sternal deposits. The differentiation of the anterior sternal epithelial cells and the mechanisms of epithelial ion transport required for the mineralization and demineralisation of the deposits was studied using various analytical light and electron microscopical techniques including polarized light microscopy, immunocytochemistry, electron microprobe analysis, electron energy loss spectroscopy and electron spectroscopic imaging. Comparative analysis of deposit morphology and the differentiation of the sternal epithelia provide information on the evolution of CaCO(3) deposit formation in relation to the degree of adaptation to terrestrial environments.

Ion photon emission microscope

DOEpatents

Doyle, Barney L.

2003-04-22

An ion beam analysis system that creates microscopic multidimensional image maps of the effects of high energy ions from an unfocussed source upon a sample by correlating the exact entry point of an ion into a sample by projection imaging of the ion-induced photons emitted at that point with a signal from a detector that measures the interaction of that ion within the sample. The emitted photons are collected in the lens system of a conventional optical microscope, and projected on the image plane of a high resolution single photon position sensitive detector. Position signals from this photon detector are then correlated in time with electrical effects, including the malfunction of digital circuits, detected within the sample that were caused by the individual ion that created these photons initially.

The history and development of the helium ion microscope.

PubMed

Economou, Nicholas P; Notte, John A; Thompson, William B

2012-01-01

The helium ion microscope has recently emerged as a commercially available instrument. However, its roots go back more than 60 years to the development of the field ion microscope in Berlin, first reported in 1951. Over the intervening years, numerous researchers have pursued the development of a gas field ionization source with the goal of producing a suitable source for an ion microscope. This proved to be an elusive goal until early in this century when a number of discoveries led to a successful source, and shortly thereafter, an instrument fully able to exploit its advantages. Many individuals and many technical advances have come together to make this new class of microscope. The long history of this quest is reviewed along with the recent advances that led to the achievement of this milestone. A brief summary of the current status of the technology and its applications are given. © Wiley Periodicals, Inc.

Track structure model of microscopic energy deposition by protons and heavy ions in segments of neuronal cell dendrites represented by cylinders or spheres

PubMed Central

Alp, Murat; Cucinotta, Francis A.

2017-01-01

Changes to cognition, including memory, following radiation exposure are a concern for cosmic ray exposures to astronauts and in Hadron therapy with proton and heavy ion beams. The purpose of the present work is to develop computational methods to evaluate microscopic energy deposition (ED) in volumes representative of neuron cell structures, including segments of dendrites and spines, using a stochastic track structure model. A challenge for biophysical models of neuronal damage is the large sizes (>100 μm) and variability in volumes of possible dendritic segments and pre-synaptic elements (spines and filopodia). We consider cylindrical and spherical microscopic volumes of varying geometric parameters and aspect ratios from 0.5 to 5 irradiated by protons, and 3He and 12C particles at energies corresponding to a distance of 1 cm to the Bragg peak, which represent particles of interest in Hadron therapy as well as space radiation exposure. We investigate the optimal axis length of dendritic segments to evaluate microscopic ED and hit probabilities along the dendritic branches at a given macroscopic dose. Because of large computation times to analyze ED in volumes of varying sizes, we developed an analytical method to find the mean primary dose in spheres that can guide numerical methods to find the primary dose distribution for cylinders. Considering cylindrical segments of varying aspect ratio at constant volume, we assess the chord length distribution, mean number of hits and ED profiles by primary particles and secondary electrons (δ-rays). For biophysical modeling applications, segments on dendritic branches are proposed to have equal diameters and axes lengths along the varying diameter of a dendritic branch. PMID:28554507

Track structure model of microscopic energy deposition by protons and heavy ions in segments of neuronal cell dendrites represented by cylinders or spheres

NASA Astrophysics Data System (ADS)

Alp, Murat; Cucinotta, Francis A.

2017-05-01

Changes to cognition, including memory, following radiation exposure are a concern for cosmic ray exposures to astronauts and in Hadron therapy with proton and heavy ion beams. The purpose of the present work is to develop computational methods to evaluate microscopic energy deposition (ED) in volumes representative of neuron cell structures, including segments of dendrites and spines, using a stochastic track structure model. A challenge for biophysical models of neuronal damage is the large sizes (> 100 μm) and variability in volumes of possible dendritic segments and pre-synaptic elements (spines and filopodia). We consider cylindrical and spherical microscopic volumes of varying geometric parameters and aspect ratios from 0.5 to 5 irradiated by protons, and 3He and 12C particles at energies corresponding to a distance of 1 cm to the Bragg peak, which represent particles of interest in Hadron therapy as well as space radiation exposure. We investigate the optimal axis length of dendritic segments to evaluate microscopic ED and hit probabilities along the dendritic branches at a given macroscopic dose. Because of large computation times to analyze ED in volumes of varying sizes, we developed an analytical method to find the mean primary dose in spheres that can guide numerical methods to find the primary dose distribution for cylinders. Considering cylindrical segments of varying aspect ratio at constant volume, we assess the chord length distribution, mean number of hits and ED profiles by primary particles and secondary electrons (δ-rays). For biophysical modeling applications, segments on dendritic branches are proposed to have equal diameters and axes lengths along the varying diameter of a dendritic branch.

Track structure model of microscopic energy deposition by protons and heavy ions in segments of neuronal cell dendrites represented by cylinders or spheres.

PubMed

Alp, Murat; Cucinotta, Francis A

2017-05-01

Changes to cognition, including memory, following radiation exposure are a concern for cosmic ray exposures to astronauts and in Hadron therapy with proton and heavy ion beams. The purpose of the present work is to develop computational methods to evaluate microscopic energy deposition (ED) in volumes representative of neuron cell structures, including segments of dendrites and spines, using a stochastic track structure model. A challenge for biophysical models of neuronal damage is the large sizes (> 100µm) and variability in volumes of possible dendritic segments and pre-synaptic elements (spines and filopodia). We consider cylindrical and spherical microscopic volumes of varying geometric parameters and aspect ratios from 0.5 to 5 irradiated by protons, and 3 He and 12 C particles at energies corresponding to a distance of 1cm to the Bragg peak, which represent particles of interest in Hadron therapy as well as space radiation exposure. We investigate the optimal axis length of dendritic segments to evaluate microscopic ED and hit probabilities along the dendritic branches at a given macroscopic dose. Because of large computation times to analyze ED in volumes of varying sizes, we developed an analytical method to find the mean primary dose in spheres that can guide numerical methods to find the primary dose distribution for cylinders. Considering cylindrical segments of varying aspect ratio at constant volume, we assess the chord length distribution, mean number of hits and ED profiles by primary particles and secondary electrons (δ-rays). For biophysical modeling applications, segments on dendritic branches are proposed to have equal diameters and axes lengths along the varying diameter of a dendritic branch. Copyright © 2017. Published by Elsevier Ltd.

Simultaneous specimen and stage cleaning device for analytical electron microscope

DOEpatents

Zaluzec, Nestor J.

1996-01-01

An improved method and apparatus are provided for cleaning both a specimen stage, a specimen and an interior of an analytical electron microscope (AEM). The apparatus for cleaning a specimen stage and specimen comprising a plasma chamber for containing a gas plasma and an air lock coupled to the plasma chamber for permitting passage of the specimen stage and specimen into the plasma chamber and maintaining an airtight chamber. The specimen stage and specimen are subjected to a reactive plasma gas that is either DC or RF excited. The apparatus can be mounted on the analytical electron microscope (AEM) for cleaning the interior of the microscope.

High dynamic range bio-molecular ion microscopy with the Timepix detector.

PubMed

Jungmann, Julia H; MacAleese, Luke; Visser, Jan; Vrakking, Marc J J; Heeren, Ron M A

2011-10-15

Highly parallel, active pixel detectors enable novel detection capabilities for large biomolecules in time-of-flight (TOF) based mass spectrometry imaging (MSI). In this work, a 512 × 512 pixel, bare Timepix assembly combined with chevron microchannel plates (MCP) captures time-resolved images of several m/z species in a single measurement. Mass-resolved ion images from Timepix measurements of peptide and protein standards demonstrate the capability to return both mass-spectral and localization information of biologically relevant analytes from matrix-assisted laser desorption ionization (MALDI) on a commercial ion microscope. The use of a MCP-Timepix assembly delivers an increased dynamic range of several orders of magnitude. The Timepix returns defined mass spectra already at subsaturation MCP gains, which prolongs the MCP lifetime and allows the gain to be optimized for image quality. The Timepix peak resolution is only limited by the resolution of the in-pixel measurement clock. Oligomers of the protein ubiquitin were measured up to 78 kDa. © 2011 American Chemical Society

Characterization of Nanopipettes.

PubMed

Perry, David; Momotenko, Dmitry; Lazenby, Robert A; Kang, Minkyung; Unwin, Patrick R

2016-05-17

Nanopipettes are widely used in electrochemical and analytical techniques as tools for sizing, sequencing, sensing, delivery, and imaging. For all of these applications, the response of a nanopipette is strongly affected by its geometry and surface chemistry. As the size of nanopipettes becomes smaller, precise geometric characterization is increasingly important, especially if nanopipette probes are to be used for quantitative studies and analysis. This contribution highlights the combination of data from voltage-scanning ion conductivity experiments, transmission electron microscopy and finite element method simulations to fully characterize nanopipette geometry and surface charge characteristics, with an accuracy not achievable using existing approaches. Indeed, it is shown that presently used methods for characterization can lead to highly erroneous information on nanopipettes. The new approach to characterization further facilitates high-level quantification of the behavior of nanopipettes in electrochemical systems, as demonstrated herein for a scanning ion conductance microscope setup.

Microscope mode secondary ion mass spectrometry imaging with a Timepix detector.

PubMed

Kiss, Andras; Jungmann, Julia H; Smith, Donald F; Heeren, Ron M A

2013-01-01

In-vacuum active pixel detectors enable high sensitivity, highly parallel time- and space-resolved detection of ions from complex surfaces. For the first time, a Timepix detector assembly was combined with a secondary ion mass spectrometer for microscope mode secondary ion mass spectrometry (SIMS) imaging. Time resolved images from various benchmark samples demonstrate the imaging capabilities of the detector system. The main advantages of the active pixel detector are the higher signal-to-noise ratio and parallel acquisition of arrival time and position. Microscope mode SIMS imaging of biomolecules is demonstrated from tissue sections with the Timepix detector.

DNA translocation measurements in solid-state nanopores fabricated using helium-ion microscope

NASA Astrophysics Data System (ADS)

Liu, Liping; Miao, Wang; Huynh, Chuong; Liu, Quanjun; Ling, Xinsheng

2012-02-01

We report high-quality DNA translocation measurements in solid-state nanopores drilled in free-standing SiN membranes by using a helium-ion beam in a Zeiss helium-ion microscope (HIM). We show that the HIM nanopores have similar performance as the TEM-drilled pores.

Failure Analysis of Heavy-Ion-Irradiated Schottky Diodes

NASA Technical Reports Server (NTRS)

Casey, Megan C.; Lauenstein, Jean-Marie; Wilcox, Edward P.; Topper, Alyson D.; Campola, Michael J.; Label, Kenneth A.

2017-01-01

In this work, we use high- and low-magnitude optical microscope images, infrared camera images, and scanning electron microscope images to identify and describe the failure locations in heavy-ion-irradiated Schottky diodes.

Automated MALDI matrix deposition method with inkjet printing for imaging mass spectrometry.

PubMed

Baluya, Dodge L; Garrett, Timothy J; Yost, Richard A

2007-09-01

Careful matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is critical for producing reproducible analyte ion signals. Traditional methods for matrix deposition are often considered an art rather than a science, with significant sample-to-sample variability. Here we report an automated method for matrix deposition, employing a desktop inkjet printer (<$200) with 5760 x 1440 dpi resolution and a six-channel piezoelectric head that delivers 3 pL/drop. The inkjet printer tray, designed to hold CDs and DVDs, was modified to hold microscope slides. Empty ink cartridges were filled with MALDI matrix solutions, including DHB in methanol/water (70:30) at concentrations up to 40 mg/mL. Various samples (including rat brain tissue sections and standards of small drug molecules) were prepared using three deposition methods (electrospray, airbrush, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed that matrix crystals were formed evenly across the sample. There was minimal background signal after storing the matrix in the cartridges over a 6-month period. Overall, the mass spectral images gathered from inkjet-printed tissue specimens were of better quality and more reproducible than from specimens prepared by the electrospray and airbrush methods.

Method for reduction of selected ion intensities in confined ion beams

DOEpatents

Eiden, Gregory C.; Barinaga, Charles J.; Koppenaal, David W.

1998-01-01

A method for producing an ion beam having an increased proportion of analyte ions compared to carrier gas ions is disclosed. Specifically, the method has the step of addition of a charge transfer gas to the carrier analyte combination that accepts charge from the carrier gas ions yet minimally accepts charge from the analyte ions thereby selectively neutralizing the carrier gas ions. Also disclosed is the method as employed in various analytical instruments including an inductively coupled plasma mass spectrometer.

Method for reduction of selected ion intensities in confined ion beams

DOEpatents

Eiden, G.C.; Barinaga, C.J.; Koppenaal, D.W.

1998-06-16

A method for producing an ion beam having an increased proportion of analyte ions compared to carrier gas ions is disclosed. Specifically, the method has the step of addition of a charge transfer gas to the carrier analyte combination that accepts charge from the carrier gas ions yet minimally accepts charge from the analyte ions thereby selectively neutralizing the carrier gas ions. Also disclosed is the method as employed in various analytical instruments including an inductively coupled plasma mass spectrometer. 7 figs.

Rapid and precise scanning helium ion microscope milling of solid-state nanopores for biomolecule detection.

PubMed

Yang, Jijin; Ferranti, David C; Stern, Lewis A; Sanford, Colin A; Huang, Jason; Ren, Zheng; Qin, Lu-Chang; Hall, Adam R

2011-07-15

We report the formation of solid-state nanopores using a scanning helium ion microscope. The fabrication process offers the advantage of high sample throughput along with fine control over nanopore dimensions, producing single pores with diameters below 4 nm. Electronic noise associated with ion transport through the resultant pores is found to be comparable with levels measured on devices made with the established technique of transmission electron microscope milling. We demonstrate the utility of our nanopores for biomolecular analysis by measuring the passage of double-strand DNA.

Formation of Metal-Adducted Analyte Ions by Flame-Induced Atmospheric Pressure Chemical Ionization Mass Spectrometry.

PubMed

Cheng, Sy-Chyi; Wang, Chin-Hsiung; Shiea, Jentaie

2016-05-17

A flame-induced atmospheric pressure chemical ionization (FAPCI) source, consisting of a miniflame, nebulizer, and heated tube, was developed to ionize analytes. The ionization was performed by reacting analytes with a charged species generated in a flame. A stainless steel needle deposited with saturated alkali chloride solution was introduced into the mini oxyacetylene flame to generate alkali ions, which were reacted with analytes (M) generated in a heated nebulizer. The alkali-adducted 18-crown-6 ether ions, including (M + Li)(+), (M + Na)(+), (M + K)(+), (M + Rb)(+), and (M + Cs)(+), were successfully detected on the FAPCI mass spectra when the corresponding alkali chloride solutions were separately introduced to the flame. When an alkali chloride mixture was introduced, all alkali-adducted analyte ions were simultaneously detected. Their intensity order was as follows: (M + Cs)(+) > (M + Rb)(+) > (M + K)(+) > (M + Na)(+) > (M + Li)(+), and this trend agreed with the lattice energies of alkali chlorides. Besides alkali ions, other transition metal ions such as Ni(+), Cu(+), and Ag(+) were generated in a flame for analyte ionization. Other than metal ions, the reactive species generated in the fossil fuel flame could also be used to ionize analytes, which formed protonated analyte ions (M + H)(+) in positive ion mode and deprotonated analyte ions (M - H)(-) in negative ion mode.

Concurrent in situ ion irradiation transmission electron microscope

DOE PAGES

Hattar, K.; Bufford, D. C.; Buller, D. L.

2014-08-29

An in situ ion irradiation transmission electron microscope has been developed and is operational at Sandia National Laboratories. This facility permits high spatial resolution, real time observation of electron transparent samples under ion irradiation, implantation, mechanical loading, corrosive environments, and combinations thereof. This includes the simultaneous implantation of low-energy gas ions (0.8–30 keV) during high-energy heavy ion irradiation (0.8–48 MeV). In addition, initial results in polycrystalline gold foils are provided to demonstrate the range of capabilities.

Using Time-of-Flight Secondary Ion Mass Spectrometry to Study Biomarkers

NASA Astrophysics Data System (ADS)

Thiel, Volker; Sjövall, Peter

2011-05-01

Time-of-flight secondary ion mass spectrometry (ToF-SIMS) is a technique designed to analyze the composition and spatial distribution of molecules and chemical structures on surfaces. These capabilities have generated much interest in its use in geobiology, in particular for the characterization of organic biomarkers (molecular biosignatures) at the microscopic level. We here discuss the strengths, weaknesses, and potential of ToF-SIMS for biomarker analyses with a focus on applications in geobiology, including biogeochemistry, organic geochemistry, geomicrobiology, and paleobiology. After describing the analytical principles of ToF-SIMS, we discuss issues of biomarker spectral formation and interpretation. Then, key applications of ToF-SIMS to soft (microbial matter, cells), hard (microbial mineral precipitates), and liquid (petroleum) samples relevant in geobiology are reviewed. Finally, we examine the potential of ToF-SIMS in biomarker research and the current limitations and obstacles for which further development would be beneficial to the field.

Focal depth measurement of scanning helium ion microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guo, Hongxuan, E-mail: Guo.hongxuan@nims.go.jp; Itoh, Hiroshi; Wang, Chunmei

2014-07-14

When facing the challenges of critical dimension measurement of complicated nanostructures, such as of the three dimension integrated circuit, characterization of the focal depth of microscopes is important. In this Letter, we developed a method for characterizing the focal depth of a scanning helium ion microscope (HIM) by using an atomic force microscope tip characterizer (ATC). The ATC was tilted in a sample chamber at an angle to the scanning plan. Secondary electron images (SEIs) were obtained at different positions of the ATC. The edge resolution of the SEIs shows the nominal diameters of the helium ion beam at differentmore » focal levels. With this method, the nominal shapes of the helium ion beams were obtained with different apertures. Our results show that a small aperture is necessary to get a high spatial resolution and high depth of field images with HIM. This work provides a method for characterizing and improving the performance of HIM.« less

Focal depth measurement of scanning helium ion microscope

NASA Astrophysics Data System (ADS)

Guo, Hongxuan; Itoh, Hiroshi; Wang, Chunmei; Zhang, Han; Fujita, Daisuke

2014-07-01

When facing the challenges of critical dimension measurement of complicated nanostructures, such as of the three dimension integrated circuit, characterization of the focal depth of microscopes is important. In this Letter, we developed a method for characterizing the focal depth of a scanning helium ion microscope (HIM) by using an atomic force microscope tip characterizer (ATC). The ATC was tilted in a sample chamber at an angle to the scanning plan. Secondary electron images (SEIs) were obtained at different positions of the ATC. The edge resolution of the SEIs shows the nominal diameters of the helium ion beam at different focal levels. With this method, the nominal shapes of the helium ion beams were obtained with different apertures. Our results show that a small aperture is necessary to get a high spatial resolution and high depth of field images with HIM. This work provides a method for characterizing and improving the performance of HIM.

Understanding Imaging and Metrology with the Helium Ion Microscope

NASA Astrophysics Data System (ADS)

Postek, Michael T.; Vladár, András E.; Ming, Bin

2009-09-01

One barrier to innovation confronting all phases of nanotechnology is the lack of accurate metrology for the characterization of nanomaterials. Ultra-high resolution microscopy is a key technology needed to achieve this goal. But, current microscope technology is being pushed to its limits. The scanning and transmission electron microscopes have incrementally improved in performance and other scanned probe technologies such as atomic force microscopy, scanning tunneling microscopy and focused ion beam microscopes have all been applied to nanotechnology with various levels of success. A relatively new tool for nanotechnology is the scanning helium ion microscope (HIM). The HIM is a new complementary imaging and metrology technology for nanotechnology which may be able to push the current resolution barrier lower. But, successful imaging and metrology with this instrument entails new ion beam/specimen interaction physics which must be fully understood. As a new methodology, HIM is beginning to show promise and the abundance of potentially advantageous applications for nanotechnology have yet to be fully exploited. This presentation will discuss some of the progress made at NIST in understanding the science behind this new technique.

Specific interaction between negative atmospheric ions and organic compounds in atmospheric pressure corona discharge ionization mass spectrometry.

PubMed

Sekimoto, Kanako; Sakai, Mami; Takayama, Mitsuo

2012-06-01

The interaction between negative atmospheric ions and various types of organic compounds were investigated using atmospheric pressure corona discharge ionization (APCDI) mass spectrometry. Atmospheric negative ions such as O(2)(-), HCO(3)(-), COO(-)(COOH), NO(2)(-), NO(3)(-), and NO(3)(-)(HNO(3)) having different proton affinities served as the reactant ions for analyte ionization in APCDI in negative-ion mode. The individual atmospheric ions specifically ionized aliphatic and aromatic compounds with various functional groups as atmospheric ion adducts and deprotonated analytes. The formation of the atmospheric ion adducts under certain discharge conditions is most likely attributable to the affinity between the analyte and atmospheric ion and the concentration of the atmospheric ion produced under these conditions. The deprotonated analytes, in contrast, were generated from the adducts of the atmospheric ions with higher proton affinity attributable to efficient proton abstraction from the analyte by the atmospheric ion.

Chemical analyses of fossil bone.

PubMed

Zheng, Wenxia; Schweitzer, Mary Higby

2012-01-01

The preservation of microstructures consistent with soft tissues, cells, and other biological components in demineralized fragments of dinosaur bone tens of millions of years old was unexpected, and counter to current hypotheses of tissue, cellular, and molecular degradation. Although the morphological similarity of these tissues to extant counterparts was unmistakable, after at least 80 million years exposed to geochemical influences, morphological similarity is insufficient to support an endogenous source. To test this hypothesis, and to characterize these materials at a molecular level, we applied multiple independent chemical, molecular, and microscopic analyses to identify the presence of original components produced by the extinct organisms. Microscopic techniques included field emission scanning electron microscopy, analytical transmission electron microscopy, transmitted light microscopy (LM), and fluorescence microscopy (FM). The chemical and molecular techniques include enzyme-linked immunosorbant assay, sodium dodecyl sulfate polyacrylamide gel electrophoresis, western blot (immunoblot), and attenuated total reflectance infrared spectroscopy. In situ analyses performed directly on tissues included immunohistochemistry and time-of-flight secondary ion mass spectrometry. The details of sample preparation and methodology are described in detail herein.

Nanofabrication with a helium ion microscope

NASA Astrophysics Data System (ADS)

Maas, Diederik; van Veldhoven, Emile; Chen, Ping; Sidorkin, Vadim; Salemink, Huub; van der Drift, Emile..; Alkemade, Paul

2010-03-01

The recently introduced helium ion microscope (HIM) is capable of imaging and fabrication of nanostructures thanks to its sub-nanometer sized ion probe. The unique interaction of the helium ions with the sample material provides very localized secondary electron emission, thus providing a valuable signal for high-resolution imaging as well as a mechanism for very precise nanofabrication. The low proximity effects, due to the low yield of backscattered ions and the confinement of the forward scattered ions into a narrow cone, enable patterning of ultra-dense sub-10 nm structures. This paper presents various nanofabrication results obtained with direct-write, with scanning helium ion beam lithography, and with helium ion beam induced deposition.

A method of mounting multiple otoliths for beam-based microchemical analyses

USGS Publications Warehouse

Donohoe, C.J.; Zimmerman, C.E.

2010-01-01

Beam-based analytical methods are widely used to measure the concentrations of elements and isotopes in otoliths. These methods usually require that otoliths be individually mounted and prepared to properly expose the desired growth region to the analytical beam. Most analytical instruments, such as LA-ICPMS and ion and electron microprobes, have sample holders that will accept only one to six slides or mounts at a time. We describe a method of mounting otoliths that allows for easy transfer of many otoliths to a single mount after they have been prepared. Such an approach increases the number of otoliths that can be analyzed in a single session by reducing the need open the sample chamber to exchange slides-a particularly time consuming step on instruments that operate under vacuum. For ion and electron microprobes, the method also greatly reduces the number of slides that must be coated with an electrical conductor prior to analysis. In this method, a narrow strip of cover glass is first glued at one end to a standard microscope slide. The otolith is then mounted in thermoplastic resin on the opposite, free end of the strip. The otolith can then be ground and flipped, if needed, by reheating the mounting medium. After otolith preparation is complete, the cover glass is cut with a scribe to free the otolith and up to 20 small otoliths can be arranged on a single petrographic slide. ?? 2010 The Author(s).

Conversion of multiple analyte cation types to a single analyte anion type via ion/ion charge inversion.

PubMed

Hassell, Kerry M; LeBlanc, Yves; McLuckey, Scott A

2009-11-01

Charge inversion ion/ion reactions can convert several cation types associated with a single analyte molecule to a single anion type for subsequent mass analysis. Specifically, analyte ions present with one of a variety of cationizing agents, such as an excess proton, excess sodium ion, or excess potassium ion, can all be converted to the deprotonated molecule, provided that a stable anion can be generated for the analyte. Multiply deprotonated species that are capable of exchanging a proton for a metal ion serve as the reagent anions for the reaction. This process is demonstrated here for warfarin and for a glutathione conjugate. Examples for several other glutathione conjugates are provided as supplementary material to demonstrate the generality of the reaction. In the case of glutathione conjugates, multiple metal ions can be associated with the singly-charged analyte due to the presence of two carboxylate groups. The charge inversion reaction involves the removal of the excess cationizing agent, as well as any metal ions associated with anionic groups to yield a singly deprotonated analyte molecule. The ability to convert multiple cation types to a single anion type is analytically desirable in cases in which the analyte signal is distributed among several cation types, as is common in the electrospray ionization of solutions with relatively high salt contents. For analyte species that undergo efficient charge inversion, such as glutathione conjugates, there is the additional potential advantage for significantly improved signal-to-noise ratios when species that give rise to 'chemical noise' in the positive ion spectrum do not undergo efficient charge inversion.

Solar Ion Sputter Deposition in the Lunar Regolith: Experimental Simulation Using Focused-Ion Beam Techniques

NASA Technical Reports Server (NTRS)

Christoffersen, R.; Rahman, Z.; Keller, L. P.

2012-01-01

As regions of the lunar regolith undergo space weathering, their component grains develop compositionally and microstructurally complex outer coatings or "rims" ranging in thickness from a few 10 s to a few 100's of nm. Rims on grains in the finest size fractions (e.g., <20 m) of mature lunar regoliths contain optically-active concentrations of nm size metallic Fe spherules, or "nanophase Fe(sup o)" that redden and attenuate optical reflectance spectral features important in lunar remote sensing. Understanding the mechanisms for rim formation is therefore a key part of connecting the drivers of mineralogical and chemical changes in the lunar regolith with how lunar terrains are observed to become space weathered from a remotely-sensed point of view. As interpreted based on analytical transmission electron microscope (TEM) studies, rims are produced from varying relative contributions from: 1) direct solar ion irradiation effects that amorphize or otherwise modify the outer surface of the original host grain, and 2) nanoscale, layer-like, deposition of extrinsic material processed from the surrounding soil. This extrinsic/deposited material is the dominant physical host for nanophase Fe(sup o) in the rims. An important lingering uncertainty is whether this deposited material condensed from regolith components locally vaporized in micrometeorite or larger impacts, or whether it formed as solar wind ions sputtered exposed soil and re-deposited the sputtered ions on less exposed areas. Deciding which of these mechanisms is dominant, or possibility exclusive, has been hampered because there is an insufficient library of chemical and microstructural "fingerprints" to distinguish deposits produced by the two processes. Experimental sputter deposition / characterization studies relevant to rim formation have particularly lagged since the early post-Apollo experiments of Hapke and others, especially with regard to application of TEM-based characterization techniques. Here we report on a novel design for simulating solar ion sputter deposition in the lunar regolith, with characterization of the resulting sputter deposits by an array of advanced analytical TEM techniques.

Scanning ion-conductance and atomic force microscope with specialized sphere-shaped nanopippettes

NASA Astrophysics Data System (ADS)

Zhukov, M. V.; Sapozhnikov, I. D.; Golubok, A. O.; Chubinskiy-Nadezhdin, V. I.; Komissarenko, F. E.; Lukashenko, S. Y.

2017-11-01

A scanning ion-conductance microscope was designed on the basis of scanning probe microscope NanoTutor. The optimal parameters of nanopipettes fabrication were found according to scanning electron microscopy diagnostics, current-distance I (Z) and current-voltage characteristics. A comparison of images of test objects, including biological samples, was carried out in the modes of optical microscopy, atomic force microscopy and scanning ion-conductance microscopy. Sphere-shaped nanopippettes probes were developed and tested to increase the stability of pipettes, reduce invasiveness and improve image quality of atomic force microscopy in tapping mode. The efficiency of sphere-shaped nanopippettes is shown.

Apparatus for reduction of selected ion intensities in confined ion beams

DOEpatents

Eiden, Gregory C.; Barinaga, Charles J.; Koppenaal, David W.

2001-01-01

An apparatus for producing an ion beam having an increased proportion of analyte ions compared to carrier gas ions is disclosed. Specifically, the apparatus has an ion trap or a collision cell containing a reagent gas wherein the reagent gas accepts charge from the analyte ions thereby selectively neutralizing the carrier gas ions. Also disclosed is the collision cell as employed in various locations within analytical instruments including an inductively coupled plasma mass spectrometer.

Highly charged ion based time of flight emission microscope

DOEpatents

Barnes, Alan V.; Schenkel, Thomas; Hamza, Alex V.; Schneider, Dieter H.; Doyle, Barney

2001-01-01

A highly charged ion based time-of-flight emission microscope has been designed, which improves the surface sensitivity of static SIMS measurements because of the higher ionization probability of highly charged ions. Slow, highly charged ions are produced in an electron beam ion trap and are directed to the sample surface. The sputtered secondary ions and electrons pass through a specially designed objective lens to a microchannel plate detector. This new instrument permits high surface sensitivity (10.sup.10 atoms/cm.sup.2), high spatial resolution (100 nm), and chemical structural information due to the high molecular ion yields. The high secondary ion yield permits coincidence counting, which can be used to enhance determination of chemical and topological structure and to correlate specific molecular species.

Structural analysis of ion-implanted chemical-vapor-deposited diamond by transmission electron microscope

NASA Astrophysics Data System (ADS)

Jiang, N.; Deguchi, M.; Wang, C. L.; Won, J. H.; Jeon, H. M.; Mori, Y.; Hatta, A.; Kitabatake, M.; Ito, T.; Hirao, T.; Sasaki, T.; Hiraki, A.

1997-04-01

A transmission electron microscope (TEM) study of ion-implanted chemical-vapor-deposited (CVD) diamond is presented. CVD diamond used for transmission electron microscope observation was directly deposited onto Mo TEM grids. As-deposited specimens were irradiated by C (100 keV) ions at room temperature with a wide range of implantation doses (10 12-10 17/cm 2). Transmission electron diffraction (TED) patterns indicate that there exists a critical dose ( Dc) for the onset of amorphization of CVD diamond as a result of ion induced damage and the value of critical dose is confirmed to be about 3 × 10 15/cm 2. The ion-induced transformation process is clearly revealed by high resolution electron microscope (HREM) images. For a higher dose implantation (7 × 10 15/cm 2) a large amount of diamond phase is transformed into amorphous carbon and many tiny misoriented diamond blocks are found to be left in the amorphous solid. The average size of these misoriented diamond blocks is only about 1-2 nm. Further bombardment (10 17/cm 2) almost kills all of the diamond phase within the irradiated volume and moreover leads to local formation of micropolycrystalline graphite.

Technical Reports - FY16 Q1 - October-December 2015

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lordi, Vincenzo; Rubenstein, Brenda M.; Ray, Keith G.

2016-01-20

Recent experiments have demonstrated that the frequency dependence of motional heating rates in ion traps can vary dramatically with temperature.1-6 More specifically, it has been shown that, at temperatures below roughly 70 K, heating rates are substantially lower than those observed at temperatures above 70 K.1,2 These observations, combined with experiments that show that ion bombardment may also reduce heating rates,4,5 suggest that one potential source of heating may be the presence of unwanted adatoms on trap surfaces. Based upon this evidence, this past quarter, we have used our previously detailed microscopic model of anomalous heating to study which adatomsmore » may be responsible for the observed temperature-dependent scaling of motional heating rates with frequency. We have also examined the validity of one of the key assumptions in our model - that surface adatom dipoles can be accurately obtained from a variational ansatz - by using more direct DFT calculations of the dipole moments. Our current results suggest that the adatoms potentially responsible for the observed motional heating rates should bind weakly to the electrode surface and likely have a mass that exceeds that of Ne. Preliminary DFT calculations suggest that an analytical adatom dipole model,9 previously used in the ion trap noise literature7 to obtain the dipole as a function of adatom-surface distance, may be insufficiently accurate. Therefore, we are working toward obtaining a tabulation of the distance-dependent dipole for several adsorbates using first principles calculations for more accurate input to the heating model. The accurate calculation of the adatom dipole is important because its fluctuation is what couples to and heats the trapped ion qubit. Future work will focus on calculating the frequency spectra of a variety of hydrocarbons, which should have the binding characteristics identified below as necessary for reproducing experimental results. Upcoming efforts will moreover be directed toward deriving an improved microscopic model of heating which will enable direct comparisons of heating rates with measured ion-surface distances and will more accurately account for experimental parameters such as the trapping frequency, ion-electrode distance, and RF power applied to the electrodes.« less

Analytical model of the optical vortex microscope.

PubMed

Płocinniczak, Łukasz; Popiołek-Masajada, Agnieszka; Masajada, Jan; Szatkowski, Mateusz

2016-04-20

This paper presents an analytical model of the optical vortex scanning microscope. In this microscope the Gaussian beam with an embedded optical vortex is focused into the sample plane. Additionally, the optical vortex can be moved inside the beam, which allows fine scanning of the sample. We provide an analytical solution of the whole path of the beam in the system (within paraxial approximation)-from the vortex lens to the observation plane situated on the CCD camera. The calculations are performed step by step from one optical element to the next. We show that at each step, the expression for light complex amplitude has the same form with only four coefficients modified. We also derive a simple expression for the vortex trajectory of small vortex displacements.

High resolution mass spectrometry method and system for analysis of whole proteins and other large molecules

DOEpatents

Reilly, Peter T. A. [Knoxville, TN; Harris, William A [Naperville, IL

2010-03-02

A matrix assisted laser desorption/ionization (MALDI) method and related system for analyzing high molecular weight analytes includes the steps of providing at least one matrix-containing particle inside an ion trap, wherein at least one high molecular weight analyte molecule is provided within the matrix-containing particle, and MALDI on the high molecular weight particle while within the ion trap. A laser power used for ionization is sufficient to completely vaporize the particle and form at least one high molecular weight analyte ion, but is low enough to avoid fragmenting the high molecular weight analyte ion. The high molecular weight analyte ion is extracted out from the ion trap, and is then analyzed using a detector. The detector is preferably a pyrolyzing and ionizing detector.

Quantum criticality of a spin-1 XY model with easy-plane single-ion anisotropy via a two-time Green function approach avoiding the Anderson-Callen decoupling

NASA Astrophysics Data System (ADS)

Mercaldo, M. T.; Rabuffo, I.; De Cesare, L.; Caramico D'Auria, A.

2016-04-01

In this work we study the quantum phase transition, the phase diagram and the quantum criticality induced by the easy-plane single-ion anisotropy in a d-dimensional quantum spin-1 XY model in absence of an external longitudinal magnetic field. We employ the two-time Green function method by avoiding the Anderson-Callen decoupling of spin operators at the same sites which is of doubtful accuracy. Following the original Devlin procedure we treat exactly the higher order single-site anisotropy Green functions and use Tyablikov-like decouplings for the exchange higher order ones. The related self-consistent equations appear suitable for an analysis of the thermodynamic properties at and around second order phase transition points. Remarkably, the equivalence between the microscopic spin model and the continuous O(2) -vector model with transverse-Ising model (TIM)-like dynamics, characterized by a dynamic critical exponent z=1, emerges at low temperatures close to the quantum critical point with the single-ion anisotropy parameter D as the non-thermal control parameter. The zero-temperature critic anisotropy parameter Dc is obtained for dimensionalities d > 1 as a function of the microscopic exchange coupling parameter and the related numerical data for different lattices are found to be in reasonable agreement with those obtained by means of alternative analytical and numerical methods. For d > 2, and in particular for d=3, we determine the finite-temperature critical line ending in the quantum critical point and the related TIM-like shift exponent, consistently with recent renormalization group predictions. The main crossover lines between different asymptotic regimes around the quantum critical point are also estimated providing a global phase diagram and a quantum criticality very similar to the conventional ones.

Modern Material Analysis Instruments Add a New Dimension to Materials Characterization and Failure Analysis

NASA Technical Reports Server (NTRS)

Panda, Binayak

2009-01-01

Modern analytical tools can yield invaluable results during materials characterization and failure analysis. Scanning electron microscopes (SEMs) provide significant analytical capabilities, including angstrom-level resolution. These systems can be equipped with a silicon drift detector (SDD) for very fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations, chambers that admit large samples, variable pressure for wet samples, and quantitative analysis software to examine phases. Advanced solid-state electronics have also improved surface and bulk analysis instruments: Secondary ion mass spectroscopy (SIMS) can quantitatively determine and map light elements such as hydrogen, lithium, and boron - with their isotopes. Its high sensitivity detects impurities at parts per billion (ppb) levels. X-ray photo-electron spectroscopy (XPS) can determine oxidation states of elements, as well as identifying polymers and measuring film thicknesses on coated composites. This technique is also known as electron spectroscopy for chemical analysis (ESCA). Scanning Auger electron spectroscopy (SAM) combines surface sensitivity, spatial lateral resolution (10 nm), and depth profiling capabilities to describe elemental compositions of near and below surface regions down to the chemical state of an atom.

Method of multiplexed analysis using ion mobility spectrometer

DOEpatents

Belov, Mikhail E [Richland, WA; Smith, Richard D [Richland, WA

2009-06-02

A method for analyzing analytes from a sample introduced into a Spectrometer by generating a pseudo random sequence of a modulation bins, organizing each modulation bin as a series of submodulation bins, thereby forming an extended pseudo random sequence of submodulation bins, releasing the analytes in a series of analyte packets into a Spectrometer, thereby generating an unknown original ion signal vector, detecting the analytes at a detector, and characterizing the sample using the plurality of analyte signal subvectors. The method is advantageously applied to an Ion Mobility Spectrometer, and an Ion Mobility Spectrometer interfaced with a Time of Flight Mass Spectrometer.

Review of microscopic plasma processes of occurring during refilling of the plasmasphere

NASA Technical Reports Server (NTRS)

Singh, N.; Torr, D. G.

1988-01-01

Refilling of the plasmashere after geomagnetic storms involves both macroscopic and microscopic plasma processes. The latter types of processes facilitate the refilling by trapping the plasma in the flux tube and by thermalizing the interhemispheric flow. A review of studies on microscopic processes is presented. The primary focus in this review is on the processes when the density is low and the plasma is collisionless. The discussion includes electrostatic shock formation, pitch angle scatterring extended ion heating and localized ion heating in the equatorial region.

SERS Detection of Dopamine Using Label-Free Acridine Red as Molecular Probe in Reduced Graphene Oxide/Silver Nanotriangle Sol Substrate

NASA Astrophysics Data System (ADS)

Luo, Yanghe; Ma, Lu; Zhang, Xinghui; Liang, Aihui; Jiang, Zhiliang

2015-05-01

The reduced graphene oxide/silver nanotriangle (rGO/AgNT) composite sol was prepared by the reduction of silver ions with sodium borohydride in the presence of H2O2 and sodium citrate. In the nanosol substrate, the molecular probe of acridine red (AR) exhibited a weak surface-enhanced Raman scattering (SERS) peak at 1506 cm-1 due to its interaction with the rGO of rGO/AgNT. Upon addition of dopamine (DA), the competitive adsorption between DA and AR with the rGO took place, and the AR molecules were adsorbed on the AgNT aggregates with a strong SERS peak at 1506 cm-1 that caused the SERS peak increase. The increased SERS intensity is linear to the DA concentration in the range of 2.5-500 μmol/L. This new analytical system was investigated by SERS, fluorescence, absorption, transmission electron microscope (TEM), and scanning electron microscope (SEM) techniques, and a SERS quantitative analysis method for DA was established, using AR as a label-free molecular probe.

Biological tissue imaging with a position and time sensitive pixelated detector.

PubMed

Jungmann, Julia H; Smith, Donald F; MacAleese, Luke; Klinkert, Ivo; Visser, Jan; Heeren, Ron M A

2012-10-01

We demonstrate the capabilities of a highly parallel, active pixel detector for large-area, mass spectrometric imaging of biological tissue sections. A bare Timepix assembly (512 × 512 pixels) is combined with chevron microchannel plates on an ion microscope matrix-assisted laser desorption time-of-flight mass spectrometer (MALDI TOF-MS). The detector assembly registers position- and time-resolved images of multiple m/z species in every measurement frame. We prove the applicability of the detection system to biomolecular mass spectrometry imaging on biologically relevant samples by mass-resolved images from Timepix measurements of a peptide-grid benchmark sample and mouse testis tissue slices. Mass-spectral and localization information of analytes at physiologic concentrations are measured in MALDI-TOF-MS imaging experiments. We show a high spatial resolution (pixel size down to 740 × 740 nm(2) on the sample surface) and a spatial resolving power of 6 μm with a microscope mode laser field of view of 100-335 μm. Automated, large-area imaging is demonstrated and the Timepix' potential for fast, large-area image acquisition is highlighted.

Generation of gas-phase ions from charged clusters: an important ionization step causing suppression of matrix and analyte ions in matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Lou, Xianwen; van Dongen, Joost L J; Milroy, Lech-Gustav; Meijer, E W

2016-12-30

Ionization in matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is a very complicated process. It has been reported that quaternary ammonium salts show extremely strong matrix and analyte suppression effects which cannot satisfactorily be explained by charge transfer reactions. Further investigation of the reasons causing these effects can be useful to improve our understanding of the MALDI process. The dried-droplet and modified thin-layer methods were used as sample preparation methods. In the dried-droplet method, analytes were co-crystallized with matrix, whereas in the modified thin-layer method analytes were deposited on the surface of matrix crystals. Model compounds, tetrabutylammonium iodide ([N(Bu) 4 ]I), cesium iodide (CsI), trihexylamine (THA) and polyethylene glycol 600 (PEG 600), were selected as the test analytes given their ability to generate exclusively pre-formed ions, protonated ions and metal ion adducts respectively in MALDI. The strong matrix suppression effect (MSE) observed using the dried-droplet method might disappear using the modified thin-layer method, which suggests that the incorporation of analytes in matrix crystals contributes to the MSE. By depositing analytes on the matrix surface instead of incorporating in the matrix crystals, the competition for evaporation/ionization from charged matrix/analyte clusters could be weakened resulting in reduced MSE. Further supporting evidence for this inference was found by studying the analyte suppression effect using the same two sample deposition methods. By comparing differences between the mass spectra obtained via the two sample preparation methods, we present evidence suggesting that the generation of gas-phase ions from charged matrix/analyte clusters may induce significant suppression of matrix and analyte ions. The results suggest that the generation of gas-phase ions from charged matrix/analyte clusters is an important ionization step in MALDI-MS. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Systematization of the mass spectra for speciation of inorganic salts with static secondary ion mass spectrometry.

PubMed

Van Ham, Rita; Van Vaeck, Luc; Adams, Freddy C; Adriaens, Annemie

2004-05-01

The analytical use of mass spectra from static secondary ion mass spectrometry for the molecular identification of inorganic analytes in real life surface layers and microobjects requires an empirical insight in the signals to be expected from a given compound. A comprehensive database comprising over 50 salts has been assembled to complement prior data on oxides. The present study allows the systematic trends in the relationship between the detected signals and molecular composition of the analyte to be delineated. The mass spectra provide diagnostic information by means of atomic ions, structural fragments, molecular ions, and adduct ions of the analyte neutrals. The prediction of mass spectra from a given analyte must account for the charge state of the ions in the salt, the formation of oxide-type neutrals from oxy salts, and the occurrence of oxidation-reduction processes.

Review of current progress in nanometrology with the helium ion microscope

NASA Astrophysics Data System (ADS)

Postek, Michael T.; Vladár, András; Archie, Charles; Ming, Bin

2011-02-01

Scanning electron microscopy has been employed as an imaging and measurement tool for more than 50 years and it continues as a primary tool in many research and manufacturing facilities across the world. A new challenger to this work is the helium ion microscope (HIM). The HIM is a new imaging and metrology technology. Essentially, substitution of the electron source with a helium ion source yields a tool visually similar in function to the scanning electron microscope, but very different in the fundamental imaging and measurement process. The imaged and measured signal originates differently than in the scanning electron microscope and that fact and its single atom source diameter may be able to push the obtainable resolution lower, provide greater depth-of-field and ultimately improve the metrology. Successful imaging and metrology with this instrument entails understanding and modeling of new ion beam/specimen interaction physics. As a new methodology, HIM is beginning to show promise and the abundance of potentially advantageous applications for nanometrology has yet to be fully exploited. This paper discusses some of the progress made at NIST in collaboration with IBM to understand the science behind this new technology.

Microscopic morphology evolution during ion beam smoothing of Zerodur® surfaces.

PubMed

Liao, Wenlin; Dai, Yifan; Xie, Xuhui; Zhou, Lin

2014-01-13

Ion sputtering of Zerodur material often results in the formation of nanoscale microstructures on the surfaces, which seriously influences optical surface quality. In this paper, we describe the microscopic morphology evolution during ion sputtering of Zerodur surfaces through experimental researches and theoretical analysis, which shows that preferential sputtering together with curvature-dependent sputtering overcomes ion-induced smoothing mechanisms leading to granular nanopatterns formation in morphology and the coarsening of the surface. Consequently, we propose a new method for ion beam smoothing (IBS) of Zerodur optics assisted by deterministic ion beam material adding (IBA) technology. With this method, Zerodur optics with surface roughness down to 0.15 nm root mean square (RMS) level is obtained through the experimental investigation, which demonstrates the feasibility of our proposed method.

An approach to estimate spatial distribution of analyte within cells using spectrally-resolved fluorescence microscopy.

PubMed

Sharma, Dharmendar Kumar; Irfanullah, Mir; Basu, Santanu Kumar; Madhu, Sheri; De, Suman; Jadhav, Sameer; Ravikanth, Mangalampalli; Chowdhury, Arindam

2017-01-18

While fluorescence microscopy has become an essential tool amongst chemists and biologists for the detection of various analyte within cellular environments, non-uniform spatial distribution of sensors within cells often restricts extraction of reliable information on relative abundance of analytes in different subcellular regions. As an alternative to existing sensing methodologies such as ratiometric or FRET imaging, where relative proportion of analyte with respect to the sensor can be obtained within cells, we propose a methodology using spectrally-resolved fluorescence microscopy, via which both the relative abundance of sensor as well as their relative proportion with respect to the analyte can be simultaneously extracted for local subcellular regions. This method is exemplified using a BODIPY sensor, capable of detecting mercury ions within cellular environments, characterized by spectral blue-shift and concurrent enhancement of emission intensity. Spectral emission envelopes collected from sub-microscopic regions allowed us to compare the shift in transition energies as well as integrated emission intensities within various intracellular regions. Construction of a 2D scatter plot using spectral shifts and emission intensities, which depend on the relative amount of analyte with respect to sensor and the approximate local amounts of the probe, respectively, enabled qualitative extraction of relative abundance of analyte in various local regions within a single cell as well as amongst different cells. Although the comparisons remain semi-quantitative, this approach involving analysis of multiple spectral parameters opens up an alternative way to extract spatial distribution of analyte in heterogeneous systems. The proposed method would be especially relevant for fluorescent probes that undergo relatively nominal shift in transition energies compared to their emission bandwidths, which often restricts their usage for quantitative ratiometric imaging in cellular media due to strong cross-talk between energetically separated detection channels.

An approach to estimate spatial distribution of analyte within cells using spectrally-resolved fluorescence microscopy

NASA Astrophysics Data System (ADS)

Sharma, Dharmendar Kumar; Irfanullah, Mir; Basu, Santanu Kumar; Madhu, Sheri; De, Suman; Jadhav, Sameer; Ravikanth, Mangalampalli; Chowdhury, Arindam

2017-03-01

While fluorescence microscopy has become an essential tool amongst chemists and biologists for the detection of various analyte within cellular environments, non-uniform spatial distribution of sensors within cells often restricts extraction of reliable information on relative abundance of analytes in different subcellular regions. As an alternative to existing sensing methodologies such as ratiometric or FRET imaging, where relative proportion of analyte with respect to the sensor can be obtained within cells, we propose a methodology using spectrally-resolved fluorescence microscopy, via which both the relative abundance of sensor as well as their relative proportion with respect to the analyte can be simultaneously extracted for local subcellular regions. This method is exemplified using a BODIPY sensor, capable of detecting mercury ions within cellular environments, characterized by spectral blue-shift and concurrent enhancement of emission intensity. Spectral emission envelopes collected from sub-microscopic regions allowed us to compare the shift in transition energies as well as integrated emission intensities within various intracellular regions. Construction of a 2D scatter plot using spectral shifts and emission intensities, which depend on the relative amount of analyte with respect to sensor and the approximate local amounts of the probe, respectively, enabled qualitative extraction of relative abundance of analyte in various local regions within a single cell as well as amongst different cells. Although the comparisons remain semi-quantitative, this approach involving analysis of multiple spectral parameters opens up an alternative way to extract spatial distribution of analyte in heterogeneous systems. The proposed method would be especially relevant for fluorescent probes that undergo relatively nominal shift in transition energies compared to their emission bandwidths, which often restricts their usage for quantitative ratiometric imaging in cellular media due to strong cross-talk between energetically separated detection channels. Dedicated to Professor Kankan Bhattacharyya.

Effects of bulk viscosity and hadronic rescattering in heavy ion collisions at energies available at the BNL Relativistic Heavy Ion Collider and at the CERN Large Hadron Collider

NASA Astrophysics Data System (ADS)

Ryu, Sangwook; Paquet, Jean-François; Shen, Chun; Denicol, Gabriel; Schenke, Björn; Jeon, Sangyong; Gale, Charles

2018-03-01

We describe ultrarelativistic heavy ion collisions at the BNL Relativistic Heavy Ion Collider and the CERN Large Hadron Collider with a hybrid model using the IP-Glasma model for the earliest stage and viscous hydrodynamics and microscopic transport for the later stages of the collision. We demonstrate that within this framework the bulk viscosity of the plasma plays an important role in describing the experimentally observed radial flow and azimuthal anisotropy simultaneously. We further investigate the dependence of observables on the temperature below which we employ the microscopic transport description.

Imaging ion and molecular transport at subcellular resolution by secondary ion mass spectrometry

NASA Astrophysics Data System (ADS)

Chandra, Subhash; Morrison, George H.

1995-05-01

The transport of K+, Na+, and Ca2+ were imaged in individual cells with a Cameca IMS-3f ion microscope. Strict cryogenic frozen freeze-dry sample preparations were employed. Ion redistribution artifacts in conventional chemical preparations are discussed. Cryogenically prepared freeze-fractured freeze-dried cultured cells allowed the three-dimensional ion microscopic imaging of elements. As smaller structures in calcium images can be resolved with the 0.5 [mu]m spatial resolution, correlative techniques are needed to confirm their identity. The potentials of reflected light microscopy, scanning electron microscopy and laser scanning confocal microscopy are discussed for microfeature recognition in freeze-fractured freeze-dried cells. The feasibility of using frozen freeze-dried cells for imaging molecular transport at subcellular resolution was tested. Ion microscopy successfully imaged the transport of the isotopically tagged (13C, 15N) amino acid, -arginine. The labeled amino acid was imaged at mass 28 with a Cs+ primary ion beam as the 28(13C15N)- species. After a 4 h exposure of LLC-PK1 kidney cells to 4 mM labeled arginine, the amino acid was localized throughout the cell with a preferential incorporation into the nucleus and nucleolus. An example is also shown of the ion microscopic imaging of sodium borocaptate, an experimental therapeutic drug for brain tumors, in cryogenically prepared frozen freeze-dried Swiss 3T3 cells.

Peak distortion effects in analytical ion chromatography.

PubMed

Wahab, M Farooq; Anderson, Jordan K; Abdelrady, Mohamed; Lucy, Charles A

2014-01-07

The elution profile of chromatographic peaks provides fundamental understanding of the processes that occur in the mobile phase and the stationary phase. Major advances have been made in the column chemistry and suppressor technology in ion chromatography (IC) to handle a variety of sample matrices and ions. However, if the samples contain high concentrations of matrix ions, the overloaded peak elution profile is distorted. Consequently, the trace peaks shift their positions in the chromatogram in a manner that depends on the peak shape of the overloading analyte. In this work, the peak shapes in IC are examined from a fundamental perspective. Three commercial IC columns AS16, AS18, and AS23 were studied with borate, hydroxide and carbonate as suppressible eluents. Monovalent ions (chloride, bromide, and nitrate) are used as model analytes under analytical (0.1 mM) to overload conditions (10-500 mM). Both peak fronting and tailing are observed. On the basis of competitive Langmuir isotherms, if the eluent anion is more strongly retained than the analyte ion on an ion exchanger, the analyte peak is fronting. If the eluent is more weakly retained on the stationary phase, the analyte peak always tails under overload conditions regardless of the stationary phase capacity. If the charge of the analyte and eluent anions are different (e.g., Br(-) vs CO3(2-)), the analyte peak shapes depend on the eluent concentration in a more complex pattern. It was shown that there are interesting similarities with peak distortions due to strongly retained mobile phase components in other modes of liquid chromatography.

Mars Surveyor Program '01 Mars Environmental Compatibility Assessment wet chemistry lab: a sensor array for chemical analysis of the Martian soil.

PubMed

Kounaves, Samuel P; Lukow, Stefan R; Comeau, Brian P; Hecht, Michael H; Grannan-Feldman, Sabrina M; Manatt, Ken; West, Steven J; Wen, Xiaowen; Frant, Martin; Gillette, Tim

2003-07-25

The Mars Environmental Compatibility Assessment (MECA) instrument was designed, built, and flight qualified for the now canceled MSP (Mars Surveyor Program) '01 Lander. The MECA package consisted of a microscope, electrometer, material patch plates, and a wet chemistry laboratory (WCL). The primary goal of MECA was to analyze the Martian soil (regolith) for possible hazards to future astronauts and to provide a better understanding of Martian regolith geochemistry. The purpose of the WCL was to analyze for a range of soluble ionic chemical species and electrochemical parameters. The heart of the WCL was a sensor array of electrochemically based ion-selective electrodes (ISE). After 20 months storage at -23 degrees C and subsequent extended freeze/thawing cycles, WCL sensors were evaluated to determine both their physical durability and analytical responses. A fractional factorial calibration of the sensors was used to obtain slope, intercept, and all necessary selectivity coefficients simultaneously for selected ISEs. This calibration was used to model five cation and three anion sensors. These data were subsequently used to determine concentrations of several ions in two soil leachate simulants (based on terrestrial seawater and hypothesized Mars brine) and four actual soil samples. The WCL results were compared to simulant and soil samples using ion chromatography and inductively coupled plasma optical emission spectroscopy. The results showed that flight qualification and prolonged low-temperature storage conditions had minimal effects on the sensors. In addition, the analytical optimization method provided quantitative and qualitative data that could be used to accurately identify the chemical composition of the simulants and soils. The WCL has the ability to provide data that can be used to "read" the chemical, geological, and climatic history of Mars, as well as the potential habitability of its regolith.

Mars Surveyor Program '01 Mars Environmental Compatibility Assessment wet chemistry lab: a sensor array for chemical analysis of the Martian soil

NASA Technical Reports Server (NTRS)

Kounaves, Samuel P.; Lukow, Stefan R.; Comeau, Brian P.; Hecht, Michael H.; Grannan-Feldman, Sabrina M.; Manatt, Ken; West, Steven J.; Wen, Xiaowen; Frant, Martin; Gillette, Tim

2003-01-01

The Mars Environmental Compatibility Assessment (MECA) instrument was designed, built, and flight qualified for the now canceled MSP (Mars Surveyor Program) '01 Lander. The MECA package consisted of a microscope, electrometer, material patch plates, and a wet chemistry laboratory (WCL). The primary goal of MECA was to analyze the Martian soil (regolith) for possible hazards to future astronauts and to provide a better understanding of Martian regolith geochemistry. The purpose of the WCL was to analyze for a range of soluble ionic chemical species and electrochemical parameters. The heart of the WCL was a sensor array of electrochemically based ion-selective electrodes (ISE). After 20 months storage at -23 degrees C and subsequent extended freeze/thawing cycles, WCL sensors were evaluated to determine both their physical durability and analytical responses. A fractional factorial calibration of the sensors was used to obtain slope, intercept, and all necessary selectivity coefficients simultaneously for selected ISEs. This calibration was used to model five cation and three anion sensors. These data were subsequently used to determine concentrations of several ions in two soil leachate simulants (based on terrestrial seawater and hypothesized Mars brine) and four actual soil samples. The WCL results were compared to simulant and soil samples using ion chromatography and inductively coupled plasma optical emission spectroscopy. The results showed that flight qualification and prolonged low-temperature storage conditions had minimal effects on the sensors. In addition, the analytical optimization method provided quantitative and qualitative data that could be used to accurately identify the chemical composition of the simulants and soils. The WCL has the ability to provide data that can be used to "read" the chemical, geological, and climatic history of Mars, as well as the potential habitability of its regolith.

Study and optimisation of SIMS performed with He+ and Ne+ bombardment

NASA Astrophysics Data System (ADS)

Pillatsch, L.; Vanhove, N.; Dowsett, D.; Sijbrandij, S.; Notte, J.; Wirtz, T.

2013-10-01

The combination of the high-brightness He+/Ne+ atomic level ion source with the detection capabilities of secondary ion mass spectrometry (SIMS) opens up the prospect of obtaining chemical information with high lateral resolution and high sensitivity on the Zeiss ORION helium ion microscope (HIM). A feasibility study with He+ and Ne+ ion bombardment is presented in order to determine the performance of SIMS analyses using the HIM. Therefore, the sputtering yields, useful yields and detection limits obtained for metallic (Al, Ni and W) as well as semiconductor samples (Si, Ge, GaAs and InP) were investigated. All the experiments were performed on a Cameca IMS4f SIMS instrument which was equipped with a caesium evaporator and oxygen flooding system. For most of the elements, useful yields in the range of 10-4 to 3 × 10-2 were measured with either O2 or Cs flooding. SIMS experiments performed directly on the ORION with a prototype secondary ion extraction and detection system lead to results that are consistent with those obtained on the IMS4f. Taking into account the obtained useful yields and the analytical conditions, such as the ion current and typical dwell time on the ORION HIM, detection limits in the at% range and better can be obtained during SIMS imaging at 10 nm lateral resolution with Ne+ bombardment and down to the ppm level when a lateral resolution of 100 nm is chosen. Performing SIMS on the HIM with a good detection limit while maintaining an excellent lateral resolution (<50 nm) is therefore very promising.

Effects of bulk viscosity and hadronic rescattering in heavy ion collisions at energies available at the BNL Relativistic Heavy Ion Collider and at the CERN Large Hadron Collider

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ryu, Sangwook; Paquet, Jean-Francois; Shen, Chun

Here, we describe ultrarelativistic heavy ion collisions at the BNL Relativistic Heavy Ion Collider and the CERN Large Hadron Collider with a hybrid model using the IP-Glasma model for the earliest stage and viscous hydrodynamics and microscopic transport for the later stages of the collision. We demonstrate that within this framework the bulk viscosity of the plasma plays an important role in describing the experimentally observed radial flow and azimuthal anisotropy simultaneously. Finally, we further investigate the dependence of observables on the temperature below which we employ the microscopic transport description.

Effects of bulk viscosity and hadronic rescattering in heavy ion collisions at energies available at the BNL Relativistic Heavy Ion Collider and at the CERN Large Hadron Collider

DOE PAGES

Ryu, Sangwook; Paquet, Jean-Francois; Shen, Chun; ...

2018-03-15

Here, we describe ultrarelativistic heavy ion collisions at the BNL Relativistic Heavy Ion Collider and the CERN Large Hadron Collider with a hybrid model using the IP-Glasma model for the earliest stage and viscous hydrodynamics and microscopic transport for the later stages of the collision. We demonstrate that within this framework the bulk viscosity of the plasma plays an important role in describing the experimentally observed radial flow and azimuthal anisotropy simultaneously. Finally, we further investigate the dependence of observables on the temperature below which we employ the microscopic transport description.

Characterization of Meteorites by Focused Ion Beam Sectioning: Recent Applications to CAIs and Primitive Meteorite Matrices

NASA Technical Reports Server (NTRS)

Christoffersen, Roy; Keller, Lindsay P.; Han, Jangmi; Rahman, Zia; Berger, Eve L.

2015-01-01

Focused ion beam (FIB) sectioning has revolutionized preparation of meteorite samples for characterization by analytical transmission electron microscopy (TEM) and other techniques. Although FIB is not "non-destructive" in the purest sense, each extracted section amounts to no more than nanograms (approximately 500 cubic microns) removed intact from locations precisely controlled by SEM imaging and analysis. Physical alteration of surrounding material by ion damage, fracture or sputter contamination effects is localized to within a few micrometers around the lift-out point. This leaves adjacent material intact for coordinate geochemical analysis by SIMS, microdrill extraction/TIMS and other techniques. After lift out, FIB sections can be quantitatively analyzed by electron microprobe prior to final thinning, synchrotron x-ray techniques, and by the full range of state-of-the-art analytical field-emission scanning transmission electron microscope (FE-STEM) techniques once thinning is complete. Multiple meteorite studies supported by FIB/FE-STEM are currently underway at NASA-JSC, including coordinated analysis of refractory phase assemblages in CAIs and fine-grained matrices in carbonaceous chondrites. FIB sectioning of CAIs has uncovered epitaxial and other overgrowth relations between corundum-hibonite-spinel consistent with hibonite preceding corundum and/or spinel in non-equilibrium condensation sequences at combinations of higher gas pressures, dust-gas enrichments or significant nebular transport. For all of these cases, the ability of FIB to allow for coordination with spatially-associated isotopic data by SIMS provides immense value for constraining the formation scenarios of the particular CAI assemblage. For carbonaceous chondrites matrix material, FIB has allowed us to obtain intact continuous sections of the immediate outer surface of Murchison (CM2) after it has been experimentally ion processed to simulate solar wind space weathering. The surface amorphization and loss of OH produced by the irradiation provides important clues regarding space weathering on primitive asteroids such as the OSIRIS-Rex target 101955 Bennu.

Experimental Investigation of Space Radiation Processing in Lunar Soil Ilmenite: Combining Perspectives from Surface Science and Transmission Electron Microscopy

NASA Technical Reports Server (NTRS)

Christoffersen, R.; Keller, L. P.; Rahman, Z.; Baragiola, R.

2010-01-01

Energetic ions mostly from the solar wind play a major role in lunar space weathering because they contribute structural and chemical changes to the space-exposed surfaces of lunar regolith grains. In mature mare soils, ilmenite (FeTiO3) grains in the finest size fraction have been shown in transmission electron microscope (TEM) studies to exhibit key differences in their response to space radiation processing relative to silicates [1,2,3]. In ilmenite, solar ion radiation alters host grain outer margins to produce 10-100 nm thick layers that are microstructurally complex, but dominantly crystalline compared to the amorphous radiation-processed rims on silicates [1,2,3]. Spatially well-resolved analytical TEM measurements also show nm-scale compositional and chemical state changes in these layers [1,3]. These include shifts in Fe/Ti ratio from strong surface Fe-enrichment (Fe/Ti >> 1), to Fe depletion (Fe/Ti < 1) at 40-50 nm below the grain surface [1,3]. These compositional changes are not observed in the radiation-processed rims on silicates [4]. Several mechanism(s) to explain the overall relations in the ilmenite grain rims by radiation processing and/or additional space weathering processes were proposed by [1], and remain under current consideration [3]. A key issue has concerned the ability of ion radiation processing alone to produce some of the deeper- penetrating compositional changes. In order to provide some experimental constraints on these questions, we have performed a combined X-ray photoelectron spectroscopy (XPS) and field-emission scanning transmission electron (FE-STEM) study of experimentally ion-irradiated ilmenite. A key feature of this work is the combination of analytical techniques sensitive to changes in the irradiated samples at depth scales going from the immediate surface (approx.5 nm; XPS), to deeper in the grain interior (5-100 nm; FE-STEM).

Extending the Dynamic Range of the Ion Trap by Differential Mobility Filtration

PubMed Central

Hall, Adam B.; Coy, Stephen L.; Kafle, Amol; Glick, James; Nazarov, Erkinjon

2013-01-01

A miniature, planar, differential ion mobility spectrometer (DMS) was interfaced to an LCQ classic ion trap to conduct selective ion filtration prior to mass analysis in order to extend the dynamic range of the trap. Space charge effects are known to limit the functional ion storage capacity of ion trap mass analyzers and this, in turn, can affect the quality of the mass spectral data generated. This problem is further exacerbated in the analysis of mixtures where the indiscriminate introduction of matrix ions results in premature trap saturation with non-targeted species, thereby reducing the number of parent ions that may be used to conduct MS/MS experiments for quantitation or other diagnostic studies. We show that conducting differential mobility-based separations prior to mass analysis allows the isolation of targeted analytes from electrosprayed mixtures preventing the indiscriminate introduction of matrix ions and premature trap saturation with analytically unrelated species. Coupling these two analytical techniques is shown to enhance the detection of a targeted drug metabolite from a biological matrix. In its capacity as a selective ion filter, the DMS can improve the analytical performance of analyzers such as quadrupole (3-D or linear) and ion cyclotron resonance (FT-ICR) ion traps that depend on ion accumulation. PMID:23797861

Development of Functional Surfaces on High-Density Polyethylene (HDPE) via Gas-Assisted Etching (GAE) Using Focused Ion Beams.

PubMed

Sezen, Meltem; Bakan, Feray

2015-12-01

Irradiation damage, caused by the use of beams in electron and ion microscopes, leads to undesired physical/chemical material property changes or uncontrollable modification of structures. Particularly, soft matter such as polymers or biological materials is highly susceptible and very much prone to react on electron/ion beam irradiation. Nevertheless, it is possible to turn degradation-dependent physical/chemical changes from negative to positive use when materials are intentionally exposed to beams. Especially, controllable surface modification allows tuning of surface properties for targeted purposes and thus provides the use of ultimate materials and their systems at the micro/nanoscale for creating functional surfaces. In this work, XeF2 and I2 gases were used in the focused ion beam scanning electron microscope instrument in combination with gallium ion etching of high-density polyethylene surfaces with different beam currents and accordingly different gas exposure times resulting at the same ion dose to optimize and develop new polymer surface properties and to create functional polymer surfaces. Alterations in the surface morphologies and surface chemistry due to gas-assisted etching-based nanostructuring with various processing parameters were tracked using high-resolution SEM imaging, complementary energy-dispersive spectroscopic analyses, and atomic force microscopic investigations.

Helium Ion Secondary Electron Mode Microscopy For Interconnect Material Imaging

NASA Astrophysics Data System (ADS)

Ogawa, Shinichi; Thompson, William; Stern, Lewis; Scipioni, Larry; Notte, John; Farkas, Lou; Barriss, Louise

2010-04-01

The recently developed helium ion microscope (HIM) is now capable of 0.35 nm secondary electron (SE) mode image resolution. When low-k dielectrics or copper interconnects in ultra large scale integrated circuits (ULSI) interconnect structures were imaged in this mode, it was found that unique pattern dimension and fidelity information at sub-nanometer resolution was available for the first time. This paper will discuss the helium ion microscope architecture and the SE imaging techniques that make the HIM observation method of particular value to the low-k dielectric and dual damascene copper interconnect technologies.

Ionization Capabilities of Hydronium Ions and High Electric Fields Produced by Atmospheric Pressure Corona Discharge.

PubMed

Sato, Natsuhiko; Sekimoto, Kanako; Takayama, Mitsuo

2016-01-01

Atmospheric pressure corona discharge (APCD) was applied to the ionization of volatile organic compounds. The mass spectra of analytes having aromatic, phenolic, anilinic, basic and aliphatic in nature were obtained by using vapor supply and liquid smear supply methods. The vapor supply method mainly gave protonated analytes [A+H] + caused by proton transfer from hydronium ion H 3 O + , except for benzene, toluene and n -hexane that have lower proton affinity. The use of the liquid smear supply method resulted in the formation of molecular ion A ·+ and/or dehydride analyte [A-H] + , according to the nature of analytes used. The formation of A ·+ without fragment ions could be explained by the electron tunneling via high electric fields 10 8  V/m at the tip of the corona needle. The dehydride analytes [A-H] + observed in the mass spectra of n -hexane, di- and tributylamines may be explained by the hydride abstraction from the alkyl chains by the hydronium ion. The hydronium ion can play the two-roles for analytes, i.e. , the proton donor to form [A+H] + and the hydride acceptor to form [A-H] + .

Ionization Capabilities of Hydronium Ions and High Electric Fields Produced by Atmospheric Pressure Corona Discharge

PubMed Central

Sato, Natsuhiko; Sekimoto, Kanako; Takayama, Mitsuo

2016-01-01

Atmospheric pressure corona discharge (APCD) was applied to the ionization of volatile organic compounds. The mass spectra of analytes having aromatic, phenolic, anilinic, basic and aliphatic in nature were obtained by using vapor supply and liquid smear supply methods. The vapor supply method mainly gave protonated analytes [A+H]+ caused by proton transfer from hydronium ion H3O+, except for benzene, toluene and n-hexane that have lower proton affinity. The use of the liquid smear supply method resulted in the formation of molecular ion A·+ and/or dehydride analyte [A−H]+, according to the nature of analytes used. The formation of A·+ without fragment ions could be explained by the electron tunneling via high electric fields 108 V/m at the tip of the corona needle. The dehydride analytes [A−H]+ observed in the mass spectra of n-hexane, di- and tributylamines may be explained by the hydride abstraction from the alkyl chains by the hydronium ion. The hydronium ion can play the two-roles for analytes, i.e., the proton donor to form [A+H]+ and the hydride acceptor to form [A−H]+. PMID:28616372

Surface topographical and structural analysis of Ag+-implanted polymethylmethacrylate

NASA Astrophysics Data System (ADS)

Arif, Shafaq; Rafique, M. Shahid; Saleemi, Farhat; Naab, Fabian; Toader, Ovidiu; Sagheer, Riffat; Bashir, Shazia; Zia, Rehana; Siraj, Khurram; Iqbal, Saman

2016-08-01

Specimens of polymethylmethacrylate (PMMA) were implanted with 400-keV Ag+ ions at different ion fluences ranging from 1 × 1014 to 5 × 1015 ions/cm2 using a 400-kV NEC ion implanter. The surface topographical features of the implanted PMMA were investigated by a confocal microscope. Modifications in the structural properties of the implanted specimens were analyzed in comparison with pristine PMMA by X-ray diffraction (XRD) and Raman spectroscopy. UV-Visible spectroscopy was applied to determine the effects of ion implantation on optical transmittance of the implanted PMMA. The confocal microscopic images revealed the formation of hillock-like microstructures along the ion track on the implanted PMMA surface. The increase in ion fluence led to more nucleation of hillocks. The XRD pattern confirmed the amorphous nature of pristine and implanted PMMA, while the Raman studies justified the transformation of Ag+-implanted PMMA into amorphous carbon at the ion fluence of ⩾5 × 1014 ions/cm2. Moreover, the decrease in optical transmittance of PMMA is associated with the formation of hillocks and ion-induced structural modifications after implantation.

Comparison of reactant and analyte ions for ⁶³Nickel, corona discharge, and secondary electrospray ionization sources with ion mobility-mass spectrometry.

PubMed

Crawford, C L; Hill, H H

2013-03-30

(63)Nickel radioactive ionization ((63)Ni) is the most common and widely used ion source for ion mobility spectrometry (IMS). Regulatory, financial, and operational concerns with this source have promoted recent development of non-radioactive sources, such as corona discharge ionization (CD), for stand-alone IMS systems. However, there has been no comparison of the negative ion species produced by all three sources in the literature. This study compares the negative reactant and analyte ions produced by three sources on an ion mobility-mass spectrometer: conventional (63)Ni, CD, and secondary electrospray ionization (SESI). Results showed that (63)Ni and SESI produced the same reactant ion species while CD produced only the nitrate monomer and dimer ions. The analyte ions produced by each ion source were the same except for the CD source which produced a different ion species for the explosive RDX than either the (63)Ni or SESI source. Accurate and reproducible reduced mobility (K0) values, including several values reported here for the first time, were found for each explosive with each ion source. Overall, the SESI source most closely reproduced the reactant ion species and analyte ion species profiles for (63)Ni. This source may serve as a non-radioactive, robust, and flexible alternative for (63)Ni. Copyright © 2013 Elsevier B.V. All rights reserved.

In-Situ atomic force microscopic observation of ion beam bombarded plant cell envelopes

NASA Astrophysics Data System (ADS)

Sangyuenyongpipat, S.; Yu, L. D.; Brown, I. G.; Seprom, C.; Vilaithong, T.

2007-04-01

A program in ion beam bioengineering has been established at Chiang Mai University (CMU), Thailand, and ion beam induced transfer of plasmid DNA molecules into bacterial cells (Escherichia coli) has been demonstrated. However, a good understanding of the fundamental physical processes involved is lacking. In parallel work, onion skin cells have been bombarded with Ar+ ions at energy 25 keV and fluence1-2 × 1015 ions/cm2, revealing the formation of microcrater-like structures on the cell wall that could serve as channels for the transfer of large macromolecules into the cell interior. An in-situ atomic force microscope (AFM) system has been designed and installed in the CMU bio-implantation facility as a tool for the observation of these microcraters during ion beam bombardment. Here we describe some of the features of the in-situ AFM and outline some of the related work.

Effect of cobalt doping on the phase transformation of TiO2 nanoparticles.

PubMed

Barakat, M A; Hayes, G; Shah, S Ismat

2005-05-01

Co-doped TiO2 nanoparticles containing 0.0085, 0.017, 0.0255, 0.034, and 0.085 mol % Co(III) ion dopant were synthesized via sol-gel and dip-coating techniques. The effects of metal ion doping on the transformation of anatase to the rutile phase have been investigated. Several analytical tools, such as X-ray diffraction (XRD), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), and energy dispersive X-ray analysis (EDAX) were used to investigate the nanoparticle structure, size distribution, and composition. Results obtained revealed that the rutile to anatase concentration ratio increases with increase of the cobalt dopant concentration and annealing temperature. The typical composition of Co-doped TiO2 was Ti(1-x)Co(x)O2, where x values ranged from 0.0085 to 0.085. The activation energy for the phase transformation from anatase to rutile was measured to be 229, 222, 211, and 195 kJ/mole for 0.0085, 0.017, 0.0255, and 0.034 mol % Co in TiO2, respectively.

Improvement in ionization efficiency of direct analysis in real time-mass spectrometry (DART-MS) by corona discharge.

PubMed

Sekimoto, Kanako; Sakakura, Motoshi; Kawamukai, Takatomo; Hike, Hiroshi; Shiota, Teruhisa; Usui, Fumihiko; Bando, Yasuhiko; Takayama, Mitsuo

2016-08-02

Herein it is shown that a combination of direct analysis in real time (DART) with a corona discharge system consisting of only a needle electrode easily improves DART ionization efficiency. Positive and negative DC corona discharges led to a formation of abundant excited helium atoms as well as the reactant ions H3O(+)(H2O)n and O2˙(-) in the DART analyte ionization area. These phenomena resulted in an increase in the absolute intensities of (de)protonated analytes by a factor of 2-20 over conventional DART. The other analyte ions detected in this corona-DART system (i.e., molecular ions, fragment ions, oxygenated (de)protonated analytes, dehydrogenated deprotonated analytes, and negative ion adducts) were quite similar to those obtained from DART alone. This indicates a lack of side reactions due to the corona discharge. The change in the relative intensities of individual analyte-related ions due to the combination of a corona discharge system with DART suggests that there is no effect of the abundant excited helium in the analyte ionization area on the fragmentation processes or enhancement of oxidation due to hydroxyl radicals HO˙. Furthermore, it was found that the corona-DART combination can be applied to the highly sensitive analysis of n-alkanes, in which the alkanes are ionized as positive ions via hydride abstraction and oxidation, independent of the type of alkane or the mass spectrometer used.

Applications of the Analytical Electron Microscope to Materials Science

NASA Technical Reports Server (NTRS)

Goldstein, J. I.

1992-01-01

In the last 20 years, the analytical electron microscope (AEM) as allowed investigators to obtain chemical and structural information from less than 50 nanometer diameter regions in thin samples of materials and to explore problems where reactions occur at boundaries and interfaces or within small particles or phases in bulk samples. Examples of the application of the AEM to materials science problems are presented in this paper and demonstrate the usefulness and the future potential of this instrument.

Simulation of a model nanopore sensor: Ion competition underlies device behavior.

PubMed

Mádai, Eszter; Valiskó, Mónika; Dallos, András; Boda, Dezső

2017-12-28

We study a model nanopore sensor with which a very low concentration of analyte molecules can be detected on the basis of the selective binding of the analyte molecules to the binding sites on the pore wall. The bound analyte ions partially replace the current-carrier cations in a thermodynamic competition. This competition depends both on the properties of the nanopore and the concentrations of the competing ions (through their chemical potentials). The output signal given by the device is the current reduction caused by the presence of the analyte ions. The concentration of the analyte ions can be determined through calibration curves. We model the binding site with the square-well potential and the electrolyte as charged hard spheres in an implicit background solvent. We study the system with a hybrid method in which we compute the ion flux with the Nernst-Planck (NP) equation coupled with the Local Equilibrium Monte Carlo (LEMC) simulation technique. The resulting NP+LEMC method is able to handle both strong ionic correlations inside the pore (including finite size of ions) and bulk concentrations as low as micromolar. We analyze the effect of bulk ion concentrations, pore parameters, binding site parameters, electrolyte properties, and voltage on the behavior of the device.

Simulation of a model nanopore sensor: Ion competition underlies device behavior

NASA Astrophysics Data System (ADS)

Mádai, Eszter; Valiskó, Mónika; Dallos, András; Boda, Dezső

2017-12-01

We study a model nanopore sensor with which a very low concentration of analyte molecules can be detected on the basis of the selective binding of the analyte molecules to the binding sites on the pore wall. The bound analyte ions partially replace the current-carrier cations in a thermodynamic competition. This competition depends both on the properties of the nanopore and the concentrations of the competing ions (through their chemical potentials). The output signal given by the device is the current reduction caused by the presence of the analyte ions. The concentration of the analyte ions can be determined through calibration curves. We model the binding site with the square-well potential and the electrolyte as charged hard spheres in an implicit background solvent. We study the system with a hybrid method in which we compute the ion flux with the Nernst-Planck (NP) equation coupled with the Local Equilibrium Monte Carlo (LEMC) simulation technique. The resulting NP+LEMC method is able to handle both strong ionic correlations inside the pore (including finite size of ions) and bulk concentrations as low as micromolar. We analyze the effect of bulk ion concentrations, pore parameters, binding site parameters, electrolyte properties, and voltage on the behavior of the device.

Anomalies in the equilibrium and nonequilibrium properties of correlated ions in complex molecular environments

NASA Astrophysics Data System (ADS)

Mahakrishnan, Sathiya; Chakraborty, Subrata; Vijay, Amrendra

2017-11-01

Emergent statistical attributes, and therefore the equations of state, of an assembly of interacting charge carriers embedded within a complex molecular environment frequently exhibit a variety of anomalies, particularly in the high-density (equivalently, the concentration) regime, which are not well understood, because they do not fall under the low-concentration phenomenologies of Debye-Hückel-Onsager and Poisson-Nernst-Planck, including their variants. To go beyond, we here use physical concepts and mathematical tools from quantum scattering theory, transport theory with the Stosszahlansatz of Boltzmann, and classical electrodynamics (Lorentz gauge) and obtain analytical expressions both for the average and the frequency-wave vector-dependent longitudinal and transverse current densities, diffusion coefficient, and the charge density, and therefore the analytical expressions for (a) the chemical potential, activity coefficient, and the equivalent conductivity for strong electrolytes and (b) the current-voltage characteristics for ion-transport processes in complex molecular environments. Using a method analogous to the notion of Debye length and thence the electrical double layer, we here identify a pair of characteristic length scales (longitudinal and the transverse), which, being wave vector and frequency dependent, manifestly exhibit nontrivial fluctuations in space-time. As a unifying theme, we advance a quantity (inverse length dimension), gscat(a ), which embodies all dynamical interactions, through various quantum scattering lengths, relevant to molecular species a, and the analytical behavior which helps us to rationalize the properties of strong electrolytes, including anomalies, in all concentration regimes. As an example, the behavior of gscat(a ) in the high-concentration regime explains the anomalous increase of the Debye length with concentration, as seen in a recent experiment on electrolyte solutions. We also put forth an extension of the standard diffusion equation, which manifestly incorporates the effects arising from the underlying microscopic collisions among constituent molecular species. Furthermore, we show a nontrivial connection between the current-voltage characteristics of electrolyte solutions and the Landauer's approach to electrical conduction in mesoscopic solids and thereby establish a definite conceptual bridge between the two disjoint subjects. For numerical insight, we present results on the aqueous solution of KCl as an example of strong electrolyte, and the transport (conduction as well as diffusion) of K+ ions in water, as an example of ion transport across the voltage-gated channels in biological cells.

Anomalies in the equilibrium and nonequilibrium properties of correlated ions in complex molecular environments.

PubMed

Mahakrishnan, Sathiya; Chakraborty, Subrata; Vijay, Amrendra

2017-11-01

Emergent statistical attributes, and therefore the equations of state, of an assembly of interacting charge carriers embedded within a complex molecular environment frequently exhibit a variety of anomalies, particularly in the high-density (equivalently, the concentration) regime, which are not well understood, because they do not fall under the low-concentration phenomenologies of Debye-Hückel-Onsager and Poisson-Nernst-Planck, including their variants. To go beyond, we here use physical concepts and mathematical tools from quantum scattering theory, transport theory with the Stosszahlansatz of Boltzmann, and classical electrodynamics (Lorentz gauge) and obtain analytical expressions both for the average and the frequency-wave vector-dependent longitudinal and transverse current densities, diffusion coefficient, and the charge density, and therefore the analytical expressions for (a) the chemical potential, activity coefficient, and the equivalent conductivity for strong electrolytes and (b) the current-voltage characteristics for ion-transport processes in complex molecular environments. Using a method analogous to the notion of Debye length and thence the electrical double layer, we here identify a pair of characteristic length scales (longitudinal and the transverse), which, being wave vector and frequency dependent, manifestly exhibit nontrivial fluctuations in space-time. As a unifying theme, we advance a quantity (inverse length dimension), g_{scat}^{(a)}, which embodies all dynamical interactions, through various quantum scattering lengths, relevant to molecular species a, and the analytical behavior which helps us to rationalize the properties of strong electrolytes, including anomalies, in all concentration regimes. As an example, the behavior of g_{scat}^{(a)} in the high-concentration regime explains the anomalous increase of the Debye length with concentration, as seen in a recent experiment on electrolyte solutions. We also put forth an extension of the standard diffusion equation, which manifestly incorporates the effects arising from the underlying microscopic collisions among constituent molecular species. Furthermore, we show a nontrivial connection between the current-voltage characteristics of electrolyte solutions and the Landauer's approach to electrical conduction in mesoscopic solids and thereby establish a definite conceptual bridge between the two disjoint subjects. For numerical insight, we present results on the aqueous solution of KCl as an example of strong electrolyte, and the transport (conduction as well as diffusion) of K^{+} ions in water, as an example of ion transport across the voltage-gated channels in biological cells.

Nanopatterning of optical surfaces during low-energy ion beam sputtering

NASA Astrophysics Data System (ADS)

Liao, Wenlin; Dai, Yifan; Xie, Xuhui

2014-06-01

Ion beam figuring (IBF) provides a highly deterministic method for high-precision optical surface fabrication, whereas ion-induced microscopic morphology evolution would occur on surfaces. Consequently, the fabrication specification for surface smoothness must be seriously considered during the IBF process. In this work, low-energy ion nanopatterning of our frequently used optical material surfaces is investigated to discuss the manufacturability of an ultrasmooth surface. The research results indicate that ion beam sputtering (IBS) can directly smooth some amorphous or amorphizable material surfaces, such as fused silica, Si, and ULE under appropriate processing conditions. However, for IBS of a Zerodur surface, preferential sputtering together with curvature-dependent sputtering overcome ion-induced smoothing mechanisms, leading to the granular nanopatterns' formation and the coarsening of the surface. Furthermore, the material property difference at microscopic scales and the continuous impurity incorporation would affect the ion beam smoothing of optical surfaces. Overall, IBS can be used as a promising technique for ultrasmooth surface fabrication, which strongly depends on processing conditions and material characters.

Biosynthesised ZnO : Dy3+ nanoparticles: Biodiesel properties and reusable catalyst for N-formylation of aromatic amines with formic acid

NASA Astrophysics Data System (ADS)

Reddy Yadav, L. S.; Raghavendra, M.; Sudheer Kumar, K. H.; Dhananjaya, N.; Nagaraju, G.

2018-04-01

ZnO nanoparticles doped with trivalent dysprosium ions (Dy3+) were prepared through the green combustion technique using E. tirucalli plant latex as a fuel. The fundamental and optical properties of the samples are examined via the X-ray diffraction, FTIR, UV-visible analytical methods and morphology by scanning electron microscope and transmission electron microscope. Rietveld refinement results show that the ZnO : Dy3+ were crystallized in the wurtzite hexagonal structure with space group P63mc (No. 186). The average particle size of ZnO : Dy3+ prepared with the different concentration of latex was found to be in the range 30-38nm, which is also confirmed by TEM analysis. A rapid and convenient method for the one-pot preparation of N-formamide derivatives aromatic amines and amino acid esters has been developed using Dy3+ doped ZnO as a catalytic agent. This method provides an efficient and much improved modification over reported protocols regarding yield, clean and work-up procedure milder reaction conditions. In this work, Pongamiapinnata oil was recycled for the preparation of biodiesel via Dy3+ doped ZnO as a catalytic agent.

Method for selective detection of explosives in mass spectrometer or ion mobility spectrometer at parts-per-quadrillion level

DOEpatents

Ewing, Robert G.; Atkinson, David A.; Clowers, Brian H.

2015-09-01

A method for selective detection of volatile and non-volatile explosives in a mass spectrometer or ion mobility spectrometer at a parts-per-quadrillion level without preconcentration is disclosed. The method comprises the steps of ionizing a carrier gas with an ionization source to form reactant ions or reactant adduct ions comprising nitrate ions (NO.sub.3.sup.-); selectively reacting the reactant ions or reactant adduct ions with at least one volatile or non-volatile explosive analyte at a carrier gas pressure of at least about 100 Ton in a reaction region disposed between the ionization source and an ion detector, the reaction region having a length which provides a residence time (tr) for reactant ions therein of at least about 0.10 seconds, wherein the selective reaction yields product ions comprising reactant ions or reactant adduct ions that are selectively bound to the at least one explosive analyte when present therein; and detecting product ions with the ion detector to determine presence or absence of the at least one explosive analyte.

Analytical electron microscopic studies and positron lifetime measurements in Al-doped MgO crystals

NASA Astrophysics Data System (ADS)

Pedrosa, M. A.; Pareja, R.; González, R.; Abraham, M. M.

1987-07-01

MgO crystals intentionally doped with Al were characterized by analytical electron microscopic examinations and positron lifetime measurements. Large spinel (MgO Al2O3) precipitates were observed in samples with high contents of Al. A well-defined crystallographic relationship between the precipitates and the matrix was found. The characteristics of positron lifetime spectra appear to depend on the valence state of the different impurities in the MgO lattice suggesting that positrons are trapped by vacancy impurity complexes.

Sampling probe for microarray read out using electrospray mass spectrometry

DOEpatents

Van Berkel, Gary J.

2004-10-12

An automated electrospray based sampling system and method for analysis obtains samples from surface array spots having analytes. The system includes at least one probe, the probe including an inlet for flowing at least one eluting solvent to respective ones of a plurality of spots and an outlet for directing the analyte away from the spots. An automatic positioning system is provided for translating the probe relative to the spots to permit sampling of any spot. An electrospray ion source having an input fluidicly connected to the probe receives the analyte and generates ions from the analyte. The ion source provides the generated ions to a structure for analysis to identify the analyte, preferably being a mass spectrometer. The probe can be a surface contact probe, where the probe forms an enclosing seal along the periphery of the array spot surface.

Compelling evidence for Lucky Survivor and gas phase protonation: the unified MALDI analyte protonation mechanism.

PubMed

Jaskolla, Thorsten W; Karas, Michael

2011-06-01

This work experimentally verifies and proves the two long since postulated matrix-assisted laser desorption/ionization (MALDI) analyte protonation pathways known as the Lucky Survivor and the gas phase protonation model. Experimental differentiation between the predicted mechanisms becomes possible by the use of deuterated matrix esters as MALDI matrices, which are stable under typical sample preparation conditions and generate deuteronated reagent ions, including the deuterated and deuteronated free matrix acid, only upon laser irradiation in the MALDI process. While the generation of deuteronated analyte ions proves the gas phase protonation model, the detection of protonated analytes by application of deuterated matrix compounds without acidic hydrogens proves the survival of analytes precharged from solution in accordance with the predictions from the Lucky Survivor model. The observed ratio of the two analyte ionization processes depends on the applied experimental parameters as well as the nature of analyte and matrix. Increasing laser fluences and lower matrix proton affinities favor gas phase protonation, whereas more quantitative analyte protonation in solution and intramolecular ion stabilization leads to more Lucky Survivors. The presented results allow for a deeper understanding of the fundamental processes causing analyte ionization in MALDI and may alleviate future efforts for increasing the analyte ion yield.

Sensitive glow discharge ion source for aerosol and gas analysis

DOEpatents

Reilly, Peter T. A. [Knoxville, TN

2007-08-14

A high sensitivity glow discharge ion source system for analyzing particles includes an aerodynamic lens having a plurality of constrictions for receiving an aerosol including at least one analyte particle in a carrier gas and focusing the analyte particles into a collimated particle beam. A separator separates the carrier gas from the analyte particle beam, wherein the analyte particle beam or vapors derived from the analyte particle beam are selectively transmitted out of from the separator. A glow discharge ionization source includes a discharge chamber having an entrance orifice for receiving the analyte particle beam or analyte vapors, and a target electrode and discharge electrode therein. An electric field applied between the target electrode and discharge electrode generates an analyte ion stream from the analyte vapors, which is directed out of the discharge chamber through an exit orifice, such as to a mass spectrometer. High analyte sensitivity is obtained by pumping the discharge chamber exclusively through the exit orifice and the entrance orifice.

Reaction chemistry and collisional processes in multiple devices for resolving isobaric interferences in ICP-MS.

PubMed

Bandura, D R; Baranov, V I; Tanner, S D

2001-07-01

A low-level review of the fundamentals of ion-molecule interactions is presented. These interactions are used to predict the efficiencies of collisional fragmentation, energy damping and reaction for a variety of neutral gases as a function of pressure in a rf-driven collision/reaction cell. It is shown that the number of collisions increases dramatically when the ion energies are reduced to near-thermal (< 0.1 eV), because of the ion-induced dipole and ion-dipole interaction. These considerations suggest that chemical reaction can be orders of magnitude more efficient at improving the analyte signal/background ratio than can collisional fragmentation. Considerations that lead to an appropriate selection of type of gas, operating pressure, and ion energies for efficient operation of the cell for the alleviation of spectral interferences are discussed. High efficiency (large differences between reaction efficiencies of the analyte and interference ions, and concomitant suppression of secondary chemistry) might be required to optimize the chemical resolution (determination of an analyte in the presence of an isobaric interference) when using ion-molecule chemistry to suppress the interfering ion. In many instances atom transfer to the analyte, which shifts the analytical m/z by the mass of the atom transferred, provides high chemical resolution, even when the efficiency of reaction is relatively low. Examples are given of oxidation, hydroxylation, and chlorination of analyte ions (V+, Fe+, As+, Se+, Sr+, Y+, and Zr+) to improve the capability of determination of complex samples. Preliminary results are given showing O-atom abstraction by CO from CaO+ to enable the determination of Fe in high-Ca samples.

Microchip and wedge ion funnels and planar ion beam analyzers using same

DOEpatents

Shvartsburg, Alexandre A; Anderson, Gordon A; Smith, Richard D

2012-10-30

Electrodynamic ion funnels confine, guide, or focus ions in gases using the Dehmelt potential of oscillatory electric field. New funnel designs operating at or close to atmospheric gas pressure are described. Effective ion focusing at such pressures is enabled by fields of extreme amplitude and frequency, allowed in microscopic gaps that have much higher electrical breakdown thresholds in any gas than the macroscopic gaps of present funnels. The new microscopic-gap funnels are useful for interfacing atmospheric-pressure ionization sources to mass spectrometry (MS) and ion mobility separation (IMS) stages including differential IMS or FAIMS, as well as IMS and MS stages in various configurations. In particular, "wedge" funnels comprising two planar surfaces positioned at an angle and wedge funnel traps derived therefrom can compress ion beams in one dimension, producing narrow belt-shaped beams and laterally elongated cuboid packets. This beam profile reduces the ion density and thus space-charge effects, mitigating the adverse impact thereof on the resolving power, measurement accuracy, and dynamic range of MS and IMS analyzers, while a greater overlap with coplanar light or particle beams can benefit spectroscopic methods.

Low-pressure barrier discharge ion source using air as a carrier gas and its application to the analysis of drugs and explosives.

PubMed

Usmanov, Dilshadbek T; Yu, Zhan; Chen, Lee Chuin; Hiraoka, Kenzo; Yamabe, Shinichi

2016-02-01

In this work, a low-pressure air dielectric-barrier discharge (DBD) ion source using a capillary with the inner diameter of 0.115 and 12 mm long applicable to miniaturized mass spectrometers was developed. The analytes, trinitrotoluene (TNT), 1,3,5-trinitroperhydro-1,3,5-triazine (RDX), 1,3,5,7-tetranitroperhydro-1,3,5,7-tetrazocine (HMX), pentaerythritol tetranitrate (PETN), nitroglycerine (NG), hexamethylene triperoxide diamine (HMTD), caffeine, cocaine and morphine, introduced through the capillary, were ionized by a low-pressure air DBD. The ion source pressures were changed by using various sizes of the ion sampling orifice. The signal intensities of those analytes showed marked pressure dependence. TNT was detected with higher sensitivity at lower pressure but vice versa for other analytes. For all analytes, a marked signal enhancement was observed when a grounded cylindrical mesh electrode was installed in the DBD ion source. Among nine analytes, RDX, HMX, NG and PETN could be detected as cluster ions [analyte + NO3 ](-) even at low pressure and high temperature up to 180 °C. The detection indicates that these cluster ions are stable enough to survive under present experimental conditions. The unexpectedly high stabilities of these cluster ions were verified by density functional theory calculation. Copyright © 2016 John Wiley & Sons, Ltd.

Combined use of optical and electron microscopic techniques for the measurement of hygroscopic property, chemical composition, and morphology of individual aerosol particles.

PubMed

Ahn, Kang-Ho; Kim, Sun-Man; Jung, Hae-Jin; Lee, Mi-Jung; Eom, Hyo-Jin; Maskey, Shila; Ro, Chul-Un

2010-10-01

In this work, an analytical method for the characterization of the hygroscopic property, chemical composition, and morphology of individual aerosol particles is introduced. The method, which is based on the combined use of optical and electron microscopic techniques, is simple and easy to apply. An optical microscopic technique was used to perform the visual observation of the phase transformation and hygroscopic growth of aerosol particles on a single particle level. A quantitative energy-dispersive electron probe X-ray microanalysis, named low-Z particle EPMA, was used to perform a quantitative chemical speciation of the same individual particles after the measurement of the hygroscopic property. To validate the analytical methodology, the hygroscopic properties of artificially generated NaCl, KCl, (NH(4))(2)SO(4), and Na(2)SO(4) aerosol particles of micrometer size were investigated. The practical applicability of the analytical method for studying the hygroscopic property, chemical composition, and morphology of ambient aerosol particles is demonstrated.

Acquisition of a High Resolution Field Emission Scanning Electron Microscope for the Analysis of Returned Samples

NASA Technical Reports Server (NTRS)

Nittler, Larry R.

2003-01-01

This grant furnished funds to purchase a state-of-the-art scanning electron microscope (SEM) to support our analytical facilities for extraterrestrial samples. After evaluating several instruments, we purchased a JEOL 6500F thermal field emission SEM with the following analytical accessories: EDAX energy-dispersive x-ray analysis system with fully automated control of instrument and sample stage; EDAX LEXS wavelength-dispersive x-ray spectrometer for high sensitivity light-element analysis; EDAX/TSL electron backscatter diffraction (EBSD) system with software for phase identification and crystal orientation mapping; Robinson backscatter electron detector; and an in situ micro-manipulator (Kleindiek). The total price was $550,000 (with $150,000 of the purchase supported by Carnegie institution matching funds). The microscope was delivered in October 2002, and most of the analytical accessories were installed by January 2003. With the exception of the wavelength spectrometer (which has been undergoing design changes) everything is working well and the SEM is in routine use in our laboratory.

Radiation damage in dielectric and semiconductor single crystals (direct observation)

NASA Astrophysics Data System (ADS)

Adawi, M. A.; Didyk, A. Yu.; Varichenko, V. S.; Zaitsev, A. M.

1998-11-01

The surfaces of boron-doped synthetic and natural diamonds have been investigated by using the scanning tunnelling microscope (STM) and the scanning electronic microscope (SEM) before and after irradiating the samples with 40Ar (25 MeV), 84Kr (210 MeV) and 125Xe (124 MeV) ions. The structures observed after irradiation showed craters with diameters ranging from 3 nm up to 20 nm, which could be interpreted as single ion tracks and multiple hits of ions at the nearest positions of the surface. In the case of argon ion irradiation, the surface was found to be completely amorphous, but after xenon irradiation one could see parts of surface without amorphism. This can be explained by the influence of high inelastic energy losses. The energy and temperature criteria of crater formation as a result of heavy ion irradiation are introduced.

Fabrication of a trimer/single atom tip for gas field ion sources by means of field evaporation without tip heating.

PubMed

Kim, Kwang-Il; Kim, Young Heon; Ogawa, Takashi; Choi, Suji; Cho, Boklae; Ahn, Sang Jung; Park, In-Yong

2018-05-11

A gas field ion source (GFIS) has many advantages that are suitable for ion microscope sources, such as high brightness and a small virtual source size, among others. In order to apply a tip-based GFIS to an ion microscope, it is better to create a trimer/single atom tip (TSAT), where the ion beam must be generated in several atoms of the tip apex. Here, unlike the conventional method which uses tip heating or a reactive gas, we show that the tip surface can be cleaned using only the field evaporation phenomenon and that the TSAT can also be fabricated using an insulating layer containing tungsten oxide, which remains after electrochemical etching. Using this method, we could get TSAT over 90% of yield. Copyright © 2018. Published by Elsevier B.V.

Modeling secondary electron emission from nanostructured materials in helium ion microscope

NASA Astrophysics Data System (ADS)

Ohya, K.; Yamanaka, T.

2013-11-01

Charging of a SiO2 layer on a Si substrate during helium (He) beam irradiation is investigated at an energy range relevant to a He ion microscope (HIM). A self-consistent calculation is performed to model the transport of the ions and secondary electrons (SEs), the charge accumulation in the layer, and the electric field below and above the surface. The calculated results are compared with those for gallium (Ga) ions at the same energy and 1 keV electrons corresponding to a low-voltage scanning electron microscope (SEM). The charging of thin layers (<250 nm) is strongly suppressed due to wide depth and lateral distributions of the He ions in the layer, the voltage of which is much lower than that for the Ga ions and the electrons, where the distributions are much more localized. When the irradiation approaches the edge of a 100-nm-high SiO2 step formed on a Si substrate, a sharp increase in the number of SEs is observed, irrespective of whether a material is charged or not. When the He ions are incident on the bottom of the step, the re-entrance of SEs emitted from the substrate into the sidewall is clearly observed, but it causes the sidewall to be charged negatively. At the positions on the SiO2 layer away from the step edge, the charging voltage becomes positive with increasing number of Ga ions and electrons. However, He ions do not induce such a voltage due to strong relaxation of positive and negative charges in the Si substrate and their recombination in the SiO2 layer.

Biomedical applications of ion-beam technology

NASA Technical Reports Server (NTRS)

Banks, B. A.; Weigand, A. J.; Gibbons, D. F.; Vankampen, C. L.; Babbush, C. A.

1979-01-01

Microscopically-rough surface texture of various biocompatible alloys and polymers produced by ion-beam sputtering may result in improvements in response of hard or soft tissue to various surgical implants.

External and internal gelation of pectin solutions: microscopic dynamics versus macroscopic rheology

NASA Astrophysics Data System (ADS)

Secchi, E.; Munarin, F.; Alaimo, M. D.; Bosisio, S.; Buzzaccaro, S.; Ciccarella, G.; Vergaro, V.; Petrini, P.; Piazza, R.

2014-11-01

Pectin is a natural biopolymer that forms, in the presence of divalent cations, ionic-bound gels typifying a large class of biological gels stabilized by non-covalent cross-links. We investigate and compare the kinetics of formation and aging of pectin gels obtained either through external gelation via perfusion of free Ca2+ ions, or by internal gelation due to the supply of the same ions from the dissolution of CaCO3 nanoparticles. The microscopic dynamics obtained with photon correlation imaging, a novel optical technique that allows obtaining the microscopic dynamics of the sample while retaining the spatial resolution of imaging techniques, is contrasted with macroscopic rheological measurements at constant strain. Pectin gelation is found to display peculiar two-stage kinetics, highlighted by non-monotonic growth in time of both microscopic correlations and gel mechanical strength. These results are compared to those found for alginate, another biopolymer extensively used in food formulation.

Fabrication of cobalt magnetic nanostructures using atomic force microscope lithography.

PubMed

Chu, Haena; Yun, Seonghun; Lee, Haiwon

2013-12-01

Cobalt nanopatterns are promising assemblies for patterned magnetic storage applications. The fabrication of cobalt magnetic nanostructures on n-tridecylamine x hydrochloride (TDA x HCl) self-assembled monolayer (SAM) modified silicon surfaces using direct writing atomic force microscope (AFM) lithography for localized electrochemical reduction of cobalt ions was demonstrated. The ions were reduced to form metal nanowires along the direction of the electricfield between the AFM tip and the substrate. In this lithography process, TDA x HCI SAMs play an important role in the lithography process for improving the resolution of cobalt nanopatterns by preventing nonspecific reduction of cobalt ions on the unwritten background. Cobalt nanowires and nanodots with width of 225 +/- 26 nm and diameter of 208 +/- 28 nm were successfully fabricated. Platinium-coated polydimethylsiloxane (PDMS) stamp was used fabricating bulk cobalt structures which can be detected by energy dispersive X-ray spectroscopy for element analysis and the physical and magnetic properties of these cobalt nanopatterns were characterized using AFM and magnetic force microscope.

Ion concentration in micro and nanoscale electrospray emitters.

PubMed

Yuill, Elizabeth M; Baker, Lane A

2018-06-01

Solution-phase ion transport during electrospray has been characterized for nanopipettes, or glass capillaries pulled to nanoscale tip dimensions, and micron-sized electrospray ionization emitters. Direct visualization of charged fluorophores during the electrospray process is used to evaluate impacts of emitter size, ionic strength, analyte size, and pressure-driven flow on heterogeneous ion transport during electrospray. Mass spectrometric measurements of positively- and negatively-charged proteins were taken for micron-sized and nanopipette emitters under low ionic strength conditions to further illustrate a discrepancy in solution-driven transport of charged analytes. A fundamental understanding of analyte electromigration during electrospray, which is not always considered, is expected to provide control over selective analyte depletion and enrichment, and can be harnessed for sample cleanup. Graphical abstract Fluorescence micrographs of ion migration in nanoscale pipettes while solution is electrosprayed.

Charge Assisted Laser Desorption/Ionization Mass Spectrometry of Droplets

PubMed Central

Jorabchi, Kaveh; Westphall, Michael S.; Smith, Lloyd M.

2008-01-01

We propose and evaluate a new mechanism to account for analyte ion signal enhancement in ultraviolet-laser desorption mass spectrometry of droplets in the presence of corona ions. Our new insights are based on timing control of corona ion production, laser desorption, and peptide ion extraction achieved by a novel pulsed corona apparatus. We demonstrate that droplet charging rather than gas-phase ion-neutral reactions is the major contributor to analyte ion generation from an electrically isolated droplet. Implications of the new mechanism, termed charge assisted laser desorption/ionization (CALDI), are discussed and contrasted to those of the laser desorption atmospheric pressure chemical ionization method (LD-APCI). It is also demonstrated that analyte ion generation in CALDI occurs with external electric fields about one order of magnitude lower than those needed for atmospheric pressure matrix assisted laser desorption/ionization or electrospray ionization of droplets. PMID:18387311

Measurement of Heavy Ion Irradiation Induced In-Plane Strain in Patterned Face-Centered-Cubic Metal Films: An in Situ Study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yu, K. Y.; Chen, Y.; Li, J.

Nanocrystalline Ag, Cu, and Ni thin films and their coarse grained counterparts are patterned in this paper using focused ion beam and then irradiated by Kr ions within an electron microscope at room temperature. Irradiation induced in-plane strain of the films is measured by tracking the location of nanosized holes. The magnitude of the strain in all specimens is linearly dose-dependent and the strain rates of nanocrystalline metals are significantly greater as compared to that of the coarse grained metals. Finally, real-time microscopic observation suggests that substantial grain boundary migration and grain rotation are responsible for the significant in-plane strain.

Measurement of Heavy Ion Irradiation Induced In-Plane Strain in Patterned Face-Centered-Cubic Metal Films: An in Situ Study

DOE PAGES

Yu, K. Y.; Chen, Y.; Li, J.; ...

2016-11-28

Nanocrystalline Ag, Cu, and Ni thin films and their coarse grained counterparts are patterned in this paper using focused ion beam and then irradiated by Kr ions within an electron microscope at room temperature. Irradiation induced in-plane strain of the films is measured by tracking the location of nanosized holes. The magnitude of the strain in all specimens is linearly dose-dependent and the strain rates of nanocrystalline metals are significantly greater as compared to that of the coarse grained metals. Finally, real-time microscopic observation suggests that substantial grain boundary migration and grain rotation are responsible for the significant in-plane strain.

Commissioning of the PRIOR proton microscope

DOE PAGES

Varentsov, D.; Antonov, O.; Bakhmutova, A.; ...

2016-02-18

Recently, a new high energy proton microscopy facility PRIOR (Proton Microscope for FAIR Facility for Anti-proton and Ion Research) has been designed, constructed, and successfully commissioned at GSI Helmholtzzentrum für Schwerionenforschung (Darmstadt, Germany). As a result of the experiments with 3.5–4.5 GeV proton beams delivered by the heavy ion synchrotron SIS-18 of GSI, 30 μm spatial and 10 ns temporal resolutions of the proton microscope have been demonstrated. A new pulsed power setup for studying properties of matter under extremes has been developed for the dynamic commissioning of the PRIOR facility. This study describes the PRIOR setup as well asmore » the results of the first static and dynamic protonradiography experiments performed at GSI.« less

Commissioning of the PRIOR proton microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Varentsov, D.; Antonov, O.; Bakhmutova, A.

Recently, a new high energy proton microscopy facility PRIOR (Proton Microscope for FAIR Facility for Anti-proton and Ion Research) has been designed, constructed, and successfully commissioned at GSI Helmholtzzentrum für Schwerionenforschung (Darmstadt, Germany). As a result of the experiments with 3.5–4.5 GeV proton beams delivered by the heavy ion synchrotron SIS-18 of GSI, 30 μm spatial and 10 ns temporal resolutions of the proton microscope have been demonstrated. A new pulsed power setup for studying properties of matter under extremes has been developed for the dynamic commissioning of the PRIOR facility. This study describes the PRIOR setup as well asmore » the results of the first static and dynamic protonradiography experiments performed at GSI.« less

Unusual analyte-matrix adduct ions and mechanism of their formation in MALDI TOF MS of benzene-1,3,5-tricarboxamide and urea compounds.

PubMed

Lou, Xianwen; Fransen, Michel; Stals, Patrick J M; Mes, Tristan; Bovee, Ralf; van Dongen, Joost J L; Meijer, E W

2013-09-01

Analyte-matrix adducts are normally absent under typical matrix assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS) conditions. Interestingly, though, in the analysis of several types of organic compounds synthesized in our laboratory, analyte-matrix adduct ion peaks were always recorded when common MALDI matrices such as 4-hydroxy-α-cyanocinnamic acid (CHCA) were used. These compounds are mainly those with a benzene-1,3,5-tricarboxamide (BTA) or urea moiety, which are important building blocks to make new functional supramolecular materials. The possible mechanism of the adduct formation was investigated. A shared feature of the compounds studied is that they can form intermolecular hydrogen bonding with matrices like CHCA. The intermolecular hydrogen bonding will make the association between analyte ions and matrix molecules stronger. As a result, the analyte ions and matrix molecules in MALDI clusters will become more difficult to be separated from each other. Furthermore, it was found that analyte ions were mainly adducted with matrix salts, which is probably due to the much lower volatility of the salts compared with that of their corresponding matrix acids. It seems that the analyte-matrix adduct formation for our compounds are caused by the incomplete evaporation of matrix molecules from the MALDI clusters because of the combined effects of enhanced intermolecular interaction between analyte-matrix and of the low volatility of matrix salts. Based on these findings, strategies to suppress the analyte-matrix adduction are briefly discussed. In return, the positive results of using these strategies support the proposed mechanism of the analyte-matrix adduct formation.

Specimen Holder for Analytical Electron Microscopes

NASA Technical Reports Server (NTRS)

Clanton, U. S.; Isaacs, A. M.; Mackinnon, I.

1985-01-01

Reduces spectral contamination by spurious X-ray. Specimen holder made of compressed carbon, securely retains standard electron microscope grid (disk) 3 mm in diameter and absorbs backscattered electrons that otherwise generate spurious X-rays. Since holder inexpensive, dedicated to single specimen when numerous samples examined.

Formation of Metal-Related Ions in Matrix-Assisted Laser Desorption Ionization.

PubMed

Lee, Chuping; Lu, I-Chung; Hsu, Hsu Chen; Lin, Hou-Yu; Liang, Sheng-Ping; Lee, Yuan-Tseh; Ni, Chi-Kung

2016-09-01

In a study of the metal-related ion generation mechanism in matrix-assisted laser desorption ionization (MALDI), crystals of matrix used in MALDI were grown from matrix- and salt-containing solutions. The intensities of metal ion and metal adducts of the matrix ion obtained from unwashed crystals were higher than those from crystals washed with deionized water, indicating that metal ions and metal adducts of the matrix ions are mainly generated from the surface of crystals. The contributions of preformed metal ions and metal adducts of the matrix ions inside the matrix crystals were minor. Metal adducts of the matrix and analyte ion intensities generated from a mixture of dried matrix, salt, and analyte powders were similar to or higher than those generated from the powder of dried droplet crystals, indicating that the contributions of the preformed metal adducts of the matrix and analyte ions were insignificant. Correlation between metal-related ion intensity fluctuation and protonated ion intensity fluctuation was observed, indicating that the generation mechanism of the metal-related ions is similar to that of the protonated ions. Because the thermally induced proton transfer model effectively describes the generation of the protonated ions, we suggest that metal-related ions are mainly generated from the salt dissolution in the matrix melted by the laser. Graphical Abstract ᅟ.

Performance of bent-crystal x-ray microscopes for high energy density physics research

DOE PAGES

Schollmeier, Marius S.; Geissel, Matthias; Shores, Jonathon E.; ...

2015-05-29

We present calculations for the field of view (FOV), image fluence, image monochromaticity, spectral acceptance, and image aberrations for spherical crystal microscopes, which are used as self-emission imaging or backlighter systems at large-scale high energy density physics facilities. Our analytic results are benchmarked with ray-tracing calculations as well as with experimental measurements from the 6.151 keV backlighter system at Sandia National Laboratories. Furthermore, the analytic expressions can be used for x-ray source positions anywhere between the Rowland circle and object plane. We discovered that this enables quick optimization of the performance of proposed but untested, bent-crystal microscope systems to findmore » the best compromise between FOV, image fluence, and spatial resolution for a particular application.« less

Piezoelectric trace vapor calibrator

NASA Astrophysics Data System (ADS)

Verkouteren, R. Michael; Gillen, Greg; Taylor, David W.

2006-08-01

The design and performance of a vapor generator for calibration and testing of trace chemical sensors are described. The device utilizes piezoelectric ink-jet nozzles to dispense and vaporize precisely known amounts of analyte solutions as monodisperse droplets onto a hot ceramic surface, where the generated vapors are mixed with air before exiting the device. Injected droplets are monitored by microscope with strobed illumination, and the reproducibility of droplet volumes is optimized by adjustment of piezoelectric wave form parameters. Complete vaporization of the droplets occurs only across a 10°C window within the transition boiling regime of the solvent, and the minimum and maximum rates of trace analyte that may be injected and evaporated are determined by thermodynamic principles and empirical observations of droplet formation and stability. By varying solution concentrations, droplet injection rates, air flow, and the number of active nozzles, the system is designed to deliver—on demand—continuous vapor concentrations across more than six orders of magnitude (nominally 290fg/lto1.05μg/l). Vapor pulses containing femtogram to microgram quantities of analyte may also be generated. Calibrated ranges of three explosive vapors at ng/l levels were generated by the device and directly measured by ion mobility spectrometry (IMS). These data demonstrate expected linear trends within the limited working range of the IMS detector and also exhibit subtle nonlinear behavior from the IMS measurement process.

Analytical and numerical treatment of drift-tearing modes in plasma slab

NASA Astrophysics Data System (ADS)

Mirnov, V. V.; Hegna, C. C.; Sovinec, C. R.; Howell, E. C.

2016-10-01

Two-fluid corrections to linear tearing modes includes 1) diamagnetic drifts that reduce the growth rate and 2) electron and ion decoupling on short scales that can lead to fast reconnection. We have recently developed an analytical model that includes effects 1) and 2) and important contribution from finite electron parallel thermal conduction. Both the tendencies 1) and 2) are confirmed by an approximate analytic dispersion relation that is derived using a perturbative approach of small ion-sound gyroradius ρs. This approach is only valid at the beginning of the transition from the collisional to semi-collisional regimes. Further analytical and numerical work is performed to cover the full interval of ρs connecting these two limiting cases. Growth rates are computed from analytic theory with a shooting method. They match the resistive MHD regime with the dispersion relations known at asymptotically large ion-sound gyroradius. A comparison between this analytical treatment and linear numerical simulations using the NIMROD code with cold ions and hot electrons in plasma slab is reported. The material is based on work supported by the U.S. DOE and NSF.

Towards the Rational Design of Ionic Liquid Matrices for Secondary Ion Mass Spectrometry: Role of the Anion

NASA Astrophysics Data System (ADS)

Dertinger, Jennifer J.; Walker, Amy V.

2013-08-01

The role of the ionic liquid (IL) anion structure on analyte signal enhancements has been systematically investigated in secondary ion mass spectrometry (SIMS) using a variety of samples, including lipids, sterols, polymers, and peptides. Twenty-four ILs were synthesized. The 12 matrix acids were cinnamic acid derivatives. Two bases were employed: 1-methylimidazole and tripropylamine. Three matrices, methylimmidazolium o-coumarate, tripropylammonium o-coumarate, and tripropylammonium 3,4,5-trimethoxycinnamate, were "universal" matrices enhancing all analytes tested. The pKa of the matrix acid does not appear to have a strong effect on analyte ion intensities. Rather, it is observed that a single hydroxyl group on the anion aromatic ring leads to significantly increased molecular ion intensities. No analyte signal enhancements were observed for -CH3, -CF3 and -OCH3 groups present on the aromatic ring. The position of the -OH group on the aromatic ring also alters molecular ion intensity enhancements. As well as the chemical identity and position of substituents, the number of moieties on the aromatic ring may affect the analyte signal enhancements observed. These observations suggest that the activation of the IL anion aromatic ring is important for optimizing analyte signal intensities. The implications for SIMS imaging of complex structures, such as biological samples, are discussed.

Automated MALDI Matrix Coating System for Multiple Tissue Samples for Imaging Mass Spectrometry

NASA Astrophysics Data System (ADS)

Mounfield, William P.; Garrett, Timothy J.

2012-03-01

Uniform matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is key for reproducible analyte ion signals. Current methods often result in nonhomogenous matrix deposition, and take time and effort to produce acceptable ion signals. Here we describe a fully-automated method for matrix deposition using an enclosed spray chamber and spray nozzle for matrix solution delivery. A commercial air-atomizing spray nozzle was modified and combined with solenoid controlled valves and a Programmable Logic Controller (PLC) to control and deliver the matrix solution. A spray chamber was employed to contain the nozzle, sample, and atomized matrix solution stream, and to prevent any interference from outside conditions as well as allow complete control of the sample environment. A gravity cup was filled with MALDI matrix solutions, including DHB in chloroform/methanol (50:50) at concentrations up to 60 mg/mL. Various samples (including rat brain tissue sections) were prepared using two deposition methods (spray chamber, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed a uniform coating of matrix crystals across the sample. Overall, the mass spectral images gathered from tissues coated using the spray chamber system were of better quality and more reproducible than from tissue specimens prepared by the inkjet deposition method.

Automated MALDI matrix coating system for multiple tissue samples for imaging mass spectrometry.

PubMed

Mounfield, William P; Garrett, Timothy J

2012-03-01

Uniform matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is key for reproducible analyte ion signals. Current methods often result in nonhomogenous matrix deposition, and take time and effort to produce acceptable ion signals. Here we describe a fully-automated method for matrix deposition using an enclosed spray chamber and spray nozzle for matrix solution delivery. A commercial air-atomizing spray nozzle was modified and combined with solenoid controlled valves and a Programmable Logic Controller (PLC) to control and deliver the matrix solution. A spray chamber was employed to contain the nozzle, sample, and atomized matrix solution stream, and to prevent any interference from outside conditions as well as allow complete control of the sample environment. A gravity cup was filled with MALDI matrix solutions, including DHB in chloroform/methanol (50:50) at concentrations up to 60 mg/mL. Various samples (including rat brain tissue sections) were prepared using two deposition methods (spray chamber, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed a uniform coating of matrix crystals across the sample. Overall, the mass spectral images gathered from tissues coated using the spray chamber system were of better quality and more reproducible than from tissue specimens prepared by the inkjet deposition method.

Buffer Gas Modifiers Effect Resolution in Ion Mobility Spectrometry through Selective Ion-Molecule Clustering Reactions

PubMed Central

Fernández-Maestre, Roberto; Wu, Ching; Hill, Herbert H.

2013-01-01

RATIONALE When polar molecules (modifiers) are introduced into the buffer gas of an ion mobility spectrometer, most ion mobilities decrease due to the formation of ion-modifier clusters. METHODS We used ethyl lactate, nitrobenzene, 2-butanol, and tetrahydrofuran-2-carbonitrile as buffer gas modifiers and electrospray ionization ion mobility spectrometry (IMS) coupled to quadrupole mass spectrometry. Ethyl lactate, nitrobenzene, and tetrahydrofuran-2-carbonitrile had not been tested as buffer gas modifiers and 2-butanol had not been used with basic amino acids. RESULTS The ion mobilities of several diamines (arginine, histidine, lysine, and atenolol) were not affected or only slightly reduced when these modifiers were introduced into the buffer gas (3.4% average reduction in an analyte's mobility for the three modifiers). Intramolecular bridges caused limited change in the ion mobilities of diamines when modifiers were added to the buffer gas; these bridges hindered the attachment of modifier molecules to the positive charge of ions and delocalized the charge, which deterred clustering. There was also a tendency towards large changes in ion mobility when the mass of the analyte decreased; ethanolamine, the smallest compound tested, had the largest reduction in ion mobility with the introduction of modifiers into the buffer gas (61%). These differences in mobilities, together with the lack of shift in bridge-forming ions, were used to separate ions that overlapped in IMS, such as isoleucine and lysine, and arginine and phenylalanine, and made possible the prediction of separation or not of overlapping ions. CONCLUSIONS The introduction of modifiers into the buffer gas in IMS can selectively alter the mobilities of analytes to aid in compound identification and/or enable the separation of overlapping analyte peaks. PMID:22956312

High Resolution Chemical Study of ALH84001

NASA Technical Reports Server (NTRS)

Conrad, Pamela G.; Douglas, Susanne; Kuhlman, Kimberly R.

2001-01-01

We have studied the chemistry of a sample of the SNC meteorite ALH84001 using an environmental scanning electron microscope (ESEM) with an energy dispersive chemical analytical detector and a focused ion beam secondary ion mass spectrometer (FIB-SIMS). Here we present the chemical data, both spectra and images, from two techniques that do not require sample preparation with a conductive coating, thus eliminating the possibility of preparation-induced textural artifacts. The FIB-SIMS instrument includes a column optimized for SEM with a quadrupole type mass spectrometer. Its spatial and spectral resolution are 20 nm and 0.4 AMU, respectively. The spatial resolution of the ESEM for chemical analysis is about 100 nm. Limits of detection for both instruments are mass dependent. Both the ESEM and the FIB-SIMS instrument revealed contrasting surficial features; crumbled, weathered appearance of the matrix in some regions as well as a rather ubiquitous presence of euhedral halite crystals, often associated with cracks or holes in the surface of the rock. Other halogen elements present in the vicinity of the NaCl crystals include K and Br. In this report, elemental inventories are shown as mass spectra and as X-ray maps.

Refined tip preparation by electrochemical etching and ultrahigh vacuum treatment to obtain atomically sharp tips for scanning tunneling microscope and atomic force microscope.

PubMed

Hagedorn, Till; El Ouali, Mehdi; Paul, William; Oliver, David; Miyahara, Yoichi; Grütter, Peter

2011-11-01

A modification of the common electrochemical etching setup is presented. The described method reproducibly yields sharp tungsten tips for usage in the scanning tunneling microscope and tuning fork atomic force microscope. In situ treatment under ultrahigh vacuum (p ≤10(-10) mbar) conditions for cleaning and fine sharpening with minimal blunting is described. The structure of the microscopic apex of these tips is atomically resolved with field ion microscopy and cross checked with field emission. © 2011 American Institute of Physics

Self-assembling cyclic tetrapeptide from alternating C-linked carbo-beta-amino acid [(S)-beta-Caa] and alpha-aminoxy acid [(R)-Ama]: a selective chloride ion receptor.

PubMed

Sharma, Gangavaram V M; Manohar, Vennampalli; Dutta, Samit Kumar; Sridhar, Bojja; Ramesh, Venna; Srinivas, Ragampeta; Kunwar, Ajit C

2010-02-19

A cyclic tetrapeptide is prepared from alternating (S)-beta-Caa (C-linked carbo-beta-amino acid) and (R)-Ama (alpha-aminoxy acid). Extensive NMR (in CDCl(3) solution) and mass spectral (MS) studies show its halide binding capacity, with a special affinity to the chloride ion. At higher concentration it was found to form molecular aggregates as evidenced from transmission electron microscopic and atomic force microscopic analysis, confirming the formation of nanorods.

Ion funnel ion trap and process

DOEpatents

Belov, Mikhail E [Richland, WA; Ibrahim, Yehia M [Richland, WA; Clowers, Biran H [West Richland, WA; Prior, David C [Hermiston, OR; Smith, Richard D [Richland, WA

2011-02-15

An ion funnel trap is described that includes a inlet portion, a trapping portion, and a outlet portion that couples, in normal operation, with an ion funnel. The ion trap operates efficiently at a pressure of .about.1 Torr and provides for: 1) removal of low mass-to-charge (m/z) ion species, 2) ion accumulation efficiency of up to 80%, 3) charge capacity of .about.10,000,000 elementary charges, 4) ion ejection time of 40 to 200 .mu.s, and 5) optimized variable ion accumulation times. Ion accumulation with low concentration peptide mixtures has shown an increase in analyte signal-to-noise ratios (SNR) of a factor of 30, and a greater than 10-fold improvement in SNR for multiply charged analytes.

Systematic investigation of ion suppression and enhancement effects of fourteen stable-isotope-labeled internal standards by their native analogues using atmospheric-pressure chemical ionization and electrospray ionization and the relevance for multi-analyte liquid chromatographic/mass spectrometric procedures.

PubMed

Remane, Daniela; Wissenbach, Dirk K; Meyer, Markus R; Maurer, Hans H

2010-04-15

In clinical and forensic toxicology, multi-analyte procedures are very useful to quantify drugs and poisons of different classes in one run. For liquid chromatographic/tandem mass spectrometric (LC/MS/MS) multi-analyte procedures, often only a limited number of stable-isotope-labeled internal standards (SIL-ISs) are available. If an SIL-IS is used for quantification of other analytes, it must be excluded that the co-eluting native analyte influences its ionization. Therefore, the effect of ion suppression and enhancement of fourteen SIL-ISs caused by their native analogues has been studied. It could be shown that the native analyte concentration influenced the extent of ion suppression and enhancement effects leading to more suppression with increasing analyte concentration especially when electrospray ionization (ESI) was used. Using atmospheric-pressure chemical ionization (APCI), methanolic solution showed mainly enhancement effects, whereas no ion suppression and enhancement effect, with one exception, occurred when plasma extracts were used under these conditions. Such differences were not observed using ESI. With ESI, eleven SIL-ISs showed relevant suppression effects, but only one analyte showed suppression effects when APCI was used. The presented study showed that ion suppression and enhancement tests using matrix-based samples of different sources are essential for the selection of ISs, particularly if used for several analytes to avoid incorrect quantification. In conclusion, only SIL-ISs should be selected for which no suppression and enhancement effects can be observed. If not enough ISs are free of ionization interferences, a different ionization technique should be considered. 2010 John Wiley & Sons, Ltd.

Ion/Neutral, Ion/Electron, Ion/Photon, and Ion/Ion Interactions in Tandem Mass Spectrometry: Do we need them all? Are they enough?

PubMed Central

McLuckey, Scott A.; Mentinova, Marija

2011-01-01

A range of strategies and tools has been developed to facilitate the determination of primary structures of analyte molecules of interest via tandem mass spectrometry (MS/MS). The two main factors that determine the primary structural information present in an MS/MS spectrum are the type of ion generated from the analyte molecule and the dissociation method. The ion-type subjected to dissociation is determined by the ionization method/conditions and ion transformation processes that might take place after initial gas-phase ion formation. Furthermore, the range of analyte-related ion types can be expanded via derivatization reactions prior to mass spectrometry. Dissociation methods include those that simply alter the population of internal states of the mass-selected ion (i.e., activation methods like collision-induced dissociation) as well as processes that rely on transformation of the ion-type prior to dissociation (e.g., electron capture dissociation). A variety of ionic interactions has been studied for the purpose of ion dissociation and ion transformation that include ion/neutral, ion/photon, ion/electron, and ion/ion interactions. A wide range of phenomena has been observed, many of which have been explored/developed as means for structural analysis. The techniques arising from these phenomena are discussed within the context of the elements of structure determination in tandem mass spectrometry, viz., ion-type definition and dissociation. Unique aspects of the various ion interactions are emphasized along with any barriers to widespread implementation. PMID:21472539

Selective determination of pyridine alkaloids in tobacco by PFTBA ions/analyte molecule reaction ionization ion trap mass spectrometry.

PubMed

Zhang, Jianxun; Ji, Houwei; Sun, Shihao; Mao, Duobin; Liu, Huwei; Guo, Yinlong

2007-10-01

The application of perfluorotributylamine (PFTBA) ions/analyte molecule reaction ionization for the selective determination of tobacco pyridine alkaloids by ion trap mass spectrometry (IT-MS) is reported. The main three PFTBA ions (CF(3)(+), C(3)F(5)(+), and C(5)F(10)N(+)) are generated in the external source and then introduced into ion trap for reaction with analytes. Because the existence of the tertiary nitrogen atom in the pyridine makes it possible for PFTBA ions to react smoothly with pyridine and forms adduct ions, pyridine alkaloids in tobacco were selectively ionized and formed quasi-molecular ion [M + H](+)and adduct ions, including [M + 69](+), [M + 131](+), and [M + 264](+), in IT-MS. These ions had distinct abundances and were regarded as the diagnostic ions of each tobacco pyridine alkaloid for quantitative analysis in selected-ion monitoring mode. Results show that the limit of detection is 0.2 microg/mL, and the relative standard deviations for the seven alkaloids are in the range of 0.71% to 6.8%, and good recovery of 95.6% and 97.2%. The proposed method provides substantially greater selectivity and sensitivity compared with the conventional approach and offers an alternative approach for analysis of tobacco alkaloids.

Ionization Suppression and Recovery in Direct Biofluid Analysis Using Paper Spray Mass Spectrometry

NASA Astrophysics Data System (ADS)

Vega, Carolina; Spence, Corina; Zhang, Chengsen; Bills, Brandon J.; Manicke, Nicholas E.

2016-04-01

Paper spray mass spectrometry is a method for the direct analysis of biofluid samples in which extraction of analytes from dried biofluid spots and electrospray ionization occur from the paper on which the dried sample is stored. We examined matrix effects in the analysis of small molecule drugs from urine, plasma, and whole blood. The general method was to spike stable isotope labeled analogs of each analyte into the spray solvent, while the analyte itself was in the dried biofluid. Intensity of the labeled analog is proportional to ionization efficiency, whereas the ratio of the analyte intensity to the labeled analog in the spray solvent is proportional to recovery. Ion suppression and recovery were found to be compound- and matrix-dependent. Highest levels of ion suppression were obtained for poor ionizers (e.g., analytes lacking basic aliphatic amine groups) in urine and approached -90%. Ion suppression was much lower or even absent for good ionizers (analytes with aliphatic amines) in dried blood spots. Recovery was generally highest in urine and lowest in blood. We also examined the effect of two experimental parameters on ion suppression and recovery: the spray solvent and the sample position (how far away from the paper tip the dried sample was spotted). Finally, the change in ion suppression and analyte elution as a function of time was examined by carrying out a paper spray analysis of dried plasma spots for 5 min by continually replenishing the spray solvent.

Concept for facilitating analyst-mediated interpretation of qualitative chromatographic-mass spectral data: an alternative to manual examination of extracted ion chromatograms.

PubMed

Borges, Chad R

2007-07-01

A chemometrics-based data analysis concept has been developed as a substitute for manual inspection of extracted ion chromatograms (XICs), which facilitates rapid, analyst-mediated interpretation of GC- and LC/MS(n) data sets from samples undergoing qualitative batchwise screening for prespecified sets of analytes. Automatic preparation of data into two-dimensional row space-derived scatter plots (row space plots) eliminates the need to manually interpret hundreds to thousands of XICs per batch of samples while keeping all interpretation of raw data directly in the hands of the analyst-saving great quantities of human time without loss of integrity in the data analysis process. For a given analyte, two analyte-specific variables are automatically collected by a computer algorithm and placed into a data matrix (i.e., placed into row space): the first variable is the ion abundance corresponding to scan number x and analyte-specific m/z value y, and the second variable is the ion abundance corresponding to scan number x and analyte-specific m/z value z (a second ion). These two variables serve as the two axes of the aforementioned row space plots. In order to collect appropriate scan number (retention time) information, it is necessary to analyze, as part of every batch, a sample containing a mixture of all analytes to be tested. When pure standard materials of tested analytes are unavailable, but representative ion m/z values are known and retention time can be approximated, data are evaluated based on two-dimensional scores plots from principal component analysis of small time range(s) of mass spectral data. The time-saving efficiency of this concept is directly proportional to the percentage of negative samples and to the total number of samples processed simultaneously.

CAMECA IMS 1300-HR3: The New Generation Ion Microprobe

NASA Astrophysics Data System (ADS)

Peres, P.; Choi, S. Y.; Renaud, L.; Saliot, P.; Larson, D. J.

2016-12-01

The success of secondary ion mass spectrometry (SIMS) in Geo- and Cosmo-chemistry relies on its performance in terms of: 1) very high sensitivity (mandatory for high precision measurements or to achieve low detection limits); 2) a broad mass range of elemental and isotopic species, from low mass (H) to high mass (U and above); 3) in-situ analysis of any solid flat polished surface; and 4) high spatial resolution from tens of microns down to sub-micron scale. The IMS 1300-HR3 (High Reproducibility, High spatial Resolution, High mass Resolution) is the latest generation of CAMECA's large geometry magnetic sector SIMS (or ion microprobe), successor to the internationally recognized IMS 1280-HR. The 1300-HR3delivers unmatched analytical performance for a wide range of applications (stable isotopes, geochronology, trace elements, nuclear safeguards and environmental studies…) due to: • High brightness RF-plasma oxygen ion source with enhanced beam density and current stability, dramatically improving spatial resolution, data reproducibility, and throughput • Automated sample loading system with motorized sample height (Z) adjustment, significantly increasing analysis precision, ease-of-use, and productivity • UV-light microscope for enhanced optical image resolution, together with dedicated software for easy sample navigation (developed by University of Wisconsin, USA) • Low noise 1012Ω resistor Faraday cup preamplifier boards for measuring low signal intensities In addition, improvements in electronics and software have been integrated into the new instrument. In order to meet a growing demand from geochronologists, CAMECA also introduces the KLEORA, which is a fully optimized ion microprobe for advanced mineral dating derived from the IMS 1300-HR3. Instrumental developments as well as data obtained for stable isotope and U-Pb dating applications will be presented in detail.

Depth-Resolved Cathodoluminescence of Thorium Dioxide

DTIC Science & Technology

2013-03-01

exhibited more of an energy dependency than the cut and polished sample. However, in a companion study, ime of flight secondary ion mass spectrometry...Ion Mass Spectrometry (TOF SIMS) ......................17 2.7 Atomic Force Microscope (AFM...1 TOF SIMS……….Time of Flight Secondary Ion Mass Spectroscopy……………….62 1 DEPTH

Newly recognized hosts for uranium in the Hanford Site vadose zone

USGS Publications Warehouse

Stubbs, J.E.; Veblen, L.A.; Elbert, D.C.; Zachara, J.M.; Davis, J.A.; Veblen, D.R.

2009-01-01

Uranium contaminated sediments from the U.S. Department of Energy's Hanford Site have been investigated using electron microscopy. Six classes of solid hosts for uranium were identified. Preliminary sediment characterization was carried out using optical petrography, and electron microprobe analysis (EMPA) was used to locate materials that host uranium. All of the hosts are fine-grained and intergrown with other materials at spatial scales smaller than the analytical volume of the electron microprobe. A focused ion beam (FIB) was used to prepare electron-transparent specimens of each host for the transmission electron microscope (TEM). The hosts were identified as: (1) metatorbernite [Cu(UO2)2(PO4)2??8H2O]; (2) coatings on sediment clasts comprised mainly of phyllosilicates; (3) an amorphous zirconium (oxyhydr)oxide found in clast coatings; (4) amorphous and poorly crystalline materials that line voids within basalt lithic fragments; (5) amorphous palagonite surrounding fragments of basaltic glass; and (6) Fe- and Mn-oxides. These findings demonstrate the effectiveness of combining EMPA, FIB, and TEM to identify solid-phase contaminant hosts. Furthermore, they highlight the complexity of U geochemistry in the Hanford vadose zone, and illustrate the importance of microscopic transport in controlling the fate of contaminant metals in the environment. ?? 2008 Elsevier Ltd.

Morphology variation, composition alteration and microstructure changes in ion-irradiated 1060 aluminum alloy

NASA Astrophysics Data System (ADS)

Wan, Hao; Si, Naichao; Wang, Quan; Zhao, Zhenjiang

2018-02-01

Morphology variation, composition alteration and microstructure changes in 1060 aluminum irradiated with 50 keV helium ions were characterized by field emission scanning electron microscopy (FESEM) equipped with x-ray elemental scanning, 3D measuring laser microscope and transmission electron microscope (TEM). The results show that, helium ions irradiation induced surface damage and Si-rich aggregates in the surfaces of irradiated samples. Increasing the dose of irradiation, more damages and Si-rich aggregates would be produced. Besides, defects such as dislocations, dislocation loops and dislocation walls were the primary defects in the ion implanted layer. The forming of surface damages were related with preferentially sputtering of Al component. While irradiation-enhanced diffusion and irradiation-induced segregation resulted in the aggregation of impurity atoms. And the aggregation ability of impurity atoms were discussed based on the atomic radius, displacement energy, lattice binding energy and surface binding energy.

Selective retention of basic compounds by metal aquo-ion affinity chromatography.

PubMed

Asakawa, Yoshiki; Yamamoto, Eiichi; Asakawa, Naoki

2014-10-01

A novel metal aquo-ion affinity chromatography has been developed for the analysis of basic compounds using heat-treated silica gel containing hydrated metal cations (metal aquo-ions) as the packing material. The packing materials of the metal aquo-ion affinity chromatography were prepared by the immobilization of a single metal component such as Fe(III), Al(III), Ag(I), and Ni(II) on silica gel followed by extensive heat treatment. The immobilized metals form aquo-ions to present cation-exchange ability for basic analytes and the cation-exchange ability for basic analytes depends on pKa of the immobilized metal species. In the present study, to evaluate the retention characteristics of metal aquo-ion affinity chromatography, the on-line solid-phase extraction of drugs was investigated. Obtained data clearly evidence the selective retention capability of metal aquo-ion affinity chromatography for basic analytes with sufficient capacity. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

From fluid dynamics to microscopic transport approach

NASA Astrophysics Data System (ADS)

Saini, Abhilasha; Bhardwaj, Sudhir; Keswani, Bright

2018-05-01

Here we are exploring the widespread features or the characteristics of the microscopic transport modeling and also the speculations made for the approach to fit it to the dynamics of high energy heavy ion collisions, when we see its expansion in space-time dimensions. The explanation of initial stages of the hot and high dense region, the hydrodynamics is instigated and further moderate stages of reaction are complemented to microscopic transport.

Atomic Oxygen (ATOX) simulation of Teflon FEP and Kapton H surfaces using a high intensity, low energy, mass selected, ion beam facility

NASA Technical Reports Server (NTRS)

Vered, R.; Grossman, E.; Lempert, G. D.; Lifshitz, Y.

1994-01-01

A high intensity (greater than 10(exp 15) ions/sq cm) low energy (down to 5 eV) mass selected ion beam (MSIB) facility was used to study the effects of ATOX on two polymers commonly used for space applications (Kapton H and Teflon FEP). The polymers were exposed to O(+) and Ne(+) fluences on 10(exp 15) - 10(exp 19) ions/sq cm, using 30eV ions. A variety of analytical methods were used to analyze the eroded surfaces including: (1) atomic force microscopy (AFM) for morphology measurements; (2) total mass loss measurements using a microbalance; (3) surface chemical composition using x-ray photoelectron spectroscopy (XPS), and (4) residual gas analysis (RGA) of the released gases during bombardment. The relative significance of the collisional and chemical degradation processes was evaluated by comparing the effects of Ne(+) and O(+) bombardment. For 30 eV ions it was found that the Kapton is eroded via chemical mechanisms while Teflon FEP is eroded via collisional mechanisms. AFM analysis was found very powerful in revealing the evolution of the damage from its initial atomic scale (roughness of approx. 1 nm) to its final microscopic scale (roughness greater than 1 micron). Both the surface morphology and the average roughness of the bombarded surfaces (averaged over 1 micron x 1 micron images by the system's computer) were determined for each sample. For 30 eV a non linear increase of the Kapton roughness with the O(+) fluence was discovered (a slow increase rate for fluences phi less than 5 x 10(exp 17) O(+)/sq cm, and a rapid increase rate for phi greater than 5 x 10(exp 17) O(+)/sq cm). Comparative studies on the same materials exposed to RF and DC oxygen plasmas indicate that the specific details of the erosion depend on the simulation facility emphasizing the advantages of the ion beam facility.

"Breath figures" on leaf surfaces-formation and effects of microscopic leaf wetness.

PubMed

Burkhardt, Juergen; Hunsche, Mauricio

2013-01-01

"Microscopic leaf wetness" means minute amounts of persistent liquid water on leaf surfaces which are invisible to the naked eye. The water is mainly maintained by transpired water vapor condensing onto the leaf surface and to attached leaf surface particles. With an estimated average thickness of less than 1 μm, microscopic leaf wetness is about two orders of magnitude thinner than morning dewfall. The most important physical processes which reduce the saturation vapor pressure and promote condensation are cuticular absorption and the deliquescence of hygroscopic leaf surface particles. Deliquescent salts form highly concentrated solutions. Depending on the type and concentration of the dissolved ions, the physicochemical properties of microscopic leaf wetness can be considerably different from those of pure water. Microscopic leaf wetness can form continuous thin layers on hydrophobic leaf surfaces and in specific cases can act similar to surfactants, enabling a strong potential influence on the foliar exchange of ions. Microscopic leaf wetness can also enhance the dissolution, the emission, and the reaction of specific atmospheric trace gases e.g., ammonia, SO2, or ozone, leading to a strong potential role for microscopic leaf wetness in plant/atmosphere interaction. Due to its difficult detection, there is little knowledge about the occurrence and the properties of microscopic leaf wetness. However, based on the existing evidence and on physicochemical reasoning it can be hypothesized that microscopic leaf wetness occurs on almost any plant worldwide and often permanently, and that it significantly influences the exchange processes of the leaf surface with its neighboring compartments, i.e., the plant interior and the atmosphere. The omission of microscopic water in general leaf wetness concepts has caused far-reaching, misleading conclusions in the past.

Interpretation of leaching data for cementitious waste forms using analytical solutions based on mass transport theory and empiricism

DOE Office of Scientific and Technical Information (OSTI.GOV)

Spence, R.D.; Godbee, H.W.; Tallent, O.K.

1989-01-01

The analysis of leaching data using analytical solutions based on mass transport theory and empiricism is presented. The waste forms leached to generate the data used in this analysis were prepared with a simulated radioactive waste slurry with traces of potassium ion, manganese ions, carbonate ions, phosphate ions, and sulfate ions solidified with several blends of cementitious materials. Diffusion coefficients were estimated from the results of ANS - 16.1 tests. Data of fraction leached versus time is presented and discussed.

Analytical model for ion stopping power and range in the therapeutic energy interval for beams of hydrogen and heavier ions

NASA Astrophysics Data System (ADS)

Donahue, William; Newhauser, Wayne D.; Ziegler, James F.

2016-09-01

Many different approaches exist to calculate stopping power and range of protons and heavy charged particles. These methods may be broadly categorized as physically complete theories (widely applicable and complex) or semi-empirical approaches (narrowly applicable and simple). However, little attention has been paid in the literature to approaches that are both widely applicable and simple. We developed simple analytical models of stopping power and range for ions of hydrogen, carbon, iron, and uranium that spanned intervals of ion energy from 351 keV u-1 to 450 MeV u-1 or wider. The analytical models typically reproduced the best-available evaluated stopping powers within 1% and ranges within 0.1 mm. The computational speed of the analytical stopping power model was 28% faster than a full-theoretical approach. The calculation of range using the analytic range model was 945 times faster than a widely-used numerical integration technique. The results of this study revealed that the new, simple analytical models are accurate, fast, and broadly applicable. The new models require just 6 parameters to calculate stopping power and range for a given ion and absorber. The proposed model may be useful as an alternative to traditional approaches, especially in applications that demand fast computation speed, small memory footprint, and simplicity.

Analytical model for ion stopping power and range in the therapeutic energy interval for beams of hydrogen and heavier ions.

PubMed

Donahue, William; Newhauser, Wayne D; Ziegler, James F

2016-09-07

Many different approaches exist to calculate stopping power and range of protons and heavy charged particles. These methods may be broadly categorized as physically complete theories (widely applicable and complex) or semi-empirical approaches (narrowly applicable and simple). However, little attention has been paid in the literature to approaches that are both widely applicable and simple. We developed simple analytical models of stopping power and range for ions of hydrogen, carbon, iron, and uranium that spanned intervals of ion energy from 351 keV u(-1) to 450 MeV u(-1) or wider. The analytical models typically reproduced the best-available evaluated stopping powers within 1% and ranges within 0.1 mm. The computational speed of the analytical stopping power model was 28% faster than a full-theoretical approach. The calculation of range using the analytic range model was 945 times faster than a widely-used numerical integration technique. The results of this study revealed that the new, simple analytical models are accurate, fast, and broadly applicable. The new models require just 6 parameters to calculate stopping power and range for a given ion and absorber. The proposed model may be useful as an alternative to traditional approaches, especially in applications that demand fast computation speed, small memory footprint, and simplicity.

Humidity Effects on Fragmentation in Plasma-Based Ambient Ionization Sources

NASA Astrophysics Data System (ADS)

Newsome, G. Asher; Ackerman, Luke K.; Johnson, Kevin J.

2016-01-01

Post-plasma ambient desorption/ionization (ADI) sources are fundamentally dependent on surrounding water vapor to produce protonated analyte ions. There are two reports of humidity effects on ADI spectra. However, it is unclear whether humidity will affect all ADI sources and analytes, and by what mechanism humidity affects spectra. Flowing atmospheric pressure afterglow (FAPA) ionization and direct analysis in real time (DART) mass spectra of various surface-deposited and gas-phase analytes were acquired at ambient temperature and pressure across a range of observed humidity values. A controlled humidity enclosure around the ion source and mass spectrometer inlet was used to create programmed humidity and temperatures. The relative abundance and fragmentation of molecular adduct ions for several compounds consistently varied with changing ambient humidity and also were controlled with the humidity enclosure. For several compounds, increasing humidity decreased protonated molecule and other molecular adduct ion fragmentation in both FAPA and DART spectra. For others, humidity increased fragment ion ratios. The effects of humidity on molecular adduct ion fragmentation were caused by changes in the relative abundances of different reagent protonated water clusters and, thus, a change in the average difference in proton affinity between an analyte and the population of water clusters. Control of humidity in ambient post-plasma ion sources is needed to create spectral stability and reproducibility.

Humidity Effects on Fragmentation in Plasma-Based Ambient Ionization Sources.

PubMed

Newsome, G Asher; Ackerman, Luke K; Johnson, Kevin J

2016-01-01

Post-plasma ambient desorption/ionization (ADI) sources are fundamentally dependent on surrounding water vapor to produce protonated analyte ions. There are two reports of humidity effects on ADI spectra. However, it is unclear whether humidity will affect all ADI sources and analytes, and by what mechanism humidity affects spectra. Flowing atmospheric pressure afterglow (FAPA) ionization and direct analysis in real time (DART) mass spectra of various surface-deposited and gas-phase analytes were acquired at ambient temperature and pressure across a range of observed humidity values. A controlled humidity enclosure around the ion source and mass spectrometer inlet was used to create programmed humidity and temperatures. The relative abundance and fragmentation of molecular adduct ions for several compounds consistently varied with changing ambient humidity and also were controlled with the humidity enclosure. For several compounds, increasing humidity decreased protonated molecule and other molecular adduct ion fragmentation in both FAPA and DART spectra. For others, humidity increased fragment ion ratios. The effects of humidity on molecular adduct ion fragmentation were caused by changes in the relative abundances of different reagent protonated water clusters and, thus, a change in the average difference in proton affinity between an analyte and the population of water clusters. Control of humidity in ambient post-plasma ion sources is needed to create spectral stability and reproducibility.

Gas-phase ion-molecule reactions for the identification of the sulfone functionality in protonated analytes in a linear quadrupole ion trap mass spectrometer.

PubMed

Tang, Weijuan; Sheng, Huaming; Kong, John Y; Yerabolu, Ravikiran; Zhu, Hanyu; Max, Joann; Zhang, Minli; Kenttämaa, Hilkka I

2016-06-30

The oxidation of sulfur atoms is an important biotransformation pathway for many sulfur-containing drugs. In order to rapidly identify the sulfone functionality in drug metabolites, a tandem mass spectrometric method based on ion-molecule reactions was developed. A phosphorus-containing reagent, trimethyl phosphite (TMP), was allowed to react with protonated analytes with various functionalities in a linear quadrupole ion trap mass spectrometer. The reaction products and reaction efficiencies were measured. Only protonated sulfone model compounds were found to react with TMP to form a characteristic [TMP adduct-MeOH] product ion. All other protonated compounds investigated, with functionalities such as sulfoxide, N-oxide, hydroxylamino, keto, carboxylic acid, and aliphatic and aromatic amino, only react with TMP via proton transfer and/or addition. The specificity of the reaction was further demonstrated by using a sulfoxide-containing anti-inflammatory drug, sulindac, as well as its metabolite sulindac sulfone. A method based on functional group-selective ion-molecule reactions in a linear quadrupole ion trap mass spectrometer has been demonstrated for the identification of the sulfone functionality in protonated analytes. A characteristic [TMP adduct-MeOH] product ion was only formed for the protonated sulfone analytes. The applicability of the TMP reagent in identifying sulfone functionalities in drug metabolites was also demonstrated. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Focussed Ion Beam Milling and Scanning Electron Microscopy of Brain Tissue

PubMed Central

Knott, Graham; Rosset, Stéphanie; Cantoni, Marco

2011-01-01

This protocol describes how biological samples, like brain tissue, can be imaged in three dimensions using the focussed ion beam/scanning electron microscope (FIB/SEM). The samples are fixed with aldehydes, heavy metal stained using osmium tetroxide and uranyl acetate. They are then dehydrated with alcohol and infiltrated with resin, which is then hardened. Using a light microscope and ultramicrotome with glass knives, a small block containing the region interest close to the surface is made. The block is then placed inside the FIB/SEM, and the ion beam used to roughly mill a vertical face along one side of the block, close to this region. Using backscattered electrons to image the underlying structures, a smaller face is then milled with a finer ion beam and the surface scrutinised more closely to determine the exact area of the face to be imaged and milled. The parameters of the microscope are then set so that the face is repeatedly milled and imaged so that serial images are collected through a volume of the block. The image stack will typically contain isotropic voxels with dimenions as small a 4 nm in each direction. This image quality in any imaging plane enables the user to analyse cell ultrastructure at any viewing angle within the image stack. PMID:21775953

Hydrolysis Studies and Quantitative Determination of Aluminum Ions Using [superscript 27]Al NMR: An Undergraduate Analytical Chemistry Experiment

ERIC Educational Resources Information Center

Curtin, Maria A.; Ingalls, Laura R.; Campbell, Andrew; James-Pederson, Magdalena

2008-01-01

This article describes a novel experiment focused on metal ion hydrolysis and the equilibria related to metal ions in aqueous systems. Using [superscript 27]Al NMR, the students become familiar with NMR spectroscopy as a quantitative analytical tool for the determination of aluminum by preparing a standard calibration curve using standard aluminum…

Low Mach-number collisionless electrostatic shocks and associated ion acceleration

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pusztai, Istvan; TenBarge, Jason; Csapó, Aletta N.

The existence and properties of low Mach-number (M >~ 1) electrostatic collisionless shocks are investigated with a semi-analytical solution for the shock structure. We show that the properties of the shock obtained in the semi-analytical model can be well reproduced in fully kinetic Eulerian Vlasov-Poisson simulations, where the shock is generated by the decay of an initial density discontinuity. By using this semi-analytical model, we also study the effect of electron-to-ion temperature ratio and presence of impurities on both the maximum shock potential and Mach number. We find that even a small amount of impurities can influence the shock propertiesmore » significantly, including the reflected light ion fraction, which can change several orders of magnitude. Electrostatic shocks in heavy ion plasmas reflect most of the hydrogen impurity ions.« less

Low Mach-number collisionless electrostatic shocks and associated ion acceleration

DOE PAGES

Pusztai, Istvan; TenBarge, Jason; Csapó, Aletta N.; ...

2017-12-19

The existence and properties of low Mach-number (M >~ 1) electrostatic collisionless shocks are investigated with a semi-analytical solution for the shock structure. We show that the properties of the shock obtained in the semi-analytical model can be well reproduced in fully kinetic Eulerian Vlasov-Poisson simulations, where the shock is generated by the decay of an initial density discontinuity. By using this semi-analytical model, we also study the effect of electron-to-ion temperature ratio and presence of impurities on both the maximum shock potential and Mach number. We find that even a small amount of impurities can influence the shock propertiesmore » significantly, including the reflected light ion fraction, which can change several orders of magnitude. Electrostatic shocks in heavy ion plasmas reflect most of the hydrogen impurity ions.« less

High temperature ion channels and pores

NASA Technical Reports Server (NTRS)

Cheley, Stephen (Inventor); Gu, Li Qun (Inventor); Bayley, Hagan (Inventor); Kang, Xiaofeng (Inventor)

2011-01-01

The present invention includes an apparatus, system and method for stochastic sensing of an analyte to a protein pore. The protein pore may be an engineer protein pore, such as an ion channel at temperatures above 55.degree. C. and even as high as near 100.degree. C. The analyte may be any reactive analyte, including chemical weapons, environmental toxins and pharmaceuticals. The analyte covalently bonds to the sensor element to produce a detectable electrical current signal. Possible signals include change in electrical current. Detection of the signal allows identification of the analyte and determination of its concentration in a sample solution. Multiple analytes present in the same solution may also be detected.

Linear electronic field time-of-flight ion mass spectrometers

DOEpatents

Funsten, Herbert O.

2010-08-24

Time-of-flight mass spectrometer comprising a first drift region and a second drift region enclosed within an evacuation chamber; a means of introducing an analyte of interest into the first drift region; a pulsed ionization source which produces molecular ions from said analyte of interest; a first foil positioned between the first drift region and the second drift region, which dissociates said molecular ions into constituent atomic ions and emits secondary electrons; an electrode which produces secondary electrons upon contact with a constituent atomic ion in second drift region; a stop detector comprising a first ion detection region and a second ion detection region; and a timing means connected to the pulsed ionization source, to the first ion detection region, and to the second ion detection region.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singh, Varinderjit; Vadas, J.; Steinbach, T. K.

Measuring the fusion excitation function for an isotopic chain of projectile nuclei provides a stringent test of a microscopic description of fusion. We report the first measurement of the fusion excitation function at near-barrier energies for the 19O+ 12C system. The measured excitation function is compared with the fusion excitation function of 18O+ 12C. A significant enhancement in the fusion probability of 19O ions with a 12C target as compared to 18O ions is observed. As a result, the experimental cross-sections observed at near-barrier energies are compared with a state-of-the-art microscopic model.

Silver-gold alloy nanoparticles as tunable substrates for systematic control of ion-desorption efficiency and heat transfer in surface-assisted laser desorption/ionization.

PubMed

Lai, Samuel Kin-Man; Cheng, Yu-Hong; Tang, Ho-Wai; Ng, Kwan-Ming

2017-08-09

Systematically controlling heat transfer in the surface-assisted laser desorption/ionization (SALDI) process and thus enhancing the analytical performance of SALDI-MS remains a challenging task. In the current study, by tuning the metal contents of Ag-Au alloy nanoparticle substrates (AgNPs, Ag55Au45NPs, Ag15Au85NPs and AuNPs, ∅: ∼2.0 nm), it was found that both SALDI ion-desorption efficiency and heat transfer can be controlled in a wide range of laser fluence (21.3 mJ cm -2 to 125.9 mJ cm -2 ). It was discovered that ion detection sensitivity can be enhanced at any laser fluence by tuning up the Ag content of the alloy nanoparticle, whereas the extent of ion fragmentation can be reduced by tuning up the Au content. The enhancement effect of Ag content on ion desorption was found to be attributable to the increase in laser absorption efficiency (at 355 nm) with Ag content. Tuning the laser absorption efficiency by changing the metal composition was also effective in controlling the heat transfer from the NPs to the analytes. The laser-induced heating of Ag-rich alloy NPs could be balanced or even overridden by increasing the Au content of NPs, resulting in the reduction of the fragmentation of analytes. In the correlation of experimental measurement with molecular dynamics simulation, the effect of metal composition on the dynamics of the ion desorption process was also elucidated. Upon increasing the Ag content, it was also found that phase transition temperatures, such as melting, vaporization and phase explosion temperature, of NPs could be reduced. This further enhanced the desorption of analyte ions via phase-transition-driven desorption processes. The significant cooling effect on the analyte ions observed at high laser fluence was also determined to be originated from the phase explosion of the NPs. This study revealed that the development of alloy nanoparticles as SALDI substrates can constitute an effective means for the systematic control of ion-desorption efficiency and the extent of heat transfer, which could potentially enhance the analytical performance of SALDI-MS.

An analytical model for scanning electron microscope Type I magnetic contrast with energy filtering

NASA Astrophysics Data System (ADS)

Chim, W. K.

1994-02-01

In this article, a theoretical model for type I magnetic contrast calculations in the scanning electron microscope with energy filtering is presented. This model uses an approximate form of the secondary electron (SE) energy distribution by Chung and Everhart [M. S. Chung and T. E. Everhart, J. Appl. Phys. 45, 707 (1974). Closed form analytical expressions for the contrast and quality factors, which take into consideration the work function and field-distance integral of the material being studied, are obtained. This analytical model is compared with that of a more accurate numerical model. Results showed that the contrast and quality factors for the analytical model differed by not more than 20% from the numerical model, with the actual difference depending on the range of filtered SE energies considered. This model has also been extended to the situation of a two-detector (i.e., detector A and B) configuration, in which enhanced magnetic contrast and quality factor can be obtained by operating in the ``A-B'' mode.

Integrated Arrays of Ion-Sensitive Electrodes

NASA Technical Reports Server (NTRS)

Buehler, Martin; Kuhlman, Kimberly

2003-01-01

The figure depicts an example of proposed compact water-quality sensors that would contain integrated arrays of ion-sensitive electrodes (ISEs). These sensors would serve as electronic "tongues": they would be placed in contact with water and used to "taste" selected dissolved ions (that is, they would be used to measure the concentrations of the ions). The selected ions could be any or all of a variety of organic and inorganic cations and anions that could be regarded as contaminants or analytes, depending on the specific application. In addition, some of the ISEs could be made sensitive to some neutral analytes

Strategy to improve the quantitative LC-MS analysis of molecular ions resistant to gas-phase collision induced dissociation: application to disulfide-rich cyclic peptides.

PubMed

Ciccimaro, Eugene; Ranasinghe, Asoka; D'Arienzo, Celia; Xu, Carrie; Onorato, Joelle; Drexler, Dieter M; Josephs, Jonathan L; Poss, Michael; Olah, Timothy

2014-12-02

Due to observed collision induced dissociation (CID) fragmentation inefficiency, developing sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) assays for CID resistant compounds is especially challenging. As an alternative to traditional LC-MS/MS, we present here a methodology that preserves the intact analyte ion for quantification by selectively filtering ions while reducing chemical noise. Utilizing a quadrupole-Orbitrap MS, the target ion is selectively isolated while interfering matrix components undergo MS/MS fragmentation by CID, allowing noise-free detection of the analyte's surviving molecular ion. In this manner, CID affords additional selectivity during high resolution accurate mass analysis by elimination of isobaric interferences, a fundamentally different concept than the traditional approach of monitoring a target analyte's unique fragment following CID. This survivor-selected ion monitoring (survivor-SIM) approach has allowed sensitive and specific detection of disulfide-rich cyclic peptides extracted from plasma.

Electrospray ion source with reduced analyte electrochemistry

DOEpatents

Kertesz, Vilmos [Knoxville, TN; Van Berkel, Gary [Clinton, TN

2011-08-23

An electrospray ion (ESI) source and method capable of ionizing an analyte molecule without oxidizing or reducing the analyte of interest. The ESI source can include an emitter having a liquid conduit, a working electrode having a liquid contacting surface, a spray tip, a secondary working electrode, and a charge storage coating covering partially or fully the liquid contacting surface of the working electrode. The liquid conduit, the working electrode and the secondary working electrode can be in liquid communication. The electrospray ion source can also include a counter electrode proximate to, but separated from, said spray tip. The electrospray ion source can also include a power system for applying a voltage difference between the working electrodes and a counter-electrode. The power system can deliver pulsed voltage changes to the working electrodes during operation of said electrospray ion source to minimize the surface potential of the charge storage coating.

Electrospray ion source with reduced analyte electrochemistry

DOEpatents

Kertesz, Vilmos; Van Berkel, Gary J

2013-07-30

An electrospray ion (ESI) source and method capable of ionizing an analyte molecule without oxidizing or reducing the analyte of interest. The ESI source can include an emitter having a liquid conduit, a working electrode having a liquid contacting surface, a spray tip, a secondary working electrode, and a charge storage coating covering partially or fully the liquid contacting surface of the working electrode. The liquid conduit, the working electrode and the secondary working electrode can be in liquid communication. The electrospray ion source can also include a counter electrode proximate to, but separated from, said spray tip. The electrospray ion source can also include a power system for applying a voltage difference between the working electrodes and a counter-electrode. The power system can deliver pulsed voltage changes to the working electrodes during operation of said electrospray ion source to minimize the surface potential of the charge storage coating.

Diaion HP-2MG modified with 2-(2,6-dichlorobenzylideneamino) benzenethiol as new adsorbent for solid phase extraction and flame atomic absorption spectrometric determination of metal ions.

PubMed

Ghaedi, M; Montazerozohori, M; Haghdoust, S; Zaare, F; Soylak, M

2013-04-01

A solid phase extraction method for enrichment-separation and the determination of cobalt (Co(2+)), copper (Cu(2+)), nickel (Ni(2+)), zinc (Zn(2+)) and lead (Pb(2+)) ions in real samples has been proposed. The influences of some analytical parameters like pH, flow rate, eluent type and interference of matrix ions on recoveries of analytes were optimized. The limits of detection were found in the range of 1.6-3.9 µg L(-1), while preconcentration factor for all understudy metal ions were found to be 166 with loading half time (t 1/2) less than 10 min. The procedure was applied for the enrichment-separation of analyte ions in environmental samples with recoveries higher than 94.8% and relative SD <4.9% (N = 5).

Collision-induced dissociation analysis of negative atmospheric ion adducts in atmospheric pressure corona discharge ionization mass spectrometry.

PubMed

Sekimoto, Kanako; Takayama, Mitsuo

2013-05-01

Collision-induced dissociation (CID) experiments were performed on atmospheric ion adducts [M + R](-) formed between various types of organic compounds M and atmospheric negative ions R(-) [such as O2(-), HCO3(-), COO(-)(COOH), NO2(-), NO3(-), and NO3(-)(HNO3)] in negative-ion mode atmospheric pressure corona discharge ionization (APCDI) mass spectrometry. All of the [M + R](-) adducts were fragmented to form deprotonated analytes [M - H](-) and/or atmospheric ions R(-), whose intensities in the CID spectra were dependent on the proton affinities of the [M - H](-) and R(-) fragments. Precursor ions [M + R](-) for which R(-) have higher proton affinities than [M - H](-) formed [M - H](-) as the dominant product. Furthermore, the CID of the adducts with HCO3(-) and NO3(-)(HNO3) led to other product ions such as [M + HO](-) and NO3(-), respectively. The fragmentation behavior of [M + R](-) for each R(-) observed was independent of analyte type (e.g., whether the analyte was aliphatic or aromatic, or possessed certain functional groups).

Surface analytical characterization of Streptavidin/poly(3-hexylthiophene) bilayers for bio-electronic applications

NASA Astrophysics Data System (ADS)

Sportelli, M. C.; Picca, R. A.; Manoli, K.; Re, M.; Pesce, E.; Tapfer, L.; Di Franco, C.; Cioffi, N.; Torsi, L.

2017-10-01

The analytical performance of bioelectronic devices is highly influenced by their fabrication methods. In particular, the final architecture of field-effect transistor biosensors combining spin-cast poly(3-hexylthiophene) (P3HT) film and a biomolecule interlayer deposited on a SiO2/Si substrate can lead to the development of highly performing sensing systems, such as for the case of streptavidin (SA) used for biotin sensing. To gain a better understanding of the quality of the interfacial area, critical is the assessment of the morphological features characteristic of the adopted biolayer deposition protocol, namely: the layer-by-layer (LbL) approach and the spin coating technique. The present study relies on a combined surface spectroscopic and morphological characterization. Specifically, X-ray photoelectron spectroscopy operated in the parallel angle-resolved mode allowed the non-destructive investigation of the in-depth chemical composition of the SA film, alone or in the presence of the P3HT overlayer. Spectroscopic data were supported and corroborated by the results obtained with a Scanning Electron and a Helium Ion microscope investigation performed on the SA layer that provided relevant information on the protein structural arrangement or on its surface morphology. Clear differences emerged between the SA layers prepared by the two approaches, with the layer-by-layer deposition resulting in a smoother and better defined bio-electronic interface. Such findings support the superior analytical performance shown by bioelectronic devices based on LbL-deposited protein layers over spin coated ones.

A comparative study on the analytical utility of atmospheric and low-pressure MALDI sources for the mass spectrometric characterization of peptides.

PubMed

Moskovets, Eugene; Misharin, Alexander; Laiko, Viktor; Doroshenko, Vladimir

2016-07-15

A comparative MS study was conducted on the analytical performance of two matrix-assisted laser desorption/ionization (MALDI) sources that operated at either low pressure (∼1Torr) or at atmospheric pressure. In both cases, the MALDI sources were attached to a linear ion trap mass spectrometer equipped with a two-stage ion funnel. The obtained results indicate that the limits of detection, in the analysis of identical peptide samples, were much lower with the source that was operated slightly below the 1-Torr pressure. In the low-pressure (LP) MALDI source, ion signals were observed at a laser fluence that was considerably lower than the one determining the appearance of ion signals in the atmospheric pressure (AP) MALDI source. When the near-threshold laser fluences were used to record MALDI MS spectra at 1-Torr and 750-Torr pressures, the level of chemical noise at the 1-Torr pressure was much lower compared to that at AP. The dependency of the analyte ion signals on the accelerating field which dragged the ions from the MALDI plate to the MS analyzer are presented for the LP and AP MALDI sources. The study indicates that the laser fluence, background gas pressure, and field accelerating the ions away from a MALDI plate were the main parameters which determined the ion yield, signal-to-noise (S/N) ratios, the fragmentation of the analyte ions, and adduct formation in the LP and AP MALDI MS methods. The presented results can be helpful for a deeper insight into the mechanisms responsible for the ion formation in MALDI. Copyright © 2016 Elsevier Inc. All rights reserved.

Dynamic multiplexed analysis method using ion mobility spectrometer

DOEpatents

Belov, Mikhail E [Richland, WA

2010-05-18

A method for multiplexed analysis using ion mobility spectrometer in which the effectiveness and efficiency of the multiplexed method is optimized by automatically adjusting rates of passage of analyte materials through an IMS drift tube during operation of the system. This automatic adjustment is performed by the IMS instrument itself after determining the appropriate levels of adjustment according to the method of the present invention. In one example, the adjustment of the rates of passage for these materials is determined by quantifying the total number of analyte molecules delivered to the ion trap in a preselected period of time, comparing this number to the charge capacity of the ion trap, selecting a gate opening sequence; and implementing the selected gate opening sequence to obtain a preselected rate of analytes within said IMS drift tube.

Emittance preservation in plasma-based accelerators with ion motion

DOE PAGES

Benedetti, C.; Schroeder, C. B.; Esarey, E.; ...

2017-11-01

In a plasma-accelerator-based linear collider, the density of matched, low-emittance, high-energy particle bunches required for collider applications can be orders of magnitude above the background ion density, leading to ion motion, perturbation of the focusing fields, and, hence, to beam emittance growth. By analyzing the response of the background ions to an ultrahigh density beam, analytical expressions, valid for nonrelativistic ion motion, are derived for the transverse wakefield and for the final (i.e., after saturation) bunch emittance. Analytical results are validated against numerical modeling. Initial beam distributions are derived that are equilibrium solutions, which require head-to-tail bunch shaping, enabling emittancemore » preservation with ion motion.« less

Ion sound instability driven by the ion flows

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koshkarov, O., E-mail: koshkarov.alexandr@usask.ca; Smolyakov, A. I.; National Research Centre

2015-05-15

Ion sound instabilities driven by the ion flow in a system of a finite length are considered by analytical and numerical methods. The ion sound waves are modified by the presence of stationary ion flow resulting in negative and positive energy modes. The instability develops due to coupling of negative and positive energy modes mediated by reflections from the boundary. It is shown that the wave dispersion due to deviation from quasineutrality is crucial for the stability. In finite length system, the dispersion is characterized by the length of the system measured in units of the Debye length. The instabilitymore » is studied analytically and the results are compared with direct, initial value numerical simulations.« less

Are clusters important in understanding the mechanisms in atmospheric pressure ionization? Part 1: Reagent ion generation and chemical control of ion populations.

PubMed

Klee, Sonja; Derpmann, Valerie; Wißdorf, Walter; Klopotowski, Sebastian; Kersten, Hendrik; Brockmann, Klaus J; Benter, Thorsten; Albrecht, Sascha; Bruins, Andries P; Dousty, Faezeh; Kauppila, Tiina J; Kostiainen, Risto; O'Brien, Rob; Robb, Damon B; Syage, Jack A

2014-08-01

It is well documented since the early days of the development of atmospheric pressure ionization methods, which operate in the gas phase, that cluster ions are ubiquitous. This holds true for atmospheric pressure chemical ionization, as well as for more recent techniques, such as atmospheric pressure photoionization, direct analysis in real time, and many more. In fact, it is well established that cluster ions are the primary carriers of the net charge generated. Nevertheless, cluster ion chemistry has only been sporadically included in the numerous proposed ionization mechanisms leading to charged target analytes, which are often protonated molecules. This paper series, consisting of two parts, attempts to highlight the role of cluster ion chemistry with regard to the generation of analyte ions. In addition, the impact of the changing reaction matrix and the non-thermal collisions of ions en route from the atmospheric pressure ion source to the high vacuum analyzer region are discussed. This work addresses such issues as extent of protonation versus deuteration, the extent of analyte fragmentation, as well as highly variable ionization efficiencies, among others. In Part 1, the nature of the reagent ion generation is examined, as well as the extent of thermodynamic versus kinetic control of the resulting ion population entering the analyzer region.

Destructive Single-Event Effects in Diodes

NASA Technical Reports Server (NTRS)

Casey, Megan C.; Lauenstein, Jean-Marie; Campola, Michael J.; Wilcox, Edward P.; Phan, Anthony M.; Label, Kenneth A.

2017-01-01

In this work, we discuss the observed single-event effects in a variety of types of diodes. In addition, we conduct failure analysis on several Schottky diodes that were heavy-ion irradiated. High- and low-magnitude optical microscope images, infrared camera images, and scanning electron microscope images are used to identify and describe the failure locations.

New light on ion channel imaging by total internal reflection fluorescence (TIRF) microscopy.

PubMed

Yamamura, Hisao; Suzuki, Yoshiaki; Imaizumi, Yuji

2015-05-01

Ion channels play pivotal roles in a wide variety of cellular functions; therefore, their physiological characteristics, pharmacological responses, and molecular structures have been extensively investigated. However, the mobility of an ion channel itself in the cell membrane has not been examined in as much detail. A total internal reflection fluorescence (TIRF) microscope allows fluorophores to be imaged in a restricted region within an evanescent field of less than 200 nm from the interface of the coverslip and plasma membrane in living cells. Thus the TIRF microscope is useful for selectively visualizing the plasmalemmal surface and subplasmalemmal zone. In this review, we focused on a single-molecule analysis of the dynamic movement of ion channels in the plasma membrane using TIRF microscopy. We also described two single-molecule imaging techniques under TIRF microscopy: fluorescence resonance energy transfer (FRET) for the identification of molecules that interact with ion channels, and subunit counting for the determination of subunit stoichiometry in a functional channel. TIRF imaging can also be used to analyze spatiotemporal Ca(2+) events in the subplasmalemma. Single-molecule analyses of ion channels and localized Ca(2+) signals based on TIRF imaging provide beneficial pharmacological and physiological information concerning the functions of ion channels. Copyright © 2015 The Authors. Production and hosting by Elsevier B.V. All rights reserved.

Benchmark solutions for the galactic heavy-ion transport equations with energy and spatial coupling

NASA Technical Reports Server (NTRS)

Ganapol, Barry D.; Townsend, Lawrence W.; Lamkin, Stanley L.; Wilson, John W.

1991-01-01

Nontrivial benchmark solutions are developed for the galactic heavy ion transport equations in the straightahead approximation with energy and spatial coupling. Analytical representations of the ion fluxes are obtained for a variety of sources with the assumption that the nuclear interaction parameters are energy independent. The method utilizes an analytical LaPlace transform inversion to yield a closed form representation that is computationally efficient. The flux profiles are then used to predict ion dose profiles, which are important for shield design studies.

Extended Lindhard-Scharf-Schiott Theory for Ion Implantation Profiles Expressed with Pearson Function

NASA Astrophysics Data System (ADS)

Suzuki, Kunihiro

2009-04-01

Ion implantation profiles are expressed by the Pearson function with first, second, third, and fourth moment parameters of Rp, ΔRp, γ, and β. We derived an analytical model for these profile moments by solving a Lindhard-Scharf-Schiott (LSS) integration equation using perturbation approximation. This analytical model reproduces Monte Carlo data that were well calibrated to reproduce a vast experimental database. The extended LSS theory is vital for instantaneously predicting ion implantation profiles with any combination of incident ions and substrate atoms including their energy dependence.

Nanostructure formation and regulation during low-energy ion beam sputtering of fused silica surfaces

NASA Astrophysics Data System (ADS)

Liao, Wenlin; Dai, Yi-Fan; Nie, Xutao; Nie, Xuqing; Xu, Mingjin

2017-12-01

Ion beam sputtering (IBS) possesses strong surface nanostructuring behaviors, where dual microscopic phenomenon can be aroused to induce the formation of ultrasmooth surfaces or regular nanostructures. Low-energy IBS of fused silica surfaces is investigated to discuss the formation mechanism and the regulation of the IBS-induced nanostructures. The research results indicate that these microscopic phenomena can be attributed to the interaction of the IBS-induced surface roughening and smoothing effects, and the interaction process strongly depends on the sputtering conditions. Alternatively, ultrasmooth surface or regular nanostructure can be selectively generated through the regulation of the nanostructuring process, and the features of the generated nanostructures, such as amplitude and period, also can be regulated. Consequently, two different technology aims of nanofabrication, including nanometer-scale and nanometer-precision fabrication, can be realized, respectively. These dual microscopic mechanisms distinguish IBS as a promising nanometer manufacturing technology for the optical surfaces.

Surface Modification Technique of Cathode Materials for LI-ION Battery

NASA Astrophysics Data System (ADS)

Jia, Yongzhong; Han, Jinduo; Jing, Yan; Jin, Shan; Qi, Taiyuan

Cathode materials for Li-ion battery LiMn2O4 and LiCo0.1Mn1.9O4 were prepared by soft chemical method. Carbon, which was made by decomposing organic compounds, was used as modifying agent. Cathode material matrix was mixed with water solution that had contained organic compound such as cane sugar, soluble amylum, levulose et al. These mixture were reacted at 150 200 °C for 0.5 4 h in a Teflon-lined autoclave to get a series of homogeneously C-coated cathode materials. The new products were analyzed by X-ray diffraction (XRD) and infrared (IR). Morphology of cathode materials was characterized by scanning electron microscope (SEM) and transition electron microscope (TEM). The new homogeneously C-coated products that were used as cathode materials of lithium-ion battery had good electrochemical stability and cycle performance. This technique has free-pollution, low cost, simpleness and easiness to realize the industrialization of the cathode materials for Li-ion battery.

Dissecting anode swelling in commercial lithium-ion batteries

NASA Astrophysics Data System (ADS)

Zhang, Ningxin; Tang, Huaqiong

2012-11-01

An innovative method is applied to investigate anode swelling during electrochemical processes in commercial lithium-ion batteries. Cathode surface is partially covered with a piece of paste to block the transportation of lithium ion from active material during charging/discharging, and the corresponding part on the anode film shows no formation of Li-graphite compounds during different electrochemical processes, which is confirmed by XRD analysis. The increases of anode thickness within and outside lithiated zone are measured, and defined as electrochemical swelling and physical swelling respectively. The microscopic lattice expansion of graphite due to lithiation process correlates to mesoscopic electrochemical swelling synchronically, while physical swelling tends to decrease steadily with time. The relationship among the microscopic stress due to lithium-ion intercalation, the mesoscopic stress resulting in anode swelling, and the macroscopic rippling of pouch cell after a large number of cycle test, is analyzed and correlated in terms of stress evolution across different scales, and suggestions for solving anode swelling are provided.

Comparison of technologies for nano device prototyping with a special focus on ion beams: A review

NASA Astrophysics Data System (ADS)

Bruchhaus, L.; Mazarov, P.; Bischoff, L.; Gierak, J.; Wieck, A. D.; Hövel, H.

2017-03-01

Nano device prototyping (NDP) is essential for realizing and assessing ideas as well as theories in the form of nano devices, before they can be made available in or as commercial products. In this review, application results patterned similarly to those in the semiconductor industry (for cell phone, computer processors, or memory) will be presented. For NDP, some requirements are different: thus, other technologies are employed. Currently, in NDP, for many applications direct write Gaussian vector scan electron beam lithography (EBL) is used to define the required features in organic resists on this scale. We will take a look at many application results carried out by EBL, self-organized 3D epitaxy, atomic probe microscopy (scanning tunneling microscope/atomic force microscope), and in more detail ion beam techniques. For ion beam techniques, there is a special focus on those based upon liquid metal (alloy) ion sources, as recent developments have significantly increased their applicability for NDP.

ANALYTICAL METHODS AND QUALITY ASSURANCE CRITERIA FOR LC/ES/MS DETERMINATION OF PFOS IN FISH

EPA Science Inventory

PFOS, perfluorooctanesulfonate, has recently received much attention from environmental researchers. Previous analytical methods were based upon complexing with a strong ion-pairing reagent and extraction into MTBE. Detection was done on a concentrate using negative ion LC/ES/MS/...

Nanoscale visualization of redox activity at lithium-ion battery cathodes.

PubMed

Takahashi, Yasufumi; Kumatani, Akichika; Munakata, Hirokazu; Inomata, Hirotaka; Ito, Komachi; Ino, Kosuke; Shiku, Hitoshi; Unwin, Patrick R; Korchev, Yuri E; Kanamura, Kiyoshi; Matsue, Tomokazu

2014-11-17

Intercalation and deintercalation of lithium ions at electrode surfaces are central to the operation of lithium-ion batteries. Yet, on the most important composite cathode surfaces, this is a rather complex process involving spatially heterogeneous reactions that have proved difficult to resolve with existing techniques. Here we report a scanning electrochemical cell microscope based approach to define a mobile electrochemical cell that is used to quantitatively visualize electrochemical phenomena at the battery cathode material LiFePO4, with resolution of ~100 nm. The technique measures electrode topography and different electrochemical properties simultaneously, and the information can be combined with complementary microscopic techniques to reveal new perspectives on structure and activity. These electrodes exhibit highly spatially heterogeneous electrochemistry at the nanoscale, both within secondary particles and at individual primary nanoparticles, which is highly dependent on the local structure and composition.

Brominated Tyrosine and Polyelectrolyte Multilayer Analysis by Laser Desorption VUV Postionization and Secondary Ion Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

University of Illinois at Chicago; Blaze, Melvin M. T.; Takahashi, Lynelle

2011-03-14

The small molecular analyte 3,5-dibromotyrosine (Br2Y) and chitosan-alginate polyelectrolyte multilayers (PEM) with and without adsorbed Br2Y were analyzed by laser desorption postionization mass spectrometry (LDPI-MS). LDPI-MS using 7.87 eV laser and tunable 8 ? 12.5 eV synchrotron vacuum ultraviolet (VUV) radiation found that desorption of clusters from Br2Y films allowed detection by≤8 eV single photon ionization. Thermal desorption and electronic structure calculations determined the ionization energy of Br2Y to be ~;;8.3?0.1 eV and further indicated that the lower ionization energies of clusters permitted their detection at≤8 eV photon energies. However, single photon ionization could only detect Br2Y adsorbed within PEMsmore » when using either higher photon energies or matrix addition to the sample. All samples were also analyzed by 25 keV Bi3 + secondary ion mass spectrometry (SIMS), with the negative ion spectra showing strong parent ion signal which complemented that observed by LDPI-MS. The negative ion SIMS depended strongly on the high electron affinity of this specific analyte and the analyte?s condensed phase environment.« less

Analytical model for describing ion guiding through capillaries in insulating polymers

NASA Astrophysics Data System (ADS)

Liu, Shi-Dong; Zhao, Yong-Tao; Wang, Yu-Yu; N, Stolterfoht; Cheng, Rui; Zhou, Xian-Ming; Xu, Hu-Shan; Xiao, Guo-Qing

2015-08-01

An analytical description for guiding of ions through nanocapillaries is given on the basis of previous work. The current entering into the capillary is assumed to be divided into a current fraction transmitted through the capillary, a current fraction flowing away via the capillary conductivity and a current fraction remaining within the capillary, which is responsible for its charge-up. The discharging current is assumed to be governed by the Frenkel-Poole process. At higher conductivities the analytical model shows a blocking of the ion transmission, which is in agreement with recent simulations. Also, it is shown that ion blocking observed in experiments is well reproduced by the analytical formula. Furthermore, the asymptotic fraction of transmitted ions is determined. Apart from the key controlling parameter (charge-to-energy ratio), the ratio of the capillary conductivity to the incident current is included in the model. Differences resulting from the nonlinear and linear limits of the Frenkel-Poole discharge are pointed out. Project supported by the Major State Basic Research Development Program of China (Grant No. 2010CB832902) and the National Natural Science Foundation of China (Grant Nos. 11275241, 11275238, 11105192, and 11375034).

Thermodynamically consistent Langevin dynamics with spatially correlated noise predicting frictionless regime and transient attraction effect

NASA Astrophysics Data System (ADS)

Majka, M.; Góra, P. F.

2016-10-01

While the origins of temporal correlations in Langevin dynamics have been thoroughly researched, the understanding of spatially correlated noise (SCN) is rather incomplete. In particular, very little is known about the relation between friction and SCN. In this article, starting from the microscopic, deterministic model, we derive the analytical formula for the spatial correlation function in the particle-bath interactions. This expression shows that SCN is the inherent component of binary mixtures, originating from the effective (entropic) interactions. Further, employing this spatial correlation function, we postulate the thermodynamically consistent Langevin equation driven by the Gaussian SCN and calculate the adequate fluctuation-dissipation relation. The thermodynamical consistency is achieved by introducing the spatially variant friction coefficient, which can be also derived analytically. This coefficient exhibits a number of intriguing properties, e.g., the singular behavior for certain types of interactions. Eventually, we apply this new theory to the system of two charged particles in the presence of counter-ions. Such particles interact via the screened-charge Yukawa potential and the inclusion of SCN leads to the emergence of the anomalous frictionless regime. In this regime the particles can experience active propulsion leading to the transient attraction effect. This effect suggests a nonequilibrium mechanism facilitating the molecular binding of the like-charged particles.

Fusion enhancement at near and sub-barrier energies in 19O + 12C

DOE PAGES

Singh, Varinderjit; Vadas, J.; Steinbach, T. K.; ...

2016-12-12

Measuring the fusion excitation function for an isotopic chain of projectile nuclei provides a stringent test of a microscopic description of fusion. We report the first measurement of the fusion excitation function at near-barrier energies for the 19O+ 12C system. The measured excitation function is compared with the fusion excitation function of 18O+ 12C. A significant enhancement in the fusion probability of 19O ions with a 12C target as compared to 18O ions is observed. As a result, the experimental cross-sections observed at near-barrier energies are compared with a state-of-the-art microscopic model.

Helium ion microscopy of graphene: beam damage, image quality and edge contrast

NASA Astrophysics Data System (ADS)

Fox, D.; Zhou, Y. B.; O'Neill, A.; Kumar, S.; Wang, J. J.; Coleman, J. N.; Duesberg, G. S.; Donegan, J. F.; Zhang, H. Z.

2013-08-01

A study to analyse beam damage, image quality and edge contrast in the helium ion microscope (HIM) has been undertaken. The sample investigated was graphene. Raman spectroscopy was used to quantify the disorder that can be introduced into the graphene as a function of helium ion dose. The effects of the dose on both freestanding and supported graphene were compared. These doses were then correlated directly to image quality by imaging graphene flakes at high magnification. It was found that a high magnification image with a good signal to noise ratio will introduce very significant sample damage. A safe imaging dose of the order of 1013 He+ cm-2 was established, with both graphene samples becoming highly defective at doses over 5 × 1014 He+ cm-2. The edge contrast of a freestanding graphene flake imaged in the HIM was then compared with the contrast of the same flake observed in a scanning electron microscope and a transmission electron microscope. Very strong edge sensitivity was observed in the HIM. This enhanced edge sensitivity over the other techniques investigated makes the HIM a powerful nanoscale dimensional metrology tool, with the capability of both fabricating and imaging features with sub-nanometre resolution.

Relating the microscopic rules in coalescence-fragmentation models to the cluster-size distribution

NASA Astrophysics Data System (ADS)

Ruszczycki, B.; Burnett, B.; Zhao, Z.; Johnson, N. F.

2009-11-01

Coalescence-fragmentation problems are now of great interest across the physical, biological, and social sciences. They are typically studied from the perspective of rate equations, at the heart of which are the rules used for coalescence and fragmentation. Here we discuss how changes in these microscopic rules affect the macroscopic cluster-size distribution which emerges from the solution to the rate equation. Our analysis elucidates the crucial role that the fragmentation rule can play in such dynamical grouping models. We focus our discussion on two well-known models whose fragmentation rules lie at opposite extremes. In particular, we provide a range of generalizations and new analytic results for the well-known model of social group formation developed by Eguíluz and Zimmermann, [Phys. Rev. Lett. 85, 5659 (2000)]. We develop analytic perturbation treatments of this original model, and extend the analytic analysis to the treatment of growing and declining populations.

Site-Specific Preparation of Intact Solid–Liquid Interfaces by Label-Free In Situ Localization and Cryo-Focused Ion Beam Lift-Out

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zachman, Michael J.; Asenath-Smith, Emily; Estroff, Lara A.

Abstract Scanning transmission electron microscopy (STEM) allows atomic scale characterization of solid–solid interfaces, but has seen limited applications to solid–liquid interfaces due to the volatility of liquids in the microscope vacuum. Although cryo-electron microscopy is routinely used to characterize hydrated samples stabilized by rapid freezing, sample thinning is required to access the internal interfaces of thicker specimens. Here, we adapt cryo-focused ion beam (FIB) “lift-out,” a technique recently developed for biological specimens, to prepare intact internal solid–liquid interfaces for high-resolution structural and chemical analysis by cryo-STEM. To guide the milling process we introduce a label-freein situmethod of localizing subsurface structuresmore » in suitable materials by energy dispersive X-ray spectroscopy (EDX). Monte Carlo simulations are performed to evaluate the depth-probing capability of the technique, and show good qualitative agreement with experiment. We also detail procedures to produce homogeneously thin lamellae, which enable nanoscale structural, elemental, and chemical analysis of intact solid–liquid interfaces by analytical cryo-STEM. This work demonstrates the potential of cryo-FIB lift-out and cryo-STEM for understanding physical and chemical processes at solid–liquid interfaces.« less

MALDI mass spectrometry of biomolecules and synthetic polymers using alkali hexacyanoferrate (II) complexes and glycerol as matrix

NASA Astrophysics Data System (ADS)

Zollner, Peter; Stubiger, Gerald; Schmid, Erich; Pittenauer, Ernst; Allmaier, Gunter

1997-12-01

K4[Fe(CN)6]/glycerol and Na4[Fe(CN)6]/glycerol have been investigated as liquid matrix systems for UV-MALDI MS applying a N2 laser. Analyte molecules were detected as sodium or potassium adduct ions and, in the case of proteins, as well as protonated molecular ions. Mass accuracies were comparable to those found with standard solid matrix systems with -0.06 to +0.05% deviation in the reflectron mode and with -0.24 to +0.13% in the linear mode. Useful results could be obtained within a mass range of 15 000 Da for single-charged proteins and 8000 Da for potassium cationized polyethylene glycols. Detection limits were found for hydrophilic compounds in the low picomol range and for lipophilic compounds as triacylglycerols or peracetylated and partially benzylated carbohydrates in the low femtomol range. As shown by scanning electron microscopic investigations, the generation of a thin homogenous matrix layer was essential for a successful mass spectrometric experiment. A very careful cleaning of the target surface with glacial acid prior to matrix deposition improved the formation of such a matrix film that maximum sensitivity as well as good reproducibility of the experiments could be achieved.

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

PubMed

Warren, Alexander D; Conway, Ulric; Arthur, Christopher J; Gates, Paul J

2016-07-01

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 © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Simulation study of the lithium ion transport mechanism in ternary polymer electrolytes: the critical role of the segmental mobility.

PubMed

Diddens, Diddo; Heuer, Andreas

2014-01-30

We present an extensive molecular dynamics (MD) simulation study of the lithium ion transport in ternary polymer electrolytes consisting of poly(ethylene oxide) (PEO), lithium-bis(trifluoromethane)sulfonimide (LiTFSI), and the ionic liquid N-methyl-N-propylpyrrolidinium bis(trifluoromethane)sulfonimide (PYR13TFSI). In particular, we focus on two different strategies by which the ternary electrolytes can be devised, namely by (a) adding the ionic liquid to PEO20LiTFSI and (b) substituting the PEO chains in PEO20LiTFSI by the ionic liquid. To grasp the changes of the overall lithium transport mechanism, we employ an analytical, Rouse-based cation transport model (Maitra et al. Phys. Rev. Lett. 2007, 98, 227802), which has originally been devised for binary PEO-based electrolytes. This model distinguishes three different microscopic transport mechanisms, each quantified by an individual time scale. In the course of our analysis, we extend this mathematical description to account for an entirely new transport mechanism, namely, the TFSI-supported diffusion of lithium ions decoupled from the PEO chains, which emerges for certain stoichiometries. We find that the segmental mobility plays a decisive role in PEO-based polymer electrolytes. That is, whereas the addition of the ionic liquid to PEO20LiTFSI plasticizes the polymer network and thus also increases the lithium diffusion, the amount of free, mobile ether oxygens reduces when substituting the PEO chains by the ionic liquid, which compensates the plasticizing effect. In total, our observations allow us to formulate some general principles about the lithium ion transport mechanism in ternary polymer electrolytes. Moreover, our insights also shed light on recent experimental observations (Joost et al. Electrochim. Acta 2012, 86, 330).

Development and Evaluation of an Externally Air-Cooled Low-Flow torch and the Attenuation of Space Charge and Matrix Effects in Inductively Coupled Plasma Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Praphairaksit, Narong

2000-09-12

An externally air-cooled low-flow torch has been constructed and successfully demonstrated for applications in inductively coupled plasma mass spectrometry (ICP-MS). The torch is cooled by pressurized air flowing at ~70 L/min through a quartz air jacket onto the exterior of the outer tube. The outer gas flow rate and operating RF forward power are reduced considerably. Although plasmas can be sustained at the operating power as low as 400 W with a 2 L/min of outer gas flow, somewhat higher power and outer gas flows are advisable. A stable and analytical useful plasma can be obtained at 850 W withmore » an outer gas flow rate of ~4 L/min. Under these conditions, the air-cooled plasma produces comparable sensitivities, doubly charged ion ratios, matrix effects and other analytical merits as those produced by a conventional torch while using significantly less argon and power requirements. Metal oxide ion ratios are slightly higher with the air-cooled plasma but can be mitigated by reducing the aerosol gas flow rate slightly with only minor sacrifice in analyte sensitivity. A methodology to alleviate the space charge and matrix effects in ICP-MS has been developed. A supplemental electron source adapted from a conventional electron impact ionizer is added to the base of the skimmer. Electrons supplied from this source downstream of the skimmer with suitable amount and energy can neutralize the positive ions in the beam extracted from the plasma and diminish the space charge repulsion between them. As a result, the overall ion transmission efficiency and consequent analyte ion sensitivities are significantly improved while other important analytical aspects, such as metal oxide ion ratio, doubly charged ion ratio and background ions remain relatively unchanged with the operation of this electron source. This technique not only improves the ion transmission efficiency but also minimizes the matrix effects drastically. The matrix-induced suppression of signal for even the most troublesome combination of light analyte and heavy matrix elements can be attenuated from 90-99% to only 2-10% for 2 mM matrix solutions with an ultrasonic nebulizer. The supplemental electron current can be adjusted to ''titrate'' out the matrix effects as desired.« less

Timeframe Dependent Fragment Ions Observed in In-Source Decay Experiments with β-Casein Using MALDI MS.

PubMed

Sekiya, Sadanori; Nagoshi, Keishiro; Iwamoto, Shinichi; Tanaka, Koichi; Takayama, Mitsuo

2015-09-01

The fragment ions observed with time-of-flight (TOF) and quadrupole ion trap (QIT) TOF mass spectrometers (MS) combined with matrix-assisted laser desorption/ionization in-source decay (MALDI-ISD) experiments of phosphorylated analytes β-casein and its model peptide were compared from the standpoint of the residence timeframe of analyte and fragment ions in the MALDI ion source and QIT cell. The QIT-TOF MS gave fragment c-, z'-, z-ANL, y-, and b-ions, and further degraded fragments originating from the loss of neutrals such as H(2)O, NH(3), CH(2)O (from serine), C2H4O (from threonine), and H(3)PO(4), whereas the TOF MS merely showed MALDI source-generated fragment c-, z'-, z-ANL, y-, and w-ions. The fragment ions observed in the QIT-TOF MS could be explained by the injection of the source-generated ions into the QIT cell or a cooperative effect of a little internal energy deposition, a long residence timeframe (140 ms) in the QIT cell, and specific amino acid effects on low-energy CID, whereas the source-generated fragments (c-, z'-, z-ANL, y-, and w-ions) could be a result of prompt radical-initiated fragmentation of hydrogen-abundant radical ions [M + H + H](+) and [M + H - H](-) within the 53 ns timeframe, which corresponds to the delayed extraction time. The further degraded fragment b/y-ions produced in the QIT cell were confirmed by positive- and negative-ion low-energy CID experiments performed on the source-generated ions (c-, z'-, and y-ions). The loss of phosphoric acid (98 u) from analyte and fragment ions can be explained by a slow ergodic fragmentation independent of positive and negative charges.

Timeframe Dependent Fragment Ions Observed in In-Source Decay Experiments with β-Casein Using MALDI MS

NASA Astrophysics Data System (ADS)

Sekiya, Sadanori; Nagoshi, Keishiro; Iwamoto, Shinichi; Tanaka, Koichi; Takayama, Mitsuo

2015-09-01

The fragment ions observed with time-of-flight (TOF) and quadrupole ion trap (QIT) TOF mass spectrometers (MS) combined with matrix-assisted laser desorption/ionization in-source decay (MALDI-ISD) experiments of phosphorylated analytes β-casein and its model peptide were compared from the standpoint of the residence timeframe of analyte and fragment ions in the MALDI ion source and QIT cell. The QIT-TOF MS gave fragment c-, z'-, z-ANL, y-, and b-ions, and further degraded fragments originating from the loss of neutrals such as H2O, NH3, CH2O (from serine), C2H4O (from threonine), and H3PO4, whereas the TOF MS merely showed MALDI source-generated fragment c-, z'-, z-ANL, y-, and w-ions. The fragment ions observed in the QIT-TOF MS could be explained by the injection of the source-generated ions into the QIT cell or a cooperative effect of a little internal energy deposition, a long residence timeframe (140 ms) in the QIT cell, and specific amino acid effects on low-energy CID, whereas the source-generated fragments (c-, z'-, z-ANL, y-, and w-ions) could be a result of prompt radical-initiated fragmentation of hydrogen-abundant radical ions [M + H + H]+ and [M + H - H]- within the 53 ns timeframe, which corresponds to the delayed extraction time. The further degraded fragment b/y-ions produced in the QIT cell were confirmed by positive- and negative-ion low-energy CID experiments performed on the source-generated ions (c-, z'-, and y-ions). The loss of phosphoric acid (98 u) from analyte and fragment ions can be explained by a slow ergodic fragmentation independent of positive and negative charges.

The “2T” ion-electron semi-analytic shock solution for code-comparison with xRAGE: A report for FY16

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferguson, Jim Michael

2016-10-05

This report documents an effort to generate the semi-analytic "2T" ion-electron shock solution developed in the paper by Masser, Wohlbier, and Lowrie, and the initial attempts to understand how to use this solution as a code-verification tool for one of LANL's ASC codes, xRAGE. Most of the work so far has gone into generating the semi-analytic solution. Considerable effort will go into understanding how to write the xRAGE input deck that both matches the boundary conditions imposed by the solution, and also what physics models must be implemented within the semi-analytic solution itself to match the model assumptions inherit withinmore » xRAGE. Therefore, most of this report focuses on deriving the equations for the semi-analytic 1D-planar time-independent "2T" ion-electron shock solution, and is written in a style that is intended to provide clear guidance for anyone writing their own solver.« less

Highly selective adsorption of hydroquinone by hydroxyethyl cellulose functionalized with magnetic/ionic liquid.

PubMed

Ding, Chaofan; Li, Yue; Wang, Yanhui; Li, Jianbo; Sun, Yuanling; Lin, Yanna; Sun, Weiyan; Luo, Chuannan

2018-02-01

Magnetic hydroxyethyl cellulose/ionic liquid (MHEC/IL) materials were fabricated through a facile and fast process and their application as excellent adsorbents for hydroquinone was also demonstrated. The thermal stability, chemical structure and magnetic property of the MHEC/IL were characterized by the Scanning electron microscope (SEM), Transmission Electron Microscope (TEM), Fourier transform infrared spectrometer (FT-IR) and X-ray diffraction (XRD), respectively. The adsorbents were used for the removal of hydroquinone from simulated wastewater with a fast solid-liquid separation in the presence of external magnetic field. The influence of various analytical parameters on the adsorption of hydroquinone such as pH, contact time and initial ion concentration were studied in detail. The results showed that the maximum adsorption capacity was 335.68mgg -1 , observed at pH 5 and temperature 30°C. Equilibrium adsorption was achieved within 30min. The kinetic data, obtained at the optimum pH 5, could be fitted with a pseudo-second order equation. Adsorption process could be well described by Freundlich adsorption isotherms. The obtained results indicated that the impregnation of the room temperature IL significantly enhances the removal efficiency of hydroquinone. The MHEC/IL may be suitable materials in phenols pollution cleanup if they are synthesized in largescale and at low price in near future. Copyright © 2017 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schollmeier, Marius S.; Geissel, Matthias; Shores, Jonathon E.

We present calculations for the field of view (FOV), image fluence, image monochromaticity, spectral acceptance, and image aberrations for spherical crystal microscopes, which are used as self-emission imaging or backlighter systems at large-scale high energy density physics facilities. Our analytic results are benchmarked with ray-tracing calculations as well as with experimental measurements from the 6.151 keV backlighter system at Sandia National Laboratories. Furthermore, the analytic expressions can be used for x-ray source positions anywhere between the Rowland circle and object plane. We discovered that this enables quick optimization of the performance of proposed but untested, bent-crystal microscope systems to findmore » the best compromise between FOV, image fluence, and spatial resolution for a particular application.« less

The Wavelength-Dispersive Spectrometer and Its Proposed Use in the Analytical Electron Microscope

NASA Technical Reports Server (NTRS)

Goldstein, Joseph I.; Lyman, Charles E.; Williams, David B.

1989-01-01

The Analytical Electron Microscope (AEM) equipped with a wavelength-dispersive spectrometer (WDS) should have the ability to resolve peaks which normally overlap in the spectra from an energy-dispersive spectrometer (EDS). With a WDS it should also be possible to measure lower concentrations of elements in thin foils due to the increased peak-to-background ratio compared with EDS. The WDS will measure X-ray from the light elements (4 less than Z less than 1O) more effectively. This paper addresses the possibility of interfacing a compact WDS with a focussing circle of approximately 4 cm to a modem AEM with a high-brightness (field emission) source of electrons.

Comparison of functional group selective ion-molecule reactions of trimethyl borate in different ion trap mass spectrometers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Habicht, S C; Vinueza, Nelson R; Amundson, Lucas M

2011-02-01

We report here a comparison of the use of diagnostic ion–molecule reactions for the identification of oxygen-containing functional groups in Fourier-transform ion cyclotron resonance (FTICR) and linear quadrupole ion trap (LQIT) mass spectrometers. The ultimate goal of this research is to be able to identify functionalities in previously unknown analytes by using many different types of mass spectrometers. Previous work has focused on the reactions of various boron reagents with protonated oxygen-containing analytes in FTICR mass spectrometers. By using a LQIT modified to allow the introduction of neutral reagents into the helium buffer gas, this methodology has been successfully implementedmore » to this type of an ion trap instrument. The products obtained from the reactions of trimethyl borate (TMB) with various protonated analytes are compared for the two instruments. Finally, the ability to integrate these reactions into LC-MS experiments on the LQIT is demonstrated.« less

Theoretical Treatment of Ion Transfers in Two Polarizable Interface Systems When the Analyte Has Access to Both Interfaces.

PubMed

Olmos, José Manuel; Molina, Ángela; Laborda, Eduardo; Millán-Barrios, Enrique; Ortuño, Joaquín Ángel

2018-02-06

A new theory is presented to tackle the study of transfer processes of hydrophilic ions in two polarizable interface systems when the analyte is initially present in both aqueous phases. The treatment is applied to macrointerfaces (linear diffusion) and microholes (highly convergent diffusion), obtaining analytical equations for the current response in any voltammetric technique. The novel equations predict two signals in the current-potential curves that are symmetric when the compositions of the aqueous phases are identical while asymmetries appear otherwise. The theoretical results show good agreement with the experimental behavior of the "double transfer voltammograms" reported by Dryfe et al. in cyclic voltammetry (CV) ( Anal. Chem. 2014 , 86 , 435 - 442 ) as well as with cyclic square wave voltammetry (cSWV) experiments performed in the current work. The theoretical treatment is also extended to the situation where the target ion is lipophilic and initially present in the organic phase. The theory predicts an opposite effect of the lipophilicity of the ion on the shape of the voltammograms, which is validated experimentally via both CV and cSWV. For the above two cases, simple and manageable expressions and diagnosis criteria are derived for the qualitative and quantitative study of ion lipophilicity. The ion-transfer potentials can be easily quantified from the separation between the two signals making use of explicit analytical equations.

An ion quencher operated lamp for multiplexed fluorescent bioassays.

PubMed

Qing, Taiping; Sun, Huanhuan; He, Xiaoxiao; Huang, Xiaoqin; He, Dinggeng; Bu, Hongchang; Qiao, Zhenzhen; Wang, Kemin

2018-02-01

A novel and adjustable lamp based on competitive interaction among dsDNA-SYBR Green I (SGI), ion quencher, and analyte was designed for bioanalysis. The "filament" and switch of the lamp could be customized by employing different dsDNA and ion quencher. The poly(AT/TA) dsDNA was successfully screened as the most effective filament of the lamp. Two common ions, Hg 2+ and Fe 3+ , were selected as the model switch, and the corresponding ligand molecules cysteine (Cys) and pyrophosphate ions (PPi) were selected as the targets. When the fluorescence-quenched dsDNA/SGI-ion complex was introduced into a target-containing system, ions could be bound by competitive molecules and separate from the complex, thereby lighting the lamp. However, no light was observed if the biomolecule could not snatch the metal ions from the complex. Under the optimal conditions, sensitive and selective detection of Cys and PPi was achieved by the lamp, with practical applications in fetal bovine serum and human urine. This ion quencher regulated lamp for fluorescent bioassays is simple in design, fast in operation, and is more convenient than other methods. Significantly, as many molecules could form stable complexes with metal ions selectively, this ion quencher operated lamp has potential for the detection of a wide spectrum of analytes. Graphical abstract A novel and adjustable lamp on the basis of competitive interaction among dsDNA-SYBR Green I, ions quencher and analyte was designed for bioanalysis. The filament and switch of lamp could be customized by employing different dsDNA and ions quencher.

Analysis of a variety of inorganic and organic additives in food products by ion-pairing liquid chromatography coupled to high-resolution mass spectrometry.

PubMed

Kaufmann, Anton; Widmer, Mirjam; Maden, Kathryn; Butcher, Patrick; Walker, Stephan

2018-03-05

A reversed-phase ion-pairing chromatographic method was developed for the detection and quantification of inorganic and organic anionic food additives. A single-stage high-resolution mass spectrometer (orbitrap ion trap, Orbitrap) was used to detect the accurate masses of the unfragmented analyte ions. The developed ion-pairing chromatography method was based on a dibutylamine/hexafluoro-2-propanol buffer. Dibutylamine can be charged to serve as a chromatographic ion-pairing agent. This ensures sufficient retention of inorganic and organic anions. Yet, unlike quaternary amines, it can be de-charged in the electrospray to prevent the formation of neutral analyte ion-pairing agent adducts. This process is significantly facilitated by the added hexafluoro-2-propanol. This approach permits the sensitive detection and quantification of additives like nitrate and mono-, di-, and triphosphate as well as citric acid, a number of artificial sweeteners like cyclamate and aspartame, flavor enhancers like glutamate, and preservatives like sorbic acid. This is a major advantage, since the currently used analytical methods as utilized in food safety laboratories are only capable in monitoring a few compounds or a particular category of food additives. Graphical abstract Deptotonation of ion pair agent in the electrospray interface.

A Simple Analytical Model for Predicting the Detectable Ion Current in Ion Mobility Spectrometry Using Corona Discharge Ionization Sources

NASA Astrophysics Data System (ADS)

Kirk, Ansgar Thomas; Kobelt, Tim; Spehlbrink, Hauke; Zimmermann, Stefan

2018-05-01

Corona discharge ionization sources are often used in ion mobility spectrometers (IMS) when a non-radioactive ion source with high ion currents is required. Typically, the corona discharge is followed by a reaction region where analyte ions are formed from the reactant ions. In this work, we present a simple yet sufficiently accurate model for predicting the ion current available at the end of this reaction region when operating at reduced pressure as in High Kinetic Energy Ion Mobility Spectrometers (HiKE-IMS) or most IMS-MS instruments. It yields excellent qualitative agreement with measurement results and is even able to calculate the ion current within an error of 15%. Additional interesting findings of this model are the ion current at the end of the reaction region being independent from the ion current generated by the corona discharge and the ion current in High Kinetic Energy Ion Mobility Spectrometers (HiKE-IMS) growing quadratically when scaling down the length of the reaction region. [Figure not available: see fulltext.

A Simple Analytical Model for Predicting the Detectable Ion Current in Ion Mobility Spectrometry Using Corona Discharge Ionization Sources.

PubMed

Kirk, Ansgar Thomas; Kobelt, Tim; Spehlbrink, Hauke; Zimmermann, Stefan

2018-05-08

Corona discharge ionization sources are often used in ion mobility spectrometers (IMS) when a non-radioactive ion source with high ion currents is required. Typically, the corona discharge is followed by a reaction region where analyte ions are formed from the reactant ions. In this work, we present a simple yet sufficiently accurate model for predicting the ion current available at the end of this reaction region when operating at reduced pressure as in High Kinetic Energy Ion Mobility Spectrometers (HiKE-IMS) or most IMS-MS instruments. It yields excellent qualitative agreement with measurement results and is even able to calculate the ion current within an error of 15%. Additional interesting findings of this model are the ion current at the end of the reaction region being independent from the ion current generated by the corona discharge and the ion current in High Kinetic Energy Ion Mobility Spectrometers (HiKE-IMS) growing quadratically when scaling down the length of the reaction region. Graphical Abstract ᅟ.

The role of light microscopy in aerospace analytical laboratories

NASA Technical Reports Server (NTRS)

Crutcher, E. R.

1977-01-01

Light microscopy has greatly reduced analytical flow time and added new dimensions to laboratory capability. Aerospace analytical laboratories are often confronted with problems involving contamination, wear, or material inhomogeneity. The detection of potential problems and the solution of those that develop necessitate the most sensitive and selective applications of sophisticated analytical techniques and instrumentation. This inevitably involves light microscopy. The microscope can characterize and often identify the cause of a problem in 5-15 minutes with confirmatory tests generally less than one hour. Light microscopy has and will make a very significant contribution to the analytical capabilities of aerospace laboratories.

SPM observation of nano-dots induced by slow highly charged ions

NASA Astrophysics Data System (ADS)

Nakamura, Nobuyuki; Terada, Masashi; Nakai, Yoichi; Kanai, Yasuyuki; Ohtani, Shunsuke; Komaki, Ken-ichiro; Yamazaki, Yasunori

2005-05-01

We have observed nano-dots on a highly oriented pyrolytic graphite (HOPG) surface produced by highly charged ion impacts with a scanning probe microscope. In order to clarify the role of potential and kinetic energies in surface modification, we have measured the kinetic energy and incident ion charge dependences of the dot size. The results showed that the potential energy or the incident ion charge has strong influence on the surface modification rather than the kinetic energy.

Solar Ion Processing of Major Element Surface Compositions of Mature Mare Soils: Insights from Combined XPS and Analytical TEM Observations

NASA Technical Reports Server (NTRS)

Christoffersen, R.; Dukes, C.; Keller, L. P.; Baragiola, R.

2012-01-01

Solar wind ions are capable of altering the sur-face chemistry of the lunar regolith by a number of mechanisms including preferential sputtering, radiation-enhanced diffusion and sputter erosion of space weathered surfaces containing pre-existing compositional profiles. We have previously reported in-situ ion irradiation experiments supported by X-ray photoelectron spectroscopy (XPS) and analytical TEM that show how solar ions potentially drive Fe and Ti reduction at the monolayer scale as well as the 10-100 nm depth scale in lunar soils [1]. Here we report experimental data on the effect of ion irradiation on the major element surface composition in a mature mare soil.

Ionization Efficiency of Doubly Charged Ions Formed from Polyprotic Acids in Electrospray Negative Mode

NASA Astrophysics Data System (ADS)

Liigand, Piia; Kaupmees, Karl; Kruve, Anneli

2016-07-01

The ability of polyprotic acids to give doubly charged ions in negative mode electrospray was studied and related to physicochemical properties of the acids via linear discriminant analysis (LDA). It was discovered that the compound has to be strongly acidic (low p K a1 and p K a2) and to have high hydrophobicity (log P ow) to become multiply charged. Ability to give multiply charged ions in ESI/MS cannot be directly predicted from the solution phase acidities. Therefore, for the first time, a quantitative model to predict the charge state of the analyte in ESI/MS is proposed and validated for small anions. Also, a model to predict ionization efficiencies of these analytes was developed. Results indicate that acidity of the analyte, its octanol-water partition coefficient, and charge delocalization are important factors that influence ionization efficiencies as well as charge states of the analytes. The pH of the solvent was also found to be an important factor influencing the ionization efficiency of doubly charged ions.

Ion acoustic shock waves in plasmas with warm ions and kappa distributed electrons and positrons

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hussain, S.; Mahmood, S.; Hafeez Ur-Rehman

2013-06-15

The monotonic and oscillatory ion acoustic shock waves are investigated in electron-positron-ion plasmas (e-p-i) with warm ions (adiabatically heated) and nonthermal kappa distributed electrons and positrons. The dissipation effects are included in the model due to kinematic viscosity of the ions. Using reductive perturbation technique, the Kadomtsev-Petviashvili-Burgers (KPB) equation is derived containing dispersion, dissipation, and diffraction effects (due to perturbation in the transverse direction) in e-p-i plasmas. The analytical solution of KPB equation is obtained by employing tangent hyperbolic (Tanh) method. The analytical condition for the propagation of oscillatory and monotonic shock structures are also discussed in detail. The numericalmore » results of two dimensional monotonic shock structures are obtained for graphical representation. The dependence of shock structures on positron equilibrium density, ion temperature, nonthermal spectral index kappa, and the kinematic viscosity of ions are also discussed.« less

Method for Continuous Monitoring of Electrospray Ion Formation

NASA Astrophysics Data System (ADS)

Metzler, Guille; Crathern, Susan; Bachmann, Lorin; Fernández-Metzler, Carmen; King, Richard

2017-10-01

A method for continuously monitoring the performance of electrospray ionization without the addition of hardware or chemistry to the system is demonstrated. In the method, which we refer to as SprayDx, cluster ions with solvent vapor natively formed by electrospray are followed throughout the collection of liquid chromatography-selected reaction monitoring data. The cluster ion extracted ion chromatograms report on the consistency of the ion formation and detection system. The data collected by the SprayDx method resemble the data collected for postcolumn infusion of analyte. The response of the cluster ions monitored reports on changes in the physical parameters of the ion source such as voltage and gas flow. SprayDx is also observed to report on ion suppression in a fashion very similar to a postcolumn infusion of analyte. We anticipate the method finding utility as a continuous readout on the performance of electrospray and other atmospheric pressure ionization processes. [Figure not available: see fulltext.

Analysis of FIB-induced damage by electron channelling contrast imaging in the SEM.

PubMed

Gutierrez-Urrutia, Ivan

2017-01-01

We have investigated the Ga + ion-damage effect induced by focused ion beam (FIB) milling in a [001] single crystal of a 316 L stainless steel by the electron channelling contrast imaging (ECCI) technique. The influence of FIB milling on the characteristic electron channelling contrast of surface dislocations was analysed. The ECCI approach provides sound estimation of the damage depth produced by FIB milling. For comparison purposes, we have also studied the same milled surface by a conventional electron backscatter diffraction (EBSD) approach. We observe that the ECCI approach provides further insight into the Ga + ion-damage phenomenon than the EBSD technique by direct imaging of FIB artefacts in the scanning electron microscope. We envisage that the ECCI technique may be a convenient tool to optimize the FIB milling settings in applications where the surface crystal defect content is relevant. © 2016 The Authors Journal of Microscopy © 2016 Royal Microscopical Society.

New approaches for metabolomics by mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vertes, Akos

Small molecules constitute a large part of the world around us, including fossil and some renewable energy sources. Solar energy harvested by plants and bacteria is converted into energy rich small molecules on a massive scale. Some of the worst contaminants of the environment and compounds of interest for national security also fall in the category of small molecules. The development of large scale metabolomic analysis methods lags behind the state of the art established for genomics and proteomics. This is commonly attributed to the diversity of molecular classes included in a metabolome. Unlike nucleic acids and proteins, metabolites domore » not have standard building blocks, and, as a result, their molecular properties exhibit a wide spectrum. This impedes the development of dedicated separation and spectroscopic methods. Mass spectrometry (MS) is a strong contender in the quest for a quantitative analytical tool with extensive metabolite coverage. Although various MS-based techniques are emerging for metabolomics, many of these approaches include extensive sample preparation that make large scale studies resource intensive and slow. New ionization methods are redefining the range of analytical problems that can be solved using MS. This project developed new approaches for the direct analysis of small molecules in unprocessed samples, as well as pushed the limits of ultratrace analysis in volume limited complex samples. The projects resulted in techniques that enabled metabolomics investigations with enhanced molecular coverage, as well as the study of cellular response to stimuli on a single cell level. Effectively individual cells became reaction vessels, where we followed the response of a complex biological system to external perturbation. We established two new analytical platforms for the direct study of metabolic changes in cells and tissues following external perturbation. For this purpose we developed a novel technique, laser ablation electrospray ionization (LAESI), for metabolite profiling of functioning cells and tissues. The technique was based on microscopic sampling of biological specimens by mid-infrared laser ablation followed by electrospray ionization of the plume and MS analysis. The two main shortcomings of this technique had been limited specificity due to the lack of a separation step, and limited molecular coverage, especially for nonpolar chemical species. To improve specificity and the coverage of the metabolome, we implemented the LAESI ion source on a mass spectrometer with ion mobility separation (IMS). In this system, the gas phase ions produced by the LAESI source were first sorted according to their collisional cross sections in a mobility cell. These separated ion packets were then subjected to MS analysis. By combining the atmospheric pressure ionization with IMS, we improved the metabolite coverage. Further enhancement of the non-polar metabolite coverage resulted from the combination of laser ablation with vacuum UV irradiation of the ablation plume. Our results indicated that this new ionization modality provided improved detection for neutral and non-polar compounds. Based on rapid progress in photonics, we had introduced another novel ion source that utilized the interaction of a laser pulse with silicon nanopost arrays (NAPA). In these nanophotonic ion sources, the structural features were commensurate with the wavelength of the laser light. The enhanced interaction resulted in high ion yields. This ultrasensitive analytical platform enabled the MS analysis of single yeast cells. We extended these NAPA studies from yeast to other microorganisms, including green algae (Chlamydomonas reinhardtii) that captured energy from sunlight on a massive scale. Combining cellular perturbations, e.g., through environmental changes, with the newly developed single cell analysis methods enabled us to follow dynamic changes induced in the cells. In effect, we were able to use individual cells as a “laboratory,” and approached the long-standing goal of establishing a “lab-in-a-cell.” Model systems for these studies included cells of cyanobacteria (Anabaena), yeast (Saccharomyces cerevisiae), green algae (C. reinhardtii) and Arabidopsis thaliana.« less

Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Mirabi, Ali; Dalirandeh, Zeinab; Rad, Ali Shokuhi

2015-05-01

A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe3O4 as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L-1 HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml-1 and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results.

A non-linear theory of the parallel firehose and gyrothermal instabilities in a weakly collisional plasma

NASA Astrophysics Data System (ADS)

Rosin, M. S.; Schekochihin, A. A.; Rincon, F.; Cowley, S. C.

2011-05-01

Weakly collisional magnetized cosmic plasmas have a dynamical tendency to develop pressure anisotropies with respect to the local direction of the magnetic field. These anisotropies trigger plasma instabilities at scales just above the ion Larmor radius ρi and much below the mean free path λmfp. They have growth rates of a fraction of the ion cyclotron frequency, which is much faster than either the global dynamics or even local turbulence. Despite their microscopic nature, these instabilities dramatically modify the transport properties and, therefore, the macroscopic dynamics of the plasma. The non-linear evolution of these instabilities is expected to drive pressure anisotropies towards marginal stability values, controlled by the plasma beta βi. Here this non-linear evolution is worked out in an ab initio kinetic calculation for the simplest analytically tractable example - the parallel (k⊥= 0) firehose instability in a high-beta plasma. An asymptotic theory is constructed, based on a particular physical ordering and leading to a closed non-linear equation for the firehose turbulence. In the non-linear regime, both the analytical theory and the numerical solution predict secular (∝t) growth of magnetic fluctuations. The fluctuations develop a k-3∥ spectrum, extending from scales somewhat larger than ρi to the maximum scale that grows secularly with time (∝t1/2); the relative pressure anisotropy (p⊥-p∥)/p∥ tends to the marginal value -2/βi. The marginal state is achieved via changes in the magnetic field, not particle scattering. When a parallel ion heat flux is present, the parallel firehose mutates into the new gyrothermal instability (GTI), which continues to exist up to firehose-stable values of pressure anisotropy, which can be positive and are limited by the magnitude of the ion heat flux. The non-linear evolution of the GTI also features secular growth of magnetic fluctuations, but the fluctuation spectrum is eventually dominated by modes around a maximal scale ˜ρilT/λmfp, where lT is the scale of the parallel temperature variation. Implications for momentum and heat transport are speculated about. This study is motivated by our interest in the dynamics of galaxy cluster plasmas (which are used as the main astrophysical example), but its relevance to solar wind and accretion flow plasmas is also briefly discussed.

Nanometric depth resolution from multi-focal images in microscopy.

PubMed

Dalgarno, Heather I C; Dalgarno, Paul A; Dada, Adetunmise C; Towers, Catherine E; Gibson, Gavin J; Parton, Richard M; Davis, Ilan; Warburton, Richard J; Greenaway, Alan H

2011-07-06

We describe a method for tracking the position of small features in three dimensions from images recorded on a standard microscope with an inexpensive attachment between the microscope and the camera. The depth-measurement accuracy of this method is tested experimentally on a wide-field, inverted microscope and is shown to give approximately 8 nm depth resolution, over a specimen depth of approximately 6 µm, when using a 12-bit charge-coupled device (CCD) camera and very bright but unresolved particles. To assess low-flux limitations a theoretical model is used to derive an analytical expression for the minimum variance bound. The approximations used in the analytical treatment are tested using numerical simulations. It is concluded that approximately 14 nm depth resolution is achievable with flux levels available when tracking fluorescent sources in three dimensions in live-cell biology and that the method is suitable for three-dimensional photo-activated localization microscopy resolution. Sub-nanometre resolution could be achieved with photon-counting techniques at high flux levels.

Nanometric depth resolution from multi-focal images in microscopy

PubMed Central

Dalgarno, Heather I. C.; Dalgarno, Paul A.; Dada, Adetunmise C.; Towers, Catherine E.; Gibson, Gavin J.; Parton, Richard M.; Davis, Ilan; Warburton, Richard J.; Greenaway, Alan H.

2011-01-01

We describe a method for tracking the position of small features in three dimensions from images recorded on a standard microscope with an inexpensive attachment between the microscope and the camera. The depth-measurement accuracy of this method is tested experimentally on a wide-field, inverted microscope and is shown to give approximately 8 nm depth resolution, over a specimen depth of approximately 6 µm, when using a 12-bit charge-coupled device (CCD) camera and very bright but unresolved particles. To assess low-flux limitations a theoretical model is used to derive an analytical expression for the minimum variance bound. The approximations used in the analytical treatment are tested using numerical simulations. It is concluded that approximately 14 nm depth resolution is achievable with flux levels available when tracking fluorescent sources in three dimensions in live-cell biology and that the method is suitable for three-dimensional photo-activated localization microscopy resolution. Sub-nanometre resolution could be achieved with photon-counting techniques at high flux levels. PMID:21247948

Microscopic dynamics of charge separation at the aqueous electrochemical interface.

PubMed

Kattirtzi, John A; Limmer, David T; Willard, Adam P

2017-12-19

We have used molecular simulation and methods of importance sampling to study the thermodynamics and kinetics of ionic charge separation at a liquid water-metal interface. We have considered this process using canonical examples of two different classes of ions: a simple alkali-halide pair, Na + I - , or classical ions, and the products of water autoionization, H 3 O + OH - , or water ions. We find that for both ion classes, the microscopic mechanism of charge separation, including water's collective role in the process, is conserved between the bulk liquid and the electrode interface. However, the thermodynamic and kinetic details of the process differ between these two environments in a way that depends on ion type. In the case of the classical ion pairs, a higher free-energy barrier to charge separation and a smaller flux over that barrier at the interface result in a rate of dissociation that is 40 times slower relative to the bulk. For water ions, a slightly higher free-energy barrier is offset by a higher flux over the barrier from longer lived hydrogen-bonding patterns at the interface, resulting in a rate of association that is similar both at and away from the interface. We find that these differences in rates and stabilities of charge separation are due to the altered ability of water to solvate and reorganize in the vicinity of the metal interface.

Microscopic dynamics of charge separation at the aqueous electrochemical interface

PubMed Central

Kattirtzi, John A.; Limmer, David T.; Willard, Adam P.

2017-01-01

We have used molecular simulation and methods of importance sampling to study the thermodynamics and kinetics of ionic charge separation at a liquid water–metal interface. We have considered this process using canonical examples of two different classes of ions: a simple alkali–halide pair, Na+I−, or classical ions, and the products of water autoionization, H3O+OH−, or water ions. We find that for both ion classes, the microscopic mechanism of charge separation, including water’s collective role in the process, is conserved between the bulk liquid and the electrode interface. However, the thermodynamic and kinetic details of the process differ between these two environments in a way that depends on ion type. In the case of the classical ion pairs, a higher free-energy barrier to charge separation and a smaller flux over that barrier at the interface result in a rate of dissociation that is 40 times slower relative to the bulk. For water ions, a slightly higher free-energy barrier is offset by a higher flux over the barrier from longer lived hydrogen-bonding patterns at the interface, resulting in a rate of association that is similar both at and away from the interface. We find that these differences in rates and stabilities of charge separation are due to the altered ability of water to solvate and reorganize in the vicinity of the metal interface. PMID:28698368

New perspectives in laser analytics: Resonance-enhanced multiphoton ionization in a Paul ion trap combined with a time-of-flight mass spectrometer

NASA Astrophysics Data System (ADS)

Bisling, Peter; Heger, Hans Jörg; Michaelis, Walfried; Weitkamp, Claus; Zobel, Harald

1995-04-01

A new laser analytical device has been developed that is based on resonance-enhanced multiphoton ionization in the very center of a radio-frequency quadrupole ion trap. Applications in speciation anlaysis of biological and enviromental samples and in materials science will all benefit from laser-optical selectivity in the resonance excitation process, combined with mass-spectropic sensivity which is further enhanced by the ion accumulation and storage capability.

Metal ion attachment to the matrix meso-tetrakis(pentafluorophenyl)porphyrin, related matrices and analytes: an experimental and theoretical study.

PubMed

van Kampen, Jeroen J A; Luider, Theo M; Ruttink, Paul J A; Burgers, Peter C

2009-11-01

In a previous study [van Kampen et al. Analytical Chemistry 2006; 78: 5403], we found that meso-tetrakis (pentafluorophenyl)porphyrin (F20TPP), in combination with lithium salts, provides an efficient matrix to cationize small molecules by Li+ attachment and that this combination can be successfully applied to the quantitative analysis of drugs, such as antiretroviral compounds using matrix-assisted laser desorption ionization in conjunction with a time-of-flight analyzer (MALDI-TOF). In the present study, we further explore the mechanism of metal ion attachment to F20TPP and analytes by MALDI-FTMS(/MS). To this end, we have studied the interaction of F20TPP and analytes with various mono-, di- and trivalent metal ions (Li+, Na+, K+, Rb+, Cs+, Co2+, Cu2+, Zn2+, Fe2+, Fe3+ and Ga3+). For the alkali cations, we find that F20TPP forms complexes only with Li+ and Na+; in addition, model analyte molecules such as poly(ethyleneglycol)s, mixed with F20TPP and the alkali cations, also only form Li+ and Na+ adducts. This contrasts sharply with the commonly used matrix 2,5-dihydroxybenzoic acid, where analytes are most efficiently cationized by Na+ or K+. Reasons for this difference are delineated. Ab initio calculations on porphyrin itself reveal that even the smallest alkali cation, Li+, does not fit in the porphyrin cavity, but lies on top of it, pushing the 21H and 23 H hydrogen atoms out of and below the plane with concomitant bending of the porphyrin skeleton in the opposite direction, i.e. toward the cation. Thus, the Li+ ion is not effectively sequestered and is in fact exposed and thus accessible for donation to analyte molecules. Interaction of F20TPP with di- and trivalent metal ions leads to protoporphyrin-metal ions, where the metal ion is captured within the protoporphyrin dianion cavity. The most intense signal is obtained when F20TPP is reacted with CuCl2 and then subjected to laser ablation. This method presents an easy general route to study the metal containing protoporphyrin molecules, which could all act as potential MALDI matrices. Copyright 2009 John Wiley & Sons, Ltd.

Color matters--material ejection and ion yields in UV-MALDI mass spectrometry as a function of laser wavelength and laser fluence.

PubMed

Soltwisch, Jens; Jaskolla, Thorsten W; Dreisewerd, Klaus

2013-10-01

The success of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) as a widely employed analytical tool in the biomolecular sciences builds strongly on an effective laser-material interaction that is resulting in a soft co-desorption and ionization of matrix and imbedded biomolecules. To obtain a maximized ion yield for the analyte(s) of interest, in general both wavelength and fluence need to be tuned to match the specific optical absorption profile of the used matrix. However, commonly only lasers with fixed emission wavelengths of either 337 or 355 nm are used for MALDI-MS. Here, we employed a wavelength-tunable dye laser and recorded both the neutral material ejection and the MS ion data in a wide wavelength and fluence range between 280 and 377.5 nm. α-Cyano-4-hydroxycinnamic acid (HCCA), 4-chloro-α-cyanocinnamic acid (ClCCA), α-cyano-2,4-difluorocinnamic acid (DiFCCA), and 2,5-dihydroxybenzoic acid (DHB) were investigated as matrices, and several peptides as analytes. Recording of the material ejection was achieved by adopting a photoacoustic approach. Relative ion yields were derived by division of photoacoustic and ion signals. In this way, distinct wavelength/fluence regions can be identified for which maximum ion yields were obtained. For the tested matrices, optimal results were achieved for wavelengths corresponding to areas of high optical absorption of the respective matrix and at fluences about a factor of 2-3 above the matrix- and wavelength-dependent ion detection threshold fluences. The material ejection as probed by the photoacoustic method is excellently fitted by the quasithermal model, while a sigmoidal function allows for an empirical description of the ion signal-fluence relationship.

Determining transport coefficients for a microscopic simulation of a hadron gas

NASA Astrophysics Data System (ADS)

Pratt, Scott; Baez, Alexander; Kim, Jane

2017-02-01

Quark-gluon plasmas produced in relativistic heavy-ion collisions quickly expand and cool, entering a phase consisting of multiple interacting hadronic resonances just below the QCD deconfinement temperature, T ˜155 MeV. Numerical microscopic simulations have emerged as the principal method for modeling the behavior of the hadronic stage of heavy-ion collisions, but the transport properties that characterize these simulations are not well understood. Methods are presented here for extracting the shear viscosity and two transport parameters that emerge in Israel-Stewart hydrodynamics. The analysis is based on studying how the stress-energy tensor responds to velocity gradients. Results are consistent with Kubo relations if viscous relaxation times are twice the collision time.

Effect of calcium/sodium ion exchange on the osmotic properties and structure of polyelectrolyte gels.

PubMed

Horkay, Ferenc; Basser, Peter J; Hecht, Anne-Marie; Geissler, Erik

2015-12-01

We discuss the main findings of a long-term research program exploring the consequences of sodium/calcium ion exchange on the macroscopic osmotic and elastic properties, and the microscopic structure of representative synthetic polyelectrolyte (sodium polyacrylate, (polyacrylic acid)) and biopolymer gels (DNA). A common feature of these gels is that above a threshold calcium ion concentration, they exhibit a reversible volume phase transition. At the macroscopic level, the concentration dependence of the osmotic pressure shows that calcium ions influence primarily the third-order interaction term in the Flory-Huggins model of polymer solutions. Mechanical tests reveal that the elastic modulus is practically unaffected by the presence of calcium ions, indicating that ion bridging does not create permanent cross-links. At the microscopic level, small-angle neutron scattering shows that polyacrylic acid and DNA gels exhibit qualitatively similar structural features in spite of important differences (e.g. chain flexibility and chemical composition) between the two polymers. The main effect of calcium ions is that the neutron scattering intensity increases due to the decrease in the osmotic modulus. At the level of the counterion cloud around dissolved macroions, anomalous small-angle X-ray scattering measurements made on DNA indicate that divalent ions form a cylindrical sheath enveloping the chain, but they are not localized. Small-angle neutron scattering and small-angle X-ray scattering provide complementary information on the structure and interactions in polymer solutions and gels. © IMechE 2015.

Direct-write three-dimensional nanofabrication of nanopyramids and nanocones on Si by nanotumefaction using a helium ion microscope

NASA Astrophysics Data System (ADS)

Zhang, L.; Heinig, N. F.; Bazargan, S.; Abd-Ellah, M.; Moghimi, N.; Leung, K. T.

2015-06-01

The recently commercialized helium ion microscope (HIM) has already demonstrated its outstanding imaging capabilities in terms of resolution, surface sensitivity, depth of field and ease of charge compensation. Here, we show its exceptional patterning capabilities by fabricating dense lines and three-dimensional (3D) nanostructures on a Si substrate. Small focusing spot size and confined ion-Si interaction volume of a high-energy helium ion beam account for the high resolution in HIM patterning. We demonstrate that a set of resolvable parallel lines with a half pitch as small as 3.5 nm can be achieved. During helium ion bombardment of the Si surface, implantation outperforms milling due to the small mass of the helium ions, which produces tumefaction instead of depression in the Si surface. The Si surface tumefaction is the result of different kinetic processes including diffusion, coalescence and nanobubble formation of the implanted ions, and is found to be very stable structurally at room temperature. Under appropriate conditions, a linear dependence of the surface swollen height on the ion doses can be observed. This relation has enabled us to fabricate nanopyramids and nanocones, thus demonstrating that HIM patterning provides a new ‘bottom-up’ approach to fabricate 3D nanostructures. This surface tumefaction method is direct, both positioning and height accurate, and free of resist, etch, mode and precursor, and it promises new applications in nanoimprint mold fabrication and photomask clear defect reparation.

In situ analysis of the organic framework in the prismatic layer of mollusc shell.

PubMed

Tong, Hua; Hu, Jiming; Ma, Wentao; Zhong, Guirong; Yao, Songnian; Cao, Nianxing

2002-06-01

A novel in situ analytic approach was constructed by means of ion sputtering, decalcification and deprotein techniques combining with scanning electron microscopy (SEM) and transmission electron microscope (TEM) ultrastructural analysis. The method was employed to determine the spatial distribution of the organic framework outside and the inner crystal and organic/inorganic interface spatial geometrical relationship in the prismatic layer of cristaris plicate (leach). The results show that there is a substructure of organic matrix in the intracrystalline region. The prismatic layer forms according to strict hierarchical configuration of regular pattern. Each unit of organic template of prismatic layer can uniquely determine the column crystal growth direction, spatial orientation and size. Cavity templates are responsible for supporting. limiting size and shape and determining the crystal growth spatial orientation, while the intracrystal organic matrix is responsible for providing nucleation point and inducing the nucleation process of calcite. The stereo hierarchical fabrication of prismatic layer was elucidated for the first time.

Multinucleon transfer dynamics in heavy-ion collisions near Coulomb-barrier energies

NASA Astrophysics Data System (ADS)

Niu, Fei; Chen, Peng-Hui; Guo, Ya-Fei; Ma, Chun-Wang; Feng, Zhao-Qing

2017-12-01

Multinucleon transfer reactions near barrier energies have been investigated with a multistep model based on the dinuclear system (DNS) concept, in which the capture of two colliding nuclei, the transfer dynamics, and the deexcitation process of primary fragments are described by an analytical formula, diffusion theory, and a statistical model, respectively. The nucleon transfer takes place after forming the DNS and is coupled to the dissipation of relative motion energy and angular momentum by solving a set of microscopically derived master equations within the potential energy surface. Specific reactions of Ca,4840+124Sn , 40Ca(40Ar,58Ni)+232Th , 40Ca(58Ni)+238U , and Ca,4840(58Ni)+248Cm near barrier energies are investigated. It is found that fragments are produced by multinucleon transfer reactions with maximal yields along the β -stability line. The isospin relaxation is particularly significant in the process of fragment formation. The incident energy dependence of heavy target-like fragments in the reaction of 58Ni+248Cm is analyzed thoroughly.

A unifying approach to lattice dynamical and electronic properties of solids

NASA Astrophysics Data System (ADS)

Falter, C.

1988-06-01

A unified analysis of lattice dynamical and electronic properties of solids with special emphasis on the interaction between electrons and phonons is presented. The article is roughly divided into two parts reflecting different points of view. The density response of the electrons provides the link between these parts. In the first part, the microscopic theory in terms of the density response in crystals is discussed. Relations are pointed out between the density response approach and the density functional theory. The latter is used for a representation of the exchange-correlation interaction and the microscopic force constants. Relevant methods, as recently proposed by various authors for the calculation of the density response in inhomogeneous solids are discussed. Particular attention is paid to the development of a renormalized response description. Applications of this method to lattice dynamical and electronic properties are presented. In the second part an alternative physical concept, the quasi-ion approach, is outlined. This concept is shown to provide a microscopic basis for electronic charge localization in crystals and proves the importance of the correlation between crystal symmetry and many-body effects. Is is derived that within linear response theory an appropriate decomposition of the valence charge density leads uniquely to a spatially localized density contribution at the individual ion which follows its motion rigidly. The composite consisting of this partial density and the ion core is taken to be an individual entity, denoted as quasi-ion, from which the crystal is built up. In a certain sense this is a generalization of Ziman's concept of neutral pseudo-atoms being approximately valid in simple metals. New insight into the bonding mechanism and charge relaxation processes is shown to follow from this concept. In particular, we discuss the covalent, ionic and metallic bonding mechanisms, using the localized picture provided by the partial densities, on the same basis. The quasi-ion approach is also applied to the calculation of phonon-induced charge density redistributions and to the construction of a simplified formulation of microscopic lattice dynamics. Investigations of the phonon dispersion for different bonding types are given within a rigid quasi-ion model and extensions of this model are outlined. Among other things, these calculations indicate that bonding dynamics of (covalent) molecules and crystals can be described by relative rotations of the quasi-ions under the condition of rotational invariance of the system. Finally, possible applications of the quasi-ion concept to an approximate formulation of anharmonic lattice dynamics and the interaction between electrons and phonons are discussed. A numerical investigation of this interaction is presented and compared with the results from the rigid-ion model. As a consequence of the quasi-ion concept a consistent calculation of the phonon dispersion, the electronic band structure and the electron-phonon interaction becomes possible.

The Quantitative Resolution of a Mixture of Group II Metal Ions by Thermometric Titration with EDTA. An Analytical Chemistry Experiment.

ERIC Educational Resources Information Center

Smith, Robert L.; Popham, Ronald E.

1983-01-01

Presents an experiment in thermometric titration used in an analytic chemistry-chemical instrumentation course, consisting of two titrations, one a mixture of calcium and magnesium, the other of calcium, magnesium, and barium ions. Provides equipment and solutions list/specifications, graphs, and discussion of results. (JM)

Increasing lanthanide luminescence by use of the RETEL effect.

PubMed

Leif, Robert C; Vallarino, Lidia M; Becker, Margie C; Yang, Sean

2006-08-01

Luminescent lanthanide complexes produce emissions with the narrowest-known width at half maximum; however, their significant use in cytometry required an increase in luminescence intensity. The companion review, Leif et al., Cytometry 2006;69A:767-778, described a new technique for the enhancement of lanthanide luminescence, the Resonance Energy Transfer Enhanced Luminescence (RETEL) effect, which increases luminescence and is compatible with standard slide microscopy. The luminescence of the europium ion macrocyclic complex, EuMac, was increased by employing the RETEL effect. After adding the nonluminescent gadolinium ion complex of the thenoyltrifluoroacetonate (TTFA) ligand or the sodium salt of TTFA in ethanol solution, the EuMac-labeled sample was allowed to dry. Both a conventional arc lamp and a time-gated UV LED served as light sources for microscopic imaging. The emission intensity was measured with a CCD camera. Multiple time-gated images were summed with special software to permit analysis and effective presentation of the final image. With the RETEL effect, the luminescence of the EuMac-streptavidin conjugate increased at least six-fold upon drying. Nuclei of apoptotic cells were stained with DAPI and tailed with 5BrdUrd to which a EuMac-anti-5BrdU conjugate was subsequently attached. Time-gated images showed the long-lived EuMac luminescence but did not show the short-lived DAPI fluorescence. Imaging of DNA-synthesizing cells with an arc lamp showed that both S phase and apoptotic cells were labeled, and that their labeling patterns were different. The images of the luminescent EuMac and fluorescent DAPI were combined to produce a color image on a white background. This combination of simple chemistry, instrumentation, and presentation should make possible the inexpensive use of the lanthanide macrocycles, Quantum Dyes, as molecular diagnostics for cytological and histopathological microscopic imaging. (c) 2006 International Society for Analytical Cytology.

La microscopie ionique analytique des tissus biologiques

NASA Astrophysics Data System (ADS)

Galle, P.

Proposed in 1960 by R. Castaing and G. Slodzian, secondary ion emission microanalysis is a microanalytical method which is now largely used for the study of inert material. The instrument called the analytical ion microscope can also be used for the study of biological spécimens ; images representing the distribution of a given stable or radioactive isotope in a tissue section are obtained with a resolution of 0.5 μm. Among the characteristics of this method, two are of particular interest in biological research : its capacity for isotopic analysis and its very high sensitivity which makes possible for the first time a chemical analysis of element at a very low or even at a trace concentration in a microvolume. Proposé en 1960 par R. Castaing et G. Slodzian, la microanalyse par émission ionique secondaire est une méthode qui permet, entre autre, d'obtenir des images représentant la distribution des isotopes présents à la surface d'un échantillon solide avec une résolution de 0,5 μm. D'intérêt très général, cette méthode a été d'abord largement utilisée pour l'étude des matériaux inertes. Elle offre en outre des possibilités entièrement nouvelles dans le domaine de la recherche biomédicale. L'instrument réalisé, le microscope ionique analytique présente deux caractéristiques particulièrement intéressantes pour la biologie : la possibilité d'analyse isotopique, et l'extrême sensibilité permettant de détecter et de localiser dans une coupe histologique des éléments à des concentrations très faibles voire à l'état de trace.

A specialized bioengineering ion beam line

NASA Astrophysics Data System (ADS)

Yu, L. D.; Sangyuenyongpipat, S.; Sriprom, C.; Thongleurm, C.; Suwanksum, R.; Tondee, N.; Prakrajang, K.; Vilaithong, T.; Brown, I. G.; Wiedemann, H.

2007-04-01

A specialized bioengineering ion beam line has recently been completed at Chiang Mai University to meet rapidly growing needs of research and application development in low-energy ion beam biotechnology. This beam line possesses special features: vertical main beam line, low-energy (30 keV) ion beams, double swerve of the beam, a fast pumped target chamber, and an in-situ atomic force microscope (AFM) system chamber. The whole beam line is situated in a bioclean environment, occupying two stories. The quality of the ion beam has been studied. It has proved that this beam line has significantly contributed to our research work on low-energy ion beam biotechnology.

Facile and green preparation of novel adsorption materials by combining sol-gel with ion imprinting technology for selective removal of Cu(II) ions from aqueous solution

NASA Astrophysics Data System (ADS)

Ren, Zhongqi; Zhu, Xinyan; Du, Jian; Kong, Delong; Wang, Nian; Wang, Zhuo; Wang, Qi; Liu, Wei; Li, Qunsheng; Zhou, Zhiyong

2018-03-01

A novel green adsorption polymer was prepared by ion imprinted technology in conjunction with sol-gel process under mild conditions for the selective removal of Cu(II) ions from aqueous solution. Effects of preparation conditions on adsorption performance of prepared polymers were studied. The ion-imprinted polymer was prepared using Cu(II) ion as template, N-[3-(2-aminoethylamino) propyl] trimethoxysilane (AAPTMS) as functional monomer and tetraethyl orthosilicate (TEOS) as cross-linker. Water was used as solvent in the whole preparation process. The imprinted and non-imprinted polymers were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), atomic force microscope (AFM), Brunauer, Emmett and Teller (BET) and zeta potential. Three-dimensional network structure was formed and functional monomer was successfully cross-linked into the network structure of polymers. Effects of adsorption conditions on adsorption performance of prepared polymers were studied too. The pH value is of great influence on adsorption behavior. Adsorption by ion-imprinted polymer was fast (adsorption equilibrium was reached within 60 min). The adsorption capacity of Cu(II) ion-imprinted polymer was always larger than that of non-imprinted polymer. Pseudo-second-order kinetics model and Freundlich isotherm model fitted well with adsorption data. The maximum adsorption capacity of Cu(II) ion-imprinted polymer was 39.82 mg·g-1. However, the preparation conditions used in this work are much milder than those reported in literatures. The Cu(II) ion-imprinted polymer showed high selectivity and relative selectivity coefficients for Pb(II), Ni(II), Cd(II) and Co(II). In addition, the prepared ion-imprinted polymer could be reused several times without significant loss of adsorption capacity.

Mass spectrometry imaging: Towards a lipid microscope?

PubMed

Touboul, David; Brunelle, Alain; Laprévote, Olivier

2011-01-01

Biological imaging techniques are the most efficient way to locally measure the variation of different parameters on tissue sections. These analyses are gaining increasing interest since 20 years and allow observing extremely complex biological phenomena at lower and lower time and resolution scale. Nevertheless, most of them only target very few compounds of interest, which are chosen a priori, due to their low resolution power and sensitivity. New chemical imaging technique has to be introduced in order to overcome these limitations, leading to more informative and sensitive analyses for biologists and physicians. Two major mass spectrometry methods can be efficiently used to generate the distribution of biological compounds over a tissue section. Matrix-Assisted Laser Desorption/Ionisation-Mass Spectrometry (MALDI-MS) needs the co-crystallization of the sample with a matrix before to be irradiated by a laser, whereas the analyte is directly desorbed by a primary ion bombardment for Secondary Ion Mass Spectrometry (SIMS) experiments. In both cases, energy used for desorption/ionization is locally deposited -some tens of microns for the laser and some hundreds of nanometers for the ion beam- meaning that small areas over the surface sample can be separately analyzed. Step by step analysis allows spectrum acquisitions over the tissue sections and the data are treated by modern informatics software in order to create ion density maps, i.e., the intensity plot of one specific ion versus the (x,y) position. Main advantages of SIMS and MALDI compared to other chemical imaging techniques lie in the simultaneous acquisition of a large number of biological compounds in mixture with an excellent sensitivity obtained by Time-of-Flight (ToF) mass analyzer. Moreover, data treatment is done a posteriori, due to the fact that no compound is selectively marked, and let us access to the localization of different lipid classes in only one complete acquisition. Copyright © 2010 Elsevier Masson SAS. All rights reserved.

Ion-Exchanged Waveguides for Signal Processing Applications - A Novel Electrolytic Process.

DTIC Science & Technology

1987-03-07

were constructed of aluminium : the thermo- limitations in the melt are not expected to dominate couple sheath was stainless steel. the exchange rate...silver ion, D is its T, C0 , and t) with Schott 8011 glass (left) and a Fisher self-diffusion coefficient, and t is the time of diffusion. microscope

Nanostructural evolution and behavior of H and Li in ion-implanted γ-LiAlO 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jiang, Weilin; Zhang, Jiandong; Edwards, Danny J.

In-situ He+ ion irradiation is performed under a helium ion microscope to study nanostructural evolution in polycrystalline gamma-LiAlO2 pellets. Various locations within a grain, across grain boundaries and at a cavity are selected. The results exhibit He bubble formation, grain-boundary cracking, nanoparticle agglomeration, increasing surface brightness with dose, and material loss from the surface. Similar brightening effects at grain boundaries are also observed under a scanning electron microscope. Li diffusion and loss from polycrystalline gamma-LiAlO2 is faster than its monocrystalline counterpart during H2+ ion implantation at elevated temperatures. There is also more significant H diffusion and release from polycrystalline pelletsmore » during thermal annealing of 300 K implanted samples. Grain boundaries and cavities could provide a faster pathway for H and Li diffusion. H release is slightly faster from the 573 K implanted monocrystalline gamma-LiAlO2 during annealing at 773 K. Metal hydrides could be formed preferentially along the grain boundaries to immobilize hydrogen.« less

Potential biomedical applications of ion beam technology

NASA Technical Reports Server (NTRS)

Banks, B. A.; Weigand, A. J.; Babbush, C. A.; Vankampen, C. L.

1976-01-01

Electron bombardment ion thrusters used as ion sources have demonstrated a unique capability to vary the surface morphology of surgical implant materials. The microscopically rough surface texture produced by ion beam sputtering of these materials may result in improvements in the biological response and/or performance of implanted devices. Control of surface roughness may result in improved attachment of the implant to soft tissue, hard tissue, bone cement, or components deposited from blood. Potential biomedical applications of ion beam texturing discussed include: vascular prostheses, artificial heart pump diaphragms, pacemaker fixation, percutaneous connectors, orthopedic pros-thesis fixtion, and dental implants.

Potential biomedical applications of ion beam technology

NASA Technical Reports Server (NTRS)

Banks, B. A.; Weigand, A. J.; Van Kampen, C. L.; Babbush, C. A.

1976-01-01

Electron bombardment ion thrusters used as ion sources have demonstrated a unique capability to vary the surface morphology of surgical implant materials. The microscopically rough surface texture produced by ion beam sputtering of these materials may result in improvements in the biological response and/or performance of implanted devices. Control of surface roughness may result in improved attachment of the implant to soft tissue, hard tissue, bone cement, or components deposited from blood. Potential biomedical applications of ion beam texturing discussed include: vascular prostheses, artificial heart pump diaphragms, pacemaker fixation, percutaneous connectors, orthopedic prosthesis fixation, and dental implants.

An ion-pair principle for enantioseparations of basic analytes by nonaqueous capillary electrophoresis using the di-n-butyl L-tartrate-boric acid complex as chiral selector.

PubMed

Wang, Li-Juan; Liu, Xiu-Feng; Lu, Qie-Nan; Yang, Geng-Liang; Chen, Xing-Guo

2013-04-05

A chiral recognition mechanism of ion-pair principle has been proposed in this study. It rationalized the enantioseparations of some basic analytes using the complex of di-n-butyl l-tartrate and boric acid as the chiral selector in methanolic background electrolytes (BGEs) by nonaqueous capillary electrophoresis (NACE). An approach of mass spectrometer (MS) directly confirmed that triethylamine promoted the formation of negatively charged di-n-butyl l-tartrate-boric acid complex chiral counter ion with a complex ratio of 2:1. And the negatively charged counter ion was the real chiral selector in the ion-pair principle enantioseparations. It was assumed that triethylamine should play its role by adjusting the apparent acidity (pH*) of the running buffer to a higher value. Consequently, the effects of various basic electrolytes including inorganic and organic ones on the enantioseparations in NACE were investigated. The results showed that most of the basic electrolytes tested were favorable for the enantioseparations of basic analytes using di-n-butyl l-tartrate-boric acid complex as the chiral ion-pair selector. Copyright © 2013 Elsevier B.V. All rights reserved.

Ion sampling and transport in Inductively Coupled Plasma Mass Spectrometry

NASA Astrophysics Data System (ADS)

Farnsworth, Paul B.; Spencer, Ross L.

2017-08-01

Quantitative accuracy and high sensitivity in inductively coupled plasma mass spectrometry (ICP-MS) depend on consistent and efficient extraction and transport of analyte ions from an inductively coupled plasma to a mass analyzer, where they are sorted and detected. In this review we examine the fundamental physical processes that control ion sampling and transport in ICP-MS and compare the results of theory and computerized models with experimental efforts to characterize the flow of ions through plasma mass spectrometers' vacuum interfaces. We trace the flow of ions from their generation in the plasma, into the sampling cone, through the supersonic expansion in the first vacuum stage, through the skimmer, and into the ion optics that deliver the ions to the mass analyzer. At each stage we consider idealized behavior and departures from ideal behavior that affect the performance of ICP-MS as an analytical tool.

Plasma ion stratification by weak planar shocks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Simakov, Andrei N.; Keenan, Brett D.; Taitano, William T.

We derive fluid equations for describing steady-state planar shocks of a moderate strength (0 < M - 1 ≲ 1 with M the shock Mach number) propagating through an unmagnetized quasineutral collisional plasma comprising two separate ion species. In addition to the standard fluid shock quantities, such as the total mass density, mass-flow velocity, and electron and average ion temperatures, the equations describe shock stratification in terms of variations in the relative concentrations and temperatures of the two ion species along the shock propagation direction. We have solved these equations analytically for weak shocks (0 < M - 1 <

Plasma Ion Stratification by Weak Planar Shocks

NASA Astrophysics Data System (ADS)

Simakov, A. N.; Keenan, B. D.; Taitano, W. T.; Chacón, L.

2017-10-01

We derive fluid equations for describing steady-state planar shocks of a moderate strength (0

Plasma ion stratification by weak planar shocks

NASA Astrophysics Data System (ADS)

Simakov, Andrei N.; Keenan, Brett D.; Taitano, William T.; Chacón, Luis

2017-09-01

We derive fluid equations for describing steady-state planar shocks of a moderate strength ( 0

Plasma ion stratification by weak planar shocks

DOE PAGES

Simakov, Andrei N.; Keenan, Brett D.; Taitano, William T.; ...

2017-08-01

We derive fluid equations for describing steady-state planar shocks of a moderate strength (0 < M - 1 ≲ 1 with M the shock Mach number) propagating through an unmagnetized quasineutral collisional plasma comprising two separate ion species. In addition to the standard fluid shock quantities, such as the total mass density, mass-flow velocity, and electron and average ion temperatures, the equations describe shock stratification in terms of variations in the relative concentrations and temperatures of the two ion species along the shock propagation direction. We have solved these equations analytically for weak shocks (0 < M - 1 <

A microarray immunoassay for simultaneous detection of proteins and bacteria

NASA Technical Reports Server (NTRS)

Delehanty, James B.; Ligler, Frances S.

2002-01-01

We report the development and characterization of an antibody microarray biosensor for the rapid detection of both protein and bacterial analytes under flow conditions. Using a noncontact microarray printer, biotinylated capture antibodies were immobilized at discrete locations on the surface of an avidin-coated glass microscope slide. Preservation of capture antibody function during the deposition process was accomplished with the use of a low-salt buffer containing sucrose and bovine serum albumin. The slide was fitted with a six-channel flow module that conducted analyte-containing solutions over the array of capture antibody microspots. Detection of bound analyte was subsequently achieved using fluorescent tracer antibodies. The pattern of fluorescent complexes was interrogated using a scanning confocal microscope equipped with a 635-nm laser. This microarray system was employed to detect protein and bacterial analytes both individually and in samples containing mixtures of analytes. Assays were completed in 15 min, and detection of cholera toxin, staphylococcal enterotoxin B, ricin, and Bacillus globigii was demonstrated at levels as low as 8 ng/mL, 4 ng/mL, 10 ng/mL, and 6.2 x 10(4) cfu/mL, respectively. The assays presented here are very fast, as compared to previously published methods for measuring antibody-antigen interactions using microarrays (minutes versus hours).

3D ToF-SIMS Analysis of Peptide Incorporation into MALDI Matrix Crystals with Sub-micrometer Resolution.

PubMed

Körsgen, Martin; Pelster, Andreas; Dreisewerd, Klaus; Arlinghaus, Heinrich F

2016-02-01

The analytical sensitivity in matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is largely affected by the specific analyte-matrix interaction, in particular by the possible incorporation of the analytes into crystalline MALDI matrices. Here we used time-of-flight secondary ion mass spectrometry (ToF-SIMS) to visualize the incorporation of three peptides with different hydrophobicities, bradykinin, Substance P, and vasopressin, into two classic MALDI matrices, 2,5-dihydroxybenzoic acid (DHB) and α-cyano-4-hydroxycinnamic acid (HCCA). For depth profiling, an Ar cluster ion beam was used to gradually sputter through the matrix crystals without causing significant degradation of matrix or biomolecules. A pulsed Bi3 ion cluster beam was used to image the lateral analyte distribution in the center of the sputter crater. Using this dual beam technique, the 3D distribution of the analytes and spatial segregation effects within the matrix crystals were imaged with sub-μm resolution. The technique could in the future enable matrix-enhanced (ME)-ToF-SIMS imaging of peptides in tissue slices at ultra-high resolution. Graphical Abstract ᅟ.

3D ToF-SIMS Analysis of Peptide Incorporation into MALDI Matrix Crystals with Sub-micrometer Resolution

NASA Astrophysics Data System (ADS)

Körsgen, Martin; Pelster, Andreas; Dreisewerd, Klaus; Arlinghaus, Heinrich F.

2016-02-01

The analytical sensitivity in matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is largely affected by the specific analyte-matrix interaction, in particular by the possible incorporation of the analytes into crystalline MALDI matrices. Here we used time-of-flight secondary ion mass spectrometry (ToF-SIMS) to visualize the incorporation of three peptides with different hydrophobicities, bradykinin, Substance P, and vasopressin, into two classic MALDI matrices, 2,5-dihydroxybenzoic acid (DHB) and α-cyano-4-hydroxycinnamic acid (HCCA). For depth profiling, an Ar cluster ion beam was used to gradually sputter through the matrix crystals without causing significant degradation of matrix or biomolecules. A pulsed Bi3 ion cluster beam was used to image the lateral analyte distribution in the center of the sputter crater. Using this dual beam technique, the 3D distribution of the analytes and spatial segregation effects within the matrix crystals were imaged with sub-μm resolution. The technique could in the future enable matrix-enhanced (ME)-ToF-SIMS imaging of peptides in tissue slices at ultra-high resolution.

Analytical Chemistry of Surfaces: Part III. Ion Spectroscopy.

ERIC Educational Resources Information Center

Hercules, David M.; Hercules, Shirley H.

1984-01-01

The fundamentals of two surface techniques--secondary-ion mass spectrometry (SIMS) and ion-scattering spectrometry (ISS)--are discussed. Examples of how these techniques have been applied to surface problems are provided. (JN)

Electrostatic shock structures in dissipative multi-ion dusty plasmas

NASA Astrophysics Data System (ADS)

Elkamash, I. S.; Kourakis, I.

2018-06-01

A comprehensive analytical model is introduced for shock excitations in dusty bi-ion plasma mixtures, taking into account collisionality and kinematic (fluid) viscosity. A multicomponent plasma configuration is considered, consisting of positive ions, negative ions, electrons, and a massive charged component in the background (dust). The ionic dynamical scale is focused upon; thus, electrons are assumed to be thermalized, while the dust is stationary. A dissipative hybrid Korteweg-de Vries/Burgers equation is derived. An analytical solution is obtained, in the form of a shock structure (a step-shaped function for the electrostatic potential, or an electric field pulse) whose maximum amplitude in the far downstream region decays in time. The effect of relevant plasma configuration parameters, in addition to dissipation, is investigated. Our work extends earlier studies of ion-acoustic type shock waves in pure (two-component) bi-ion plasma mixtures.

Optical Properties of Silver Nanoparticulate Glasses

NASA Astrophysics Data System (ADS)

Evans, Rachel N.; Cannavino, Sarah A.; King, Christy A.; Lamartina, Joseph A.; Magruder, Robert H.; Ferrara, Davon W.

The ion exchange method of embedding metal nanoparticles (NPs) into float glass is an often used technique of fabricating colored glasses and graded-index waveguides. The depth and size of NP formation in the glass depends on the concentration and temperature of metal ions in the molten bath. In this study we explore the dichroic properties of silver metal ion exchange restricted to only one side of a glass microscope slide using reflection and transmission spectroscopy and its dependence on temperature, concentration of silver ions, and length of time in the molten bath.

The use of isoprene as a novel dopant in negative ion atmospheric pressure photoionization mass spectrometry coupled to high-performance liquid chromatography.

PubMed

Dousty, Faezeh; O'Brien, Rob

2015-06-15

As in the case with positive ion atmospheric pressure photoionization (PI-APPI), the addition of dopants significantly improves the sensitivity of negative ion APPI (NI-APPI). However, the research on dopant-assisted-NI-APPI has been quite limited compared to the studies on dopant-assisted PI-APPI. This work presents the potential of isoprene as a novel dopant for NI-APPI. Thirteen compounds, possessing suitable gas-phase ion energetic properties in order to make stable negative ions, were selected. Dopants were continuously introduced into a tee junction prior to the ion source through a fused-silica capillary, while analytes were directly injected into the same tee. Then both were mixed with the continuous solvent from high-performance liquid chromatography (HPLC), nebulized, and entered the source. The nebulized stream was analyzed by APPI tandem quadrupole mass spectrometry in the negative ion mode. The results obtained using isoprene were compared with those obtained by using toluene as a dopant and dopant-free NI-APPI. Isoprene enhanced the ionization intensities of the studied compounds, which were found to be comparable and, in some cases, more effective than toluene. The mechanisms leading to the observed set of negative analyte ions were also discussed. Because in NI-APPI, thermal electrons, which are produced during the photoionization of a dopant, are considered the main reagent ions, both isoprene and toluene promoted the ionization of analytes through the same mechanisms, as expected. Isoprene was shown to perform well as a novel dopant for NI-APPI. Isoprene has a high photoabsorption cross section in the VUV region; therefore, its photoionization leads to a highly effective production of thermal electrons, which further promotes the ionization of analytes. In addition, isoprene is environmentally benign and less toxic compared to currently used dopants. Copyright © 2015 John Wiley & Sons, Ltd.

An analytic model for accurate spring constant calibration of rectangular atomic force microscope cantilevers.

PubMed

Li, Rui; Ye, Hongfei; Zhang, Weisheng; Ma, Guojun; Su, Yewang

2015-10-29

Spring constant calibration of the atomic force microscope (AFM) cantilever is of fundamental importance for quantifying the force between the AFM cantilever tip and the sample. The calibration within the framework of thin plate theory undoubtedly has a higher accuracy and broader scope than that within the well-established beam theory. However, thin plate theory-based accurate analytic determination of the constant has been perceived as an extremely difficult issue. In this paper, we implement the thin plate theory-based analytic modeling for the static behavior of rectangular AFM cantilevers, which reveals that the three-dimensional effect and Poisson effect play important roles in accurate determination of the spring constants. A quantitative scaling law is found that the normalized spring constant depends only on the Poisson's ratio, normalized dimension and normalized load coordinate. Both the literature and our refined finite element model validate the present results. The developed model is expected to serve as the benchmark for accurate calibration of rectangular AFM cantilevers.

Secondary electron imaging of monolayer materials inside a transmission electron microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cretu, Ovidiu, E-mail: cretu.ovidiu@nims.go.jp; Lin, Yung-Chang; Suenaga, Kazutomo

2015-08-10

A scanning transmission electron microscope equipped with a backscattered and secondary electron detector is shown capable to image graphene and hexagonal boron nitride monolayers. Secondary electron contrasts of the two lightest monolayer materials are clearly distinguished from the vacuum level. A signal difference between these two materials is attributed to electronic structure differences, which will influence the escape probabilities of the secondary electrons. Our results show that the secondary electron signal can be used to distinguish between the electronic structures of materials with atomic layer sensitivity, enhancing its applicability as a complementary signal in the analytical microscope.

Vacancy Transport and Interactions on Metal Surfaces

DTIC Science & Technology

2014-03-06

prevent obtaining systematical pictures with atomic scale resolution. Thus the experiments on adatom and mono -vacancy surface diffusion on Ag(110) were...vacuum conditions with atomic scale resolution with Scanning Tunneling Microscope (STM) and Field Ion Microscope (FIM). For each investigated material...experimental conditions for creation of surface vacancies on Au(100) has been determined and observations of surface diffusion of mono vacancies has been

The microscopic Z-pinch process of current-carrying rarefied deuterium plasma shell

NASA Astrophysics Data System (ADS)

Ning, Cheng; Feng, Zhixing; Xue, Chuang; Li, Baiwen

2015-02-01

For insight into the microscopic mechanism of Z-pinch dynamic processes, a code of two-dimensional particle-in-cell (PIC) simulation has been developed in cylindrical coordinates. In principle, the Z-pinch of current-carrying rarefied deuterium plasma shell has been simulated by means of this code. Many results related to the microscopic processes of the Z-pinch are obtained. They include the spatio-temporal distributions of electromagnetic field, current density, forces experienced by the ions and electrons, positions and energy distributions of particles, and trailing mass and current. In radial direction, the electric and magnetic forces exerted on the electrons are comparable in magnitude, while the forces exerted on the ions are mainly the electric forces. So in the Z-pinch process, the electrons are first accelerated in Z direction and get higher velocities; then, they are driven inwards to the axis at the same time by the radial magnetic forces (i.e., Lorentz forces) of them. That causes the separations between the electrons and ions because the ion mass is much larger than the electron's, and in turn a strong electrostatic field is produced. The produced electrostatic field attracts the ions to move towards the electrons. When the electrons are driven along the radial direction to arrive at the axis, they shortly move inversely due to the static repellency among them and their tiny mass, while the ions continue to move inertially inwards, and later get into stagnation, and finally scatter outwards. Near the stagnation, the energies of the deuterium ions mostly range from 0.3 to 6 keV, while the electron energies are mostly from 5 to 35 keV. The radial components, which can contribute to the pinched plasma temperature, of the most probable energies of electron and ion at the stagnation are comparable to the Bennett equilibrium temperature (about 1 keV), and also to the highest temperatures of electron and ion obtained in one dimensional radiation magnetohydrodynamic simulation of the plasma shell Z-pinch. The trailing mass is about 20% of the total mass of the shell, and the maximum trailing current is about 7% of the driven current under our trailing definition. Our PIC simulation also demonstrates that the plasma shell first experiences a snow-plow like implosion process, which is relatively stable.

Electrochemical Ionization and Analyte Charging in the Array of Micromachined UltraSonic Electrospray (AMUSE) Ion Source

PubMed Central

Forbes, Thomas P.; Degertekin, F. Levent; Fedorov, Andrei G.

2010-01-01

Electrochemistry and ion transport in a planar array of mechanically-driven, droplet-based ion sources are investigated using an approximate time scale analysis and in-depth computational simulations. The ion source is modeled as a controlled-current electrolytic cell, in which the piezoelectric transducer electrode, which mechanically drives the charged droplet generation using ultrasonic atomization, also acts as the oxidizing/corroding anode (positive mode). The interplay between advective and diffusive ion transport of electrochemically generated ions is analyzed as a function of the transducer duty cycle and electrode location. A time scale analysis of the relative importance of advective vs. diffusive ion transport provides valuable insight into optimality, from the ionization prospective, of alternative design and operation modes of the ion source operation. A computational model based on the solution of time-averaged, quasi-steady advection-diffusion equations for electroactive species transport is used to substantiate the conclusions of the time scale analysis. The results show that electrochemical ion generation at the piezoelectric transducer electrodes located at the back-side of the ion source reservoir results in poor ionization efficiency due to insufficient time for the charged analyte to diffuse away from the electrode surface to the ejection location, especially at near 100% duty cycle operation. Reducing the duty cycle of droplet/analyte ejection increases the analyte residence time and, in turn, improves ionization efficiency, but at an expense of the reduced device throughput. For applications where this is undesirable, i.e., multiplexed and disposable device configurations, an alternative electrode location is incorporated. By moving the charging electrode to the nozzle surface, the diffusion length scale is greatly reduced, drastically improving ionization efficiency. The ionization efficiency of all operating conditions considered is expressed as a function of the dimensionless Peclet number, which defines the relative effect of advection as compared to diffusion. This analysis is general enough to elucidate an important role of electrochemistry in ionization efficiency of any arrayed ion sources, be they mechanically-driven or electrosprays, and is vital for determining optimal design and operation conditions. PMID:20607111

Quantification of Carbohydrates and Related Materials Using Sodium Ion Adducts Produced by Matrix-Assisted Laser Desorption Ionization

NASA Astrophysics Data System (ADS)

Ahn, Sung Hee; Park, Kyung Man; Moon, Jeong Hee; Lee, Seong Hoon; Kim, Myung Soo

2016-11-01

The utility of sodium ion adducts produced by matrix-assisted laser desorption ionization for the quantification of analytes with multiple oxygen atoms was evaluated. Uses of homogeneous solid samples and temperature control allowed the acquisition of reproducible spectra. The method resulted in a direct proportionality between the ion abundance ratio I([A + Na]+)/I([M + Na]+) and the analyte concentration, which could be used as a calibration curve. This was demonstrated for carbohydrates, glycans, and polyether diols with dynamic range exceeding three orders of magnitude.

High resolution Thomson Parabola Spectrometer for full spectral capture of multi-species ion beams.

PubMed

Alejo, A; Kar, S; Tebartz, A; Ahmed, H; Astbury, S; Carroll, D C; Ding, J; Doria, D; Higginson, A; McKenna, P; Neumann, N; Scott, G G; Wagner, F; Roth, M; Borghesi, M

2016-08-01

We report on the experimental characterisation of laser-driven ion beams using a Thomson Parabola Spectrometer (TPS) equipped with trapezoidally shaped electric plates, proposed by Gwynne et al. [Rev. Sci. Instrum. 85, 033304 (2014)]. While a pair of extended (30 cm long) electric plates was able to produce a significant increase in the separation between neighbouring ion species at high energies, deploying a trapezoidal design circumvented the spectral clipping at the low energy end of the ion spectra. The shape of the electric plate was chosen carefully considering, for the given spectrometer configuration, the range of detectable ion energies and species. Analytical tracing of the ion parabolas matches closely with the experimental data, which suggests a minimal effect of fringe fields on the escaping ions close to the wedged edge of the electrode. The analytical formulae were derived considering the relativistic correction required for the high energy ions to be characterised using such spectrometer.

High resolution Thomson Parabola Spectrometer for full spectral capture of multi-species ion beams

NASA Astrophysics Data System (ADS)

Alejo, A.; Kar, S.; Tebartz, A.; Ahmed, H.; Astbury, S.; Carroll, D. C.; Ding, J.; Doria, D.; Higginson, A.; McKenna, P.; Neumann, N.; Scott, G. G.; Wagner, F.; Roth, M.; Borghesi, M.

2016-08-01

We report on the experimental characterisation of laser-driven ion beams using a Thomson Parabola Spectrometer (TPS) equipped with trapezoidally shaped electric plates, proposed by Gwynne et al. [Rev. Sci. Instrum. 85, 033304 (2014)]. While a pair of extended (30 cm long) electric plates was able to produce a significant increase in the separation between neighbouring ion species at high energies, deploying a trapezoidal design circumvented the spectral clipping at the low energy end of the ion spectra. The shape of the electric plate was chosen carefully considering, for the given spectrometer configuration, the range of detectable ion energies and species. Analytical tracing of the ion parabolas matches closely with the experimental data, which suggests a minimal effect of fringe fields on the escaping ions close to the wedged edge of the electrode. The analytical formulae were derived considering the relativistic correction required for the high energy ions to be characterised using such spectrometer.

High resolution Thomson Parabola Spectrometer for full spectral capture of multi-species ion beams

DOE Office of Scientific and Technical Information (OSTI.GOV)

Alejo, A.; Kar, S., E-mail: s.kar@qub.ac.uk; Ahmed, H.

2016-08-15

We report on the experimental characterisation of laser-driven ion beams using a Thomson Parabola Spectrometer (TPS) equipped with trapezoidally shaped electric plates, proposed by Gwynne et al. [Rev. Sci. Instrum. 85, 033304 (2014)]. While a pair of extended (30 cm long) electric plates was able to produce a significant increase in the separation between neighbouring ion species at high energies, deploying a trapezoidal design circumvented the spectral clipping at the low energy end of the ion spectra. The shape of the electric plate was chosen carefully considering, for the given spectrometer configuration, the range of detectable ion energies and species.more » Analytical tracing of the ion parabolas matches closely with the experimental data, which suggests a minimal effect of fringe fields on the escaping ions close to the wedged edge of the electrode. The analytical formulae were derived considering the relativistic correction required for the high energy ions to be characterised using such spectrometer.« less

Comparison of thermal analytic model with experimental test results for 30-sentimeter-diameter engineering model mercury ion thruster

NASA Technical Reports Server (NTRS)

Oglebay, J. C.

1977-01-01

A thermal analytic model for a 30-cm engineering model mercury-ion thruster was developed and calibrated using the experimental test results of tests of a pre-engineering model 30-cm thruster. A series of tests, performed later, simulated a wide range of thermal environments on an operating 30-cm engineering model thruster, which was instrumented to measure the temperature distribution within it. The modified analytic model is described and analytic and experimental results compared for various operating conditions. Based on the comparisons, it is concluded that the analytic model can be used as a preliminary design tool to predict thruster steady-state temperature distributions for stage and mission studies and to define the thermal interface bewteen the thruster and other elements of a spacecraft.

High throughput on-chip analysis of high-energy charged particle tracks using lensfree imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Luo, Wei; Shabbir, Faizan; Gong, Chao

2015-04-13

We demonstrate a high-throughput charged particle analysis platform, which is based on lensfree on-chip microscopy for rapid ion track analysis using allyl diglycol carbonate, i.e., CR-39 plastic polymer as the sensing medium. By adopting a wide-area opto-electronic image sensor together with a source-shifting based pixel super-resolution technique, a large CR-39 sample volume (i.e., 4 cm × 4 cm × 0.1 cm) can be imaged in less than 1 min using a compact lensfree on-chip microscope, which detects partially coherent in-line holograms of the ion tracks recorded within the CR-39 detector. After the image capture, using highly parallelized reconstruction and ion track analysis algorithms running on graphics processingmore » units, we reconstruct and analyze the entire volume of a CR-39 detector within ∼1.5 min. This significant reduction in the entire imaging and ion track analysis time not only increases our throughput but also allows us to perform time-resolved analysis of the etching process to monitor and optimize the growth of ion tracks during etching. This computational lensfree imaging platform can provide a much higher throughput and more cost-effective alternative to traditional lens-based scanning optical microscopes for ion track analysis using CR-39 and other passive high energy particle detectors.« less

Subsurface examination of a foliar biofilm using scanning electron- and focused-ion-beam microscopy

USDA-ARS?s Scientific Manuscript database

The dual beam scanning electron microscope, equipped with both a focused ion- and scanning electron- beam (FIB SEM) is a novel tool for the exploration of the subsurface structure of biological tissues. The FIB is capable of removing small cross sections to view the subsurface features and may be s...

Determination of the sequence of intersecting lines using Focused Ion Beam/Scanning Electron Microscope.

PubMed

Kim, Jiye; Kim, MinJung; An, JinWook; Kim, Yunje

2016-05-01

The aim of this study was to verify that the combination of focused ion beam (FIB) and scanning electron microscope/energy-dispersive X-ray (SEM/EDX) could be applied to determine the sequence of line crossings. The samples were transferred into FIB/SEM for FIB milling and an imaging operation. EDX was able to explore the chemical components and the corresponding elemental distribution in the intersection. The technique was successful in determining the sequence of heterogeneous line intersections produced using gel pens and red sealing ink with highest success rate (100% correctness). These observations show that the FIB/SEM was the appropriate instrument for an overall examination of document. © 2016 American Academy of Forensic Sciences.

Recovery of Background Structures in Nanoscale Helium Ion Microscope Imaging.

PubMed

Carasso, Alfred S; Vladár, András E

2014-01-01

This paper discusses a two step enhancement technique applicable to noisy Helium Ion Microscope images in which background structures are not easily discernible due to a weak signal. The method is based on a preliminary adaptive histogram equalization, followed by 'slow motion' low-exponent Lévy fractional diffusion smoothing. This combined approach is unexpectedly effective, resulting in a companion enhanced image in which background structures are rendered much more visible, and noise is significantly reduced, all with minimal loss of image sharpness. The method also provides useful enhancements of scanning charged-particle microscopy images obtained by composing multiple drift-corrected 'fast scan' frames. The paper includes software routines, written in Interactive Data Language (IDL),(1) that can perform the above image processing tasks.

Effect of Curcumin on the metal ion induced fibrillization of Amyloid-β peptide

NASA Astrophysics Data System (ADS)

Banerjee, Rona

2014-01-01

The effect of Curcumin on Cu(II) and Zn(II) induced oligomerization and protofibrillization of the amyloid-beta (Aβ) peptide has been studied by spectroscopic and microscopic methods. Curcumin could significantly reduce the β-sheet content of the peptide in a time dependent manner. It also plays an antagonistic role in β-sheet formation that is promoted by metal ions like Cu(II) and Zn(II) as observed by Circular Dichroism (CD) spectroscopy. Atomic force microscopic (AFM) images show that spontaneous fibrillization of the peptide occurs in presence of Cu(II) and Zn(II) but is inhibited on incubation of the peptide with Curcumin indicating the beneficial role of Curcumin in preventing the aggregation of Aβ peptide.

An analytical expression for ion velocities at the wall including the sheath electric field and surface biasing for erosion modeling at JET ILW

DOE PAGES

Borodkina, I.; Borodin, D.; Brezinsek, S.; ...

2017-04-12

For simulation of plasma-facing component erosion in fusion experiments, an analytical expression for the ion velocity just before the surface impact including the local electric field and an optional surface biasing effect is suggested. Energy and angular impact distributions and the resulting effective sputtering yields were produced for several experimental scenarios at JET ILW mostly involving PFCs exposed to an oblique magnetic field. The analytic solution has been applied as an improvement to earlier ERO modelling of localized, Be outer limiter, RF-enhanced erosion, modulated by toggling of a remote, however magnetically connected ICRH antenna. The effective W sputtering yields duemore » to D and Be ion impact in Type-I and Type-III ELMs and inter-ELM conditions were also estimated using the analytical approach and benchmarked by spectroscopy. The intra-ELM W sputtering flux increases almost 10 times in comparison to the inter-ELM flux.« less

Fast semi-analytical method for precise prediction of ion energy distribution functions and sheath electric field in multi-frequency capacitively coupled plasmas

NASA Astrophysics Data System (ADS)

Chen, Wencong; Zhang, Xi; Diao, Dongfeng

2018-05-01

We propose a fast semi-analytical method to predict ion energy distribution functions and sheath electric field in multi-frequency capacitively coupled plasmas, which are difficult to measure in commercial plasma reactors. In the intermediate frequency regime, the ion density within the sheath is strongly modulated by the low-frequency sheath electric field, making the time-independent ion density assumption employed in conventional models invalid. Our results are in a good agreement with experimental measurements and computer simulations. The application of this method will facilitate the understanding of ion–material interaction mechanisms and development of new-generation plasma etching devices.

Analytical and Experimental Nanomechanical Approaches to Understanding the Ductile-to-Brittle Transition

NASA Astrophysics Data System (ADS)

Hintsala, Eric Daniel

This dissertation presents progress towards understanding the ductile-to-brittle transition (DBT) using a mixture of nanomechanical experiments and an analytical model. The key concept is dislocation shielding of crack tips, which is occurs due to a dislocation back stress. In order to properly evaluate the role of these interactions, in-situ experiments are ideal by reducing the number of interacting dislocations and allowing direct observation of cracking behavior and the dislocations themselves. First, in-situ transmission electron microscope (TEM) compression experiments of plasma-synthesized silicon nanocubes (NCs) are presented which shows plastic strains greater than 50% in a semi-brittle material. The mechanical properties are discussed and plasticity mechanisms are identified using post-mortem imaging with a combination of dark field and high-resolution imaging. This observations help to develop a back stress model which is used to fit the hardening regime. This represents the first study of its kind where back stresses are used in a discrete manner to match hardening rates. However, the important measurable quantities for evaluating the DBT include fracture toughness values and energetic activation parameters for cracking and plasticity. In order to do this, a new method for doing in-situ fracture experiments is explored. This method is pre-notched three point bending experiments, which were fabricated by focused ion beam (FIB) milling. Two different materials are evaluated: a model ductile material, Nitronic 50, an austenitic steel alloy, and a model brittle material, silicon. These experiments are performed in-situ scanning electron microscope (SEM) and TEM and explore different aspects including electron backscatter diffraction (EBSD) to track deformation in SEM scale experiments, pre-notching using a converged TEM beam to produce sharper notches better replicating natural cracks, etching procedures to reduce residual FIB damage and elevated temperature experiments. Lastly, an analytical method to predict DBTs is presented which can account for effects of strain rate, temperature and impurity presence. The model is tested by pre-existing data on macroscopic compact tension specimens of single crystal Fe-3%Si. Next, application of the model to nano/micro scale fracture toughness experiments is explored and the large number of confounding variables is discussed in detail. A first attempt at fitting is also presented.

Characterization and source term assessments of radioactive particles from Marshall Islands using non-destructive analytical techniques

NASA Astrophysics Data System (ADS)

Jernström, J.; Eriksson, M.; Simon, R.; Tamborini, G.; Bildstein, O.; Marquez, R. Carlos; Kehl, S. R.; Hamilton, T. F.; Ranebo, Y.; Betti, M.

2006-08-01

Six plutonium-containing particles stemming from Runit Island soil (Marshall Islands) were characterized by non-destructive analytical and microanalytical methods. Composition and elemental distribution in the particles were studied with synchrotron radiation based micro X-ray fluorescence spectrometry. Scanning electron microscope equipped with energy dispersive X-ray detector and with wavelength dispersive system as well as a secondary ion mass spectrometer were used to examine particle surfaces. Based on the elemental composition the particles were divided into two groups: particles with pure Pu matrix, and particles where the plutonium is included in Si/O-rich matrix being more heterogenously distributed. All of the particles were identified as nuclear fuel fragments of exploded weapon components. As containing plutonium with low 240Pu/ 239Pu atomic ratio, less than 0.065, which corresponds to weapons-grade plutonium or a detonation with low fission yield, the particles were identified to originate from the safety test and low-yield tests conducted in the history of Runit Island. The Si/O-rich particles contained traces of 137Cs ( 239 + 240 Pu/ 137Cs activity ratio higher than 2500), which indicated that a minor fission process occurred during the explosion. The average 241Am/ 239Pu atomic ratio in the six particles was 3.7 × 10 - 3 ± 0.2 × 10 - 3 (February 2006), which indicated that plutonium in the different particles had similar age.

Transmission geometry laserspray ionization vacuum using an atmospheric pressure inlet.

PubMed

Lutomski, Corinne A; El-Baba, Tarick J; Inutan, Ellen D; Manly, Cory D; Wager-Miller, James; Mackie, Ken; Trimpin, Sarah

2014-07-01

This represents the first report of laserspray ionization vacuum (LSIV) with operation directly from atmospheric pressure for use in mass spectrometry. Two different types of electrospray ionization source inlets were converted to LSIV sources by equipping the entrance of the atmospheric pressure inlet aperture with a customized cone that is sealed with a removable glass plate holding the matrix/analyte sample. A laser aligned in transmission geometry (at 180° relative to the inlet) ablates the matrix/analyte sample deposited on the vacuum side of the glass slide. Laser ablation from vacuum requires lower inlet temperature relative to laser ablation at atmospheric pressure. However, higher inlet temperature is required for high-mass analytes, for example, α-chymotrypsinogen (25.6 kDa). Labile compounds such as gangliosides and cardiolipins are detected in the negative ion mode directly from mouse brain tissue as intact doubly deprotonated ions. Multiple charging enhances the ion mobility spectrometry separation of ions derived from complex tissue samples.

Transmission Geometry Laserspray Ionization Vacuum Using an Atmospheric Pressure Inlet

PubMed Central

2015-01-01

This represents the first report of laserspray ionization vacuum (LSIV) with operation directly from atmospheric pressure for use in mass spectrometry. Two different types of electrospray ionization source inlets were converted to LSIV sources by equipping the entrance of the atmospheric pressure inlet aperture with a customized cone that is sealed with a removable glass plate holding the matrix/analyte sample. A laser aligned in transmission geometry (at 180° relative to the inlet) ablates the matrix/analyte sample deposited on the vacuum side of the glass slide. Laser ablation from vacuum requires lower inlet temperature relative to laser ablation at atmospheric pressure. However, higher inlet temperature is required for high-mass analytes, for example, α-chymotrypsinogen (25.6 kDa). Labile compounds such as gangliosides and cardiolipins are detected in the negative ion mode directly from mouse brain tissue as intact doubly deprotonated ions. Multiple charging enhances the ion mobility spectrometry separation of ions derived from complex tissue samples. PMID:24896880

Bio-reinforced self-healing concrete using magnetic iron oxide nanoparticles.

PubMed

Seifan, Mostafa; Sarmah, Ajit K; Ebrahiminezhad, Alireza; Ghasemi, Younes; Samani, Ali Khajeh; Berenjian, Aydin

2018-03-01

Immobilization has been reported as an efficient technique to address the bacterial vulnerability for application in bio self-healing concrete. In this study, for the first time, magnetic iron oxide nanoparticles (IONs) are being practically employed as the protective vehicle for bacteria to evaluate the self-healing performance in concrete environment. Magnetic IONs were successfully synthesized and characterized using different techniques. The scanning electron microscope (SEM) images show the efficient adsorption of nanoparticles to the Bacillus cells. Microscopic observation illustrates that the incorporation of the immobilized bacteria in the concrete matrix resulted in a significant crack healing behavior, while the control specimen had no healing characteristics. Analysis of bio-precipitates revealed that the induced minerals in the cracks were calcium carbonate. The effect of magnetic immobilized cells on the concrete water absorption showed that the concrete specimens supplemented with decorated bacteria with IONs had a higher resistance to water penetration. The initial and secondary water absorption rates in bio-concrete specimens were 26% and 22% lower than the control specimens. Due to the compatible behavior of IONs with the concrete compositions, the results of this study proved the potential application of IONs for developing a new generation of bio self-healing concrete.

Coated-Wire Ion Selective Electrodes and Their Application to the Teaching Laboratory.

ERIC Educational Resources Information Center

Martin, Charles R.; Freiser, Henry

1980-01-01

Describes the procedures for construction of a nitrate coated-wire ion selective electrode and suggests experiments for evaluation of electrode response and illustration of typical analytical applications of ion selective electrodes. (CS)

Infrared Ion Spectroscopy at Felix: Applications in Peptide Dissociation and Analytical Chemistry

NASA Astrophysics Data System (ADS)

Oomens, Jos

2016-06-01

Infrared free electron lasers such as those in Paris, Berlin and Nijmegen have been at the forefront of the development of infrared ion spectroscopy. In this contribution, I will give an overview of new developments in IR spectroscopy of stored ions at the FELIX Laboratory. In particular, I will focus on recent developments made possible by the coupling of a new commercial ion trap mass spectrometer to the FELIX beamline. The possibility to record IR spectra of mass-selected molecular ions and their reaction products has in recent years shed new light on our understanding of collision induced dissociation (CID) reactions of protonated peptides in mass spectrometry (MS). We now show that it is possible to record IR spectra for the products of electron transfer dissociation (ETD) reactions [M + nH]n+ + A- → [M + nH](n-1)+ + A → {dissociation of analyte} These reactions are now widely used in novel MS-based protein sequencing strategies, but involve complex radical chemistry. The spectroscopic results allow stringent verification of computationally predicted product structures and hence reaction mechanisms and H-atom migration. The sensitivity and high dynamic range of a commercial mass spectrometer also allows us to apply infrared ion spectroscopy to analytes in complex "real-life" mixtures. The ability to record IR spectra with the sensitivity of mass-spectrometric detection is unrivalled in analytical sciences and is particularly useful in the identification of small (biological) molecules, such as in metabolomics. We report preliminary results of a pilot study on the spectroscopic identification of small metabolites in urine and plasma samples.

Ion beam sputter modification of the surface morphology of biological implants

NASA Technical Reports Server (NTRS)

Weigand, A. J.; Banks, B. A.

1976-01-01

The surface chemistry and texture of materials used for biological implants may significantly influence their performance and biocompatibility. Recent interest in the microscopic control of implant surface texture has led to the evaluation of ion beam sputtering as a potentially useful surface roughening technique. Ion sources, similar to electron bombardment ion thrusters designed for propulsive applications, are used to roughen the surfaces of various biocompatible alloys or polymer materials. These materials are typically used for dental implants, orthopedic prostheses, vascular prostheses, and artificial heart components. Masking techniques and resulting surface textures are described along with progress concerning evaluation of the biological response to the ion beam sputtered surfaces.

Ion-beam-sputter modification of the surface morphology of biological implants

NASA Technical Reports Server (NTRS)

Weigand, A. J.; Banks, B. A.

1977-01-01

The surface chemistry and texture of materials used for biological implants may significantly influence their performance and biocompatibility. Recent interest in the microscopic control of implant surface texture has led to the evaluation of ion-beam sputtering as a potentially useful surface roughening technique. Ion sources, similar to electron-bombardment ion thrusters designed for propulsive applications, are used to roughen the surfaces of various biocompatible alloys or polymer materials. These materials are typically used for dental implants, orthopedic prostheses, vascular prostheses, and artificial heart components. Masking techniques and resulting surface textures are described along with progress concerning evaluation of the biological response to the ion-beam-sputtered surfaces.

Concomitant Ion Effects on Isotope Ratio Measurements with Liquid Sampling – Atmospheric Pressure Glow Discharge Ion Source Orbitrap Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoegg, Edward D.; Marcus, R. Kenneth; Hager, Georg

2018-02-28

In an effort to understand and improve the accuracy and precision of the liquid sampling- atmospheric pressure glow discharge (LS-APGD)/Orbitrap system, effects of concomitant ions on the acquired mass spectra are examined and presented. The LS-APGD/ Orbitrap instrument system is capable of high quality isotope ratio measurements, which are of high analytical interest for nuclear non-proliferation detection applications. The presence of background and concomitant ions (water clusters, matrix, and other analytes) has presented limitations in earlier studies. In order to mitigate these effects, an alternative quadrupole-Orbitrap hybrid mass spectrometer was employed in this study. This instrument configuration has a quadrupolemore » mass filter preceding the Orbitrap to filter-out undesired non-analyte ions. Results are presented for the analysis of U in the presence of Rb, Ag, Ba, and Pb as concomitants, each present at 5 µg/mL concentration. Progressive filtering of each concomitant ion shows steadily improved U isotope ratio performance. Ultimately, a 235U/238U ratio of 0.007133, with a relative accuracy of -2.1% and a relative standard deviation of 0.087% was achieved using this system, along with improved calibration linearity and lowered limits of detection. The resultant performance compares very favorably with other commonly accepted isotope ratio measurement platforms - surprisingly so for an ion trap type mass spectrometry instrument.« less

Zn deposition at the bone cartilage interface in equine articular cartilage

NASA Astrophysics Data System (ADS)

Bradley, D. A.; Moger, C. J.; Winlove, C. P.

2007-09-01

In articular cartilage metalloproteinases, a family of enzymes whose function relies on the presence of divalent cations such as Zn and Ca plays a central role in the normal processes of growth and remodelling and in the degenerative and inflammatory processes of arthritis. Another important enzyme, alkaline phosphatase, involved in cartilage mineralisation also relies on metallic cofactors. The local concentration of divalent cations is therefore of considerable interest in cartilage pathophysiology and several authors have used synchrotron X-ray fluorescence (XRF) to map metal ion distributions in bone and cartilage. We report use of a bench-top XRF analytical microscope, providing spatial resolution of 10 μm and applicable to histological sections, facilitating correlation of the distribution with structural features. The study seeks to establish the elemental distribution in normal tissue as a precursor to investigation of changes in disease. For six samples prepared from equine metacarpophalangeal joint, we observed increased concentration of Zn and Sr ions around the tidemark between normal and mineralised cartilage. This is believed to be an active site of remodelling but its composition has hitherto lacked detailed characterization. We also report preliminary results on two of the samples using Proton-Induced X-ray Emission (PIXE). This confirms our previous observations using synchrotron-based XRF of enhanced deposition of Sr and Zn at the surface of the subchondral bone and in articular cartilage.

Synthesis, characterization and analytical application of hybrid; acrylamide zirconium (IV) arsenate a cation exchanger, effect of dielectric constant on distribution coefficient of metal ions.

PubMed

Nabi, Syed A; Shalla, Aabid H

2009-04-30

A new hybrid inorganic-organic cation exchanger acrylamide zirconium (IV) arsenate has been synthesized, characterized and its analytical application explored. The effect of experimental parameters such as mixing ratio of reagents, temperature, and pH on the properties of material has been studied. FTIR, TGA, X-ray, UV-vis spectrophotometry, SEM and elemental analysis were used to determine the physiochemical properties of this hybrid ion exchanger. The material behaves as a monofunctional acid with ion-exchange capacity of 1.65 meq/g for Na(+) ions. The chemical stability data reveals that the exchanger is quite stable in mineral acids, bases and fairly stable in organic solvents, while as thermal analysis shows that the material retain 84% of its ion-exchange capacity up to 600 degrees C. Adsorption behavior of metal ions in solvents with increasing dielectric constant has also been explored. The sorption studies reveal that the material is selective for Pb(2+) ions. The analytical utility of the material has been explored by achieving some binary separations of metal ions on its column. Pb(2+) has been selectively removed from synthetic mixtures containing Mg(2+), Ca(2+), Sr(2+), Zn(2+) and Cu(2+), Al(3+), Ni(2+), Fe(3+). In order to demonstrate practical utility of the material quantitative separation of the Cu(2+) and Zn(2+) in brass sample has been achieved on its columns.

U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

NASA Astrophysics Data System (ADS)

Bischoff, James L.; Wooden, Joe; Murphy, Fred; Williams, Ross W.

2005-04-01

We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ˜60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few μm deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems.

U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

USGS Publications Warehouse

Bischoff, J.L.; Wooden, J.; Murphy, F.; Williams, Ross W.

2005-01-01

We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ???60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few ??m deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems. Copyright ?? 2005 Elsevier Ltd.

Investigation of argon ion sputtering on the secondary electron emission from gold samples

NASA Astrophysics Data System (ADS)

Yang, Jing; Cui, Wanzhao; Li, Yun; Xie, Guibai; Zhang, Na; Wang, Rui; Hu, Tiancun; Zhang, Hongtai

2016-09-01

Secondary electron (SE) yield, δ, is a very sensitive surface property. The values of δ often are not consistent for even identical materials. The influence of surface changes on the SE yield was investigated experimentally in this article. Argon ion sputtering was used to remove the contamination from the surface. Surface composition was monitored by X-ray photoelectron spectroscopy (XPS) and surface topography was scanned by scanning electron microscope (SEM) and atomic force microscope (AFM) before and after every sputtering. It was found that argon sputtering can remove contamination and roughen the surface. An ;equivalent work function; is presented in this thesis to establish the relationship between SE yield and surface properties. Argon ion sputtering of 1.5keV leads to a significant increase of so called ;work function; (from 3.7 eV to 6.0 eV), and a decrease of SE yield (from 2.01 to 1.54). These results provided a new insight into the influence of surface changes on the SE emission.

Helium Ion Beam Microscopy for Copper Grain Identification in BEOL Structures

NASA Astrophysics Data System (ADS)

van den Boom, Ruud J. J.; Parvaneh, Hamed; Voci, Dave; Huynh, Chuong; Stern, Lewis; Dunn, Kathleen A.; Lifshin, Eric

2009-09-01

Grain size determination in advanced metallization structures requires a technique with resolution ˜2 nm, with a high signal-to-noise ratio and high orientation-dependant contrast for unambiguous identification of grain boundaries. Ideally, such a technique would also be capable of high-throughput and rapid time-to-knowledge. The Helium Ion Microscope (HIM) offers one possibility for achieving these aims in a single platform. This article compares the performance of the HIM with Focused Ion Beam, Scanning Electron and Transmission Electron Microscopes, in terms of achievable image resolution and contrast, using plan-view and cross-sectional imaging of electroplated samples. Although the HIM is capable of sub-nanometer beam diameter, the low signal-to-noise ratio in the images necessitates signal averaging, which degrades the measured image resolution to 6-8 nm. Strategies for improving S/N are discussed in light of the trade-off between beam current and probe size, accelerating voltage, and dwell time.

Modeling of Yb3+/Er3+-codoped microring resonators

NASA Astrophysics Data System (ADS)

Vallés, Juan A.; Gălătuş, Ramona

2015-03-01

The performance of a highly Yb3+/Er3+-codoped phosphate glass add-drop microring resonator is numerically analyzed. The model assumes resonant behaviour of both pump and signal powers and the dependences of pump intensity build-up inside the microring resonator and of the signal transfer functions to the device through and drop ports are evaluated. Detailed equations for the evolution of the rare-earth ions levels population densities and the propagation of the optical powers inside the microring resonator are included in the model. Moreover, due to the high dopant concentrations considered, the microscopic statistical formalism based on the statistical average of the excitation probability of the Er3+ ion in a microscopic level has been used to describe energy-transfer inter-atomic mechanisms. Realistic parameters and working conditions are used for the calculations. Requirements to achieve amplification and laser oscillation within these devices are obtainable as a function of rare earth ions concentration and coupling losses.

A sample preparation method for recovering suppressed analyte ions in MALDI TOF MS.

PubMed

Lou, Xianwen; de Waal, Bas F M; Milroy, Lech-Gustav; van Dongen, Joost L J

2015-05-01

In matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS), analyte signals can be substantially suppressed by other compounds in the sample. In this technical note, we describe a modified thin-layer sample preparation method that significantly reduces the analyte suppression effect (ASE). In our method, analytes are deposited on top of the surface of matrix preloaded on the MALDI plate. To prevent embedding of analyte into the matrix crystals, the sample solution were prepared without matrix and efforts were taken not to re-dissolve the preloaded matrix. The results with model mixtures of peptides, synthetic polymers and lipids show that detection of analyte ions, which were completely suppressed using the conventional dried-droplet method, could be effectively recovered by using our method. Our findings suggest that the incorporation of analytes in the matrix crystals has an important contributory effect on ASE. By reducing ASE, our method should be useful for the direct MALDI MS analysis of multicomponent mixtures. Copyright © 2015 John Wiley & Sons, Ltd.

WE-H-BRA-09: Application of a Modified Microdosimetric-Kinetic Model to Analyze Relative Biological Effectiveness of Ions Relevant to Light Ion Therapy Using the Particle Heavy Ion Transport System

DOE Office of Scientific and Technical Information (OSTI.GOV)

Butkus, M; Palmer, T

Purpose: To evaluate the dose and biological effectiveness of various ions that could potentially be used for actively scanned particle therapy. Methods: The PHITS Monte Carlo code paired with a microscopic analytical function was used to determine probability distribution functions of the lineal energy in 0.3µm diameter spheres throughout a water phantom. Twenty million primary particles for 1H beams and ten million particles for 4He, 7Li, 10B, 12C, 14N, 16O, and 20Ne were simulated for 0.6cm diameter pencil beams. Beam energies corresponding to Bragg peak depths of 50, 100, 150, 200, 250, and 300mm were used and evaluated transversely everymore » millimeter and radially in annuli with outer radius of 1.0, 2.0, 3.0, 3.2, 3.4, 3.6, 4.0, 5.0, 10.0, 15.0, 20.0 and 25.0mm. The acquired probability distributions were reduced to dose-mean lineal energies and applied to the modified microdosimetric kinetic model for five different cell types to calculate relative biological effectiveness (RBE) compared to 60Co beams at the 10% survival threshold. The product of the calculated RBEs and the simulated physical dose was taken to create biological dose and comparisons were then made between the various ions. Results: Transversely, the 10B beam was seen to minimize relative biological dose in both the constant and accelerated dose change regions, proximal to the Bragg Peak, for all beams traveling greater than 50mm. For the 50mm beam, 7Li was seen to provide the most optimal biological dose profile. Radially small fluctuations (<4.2%) were seen in RBE while physical dose was greater than 1% for all beams. Conclusion: Even with the growing usage of 12C, it may not be the most optimal ion in all clinical situations. Boron was calculated to have slightly enhanced RBE characteristics, leading to lower relative biological doses.« less

Electron cooling of a bunched ion beam in a storage ring

NASA Astrophysics Data System (ADS)

Zhao, He; Mao, Lijun; Yang, Jiancheng; Xia, Jiawen; Yang, Xiaodong; Li, Jie; Tang, Meitang; Shen, Guodong; Ma, Xiaoming; Wu, Bo; Wang, Geng; Ruan, Shuang; Wang, Kedong; Dong, Ziqiang

2018-02-01

A combination of electron cooling and rf system is an effective method to compress the beam bunch length in storage rings. A simulation code based on multiparticle tracking was developed to calculate the bunched ion beam cooling process, in which the electron cooling, intrabeam scattering (IBS), ion beam space-charge field, transverse and synchrotron motion are considered. Meanwhile, bunched ion beam cooling experiments have been carried out in the main cooling storage ring (CSRm) of the Heavy Ion Research Facility in Lanzhou, to investigate the minimum bunch length obtained by the cooling method, and study the dependence of the minimum bunch length on beam and machine parameters. The experiments show comparable results to those from simulation. Based on these simulations and experiments, we established an analytical model to describe the limitation of the bunch length of the cooled ion beam. It is observed that the IBS effect is dominant for low intensity beams, and the space-charge effect is much more important for high intensity beams. Moreover, the particles will not be bunched for much higher intensity beam. The experimental results in CSRm show a good agreement with the analytical model in the IBS dominated regime. The simulation work offers us comparable results to those from the analytical model both in IBS dominated and space-charge dominated regimes.

Estimation of changes in nickel and chromium content in nickel-titanium and stainless steel orthodontic wires used during orthodontic treatment: An analytical and scanning electron microscopic study.

PubMed

Kararia, Vandana; Jain, Pradeep; Chaudhary, Seema; Kararia, Nitin

2015-01-01

The biocompatibility of orthodontic dental alloys has been investigated over the past 20 years, but the results have been inconclusive. The study compares standard 3 M Unitek nickel-titanium (NiTi) and stainless steel archwires with locally available JJ orthodontics wires. Scanning electron microscope (SEM) study of surface changes and complexometric titration to study compositional change was performed. Ten archwires each of group 1-3 M 0.016" NiTi, group 2-JJ 0.016" NiTi, group 3-3 M 0.019" *0.025" SS and group 4-JJ SS contributed a 10 mm piece of wire for analysis prior to insertion in the patient and 6 weeks post insertion. SEM images were recorded at ×2000, ×4000 and ×6000 magnification. The same samples were subjected to complexiometric titration using ethylenediaminetetraacetic acid to gauge the actual change in the composition. The SEM images of all the archwires showed marked changes with deep scratches and grooves and dark pitting corrosion areas post intraoral use. 3M wires showed an uniform criss-cross pattern in as received wires indicating a coating which was absent after intraoral use. There was a significant release of Nickel and Chromium from both group 3 and 4. Group 2 wires released ions significantly more than group 1 (P = 0.0). Extensive and stringent trials are required before certifying any product to be used in Orthodontics.

High-pressure ion source combined with an in-axis ion trap mass spectrometer. 1. Instrumentation and applications

PubMed

Mathurin; Faye; Brunot; Tabet; Wells; Fuche

2000-10-15

A new combination of a dual EI/CI ion source with a quadrupole ion trap mass spectrometer has been realized in order to efficiently produce negative ions in the reaction cell. Analysis of volatile compounds was performed under negative ion chemical ionization (NICI) during a reaction period where selected reactant negative ions, previously produced in the external ion source, were allowed to interact with molecules, introduced by hyphenated techniques such as gas chromatography. The O2*-, CH3O-, and Cl- reactant ions were used in this study to ensure specific ion/molecule interactions such as proton transfer, nucleophilic displacement, or charge exchange processes, respectively leading to even-electron species, i.e., deprotonated [M - H]- molecules, diagnostic [M - R]- ions, or odd-electron M*- molecular species. The reaction orientation depends on the thermochemistry of reactions within kinetic controls. First analytical results are presented here for the trace-level detection of several contaminants under NICI/Cl- conditions. Phosphorus-containing compounds (malathion, ethyl parathion, and methyl parathion as representative for pesticides) and nitro-containing compounds (2,4,6-trinitrotoluene for explosive material) have been chosen in order to explore the analytical ability of this promising instrumental coupling.

Particle nonuniformity effects on particle cloud flames in low gravity

NASA Technical Reports Server (NTRS)

Berlad, A. L.; Tangirala, V.; Seshadri, K.; Facca, L. T.; Ogrin, J.; Ross, H.

1991-01-01

Experimental and analytical studies of particle cloud combustion at reduced gravity reveal the substantial roles that particle cloud nonuniformities may play in particle cloud combustion. Macroscopically uniform, quiescent particle cloud systems (at very low gravitational levels and above) sustain processes which can render them nonuniform on both macroscopic and microscopic scales. It is found that a given macroscopically uniform, quiescent particle cloud flame system can display a range of microscopically nonuniform features which lead to a range of combustion features. Microscopically nonuniform particle cloud distributions are difficult experimentally to detect and characterize. A uniformly distributed lycopodium cloud of particle-enriched microscopic nonuniformities in reduced gravity displays a range of burning velocities for any given overall stoichiometry. The range of observed and calculated burning velocities corresponds to the range of particle enriched concentrations within a characteristic microscopic nonuniformity. Sedimentation effects (even in reduced gravity) are also examined.

A Statistical Physicist's Approach to Biological Motion: From the the Kinesin Walk to Muscle Contraction

NASA Astrophysics Data System (ADS)

Vicsek, Tamas

1997-03-01

It is demonstrated that a wide range of experimental results on biological motion can be successfully interpreted in terms of statistical physics motivated models taking into account the relevant microscopic details of motor proteins and allowing analytic solutions. Two important examples are considered, i) the motion of a single kinesin molecule along microtubules inside individual cells and ii) muscle contraction which is a macroscopic phenomenon due to the collective action of a large number of myosin heads along actin filaments. i) Recently individual two-headed kinesin molecules have been studied in in vitro motility assays revealing a number of their peculiar transport properties. Here we propose a simple and robust model for the kinesin stepping process with elastically coupled Brownian heads showing all of these properties. The analytic treatment of our model results in a very good fit to the experimental data and practically has no free parameters. ii) Myosin is an ATPase enzyme that converts the chemical energy stored in ATP molecules into mechanical work. During muscle contraction, the myosin cross-bridges attach to the actin filaments and exert force on them yielding a relative sliding of the actin and myosin filaments. In this paper we present a simple mechanochemical model for the cross-bridge interaction involving the relevant kinetic data and providing simple analytic solutions for the mechanical properties of muscle contraction, such as the force-velocity relationship or the relative number of the attached cross-bridges. So far the only analytic formula which could be fitted to the measured force-velocity curves has been the well known Hill equation containing parameters lacking clear microscopic origin. The main advantages of our new approach are that it explicitly connects the mechanical data with the kinetic data and the concentration of the ATP and ATPase products and as such it leads to new analytic solutions which agree extremely well with a wide range of experimental curves, while the parameters of the corresponding expressions have well defined microscopic meaning.

Nonlinear field equations for aligning self-propelled rods.

PubMed

Peshkov, Anton; Aranson, Igor S; Bertin, Eric; Chaté, Hugues; Ginelli, Francesco

2012-12-28

We derive a set of minimal and well-behaved nonlinear field equations describing the collective properties of self-propelled rods from a simple microscopic starting point, the Vicsek model with nematic alignment. Analysis of their linear and nonlinear dynamics shows good agreement with the original microscopic model. In particular, we derive an explicit expression for density-segregated, banded solutions, allowing us to develop a more complete analytic picture of the problem at the nonlinear level.

Self-regenerating Nanotips: Indestructable Field-emission Cathodes for Low-power Electric Propulsion

DTIC Science & Technology

2010-09-27

Field Emission Scanning Electron Microscope. The chamber was evacuated using a series of three ion pumps and vacuum pressure of 10-7 Torr was...backed by a 110-L/min dry scroll pump . The chamber is also equipped with a 300-L/s combination ion/sublimation pump that can maintain pressure of...Torr for 2 to 24 hours and then the ion pump was turned off to let the vacuum pressure slowly increase while observing the electron emission

Proxy-SU(3) symmetry in heavy deformed nuclei

NASA Astrophysics Data System (ADS)

Bonatsos, Dennis; Assimakis, I. E.; Minkov, N.; Martinou, Andriana; Cakirli, R. B.; Casten, R. F.; Blaum, K.

2017-06-01

Background: Microscopic calculations of heavy nuclei face considerable difficulties due to the sizes of the matrices that need to be solved. Various approximation schemes have been invoked, for example by truncating the spaces, imposing seniority limits, or appealing to various symmetry schemes such as pseudo-SU(3). This paper proposes a new symmetry scheme also based on SU(3). This proxy-SU(3) can be applied to well-deformed nuclei, is simple to use, and can yield analytic predictions. Purpose: To present the new scheme and its microscopic motivation, and to test it using a Nilsson model calculation with the original shell model orbits and with the new proxy set. Method: We invoke an approximate, analytic, treatment of the Nilsson model, that allows the above vetting and yet is also transparent in understanding the approximations involved in the new proxy-SU(3). Results: It is found that the new scheme yields a Nilsson diagram for well-deformed nuclei that is very close to the original Nilsson diagram. The specific levels of approximation in the new scheme are also shown, for each major shell. Conclusions: The new proxy-SU(3) scheme is a good approximation to the full set of orbits in a major shell. Being able to replace a complex shell model calculation with a symmetry-based description now opens up the possibility to predict many properties of nuclei analytically and often in a parameter-free way. The new scheme works best for heavier nuclei, precisely where full microscopic calculations are most challenged. Some cases in which the new scheme can be used, often analytically, to make specific predictions, are shown in a subsequent paper.

Control of Analyte Electrolysis in Electrospray Ionization Mass Spectrometry Using Repetitively Pulsed High Voltage

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kertesz, Vilmos; Van Berkel, Gary J

2011-01-01

Analyte electrolysis using a repetitively pulsed high voltage ion source was investigated and compared to that using a regular, continuously operating direct current high voltage ion source in electrospray ionization mass spectrometry. The extent of analyte electrolysis was explored as a function of the length and frequency of the high voltage pulse using the model compound reserpine in positive ion mode. Using +5 kV as the maximum high voltage amplitude, reserpine was oxidized to its 2, 4, 6 and 8-electron oxidation products when direct current high voltage was employed. In contrast, when using a pulsed high voltage, oxidation of reserpinemore » was eliminated by employing the appropriate high voltage pulse length and frequency. This effect was caused by inefficient mass transport of the analyte to the electrode surface during the duration of the high voltage pulse and the subsequent relaxation of the emitter electrode/ electrolyte interface during the time period when the high voltage was turned off. This mode of ESI source operation allows for analyte electrolysis to be quickly and simply switched on or off electronically via a change in voltage pulse variables.« less

Enhancing image contrast of carbon nanotubes on cellular background using helium ion microscope by varying helium ion fluence.

PubMed

Dykas, M M; Poddar, K; Yoong, S L; Viswanathan, V; Mathew, S; Patra, A; Saha, S; Pastorin, G; Venkatesan, T

2018-01-01

Carbon nanotubes (CNTs) have become an important nano entity for biomedical applications. Conventional methods of their imaging, often cannot be applied in biological samples due to an inadequate spatial resolution or poor contrast between the CNTs and the biological sample. Here we report a unique and effective detection method, which uses differences in conductivities of carbon nanotubes and HeLa cells. The technique involves the use of a helium ion microscope to image the sample with the surface charging artefacts created by the He + and neutralised by electron flood gun. This enables us to obtain a few nanometre resolution images of CNTs in HeLa Cells with high contrast, which was achieved by tailoring the He + fluence. Charging artefacts can be efficiently removed for conductive CNTs by a low amount of electrons, the fluence of which is not adequate to discharge the cell surface, resulting in high image contrast. Thus, this technique enables rapid detection of any conducting nano structures on insulating cellular background even in large fields of view and fine spatial resolution. The technique demonstrated has wider applications for researchers seeking enhanced contrast and high-resolution imaging of any conducting entity in a biological matrix - a commonly encountered issue of importance in drug delivery, tissue engineering and toxicological studies. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Microscopic study of heavy-ion reactions with n-rich nuclei: dynamic excitation energy and capture

NASA Astrophysics Data System (ADS)

Oberacker, Volker; Umar, A. S.

2010-11-01

Heavy-ion reactions at RIB facilities allow us to form new exotic neutron-rich nuclei. These experiments present numerous challenges for a microscopic theoretical description. We study reactions between neutron-rich ^132Sn nuclei and ^96Zr within a dynamic microscopic theory, and we compare the properties to those of the stable system ^124Sn+^96Zr. The calculations are carried out on a 3-D lattice using the density-constrained Time-Dependent Hartree-Fock (DC-TDHF) method [1- 3]. In particular, we calculate the dynamic excitation energy E^*(t) and the quadrupole moment of the dinuclear system Q20(t) during the initial stages of the collision. Regarding the heavy-ion interaction potential V(R), we find that the fusion barrier height and width increase dramatically with increasing beam energy. The fusion barriers of the neutron-rich system ^132Sn+^96Zr are systematically 1-2 MeV higher than those of the stable system. Large differences (9 MeV) are found in the interaction barriers of the two systems. Capture cross sections are analyzed in terms of dynamic effects and a comparison with recently measured capture-fission data is given. [1] Umar and Oberacker, PRC 76, 014614 (2007). [2] Umar, Oberacker, Maruhn, and Reinhard, PRC 80, 041601(R) (2009). [3] Umar, Maruhn, Itagaki, and Oberacker, PRL 104, 212503 (2010).

An Improved Analytic Model for Microdosimeter Response

NASA Technical Reports Server (NTRS)

Shinn, Judy L.; Wilson, John W.; Xapsos, Michael A.

2001-01-01

An analytic model used to predict energy deposition fluctuations in a microvolume by ions through direct events is improved to include indirect delta ray events. The new model can now account for the increase in flux at low lineal energy when the ions are of very high energy. Good agreement is obtained between the calculated results and available data for laboratory ion beams. Comparison of GCR (galactic cosmic ray) flux between Shuttle TEPC (tissue equivalent proportional counter) flight data and current calculations draws a different assessment of developmental work required for the GCR transport code (HZETRN) than previously concluded.

Method for imaging liquid and dielectric materials with scanning polarization force microscopy

DOEpatents

Hu, Jun; Ogletree, D. Frank; Salmeron, Miguel; Xiao, Xudong

1999-01-01

The invention images dielectric polarization forces on surfaces induced by a charged scanning force microscope (SFM) probe tip. On insulators, the major contribution to the surface polarizability at low frequencies is from surface ions. The mobility of these ions depends strongly on the humidity. Using the inventive SFM, liquid films, droplets, and other weakly adsorbed materials have been imaged.

Apparatus for imaging liquid and dielectric materials with scanning polarization force microscopy

DOEpatents

Hu, Jun; Ogletree, D. Frank; Salmeron, Miguel; Xiao, Xudong

1998-01-01

The invention images dielectric polarization forces on surfaces induced by a charged scanning force microscope (SFM) probe tip. On insulators, the major contribution to the surface polarizability at low frequencies is from surface ions. The mobility of these ions depends strongly on the humidity. Using the inventive SFM, liquid films, droplets, and other weakly adsorbed materials have been imaged.

Microscopic evidence that the nitromethane aci ion is a rate controlling species in the detonation of liquid nitromethane

DOE Office of Scientific and Technical Information (OSTI.GOV)

Engelke, R.; Earl, W.L.; Rohlfing, C.M.

1986-01-01

We present microscopic evidence that the aci ion (H/sub 2/CNO/sup -//sub 2/) of nitromethane (H/sub 3/CNO/sub 2/) plays an important role in the detonation kinetics of liquid-phase nitromethane. It is known from previous detonation experiments that very minute additions of organic bases (e.g., amines) have a profound effect on the detonation properties of nitromethane; i.e., the explosive is strongly sensitized. Here we show that, under conditions similar to the detonation experiments, the only new chemical species generated in nitromethane by the bases sodium hydroxide (NaOH), diethylenetriamine (NH/sub 2/CH/sub 2/CH/sub 2/NHCH/sub 2/CH/sub 2/NH/sub 2/), and pyridine (C/sub 5/H/sub 5/N) is themore » aci ion, within the sensitivity of the experiments. The primary tool used to demonstrate this is /sup 13/C NMR spectroscopy. Ab initio quantum-mechanical calculations of the chemical shifts are used to support the experimental interpretation. Qualitative arguments concerning the increased reactivity of the aci ion, relative to normal nitromethane, are given. We review earlier work and relate it to the current findings.« less

Helium-ion microscopy, helium-ion irradiation and nanoindentation of Eurofer 97 and ODS Eurofer

NASA Astrophysics Data System (ADS)

Bergner, F.; Hlawacek, G.; Heintze, C.

2018-07-01

Understanding of unsolved details of helium embrittlement requires experimental evidence for dedicated sets of materials and over a wide range of irradiation conditions. The study is focussed on the comparison of a reduced-activation ferritic-martensitic 9%Cr steel (Eurofer 97) with its oxide dispersion strengthened counterpart (ODS Eurofer) with respect to irradiation-induced hardening. Imaging and He-ion irradiation in the He-ion microscope at 30 °C in a wide range of appm He (from 0.9 × 102 to 1.8 × 106) and displacements per atom (dpa) (from 3 × 10-3 to 65) were combined with post-irradiation nanoindentation in order to detect blistering and irradiation-induced hardness changes. The applicability of this combination of techniques is demonstrated and pros and cons are discussed. We have found that the indentation hardness increases significantly after in-microscope irradiation to 3 dpa (0.9 × 105 appm He). The irradiation-induced hardness increase is higher and the onset of significant hardening tends to occur at lower fluence for Eurofer 97 than for ODS Eurofer, indicating that the presence of oxide nanoparticles is efficient to reduce the detrimental effect of He under the applied irradiation conditions.

Direct observation of dopant distribution in GaAs compound semiconductors using phase-shifting electron holography and Lorentz microscopy.

PubMed

Sasaki, Hirokazu; Otomo, Shinya; Minato, Ryuichiro; Yamamoto, Kazuo; Hirayama, Tsukasa

2014-06-01

Phase-shifting electron holography and Lorentz microscopy were used to map dopant distributions in GaAs compound semiconductors with step-like dopant concentration. Transmission electron microscope specimens were prepared using a triple beam focused ion beam (FIB) system, which combines a Ga ion beam, a scanning electron microscope, and an Ar ion beam to remove the FIB damaged layers. The p-n junctions were clearly observed in both under-focused and over-focused Lorentz microscopy images. A phase image was obtained by using a phase-shifting reconstruction method to simultaneously achieve high sensitivity and high spatial resolution. Differences in dopant concentrations between 1 × 10(19) cm(-3) and 1 × 10(18) cm(-3) regions were clearly observed by using phase-shifting electron holography. We also interpreted phase profiles quantitatively by considering inactive layers induced by ion implantation during the FIB process. The thickness of an inactive layer at different dopant concentration area can be measured from the phase image. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Tunicamycin Enhances Neuroinvasion and Pathogenicity in Mice with Venezuelan Equine Encephalitis Virus

DTIC Science & Technology

2003-01-01

H. Analytical Tests 35 1. Virus Titrations 35 2. RNA Analysis 37 3. Determination of TNF-a and Total Nitrite Levels 37...fluorescent microscope. H. Analytical Tests 1. Virus Titrations For determination of virus titers, brain samples were homogenized in Eppendorf tubes...tissues were mounted on silane-coated slides (Sigma Diagnostics , St. Louis, MO) and labeled for VEE virus antigen by immunohistochemistry. Additional

Microscopic saw mark analysis: an empirical approach.

PubMed

Love, Jennifer C; Derrick, Sharon M; Wiersema, Jason M; Peters, Charles

2015-01-01

Microscopic saw mark analysis is a well published and generally accepted qualitative analytical method. However, little research has focused on identifying and mitigating potential sources of error associated with the method. The presented study proposes the use of classification trees and random forest classifiers as an optimal, statistically sound approach to mitigate the potential for error of variability and outcome error in microscopic saw mark analysis. The statistical model was applied to 58 experimental saw marks created with four types of saws. The saw marks were made in fresh human femurs obtained through anatomical gift and were analyzed using a Keyence digital microscope. The statistical approach weighed the variables based on discriminatory value and produced decision trees with an associated outcome error rate of 8.62-17.82%. © 2014 American Academy of Forensic Sciences.

Recovery of Background Structures in Nanoscale Helium Ion Microscope Imaging

PubMed Central

Carasso, Alfred S; Vladár, András E

2014-01-01

This paper discusses a two step enhancement technique applicable to noisy Helium Ion Microscope images in which background structures are not easily discernible due to a weak signal. The method is based on a preliminary adaptive histogram equalization, followed by ‘slow motion’ low-exponent Lévy fractional diffusion smoothing. This combined approach is unexpectedly effective, resulting in a companion enhanced image in which background structures are rendered much more visible, and noise is significantly reduced, all with minimal loss of image sharpness. The method also provides useful enhancements of scanning charged-particle microscopy images obtained by composing multiple drift-corrected ‘fast scan’ frames. The paper includes software routines, written in Interactive Data Language (IDL),1 that can perform the above image processing tasks. PMID:26601050

Recent progress in understanding the imaging and metrology using the helium ion microscope

NASA Astrophysics Data System (ADS)

Postek, Michael T.; Vladar, Andras E.; Ming, Bin

2009-05-01

Nanotechnology is pushing imaging and measurement instrument technology to high levels of required performance. As this continues, new barriers confronting innovation in this field are encountered. Particle beam instrument resolution remains one of these barriers. A new tool for imaging and metrology for nanotechnology is the scanning Helium Ion Microscope (HIM). The HIM is a new approach to imaging and metrology for nanotechnology which may be able to push this barrier lower. As a new methodology, it is just beginning to show promise and the number of potentially advantageous applications for nanotechnology and nanometrology has yet to be fully exploited. This presentation will discuss some of the progress made at NIST in collaboration with the manufacturing community in understanding the imaging and metrology for this new technology.

Tuning wettability of hydrogen titanate nanowire mesh by Na+ irradiation

NASA Astrophysics Data System (ADS)

Das, Pritam; Chatterjee, Shyamal

2018-04-01

Hydrogen titanate (HT) nanowires have been widely studied for remarkable properties and various potential applications. However, a handful studies are available related to ion beam induced structural changes and influence on wetting behavior of the HT nanowire surface. In this work, we exposed HT nanowires to 5 keV Na+ at an ion fluence of 1×1016 ions.cm-2. Scanning electron microscope shows that at this ion fluence nanowires are bent arbitrarily and they are welded to each other forming an interlinked network structure. Computer simulation shows that ion beam induces defect formation in the nanowires, which plays major role in such structural modifications. An interesting alteration of surface wetting property is observed due to ion irradiation. The hydrophilic pristine surface turns into hydrophobic after ion irradiation.

Investigations of Some Liquid Matrixes for Analyte Quantification by MALDI

NASA Astrophysics Data System (ADS)

Moon, Jeong Hee; Park, Kyung Man; Ahn, Sung Hee; Lee, Seong Hoon; Kim, Myung Soo

2015-06-01

Sample inhomogeneity is one of the obstacles preventing the generation of reproducible mass spectra by MALDI and to their use for the purpose of analyte quantification. As a potential solution to this problem, we investigated MALDI with some liquid matrixes prepared by nonstoichiometric mixing of acids and bases. Out of 27 combinations of acids and bases, liquid matrixes could be produced from seven. When the overall spectral features were considered, two liquid matrixes using α-cyano-4-hydroxycinnamic acid as the acid and 3-aminoquinoline and N,N-diethylaniline as bases were the best choices. In our previous study of MALDI with solid matrixes, we found that three requirements had to be met for the generation of reproducible spectra and for analyte quantification: (1) controlling the temperature by fixing the total ion count, (2) plotting the analyte-to-matrix ion ratio versus the analyte concentration as the calibration curve, and (3) keeping the matrix suppression below a critical value. We found that the same requirements had to be met in MALDI with liquid matrixes as well. In particular, although the liquid matrixes tested here were homogeneous, they failed to display spot-to-spot spectral reproducibility unless the first requirement above was met. We also found that analyte-derived ions could not be produced efficiently by MALDI with the above liquid matrixes unless the analyte was sufficiently basic. In this sense, MALDI processes with solid and liquid matrixes should be regarded as complementary techniques rather than as competing ones.

Investigations of Some Liquid Matrixes for Analyte Quantification by MALDI.

PubMed

Moon, Jeong Hee; Park, Kyung Man; Ahn, Sung Hee; Lee, Seong Hoon; Kim, Myung Soo

2015-10-01

Sample inhomogeneity is one of the obstacles preventing the generation of reproducible mass spectra by MALDI and to their use for the purpose of analyte quantification. As a potential solution to this problem, we investigated MALDI with some liquid matrixes prepared by nonstoichiometric mixing of acids and bases. Out of 27 combinations of acids and bases, liquid matrixes could be produced from seven. When the overall spectral features were considered, two liquid matrixes using α-cyano-4-hydroxycinnamic acid as the acid and 3-aminoquinoline and N,N-diethylaniline as bases were the best choices. In our previous study of MALDI with solid matrixes, we found that three requirements had to be met for the generation of reproducible spectra and for analyte quantification: (1) controlling the temperature by fixing the total ion count, (2) plotting the analyte-to-matrix ion ratio versus the analyte concentration as the calibration curve, and (3) keeping the matrix suppression below a critical value. We found that the same requirements had to be met in MALDI with liquid matrixes as well. In particular, although the liquid matrixes tested here were homogeneous, they failed to display spot-to-spot spectral reproducibility unless the first requirement above was met. We also found that analyte-derived ions could not be produced efficiently by MALDI with the above liquid matrixes unless the analyte was sufficiently basic. In this sense, MALDI processes with solid and liquid matrixes should be regarded as complementary techniques rather than as competing ones.

Identification of Carboxylate, Phosphate, and Phenoxide Functionalities in Deprotonated Molecules Related to Drug Metabolites via Ion-Molecule Reactions with water and Diethylhydroxyborane

NASA Astrophysics Data System (ADS)

Zhu, Hanyu; Ma, Xin; Kong, John Y.; Zhang, Minli; Kenttämaa, Hilkka I.

2017-10-01

Tandem mass spectrometry based on ion-molecule reactions has emerged as a powerful tool for structural elucidation of ionized analytes. However, most currently used reagents were designed to react with protonated analytes, making them suboptimal for acidic analytes that are preferentially detected in negative ion mode. In this work we demonstrate that the phenoxide, carboxylate, and phosphate functionalities can be identified in deprotonated molecules by use of a combination of two reagents, diethylmethoxyborane (DEMB) and water. A novel reagent introduction setup that allowed DEMB and water to be separately introduced into the ion trap region of the mass spectrometer was developed to facilitate fundamental studies of this reaction. A new reagent, diethylhydroxyborane (DEHB), was generated inside the ion trap by hydrolysis of DEMB on introduction of water. Most carboxylates and phenoxides formed a DEHB adduct, followed by addition of one water molecule and subsequent ethane elimination (DEHB adduct +H2O - CH3CH3) as the major product ion. Phenoxides with a hydroxy group adjacent to the deprotonation site and phosphates formed a DEHB adduct, followed by ethane elimination (DEHB adduct - CH3CH3). Deprotonated molecules with strong intramolecular hydrogen bonds or without the aforementioned functionalities, including sulfates, were unreactive toward DEHB/H2O. Reaction mechanisms were explored via isotope labeling experiments and quantum chemical calculations. The mass spectrometry method allowed the differentiation of phenoxide-, carboxylate-, phosphate-, and sulfate-containing analytes. Finally, it was successfully coupled with high-performance liquid chromatography for the analysis of a mixture containing hymecromone, a biliary spasm drug, and its three possible metabolites. [Figure not available: see fulltext.

Prize for Industrial Applications of Physics Talk: Low energy spread Ion source for focused ion beam systems-Search for the holy grail

NASA Astrophysics Data System (ADS)

Ward, Bill

2011-03-01

In this talk I will cover my personal experiences as a serial entrepreneur and founder of a succession of focused ion beam companies (1). Ion Beam Technology, which developed a 200kv (FIB) direct ion implanter (2). Micrion, where the FIB found a market in circuit edit and mask repair, which eventually merged with FEI corporation. and (3). ALIS Corporation which develop the Orion system, the first commercially successful sub-nanometer helium ion microscope, that was ultimately acquired by Carl Zeiss corporation. I will share this adventure beginning with my experiences in the early days of ion beam implantation and e-beam lithography which lead up to the final breakthrough understanding of the mechanisms that govern the successful creation and operation of a single atom ion source.

Formation of a periodic diffractive structure based on poly(methyl methacrylate) with ion-implanted silver nanoparticles

NASA Astrophysics Data System (ADS)

Galyautdinov, M. F.; Nuzhdin, V. I.; Fattakhov, Ya. V.; Farrakhov, B. F.; Valeev, V. F.; Osin, Yu. N.; Stepanov, A. L.

2016-02-01

We propose to form optical diffractive elements on the surface of poly(methyl methacrylate) (PMMA) by implanting the polymer with silver ions ( E = 30 keV; D = 5.0 × 1014 to 1.5 × 1017 ion/cm2; I = 2 μA/cm2) through a nickel grid (mask). Ion implantation leads to the nucleation and growth of silver nanoparticles in unmasked regions of the polymer. The formation of periodic surface microstructures during local sputtering of the polymer by incident ions was monitored using an optical microscope. The diffraction efficiency of obtained gratings is demonstrated under conditions of their probing with semiconductor laser radiation in the visible spectral range.

Nanopore fabrication and characterization by helium ion microscopy

NASA Astrophysics Data System (ADS)

Emmrich, D.; Beyer, A.; Nadzeyka, A.; Bauerdick, S.; Meyer, J. C.; Kotakoski, J.; Gölzhäuser, A.

2016-04-01

The Helium Ion Microscope (HIM) has the capability to image small features with a resolution down to 0.35 nm due to its highly focused gas field ionization source and its small beam-sample interaction volume. In this work, the focused helium ion beam of a HIM is utilized to create nanopores with diameters down to 1.3 nm. It will be demonstrated that nanopores can be milled into silicon nitride, carbon nanomembranes, and graphene with well-defined aspect ratio. To image and characterize the produced nanopores, helium ion microscopy and high resolution scanning transmission electron microscopy were used. The analysis of the nanopores' growth behavior allows inferring on the profile of the helium ion beam.

High Resolution Studies of the Origins of Polyatomic Ions in Inductively Coupled Plasma-Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferguson, Jill Wisnewski

2006-01-01

The inductively coupled plasma (ICP) is an atmospheric pressure ionization source. Traditionally, the plasma is sampled via a sampler cone. A supersonic jet develops behind the sampler, and this region is pumped down to a pressure of approximately one Torr. A skimmer cone is located inside this zone of silence to transmit ions into the mass spectrometer. The position of the sampler and skimmer cones relative to the initial radiation and normal analytical zones of the plasma is key to optimizing the useful analytical signal [1]. The ICP both atomizes and ionizes the sample. Polyatomic ions form through ion-molecule interactionsmore » either in the ICP or during ion extraction [l]. Common polyatomic ions that inhibit analysis include metal oxides (MO +), adducts with argon, the gas most commonly used to make up the plasma, and hydride species. While high resolution devices can separate many analytes from common interferences, this is done at great cost in ion transmission efficiency--a loss of 99% when using high versus low resolution on the same instrument [2]. Simple quadrupole devices, which make up the bulk of ICP-MS instruments in existence, do not present this option. Therefore, if the source of polyatomic interferences can be determined and then manipulated, this could potentially improve the figures of merit on all ICP-MS devices, not just the high resolution devices often utilized to study polyatomic interferences.« less

37Cl/35Cl isotope ratio analysis in perchlorate by ion chromatography/multi collector -ICPMS: Analytical performance and implication for biodegradation studies.

PubMed

Zakon, Yevgeni; Ronen, Zeev; Halicz, Ludwik; Gelman, Faina

2017-10-01

In the present study we propose a new analytical method for 37 Cl/ 35 Cl analysis in perchlorate by Ion Chromatography(IC) coupled to Multicollector Inductively Coupled Plasma Mass Spectrometry (MC-ICPMS). The accuracy of the analytical method was validated by analysis of international perchlorate standard materials USGS-37 and USGS -38; analytical precision better than ±0.4‰ was achieved. 37 Cl/ 35 Cl isotope ratio analysis in perchlorate during laboratory biodegradation experiment with microbial cultures enriched from the contaminated soil in Israel resulted in isotope enrichment factor ε 37 Cl = -13.3 ± 1‰, which falls in the range reported previously for perchlorate biodegradation by pure microbial cultures. The proposed analytical method may significantly simplify the procedure for isotope analysis of perchlorate which is currently applied in environmental studies. Copyright © 2017. Published by Elsevier Ltd.

Direct-injection mass spectrometric method for the rapid identification of fentanyl and norfentanyl in postmortem urine of six drug-overdose cases.

PubMed

Peer, Cody J; Shakleya, Diaa M; Younis, Islam R; Kraner, James C; Callery, Patrick S

2007-10-01

A rapid mass spectrometric method was developed for the identification of fentanyl and its major hepatic metabolite norfentanyl in postmortem urine of six drug-overdose victims involving fentanyl use. To reduce matrix effects or ion suppression, sample preparation consisted of centrifugation and solid-phase extraction. Deuterium-labeled internal standards ((2)H(5)-fentanyl and (2)H(5)-norfentanyl) were used to compensate for instrument variation in signal, analyte recovery during sample preparation, and ion suppression. Structural information for fentanyl and norfentanyl were collected using mass spectrometry (MS) with electrospray ionization (ESI) operated in the positive ion mode. Fentanyl (m/z 337) was found in each of the six overdose cases by the appearance of the MS-MS daughter ion on both an ion trap and a triple-quadrupole MS resulting from the fragmentation pathway of fentanyl (m/z 337 --> 188). Norfentanyl was detected in all six cases by the appearance of the MH(+) ion, m/z 233, with a single-quadrupole MS and confirmed in an ion trap MS. Ion suppression, as determined by the comparison of ion intensities from spiked samples in water with postmortem urine from the cases, ranged from 18% to 98% in three ESI sources. The use of stable isotope-labeled internal standards obviates sample preparation because ratios of analyte/internal standard remain constant in the presence of extensive matrix effects. This MS method provided sufficient sensitivity and selectivity for the rapid identification of fentanyl and norfentanyl in urine at levels >/= 10 ng/mL without prior analyte resolution by chromatography and with a total analysis time of less than 1 h.

Stochastic dynamics and logistic population growth

NASA Astrophysics Data System (ADS)

Méndez, Vicenç; Assaf, Michael; Campos, Daniel; Horsthemke, Werner

2015-06-01

The Verhulst model is probably the best known macroscopic rate equation in population ecology. It depends on two parameters, the intrinsic growth rate and the carrying capacity. These parameters can be estimated for different populations and are related to the reproductive fitness and the competition for limited resources, respectively. We investigate analytically and numerically the simplest possible microscopic scenarios that give rise to the logistic equation in the deterministic mean-field limit. We provide a definition of the two parameters of the Verhulst equation in terms of microscopic parameters. In addition, we derive the conditions for extinction or persistence of the population by employing either the momentum-space spectral theory or the real-space Wentzel-Kramers-Brillouin approximation to determine the probability distribution function and the mean time to extinction of the population. Our analytical results agree well with numerical simulations.

Combined analysis of 1,3-benzodioxoles by crystalline sponge X-ray crystallography and laser desorption ionization mass spectrometry.

PubMed

Hayashi, Yukako; Ohara, Kazuaki; Taki, Rika; Saeki, Tomomi; Yamaguchi, Kentaro

2018-03-12

The crystalline sponge (CS) method, which employs single-crystal X-ray diffraction to determine the structure of an analyte present as a liquid or an oil and having a low melting point, was used in combination with laser desorption ionization mass spectrometry (LDI-MS). 1,3-Benzodioxole derivatives were encapsulated in CS and their structures were determined by combining X-ray crystallography and MS. After the X-ray analysis, the CS was subjected to imaging mass spectrometry (IMS) with an LDI spiral-time-of-flight mass spectrometer (TOF-MS). The ion detection area matched the microscopic image of the encapsulated CS. In addition, the accumulated 1D mass spectra showed that fragmentation of the guest molecule (hereafter, guest) can be easily visualized without any interference from the fragment ions of CS except for two strong ion peaks derived from the tridentate ligand TPT (2,4,6-tris(4-pyridyl)-1,3,5-triazine) of the CS and its fragment. X-ray analysis clearly showed the presence of the guest as well as the π-π, CH-halogen, and CH-O interactions between the guest and the CS framework. However, some guests remained randomly diffused in the nanopores of CS. In addition, the detection limit was less than sub-pmol order based on the weight and density of CS determined by X-ray analysis. Spectroscopic data, such as UV-vis and NMR, also supported the encapsulation of the guest through the interaction between the guest and CS components. The results denote that the CS-LDI-MS method, which combines CS, X-ray analysis and LDI-MS, is effective for structure determination.

Quantitative imaging of magnesium distribution at single-cell resolution in brain tumors and infiltrating tumor cells with secondary ion mass spectrometry (SIMS)

PubMed Central

Chandra, Subhash; Parker, Dylan J.; Barth, Rolf F.; Pannullo, Susan C.

2016-01-01

Glioblastoma multiforme (GBM) is one of the deadliest forms of human brain tumors. The infiltrative pattern of growth of these tumors includes the spread of individual and/or clusters of tumor cells at some distance from the main tumor mass in parts of the brain protected by an intact blood-brain-barrier. Pathophysiological studies of GBM could be greatly enhanced by analytical techniques capable of in situ single-cell resolution measurements of infiltrating tumor cells. Magnesium homeostasis is an area of active investigation in high grade gliomas. In the present study, we have used the F98 rat glioma as a model of human GBM and an elemental/isotopic imaging technique of secondary ion mass spectrometry (SIMS), a CAMECA IMS-3f ion microscope, for studying Mg distributions with single-cell resolution in freeze-dried brain tissue cryosections. Quantitative observations were made on tumor cells in the main tumor mass, contiguous brain tissue, and infiltrating tumor cells in adjacent normal brain. The brain tissue contained a significantly lower total Mg concentration of 4.70 ± 0.93 mmol/Kg wet weight (mean ± SD) in comparison to 11.64 ± 1.96 mmol/Kg wet weight in tumor cells of the main tumor mass and 10.72 ± 1.76 mmol/Kg wet weight in infiltrating tumor cells (p<0.05). The nucleus of individual tumor cells contained elevated levels of bound Mg. These observations demonstrate enhanced Mg-influx and increased binding of Mg in tumor cells and provide strong support for further investigation of GBMs for altered Mg homeostasis and activation of Mg-transporting channels as possible therapeutic targets. PMID:26703785

Verification of high efficient broad beam cold cathode ion source

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abdel Reheem, A. M., E-mail: amreheem2009@yahoo.com; Radiation Physics Department, National Center for Radiation Research and Technology; Ahmed, M. M.

2016-08-15

An improved form of cold cathode ion source has been designed and constructed. It consists of stainless steel hollow cylinder anode and stainless steel cathode disc, which are separated by a Teflon flange. The electrical discharge and output characteristics have been measured at different pressures using argon, nitrogen, and oxygen gases. The ion exit aperture shape and optimum distance between ion collector plate and cathode disc are studied. The stable discharge current and maximum output ion beam current have been obtained using grid exit aperture. It was found that the optimum distance between ion collector plate and ion exit aperturemore » is equal to 6.25 cm. The cold cathode ion source is used to deposit aluminum coating layer on AZ31 magnesium alloy using argon ion beam current which equals 600 μA. Scanning electron microscope and X-ray diffraction techniques used for characterizing samples before and after aluminum deposition.« less

Composite glycerol/graphite/aromatic acid matrices for thin-layer chromatography/matrix-assisted laser desorption/ionization mass spectrometry of heterocyclic compounds.

PubMed

Esparza, Cesar; Borisov, R S; Varlamov, A V; Zaikin, V G

2016-10-28

New composite matrices have been suggested for the analysis of mixtures of different synthetic organic compounds (N-containing heterocycles and erectile dysfunction drugs) by thin layer chromatography/matrix-assisted laser desorption ionization time-of-flight mass spectrometry (TLC/MALDI-TOF). Different mixtures of classical MALDI matrices and graphite particles dispersed in glycerol were used for the registration of MALDI mass spectra directly from TLC plates after analytes separation. In most of cases, the mass spectra possessed [M+H] + ions; however, for some analytes only [M+Na] + and [M+K] + ions were observed. These ions have been used to generate visualized TLC chromatograms. The described approach increases the desorption/ionization efficiencies of analytes separated by TLC, prevent spot blurring, simplifies and decrease time for sample preparation. Copyright © 2016 Elsevier B.V. All rights reserved.

High aspect ratio AFM Probe processing by helium-ion-beam induced deposition.

PubMed

Onishi, Keiko; Guo, Hongxuan; Nagano, Syoko; Fujita, Daisuke

2014-11-01

A Scanning Helium Ion Microscope (SHIM) is a high resolution surface observation instrument similar to a Scanning Electron Microscope (SEM) since both instruments employ finely focused particle beams of ions or electrons [1]. The apparent difference is that SHIMs can be used not only for a sub-nanometer scale resolution microscopic research, but also for the applications of very fine fabrication and direct lithography of surfaces at the nanoscale dimensions. On the other hand, atomic force microscope (AFM) is another type of high resolution microscopy which can measure a three-dimensional surface morphology by tracing a fine probe with a sharp tip apex on a specimen's surface.In order to measure highly uneven and concavo-convex surfaces by AFM, the probe of a high aspect ratio with a sharp tip is much more necessary than the probe of a general quadrangular pyramid shape. In this paper we report the manufacture of the probe tip of the high aspect ratio by ion-beam induced gas deposition using a nanoscale helium ion beam of SHIM.Gas of platinum organic compound was injected into the sample surface neighborhood in the vacuum chamber of SHIM. The decomposition of the gas and the precipitation of the involved metal brought up a platinum nano-object in a pillar shape on the normal commercial AFM probe tip. A SHIM system (Carl Zeiss, Orion Plus) equipped with the gas injection system (OmniProbe, OmniGIS) was used for the research. While the vacuum being kept to work, we injected platinum organic compound ((CH3)3(CH3C5H4)Pt) into the sample neighborhood and irradiated the helium ion beam with the shape of a point on the apex of the AFM probe tip. It is found that we can control the length of the Pt nano-pillar by irradiation time of the helium ion beam. The AFM probe which brought up a Pt nano-pillar is shown in Figure 1. It is revealed that a high-aspect-ratio Pt nano-pillar of ∼40nm diameter and up to ∼2000 nm length can be grown. In addition, for possible heating by the helium ion beam, it was observed that an original probe shape was transformed. AFM measurement of a reference sample (pitch 100-500 nm, depth 100 nm) of the lines and spaces was performed using the above probes. The conventional probes which did not bring up platinum was not able to get into the ditch enough. Therefore it was found that a salient was big and a reentrant was shallow. On the other hand, the probe which brought up platinum was able to enter enough to the depths of the ditch.jmicro;63/suppl_1/i30-a/DFU075F1F1DFU075F1Fig.1.SHIM image of the AFM probe with the Pt nano-pillar fabricated by ion-beam induced deposition. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

TLD efficiency calculations for heavy ions: an analytical approach

DOE PAGES

Boscolo, Daria; Scifoni, Emanuele; Carlino, Antonio; ...

2015-12-18

The use of thermoluminescent dosimeters (TLDs) in heavy charged particles’ dosimetry is limited by their non-linear dose response curve and by their response dependence on the radiation quality. Thus, in order to use TLDs with particle beams, a model that can reproduce the behavior of these detectors under different conditions is needed. Here a new, simple and completely analytical algorithm for the calculation of the relative TL-efficiency depending on the ion charge Z and energy E is presented. In addition, the detector response is evaluated starting from the single ion case, where the computed effectiveness values have been compared withmore » experimental data as well as with predictions from a different method. The main advantage of this approach is that, being fully analytical, it is computationally fast and can be efficiently integrated into treatment planning verification tools. In conclusion, the calculated efficiency values have been then implemented in the treatment planning code TRiP98 and dose calculations on a macroscopic target irradiated with an extended carbon ion field have been performed and verified against experimental data.« less

Method for imaging liquid and dielectric materials with scanning polarization force microscopy

DOEpatents

Hu, J.; Ogletree, D.F.; Salmeron, M.; Xiao, X.

1999-03-09

The invention images dielectric polarization forces on surfaces induced by a charged scanning force microscope (SFM) probe tip. On insulators, the major contribution to the surface polarizability at low frequencies is from surface ions. The mobility of these ions depends strongly on the humidity. Using the inventive SFM, liquid films, droplets, and other weakly adsorbed materials have been imaged. 9 figs.

Apparatus for imaging liquid and dielectric materials with scanning polarization force microscopy

DOEpatents

Hu, J.; Ogletree, D.F.; Salmeron, M.; Xiao, X.

1998-04-28

The invention images dielectric polarization forces on surfaces induced by a charged scanning force microscope (SFM) probe tip. On insulators, the major contribution to the surface polarizability at low frequencies is from surface ions. The mobility of these ions depends strongly on the humidity. Using the inventive SFM, liquid films, droplets, and other weakly adsorbed materials have been imaged. 9 figs.

Peculiar Traits of Coarse AP

DTIC Science & Technology

2014-01-01

propellant. Since coarse AP in particles larger than about 150 microns are used in great majority for AP oxidized solid propellants, the nature of...Microscopic amounts of liquid containing water were contained in the reactive centers. The maximum size for reactive centers was reasoned to be...bond in the original chlorate ion. Oxygen atom swapping between chlorate and perchlorate ions would provide chlorate migration without use of forces

Development of Wien filter for small ion gun of surface analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bahng, Jungbae; Busan Center, Korea Basic Science Institute, Busan 609-735; Hong, Jonggi

The gas cluster ion beam (GCIB) and liquid metal ion beam have been studied in the context of ion beam usage for analytical equipment in applications such as X-ray photoelectron spectroscopy and secondary ion mass spectroscopy (SIMS). In particular, small ion sources are used for the secondary ion generation and ion etching. To set the context to this study, the SIMS project has been launched to develop ion-gun based analytical equipment for the Korea Basic Science Institute. The objective of the first stage of the project is the generation of argon beams with a GCIB system [A. Kirkpatrick, Nucl. Instrum.more » Methods Phys. Res., Sect. B 206, 830–837 (2003)] that consists of a nozzle, skimmer, ionizer, acceleration tube, separation system, transport system, and target. The Wien filter directs the selected cluster beam to the target system by exploiting the velocity difference of the generated particles from GCIB. In this paper, we present the theoretical modeling and three-dimensional electromagnetic analysis of the Wien filter, which can separate Ar{sup +}{sub 2500} clusters from Ar{sup +}{sub 2400} to Ar{sup +}{sub 2600} clusters with a 1-mm collimator.« less

Cross-sectional transmission electron microscopic study of irradiation induced nano-crystallization of nickel in a W/Ni multilayer.

PubMed

Bagchi, Sharmistha; Lalla, N P

2008-06-11

The present study reports the cross-sectional transmission electron microscopic investigations of swift heavy ion-irradiation induced nano-size recrystallization of Ni in a nearly immiscible W/Ni multilayer structure. Multilayer structures (MLS) of [W(25 Å)/Ni(25 Å)](10BL) were grown on Si-(100) substrate by the ion-beam sputtering technique. The as-synthesized MLS were subjected to 120 MeV-Au(9+) ion-irradiation to a fluence of ∼5 × 10(13) ions cm(-2). Wide-angle x-ray diffraction studies of pristine as well as irradiated W/Ni multilayers show deterioration of the superlattice structure, whereas x-ray reflectivity (XRR) measurement reveals a nearly unaffected microstructure after irradiation. Analysis of the XRR data using 'Parratt's formalism' does show a significant increase of W/Ni interface roughness. Cross-sectional transmission electron microscopy (TEM) studies carried out in diffraction and imaging modes (including bright-field and dark-field imaging), show that at high irradiation dose the intralayer microstructure of Ni becomes nano-crystalline (1-2 nm). During these irradiation induced changes of the intralayer microstructure, the interlayer definition of the W and Ni layers still remains intact. The observed nano-recrystallization of Ni has been attributed to competition between low miscibility of the W/Ni interface and the ion-beam induced mixing kinetics.

Anisotropic distribution function of minority tail ions generated by strong ion-cyclotron resonance heating

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chang, C.S.; Colestock, P.

1989-05-01

The highly anisotropic particle distribution function of minority tail ions driven by ion-cyclotron resonance heating at the fundamental harmonic is calculated in a two-dimensional velocity space. It is assumed that the heating is strong enough to drive most of the resonant ions above the in-electron critical slowing-down energy. Simple analytic expressions for the tail distribution are obtained fro the case when the Doppler effect is sufficiently large to flatten the sharp pitch angle dependence in the bounce averaged qualilinear heating coefficient, D/sub b/, and for the case when D/sub b/ is assumed to be constant in pitch angle and energy.more » It is found that a simple constant-D/sub b/ solution can be used instead of the more complicated sharp-D/sub b/ solution for many analytic purposes. 4 refs., 4 figs.« less

Reactive ion etched substrates and methods of making and using

DOEpatents

Rucker, Victor C [San Francisco, CA; Shediac, Rene [Oakland, CA; Simmons, Blake A [San Francisco, CA; Havenstrite, Karen L [New York, NY

2007-08-07

Disclosed herein are substrates comprising reactive ion etched surfaces and specific binding agents immobilized thereon. The substrates may be used in methods and devices for assaying or isolating analytes in a sample. Also disclosed are methods of making the reactive ion etched surfaces.

High frequency fishbone driven by passing energetic ions in tokamak plasmas

NASA Astrophysics Data System (ADS)

Wang, Feng; Yu, L. M.; Fu, G. Y.; Shen, Wei

2017-05-01

High frequency fishbone instability driven by passing energetic ions was first reported in the Princeton beta experiment with tangential neutral-beam-injection (Heidbrink et al 1986 Phys. Rev. Lett. 57 835-8). It could play an important role for ITER-like burning plasmas, where α particles are mostly passing particles. In this work, a generalized energetic ion distribution function and finite drift orbit width effect are considered to improve the theoretical model for passing particle driving fishbone instability. For purely passing energetic ions with zero drift orbit width, the kinetic energy δ {{W}k} is derived analytically. The derived analytic expression is more accurate as compared to the result of previous work (Wang 2001 Phys. Rev. Lett. 86 5286-8). For a generalized energetic ion distribution function, the fishbone dispersion relation is derived and is solved numerically. Numerical results show that broad and off-axis beam density profiles can significantly increase the beam ion beta threshold {βc} for instability and decrease mode frequency.

High frequency fishbone driven by passing energetic ions in tokamak plasmas

DOE PAGES

Wang, Feng; Yu, L. M.; Fu, G. Y.; ...

2017-03-22

High frequency fishbone instability driven by passing energetic ions was first reported in the Princeton beta experiment with tangential neutral-beam-injection (Heidbrink et al 1986 Phys. Rev. Lett. 57 835–8). It could play an important role for ITER-like burning plasmas, where α particles are mostly passing particles. In this work, a generalized energetic ion distribution function and finite drift orbit width effect are considered to improve the theoretical model for passing particle driving fishbone instability. For purely passing energetic ions with zero drift orbit width, the kinetic energymore » $$\\delta {{W}_{k}}$$ is derived analytically. The derived analytic expression is more accurate as compared to the result of previous work. For a generalized energetic ion distribution function, the fishbone dispersion relation is derived and is solved numerically. As a result, numerical results show that broad and off-axis beam density profiles can significantly increase the beam ion beta threshold $${{\\beta}_{c}}$$ for instability and decrease mode frequency.« less

Superstatistical Energy Distributions of an Ion in an Ultracold Buffer Gas

NASA Astrophysics Data System (ADS)

Rouse, I.; Willitsch, S.

2017-04-01

An ion in a radio frequency ion trap interacting with a buffer gas of ultracold neutral atoms is a driven dynamical system which has been found to develop a nonthermal energy distribution with a power law tail. The exact analytical form of this distribution is unknown, but has often been represented empirically by q -exponential (Tsallis) functions. Based on the concepts of superstatistics, we introduce a framework for the statistical mechanics of an ion trapped in an rf field subject to collisions with a buffer gas. We derive analytic ion secular energy distributions from first principles both neglecting and including the effects of the thermal energy of the buffer gas. For a buffer gas with a finite temperature, we prove that Tsallis statistics emerges from the combination of a constant heating term and multiplicative energy fluctuations. We show that the resulting distributions essentially depend on experimentally controllable parameters paving the way for an accurate control of the statistical properties of ion-atom hybrid systems.

Analytical and numerical studies of positive ion beam expansion for surface treatment applications

NASA Astrophysics Data System (ADS)

Lounes-Mahloul, Soumya; Bendib, Abderrezeg; Oudini, Noureddine

2018-01-01

The aim of this work is to study the expansion in vacuum, of a positive ion beam with the use of one dimensional (1D) analytic model and a two dimensional Particle-In-Cell (2D-PIC) simulation. The ion beam is extracted and accelerated from preformed plasma by an extraction system composed of two polarized parallel perforated grids. The results obtained with both approaches reveal the presence of a potential barrier downstream the extraction system which tends to reflect the ion flux. The dependence of the critical distance for which all extracted ions are reflected, is investigated as a function of the extracted ion beam current density. In particular, it is shown that the 1D model recovers the well-known Child-Langmuir law and that the 2D simulation presents a significant discrepancy with respect to the 1D prediction. Indeed, for a given value of current density, the transverse effects lead to a greater critical distance.

Pre-concentration technique for reduction in "Analytical instrument requirement and analysis"

NASA Astrophysics Data System (ADS)

Pal, Sangita; Singha, Mousumi; Meena, Sher Singh

2018-04-01

Availability of analytical instruments for a methodical detection of known and unknown effluents imposes a serious hindrance in qualification and quantification. Several analytical instruments such as Elemental analyzer, ICP-MS, ICP-AES, EDXRF, ion chromatography, Electro-analytical instruments which are not only expensive but also time consuming, required maintenance, damaged essential parts replacement which are of serious concern. Move over for field study and instant detection installation of these instruments are not convenient to each and every place. Therefore, technique such as pre-concentration of metal ions especially for lean stream elaborated and justified. Chelation/sequestration is the key of immobilization technique which is simple, user friendly, most effective, least expensive, time efficient; easy to carry (10g - 20g vial) to experimental field/site has been demonstrated.

Size, weight and position: ion mobility spectrometry and imaging MS combined.

PubMed

Kiss, András; Heeren, Ron M A

2011-03-01

Size, weight and position are three of the most important parameters that describe a molecule in a biological system. Ion mobility spectrometry is capable of separating molecules on the basis of their size or shape, whereas imaging mass spectrometry is an effective tool to measure the molecular weight and spatial distribution of molecules. Recent developments in both fields enabled the combination of the two technologies. As a result, ion-mobility-based imaging mass spectrometry is gaining more and more popularity as a (bio-)analytical tool enabling the determination of the size, weight and position of several molecules simultaneously on biological surfaces. This paper reviews the evolution of ion-mobility-based imaging mass spectrometry and provides examples of its application in analytical studies of biological surfaces.

Copper(II)-rubeanic acid coprecipitation system for separation-preconcentration of trace metal ions in environmental samples for their flame atomic absorption spectrometric determinations.

PubMed

Soylak, Mustafa; Erdogan, Nilgun D

2006-09-21

A simple and facile preconcentration procedure based on the coprecipitation of trace heavy metal ions with copper(II)-rubeanic acid complex has been developed. The analytical parameters including pH, amounts of rubeanic acid, sample volume, etc. was investigated for the quantitative recoveries of Pb(II), Fe(III), Cd(II), Au(III), Pd(II) and Ni(II). No interferic effects were observed from the concomitant ions. The detection limits for analyte ions by 3 sigma were in the range of 0.14 microg/l for iron-3.4 microg/l for lead. The proposed coprecipitation method was successfully applied to water samples from Palas Lake-Kayseri, soil and sediment samples from Kayseri and Yozgat-Turkey.

Solid-phase extraction of some heavy metal ions on a double-walled carbon nanotube disk and determination by flame atomic absorption spectrometry.

PubMed

Karatepe, Aslihan; Soylak, Mustafa; Elçi, Latif

2011-01-01

A new preconcentration method was developed for the determination of trace amounts of Cu(II), Fe(III), Pb(II), Ni(II), and Cd(II) on a double-walled carbon nanotube disk. 4-(2-Thiazolylazo) resorcinol was used as a complexing reagent. The effects of parameters, including pH of the solutions, amounts of complexing reagent, eluent type, sample volume, flow rates of solutions, and matrix ions were examined for quantitative recoveries of the studied analyte ions. The retained metal ions were eluted by 2 M HNO3. The LOD values for the analytes were in the range of 0.7-4.4 microg/mL. Natural water samples and standard reference materials were analyzed by the presented method.

Semi-analytical model for a static sheath including a weakly collisional presheath

NASA Astrophysics Data System (ADS)

Shirafuji, Tatsuru; Denpoh, Kazuki

2018-06-01

A semi-analytical static sheath (SASS) model can provide a spatial potential profile on a biased surface with microstructures, which can be used for predicting ion trajectories on the surface. However, two- or three-dimensional SASS models require a search procedure for a sheath edge equipotential profile, at which ions have the Bohm velocity, as the starting positions for calculating ion trajectories. This procedure can be troublesome when surface microstructures have complex structures. This difficulty is due to the fact that the SASS model cannot handle a presheath region. In this work, we propose a modified SASS model that can handle a presheath region. By using the modified SASS model, ion trajectories can be calculated from edges with arbitrary geometry without searching for the equipotential profile corresponding to sheath edges.

Integration of paper spray ionization high-field asymmetric waveform ion mobility spectrometry for forensic applications.

PubMed

Tsai, Chia-Wei; Tipple, Christopher A; Yost, Richard A

2018-04-15

Paper spray ionization (PSI) is an attractive ambient ionization source for mass spectrometry (MS) since it allows the combination of surface sampling and ionization. The minimal sample preparation inherent in this approach greatly reduces the time needed for analysis. However, the ions generated from interfering compounds in the sample and the paper substrate may interfere with the analyte ions. Therefore, the integration of PSI with high-field asymmetric ion mobility spectrometry (FAIMS) is of significant interest since it should reduce the background ions entering the mass analyzer without complicating the analysis or increasing analysis time. Here we demonstrate the integration of PSI with FAIMS/MS and its potential for analysis of samples of forensic interest. In this work, the parameters that can influence the integration, including sampling and ionization by paper spray, the FAIMS separation of analytes from each other and background interferences, and the length of time that a usable signal can be observed for explosives on paper, were evaluated with the integrated system. In the negative ion analysis of 2,4,6-trinitrotoluene (TNT), pentaerythritol tetranitrate (PETN), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX), and 1,3,5-trinitroperhydro-1,3,5-triazine (RDX), amounts as low as 1 ng on paper were readily observed. The successful positive ion separation of a set of illicit drugs including heroin, methamphetamine, and cocaine was also achieved. In addition, the positive ion analysis of the chemical warfare agent simulants dimethyl methylphosphonate (DMMP) and diisopropyl methylphosphonate (DIMP) was evaluated. The integration of PSI-FAIMS/MS was demonstrated for the analyses of explosives in negative ion mode and for illicit drugs and CW simulants in positive mode. Paper background ions that could interfere with these analyses were separated by FAIMS. The compensation voltage of an ion obtained by FAIMS provided an additional identification parameter to be combined with the mass spectrum for each analyte. Copyright © 2018 John Wiley & Sons, Ltd.

Macroscopic irreversibility and microscopic paradox: A Constructal law analysis of atoms as open systems

PubMed Central

Lucia, Umberto

2016-01-01

The relation between macroscopic irreversibility and microscopic reversibility is a present unsolved problem. Constructal law is introduced to develop analytically the Einstein’s, Schrödinger’s, and Gibbs’ considerations on the interaction between particles and thermal radiation (photons). The result leads to consider the atoms and molecules as open systems in continuous interaction with flows of photons from their surroundings. The consequent result is that, in any atomic transition, the energy related to the microscopic irreversibility is negligible, while when a great number of atoms (of the order of Avogadro’s number) is considered, this energy related to irreversibility becomes so large that its order of magnitude must be taken into account. Consequently, macroscopic irreversibility results related to microscopic irreversibility by flows of photons and amount of atoms involved in the processes. PMID:27762333

Self-consistent simulation of high-frequency driven plasma sheaths

NASA Astrophysics Data System (ADS)

Shihab, Mohammed; Eremin, Denis; Mussenbrock, Thomas; Brinkmann, Ralf

2011-10-01

Low pressure capacitively coupled plasmas are widely used in plasma processing and microelectronics industry. Understanding the dynamics of the boundary sheath is a fundamental problem. It controls the energy and angular distribution of ions bombarding the electrode, which in turn affects the surface reaction rate and the profile of microscopic features. In this contribution, we investigate the dynamics of plasma boundary sheaths by means of a kinetic self-consistent model, which is able to resolve the ion dynamics. Asymmetric sheath dynamics is observed for the intermediate RF regime, i.e., in the regime where the ion plasma frequency is equal to the driving frequency. The ion inertia causes an additional phase difference between the expansion and the contraction phase of the plasma sheath and an asymmetry for the ion energy distribution bimodal shape. A comparison with experimental results and particle in cell simulations is performed. Low pressure capacitively coupled plasmas are widely used in plasma processing and microelectronics industry. Understanding the dynamics of the boundary sheath is a fundamental problem. It controls the energy and angular distribution of ions bombarding the electrode, which in turn affects the surface reaction rate and the profile of microscopic features. In this contribution, we investigate the dynamics of plasma boundary sheaths by means of a kinetic self-consistent model, which is able to resolve the ion dynamics. Asymmetric sheath dynamics is observed for the intermediate RF regime, i.e., in the regime where the ion plasma frequency is equal to the driving frequency. The ion inertia causes an additional phase difference between the expansion and the contraction phase of the plasma sheath and an asymmetry for the ion energy distribution bimodal shape. A comparison with experimental results and particle in cell simulations is performed. The financial support from the Federal Ministry of Education and Research within the frame of the project ``Plasma-Technology-Grid'' and the support of the DFG via the collaborative research center SFB-TR87 is gratefully acknowledged.

1300931

NASA Image and Video Library

2013-08-15

OVERVIEW OF THE MATERIALS DIAGNOSTIC LABORATORY. THE NEAR END SHOWS THE SURFACE ANALYSIS INSTRUMENTS SUCH AS THE SECONDARY ION MASS SPECTROSCOPE (CLOSEST) AND THE TWO ELECTRON SPECTROSCOPY INSTRUMENTS, WHILE THE FAR END SHOWS THE NEW SCANNING ELECTRON MICROSCOPES

Electron microscope aperture system

NASA Technical Reports Server (NTRS)

Heinemann, K. (Inventor)

1976-01-01

An electron microscope including an electron source, a condenser lens having either a circular aperture for focusing a solid cone of electrons onto a specimen or an annular aperture for focusing a hollow cone of electrons onto the specimen, and an objective lens having an annular objective aperture, for focusing electrons passing through the specimen onto an image plane are described. The invention also entails a method of making the annular objective aperture using electron imaging, electrolytic deposition and ion etching techniques.

A second-order theory for transverse ion heating and momentum coupling due to electrostatic ion cyclotron waves

NASA Technical Reports Server (NTRS)

Miller, Ronald H.; Winske, Dan; Gary, S. P.

1992-01-01

A second-order theory for electrostatic instabilities driven by counterstreaming ion beams is developed which describes momentum coupling and heating of the plasma via wave-particle interactions. Exchange rates between the waves and particles are derived, which are suitable for the fluid equations simulating microscopic effects on macroscopic scales. Using a fully kinetic simulation, the electrostatic ion cyclotron instability due to counterstreaming H(+) beams has been simulated. A power spectrum from the kinetic simulation is used to evaluate second-order exchange rates. The calculated heating and momentum loss from second-order theory is compared to the numerical simulation.

Electron-ion relaxation in a dense plasma. [supernovae core physics

NASA Technical Reports Server (NTRS)

Littleton, J. E.; Buchler, J.-R.

1974-01-01

The microscopic physics of the thermonuclear runaway in highly degenerate carbon-oxygen cores is investigated to determine if and how a detonation wave is generated. An expression for the electron-ion relaxation time is derived under the assumption of large degeneracy and extreme relativity of the electrons in a two-temperature plasma. Since the nuclear burning time proves to be several orders of magnitude shorter than the relaxation time, it is concluded that in studying the structure of the detonation wave the electrons and ions must be treated as separate fluids.

Collisionless dissipation in quasi-perpendicular shocks. [in terresrial bow waves

NASA Technical Reports Server (NTRS)

Forslund, D. W.; Quest, K. B.; Brackbill, J. U.; Lee, K.

1984-01-01

Microscopic dissipation processes in quasi-perpendicular shocks are studied by two-dimensional plasma simulations in which electrons and ions are treated as particles moving in self-consistent electric and magnetic fields. Cross-field currents induce substantial turbulence at the shock front reducing the reflected ion fraction, increasing the bulk ion temperature behind the shock, doubling the average magnetic ramp thickness, and enhancing the upstream field aligned electron heat flow. The short scale length magnetic fluctuations observed in the bow shock are probably associated with this turbulence.

Sensitive ionization of non-volatile analytes using protein solutions as spray liquid in desorption electrospray ionization mass spectrometry.

PubMed

Zhu, Zhiqiang; Han, Jing; Zhang, Yan; Zhou, Yafei; Xu, Ning; Zhang, Bo; Gu, Haiwei; Chen, Huanwen

2012-12-15

Desorption electrospray ionization (DESI) is the most popular ambient ionization technique for direct analysis of complex samples without sample pretreatment. However, for many applications, especially for trace analysis, it is of interest to improve the sensitivity of DESI-mass spectrometry (MS). In traditional DESI-MS, a mixture of methanol/water/acetic acid is usually used to generate the primary ions. In this article, dilute protein solutions were electrosprayed in the DESI method to create multiply charged primary ions for the desorption ionization of trace analytes on various surfaces (e.g., filter paper, glass, Al-foil) without any sample pretreatment. The analyte ions were then detected and structurally characterized using a LTQ XL mass spectrometer. Compared with the methanol/water/acetic acid (49:49:2, v/v/v) solution, protein solutions significantly increased the signal levels of non-volatile compounds such as benzoic acid, TNT, o-toluidine, peptide and insulin in either positive or negative ion detection mode. For all the analytes tested, the limits of detection (LODs) were reduced to about half of the original values which were obtained using traditional DESI. The results showed that the signal enhancement is highly correlated with the molecular weight of the proteins and the selected solid surfaces. The proposed DESI method is a universal strategy for rapid and sensitive detection of trace amounts of strongly bound and/or non-volatile analytes, including explosives, peptides, and proteins. The results indicate that the sensitivity of DESI can be further improved by selecting larger proteins and appropriate solid surfaces. Copyright © 2012 John Wiley & Sons, Ltd.

Transition from ideal to viscous Mach cones in a kinetic transport approach

NASA Astrophysics Data System (ADS)

Bouras, I.; El, A.; Fochler, O.; Niemi, H.; Xu, Z.; Greiner, C.

2012-04-01

Using a microscopic transport model we investigate the evolution of conical structures originating from the supersonic projectile moving through the hot matter of ultrarelativistic particles. Using different scenarios for the interaction between projectile and matter, and different transport properties of the matter, we study the formation and structure of Mach cones. Especially, a dependence of the Mach cone angle on the details and rate of the energy deposition from projectile to the matter is investigated. Furthermore, the two-particle correlations extracted from the numerical calculations are compared to an analytical approximation. We find that the propagation of a high energetic particle through the matter does not lead to the appearance of a double peak structure as observed in the ultrarelativistic heavy-ion collision experiments. The reason is the strongly forward-peaked energy and momentum deposition in the head shock region. In addition, by adjusting the cross section we investigate the influence of the viscosity to the structure of Mach cones. A clear and unavoidable smearing of the profile depending on a finite ratio of shear viscosity to entropy density is clearly visible.

Corrosion behavior of high-nickel and chromium alloys in natural Baltic seawater

DOE Office of Scientific and Technical Information (OSTI.GOV)

Birn, J.; Janik-Czachor, M.; Wolowik, A.

Effect of Cl{sup {minus}} ion concentration (O M sodium chloride [NaCl] to 2 M NaCl) and temperature (25 C to 75 C) on stability of the passive state of high-Ni and Cr alloys: NI-1 ({approximately} 16% Mo), CR-2 ({approximately} 6.2% Mo), and NI-3 (3.5% Mo) were investigated in acidic and neutral electrolytes in strictly controlled electrochemical conditions. The anodic behavior of the alloys appeared to depend mostly upon Mo content in the alloy. Thus, the NI-1 was the most stable alloy under the applied experimental conditions. The other alloys were also quite resistant, undergoing pitting only at elevated temperatures, atmore » high anodic potentials, and at a chloride concentration not lower than 1 M. In natural Baltic seawater, these alloys did not exhibit any tendency to pitting, in qualitative agreement with the accelerated electrochemical tests. Complementary microscopic and surface analytical (AES) investigations were carried out to correlate the anodic and corrosion behavior of these materials with their composition and structure, and the composition of the passivating films formed at their surfaces.« less

Enhancement of Compound Selectivity Using a Radio Frequency Ion-Funnel Proton Transfer Reaction Mass Spectrometer: Improved Specificity for Explosive Compounds.

PubMed

González-Méndez, Ramón; Watts, Peter; Olivenza-León, David; Reich, D Fraser; Mullock, Stephen J; Corlett, Clive A; Cairns, Stuart; Hickey, Peter; Brookes, Matthew; Mayhew, Chris A

2016-11-01

A key issue with any analytical system based on mass spectrometry with no initial separation of compounds is to have a high level of confidence in chemical assignment. This is particularly true for areas of security, such as airports, and recent terrorist attacks have highlighted the need for reliable analytical instrumentation. Proton transfer reaction mass spectrometry is a useful technology for these purposes because the chances of false positives are small owing to the use of a mass spectrometric analysis. However, the detection of an ion at a given m/z for an explosive does not guarantee that that explosive is present. There is still some ambiguity associated with any chemical assignment owing to the presence of isobaric compounds and, depending on mass resolution, ions with the same nominal m/z. In this article we describe how for the first time the use of a radio frequency ion-funnel (RFIF) in the reaction region (drift tube) of a proton transfer reaction-time-of-flight-mass spectrometer (PTR-ToF-MS) can be used to enhance specificity by manipulating the ion-molecule chemistry through collisional induced processes. Results for trinitrotoluene, dinitrotoluenes, and nitrotoluenes are presented to demonstrate the advantages of this new RFIF-PTR-ToF-MS for analytical chemical purposes.

Ion-pairing HPLC methods to determine EDTA and DTPA in small molecule and biological pharmaceutical formulations.

PubMed

Wang, George; Tomasella, Frank P

2016-06-01

Ion-pairing high-performance liquid chromatography-ultraviolet (HPLC-UV) methods were developed to determine two commonly used chelating agents, ethylenediaminetetraacetic acid (EDTA) in Abilify® (a small molecule drug with aripiprazole as the active pharmaceutical ingredient) oral solution and diethylenetriaminepentaacetic acid (DTPA) in Yervoy® (a monoclonal antibody drug with ipilimumab as the active pharmaceutical ingredient) intravenous formulation. Since the analytes, EDTA and DTPA, do not contain chromophores, transition metal ions (Cu 2+ , Fe 3+ ) which generate highly stable metallocomplexes with the chelating agents were added into the sample preparation to enhance UV detection. The use of metallocomplexes with ion-pairing chromatography provides the ability to achieve the desired sensitivity and selectivity in the development of the method. Specifically, the sample preparation involving metallocomplex formation allowed sensitive UV detection. Copper was utilized for the determination of EDTA and iron was utilized for the determination of DTPA. In the case of EDTA, a gradient mobile phase separated the components of the formulation from the analyte. In the method for DTPA, the active drug substance, ipilimumab, was eluted in the void. In addition, the optimization of the concentration of the ion-pairing reagent was discussed as a means of enhancing the retention of the aminopolycarboxylic acids (APCAs) including EDTA and DTPA and the specificity of the method. The analytical method development was designed based on the chromatographic properties of the analytes, the nature of the sample matrix and the intended purpose of the method. Validation data were presented for the two methods. Finally, both methods were successfully utilized in determining the fate of the chelates.

ANALYSIS OF ELECTROLESS NICKEL SOLUTIONS BY ANION CHROMATOGRAPHY

EPA Science Inventory

The principal appeal of ion chromatography (IC) as analytical technique lies in the ability to rapidly analyze a mixture of ions of widely varying concentrations and properties in a single elution. It is therefore not surprising that IC has been hampered by the similar ion exchan...

Physicochemical characterisation of natural K-clinoptilolite and heavy-metal forms from Gördes (Manisa, western Turkey)

NASA Astrophysics Data System (ADS)

Ünaldı, Tevfik; Mızrak, İbrahim; Kadir, Selahattin

2013-12-01

Physicochemical characterisation of natural K-clinoptilolite and heavy-metal (Ag+, Cd2+, Cr3+ and Co3+) forms was accomplished through ion exchange by batch, X-ray diffractometric (XRD), X-ray fluorescence (XRF), infrared-spectral (FT-IR), differential thermal analysis-thermal gravimetric (DTA-TG) and scanning-electron microscopic (SEM) methods. Increasing the normality in the cases of heavy-metal forms resulted in decrease in crystallinity and increases in unit-cell volume, rate of ion exchange, and percentage of ion selectivity. In this study, the order of ion-selectivity percentages (rather than ion selectivity) of heavy-metal forms was determined to be Ag+ > Cd2+ > Cr3+ > Co3+. This finding is consistent with the results of worldwide research on the order of ion selectivity in modified clinoptilolite.

A study of structural and mechanical properties of nano-crystalline tungsten nitride film synthesis by plasma focus

NASA Astrophysics Data System (ADS)

Hussnain, Ali; Singh Rawat, Rajdeep; Ahmad, Riaz; Hussain, Tousif; Umar, Z. A.; Ikhlaq, Uzma; Chen, Zhong; Shen, Lu

2015-02-01

Nano-crystalline tungsten nitride thin films are synthesized on AISI-304 steel at room temperature using Mather-type plasma focus system. The surface properties of the exposed substrate against different deposition shots are examined for crystal structure, surface morphology and mechanical properties using X-ray diffraction (XRD), atomic force microscope, field emission scanning electron microscope and nano-indenter. The XRD results show the growth of WN and WN2 phases and the development of strain/stress in the deposited films by varying the number of deposition shots. Morphology of deposited films shows the significant change in the surface structure with different ion energy doses (number of deposition shots). Due to the effect of different ion energy doses, the strain/stress developed in the deposited film leads to an improvement of hardness of deposited films.

Surface modification of LiNbO3 and KTa1-xNbxO3 crystals irradiated by intense pulsed ion beam

NASA Astrophysics Data System (ADS)

Cui, Xiaojun; Shen, Jie; Zhong, Haowen; Zhang, Jie; Yu, Xiao; Liang, Guoying; Qu, Miao; Yan, Sha; Zhang, Xiaofu; Le, Xiaoyun

2017-10-01

In this work, we studied the surface modification of LiNbO3 and KTa1-xNbxO3 irradiated by intense pulsed ion beam, which was mainly composed of H+ (70%) and Cn+ (30%) at an acceleration voltage of about 450 kV. The surface morphologies, microstructural evolution and elemental analysis of the sample surfaces after IPIB irradiation have been analyzed by scanning electron microscope, atomic force microscope, X-ray diffraction and energy dispersive spectrometer techniques, respectively. The results show that the surface morphologies have significant difference impacted by the irradiation effect. Regular gully damages range from 200 to 400 nm in depth appeared in LiNbO3 under 2 J/cm2 energy density for 1 pulse, block cracking appeared in KTa1-xNbxO3 at the same condition. Surface of the crystals have melted and were darkened with the increasing number up to 5 pulses. Crystal lattice arrangement is believed to be the dominant reason for the different experimental results irradiated by intense pulsed ion beam.

Helium ion microscopy and energy selective scanning electron microscopy - two advanced microscopy techniques with complementary applications

NASA Astrophysics Data System (ADS)

Rodenburg, C.; Jepson, M. A. E.; Boden, Stuart A.; Bagnall, Darren M.

2014-06-01

Both scanning electron microscopes (SEM) and helium ion microscopes (HeIM) are based on the same principle of a charged particle beam scanning across the surface and generating secondary electrons (SEs) to form images. However, there is a pronounced difference in the energy spectra of the emitted secondary electrons emitted as result of electron or helium ion impact. We have previously presented evidence that this also translates to differences in the information depth through the analysis of dopant contrast in doped silicon structures in both SEM and HeIM. Here, it is now shown how secondary electron emission spectra (SES) and their relation to depth of origin of SE can be experimentally exploited through the use of energy filtering (EF) in low voltage SEM (LV-SEM) to access bulk information from surfaces covered by damage or contamination layers. From the current understanding of the SES in HeIM it is not expected that EF will be as effective in HeIM but an alternative that can be used for some materials to access bulk information is presented.

Analytical transmission cross-coefficients for pink beam X-ray microscopy based on compound refractive lenses.

PubMed

Falch, Ken Vidar; Detlefs, Carsten; Snigirev, Anatoly; Mathiesen, Ragnvald H

2018-01-01

Analytical expressions for the transmission cross-coefficients for x-ray microscopes based on compound refractive lenses are derived based on Gaussian approximations of the source shape and energy spectrum. The effects of partial coherence, defocus, beam convergence, as well as lateral and longitudinal chromatic aberrations are accounted for and discussed. Taking the incoherent limit of the transmission cross-coefficients, a compact analytical expression for the modulation transfer function of the system is obtained, and the resulting point, line and edge spread functions are presented. Finally, analytical expressions for optimal numerical aperture, coherence ratio, and bandwidth are given. Copyright © 2017 Elsevier B.V. All rights reserved.

New Cs sputter ion source with polyatomic ion beams for secondary ion mass spectrometry applications

NASA Astrophysics Data System (ADS)

Belykh, S. F.; Palitsin, V. V.; Veryovkin, I. V.; Kovarsky, A. P.; Chang, R. J. H.; Adriaens, A.; Dowsett, M. G.; Adams, F.

2007-08-01

A simple design for a cesium sputter ion source compatible with vacuum and ion-optical systems as well as with electronics of the commercially available Cameca IMS-4f instrument is reported. This ion source has been tested with the cluster primary ions of Sin- and Cun-. Our experiments with surface characterization and depth profiling conducted to date demonstrate improvements of the analytical capabilities of the secondary ion mass spectrometry instrument due to the nonadditive enhancement of secondary ion emission and shorter ion ranges of polyatomic projectiles compared to atomic ones with the same impact energy.

Discriminant analysis of fused positive and negative ion mobility spectra using multivariate self-modeling mixture analysis and neural networks.

PubMed

Chen, Ping; Harrington, Peter B

2008-02-01

A new method coupling multivariate self-modeling mixture analysis and pattern recognition has been developed to identify toxic industrial chemicals using fused positive and negative ion mobility spectra (dual scan spectra). A Smiths lightweight chemical detector (LCD), which can measure positive and negative ion mobility spectra simultaneously, was used to acquire the data. Simple-to-use interactive self-modeling mixture analysis (SIMPLISMA) was used to separate the analytical peaks in the ion mobility spectra from the background reactant ion peaks (RIP). The SIMPLSIMA analytical components of the positive and negative ion peaks were combined together in a butterfly representation (i.e., negative spectra are reported with negative drift times and reflected with respect to the ordinate and juxtaposed with the positive ion mobility spectra). Temperature constrained cascade-correlation neural network (TCCCN) models were built to classify the toxic industrial chemicals. Seven common toxic industrial chemicals were used in this project to evaluate the performance of the algorithm. Ten bootstrapped Latin partitions demonstrated that the classification of neural networks using the SIMPLISMA components was statistically better than neural network models trained with fused ion mobility spectra (IMS).

Electron-Impact-Ionization and Electron-Attachment Cross Sections of Radicals Important in Transient Gaseous Discharges.

DTIC Science & Technology

1988-02-05

for understanding the microscopic processes of electrical discharges and for designing gaseous discharge switches. High power gaseous discharge switches...half-maximum) energy resolution. The electron gun and ion extraction were of the same design of Srivastava at the Jet Propulsion Laboratory. Ions...photons. - The observed current switching can be applied to the design of discharge switches. Elec- tron transport parameters are needed for the

Quantum Computing in Diamond

DTIC Science & Technology

2007-05-28

104 N2 103 N2 (a) (b) (c) Fig. 1: Confocal microscope images of NV centers created in bulk diamond through ion implantation of (a) gallium ions...nitrogen defects in diamond by chemical vapour deposition, J. R. Rabeau, S. Prawer, Y.L. Chin, F. Jelezko, T. Gaebel, and J. Wrachtrup, Applied...Physics Letters, 86, 31926, (2005) 2. Diamond Chemical Vapour Deposition on Opitcal Fibres for Fluorescence Waveguiding, J.R. Rabeau, S.T

Deprotonation effect of tetrahydrofuran-2-carbonitrile buffer gas dopant in ion mobility spectrometry.

PubMed

Fernandez-Maestre, Roberto; Meza-Morelos, Dairo; Wu, Ching

2016-06-15

When dopants are introduced into the buffer gas of an ion mobility spectrometer, spectra are simplified due to charge competition. We used electrospray ionization to inject tetrahydrofuran-2-carbonitrile (F, 2-furonitrile or 2-furancarbonitrile) as a buffer gas dopant into an ion mobility spectrometer coupled to a quadrupole mass spectrometer. Density functional theory was used for theoretical calculations of dopant-ion interaction energies and proton affinities, using the hybrid functional X3LYP/6-311++(d,p) with the Gaussian 09 program that accounts for the basis set superposition error; analytes structures and theoretical calculations with Gaussian were used to explain the behavior of the analytes upon interaction with F. When F was used as a dopant at concentrations below 1.5 mmol m(-3) in the buffer gas, ions were not observed for α-amino acids due to charge competition with the dopant; this deprotonation capability arises from the production of a dimer with a high formation energy that stabilized the positive charge and created steric hindrance that deterred the equilibrium with analyte ions. F could not completely strip other compounds of their charge because they either showed steric hindrance at the charge site that deterred the approach of the dopant (2,4-lutidine, and DTBP), formed intramolecular bonds that stabilized the positive charge (atenolol), had high proton affinity (2,4-lutidine, DTBP, valinol and atenolol), or were inherently ionic (tetraalkylammonium ions). This selective deprotonation suggests the use of F to simplify spectra of complex mixtures in ion mobility and mass spectrometry in metabolomics, proteomics and other studies that generate complex spectra with thousands of peaks. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Testing the Applicability of Nernst-Planck Theory in Ion Channels: Comparisons with Brownian Dynamics Simulations

PubMed Central

Song, Chen; Corry, Ben

2011-01-01

The macroscopic Nernst-Planck (NP) theory has often been used for predicting ion channel currents in recent years, but the validity of this theory at the microscopic scale has not been tested. In this study we systematically tested the ability of the NP theory to accurately predict channel currents by combining and comparing the results with those of Brownian dynamics (BD) simulations. To thoroughly test the theory in a range of situations, calculations were made in a series of simplified cylindrical channels with radii ranging from 3 to 15 Å, in a more complex ‘catenary’ channel, and in a realistic model of the mechanosensitive channel MscS. The extensive tests indicate that the NP equation is applicable in narrow ion channels provided that accurate concentrations and potentials can be input as the currents obtained from the combination of BD and NP match well with those obtained directly from BD simulations, although some discrepancies are seen when the ion concentrations are not radially uniform. This finding opens a door to utilising the results of microscopic simulations in continuum theory, something that is likely to be useful in the investigation of a range of biophysical and nano-scale applications and should stimulate further studies in this direction. PMID:21731672

Testing the applicability of Nernst-Planck theory in ion channels: comparisons with Brownian dynamics simulations.

PubMed

Song, Chen; Corry, Ben

2011-01-01

The macroscopic Nernst-Planck (NP) theory has often been used for predicting ion channel currents in recent years, but the validity of this theory at the microscopic scale has not been tested. In this study we systematically tested the ability of the NP theory to accurately predict channel currents by combining and comparing the results with those of Brownian dynamics (BD) simulations. To thoroughly test the theory in a range of situations, calculations were made in a series of simplified cylindrical channels with radii ranging from 3 to 15 Å, in a more complex 'catenary' channel, and in a realistic model of the mechanosensitive channel MscS. The extensive tests indicate that the NP equation is applicable in narrow ion channels provided that accurate concentrations and potentials can be input as the currents obtained from the combination of BD and NP match well with those obtained directly from BD simulations, although some discrepancies are seen when the ion concentrations are not radially uniform. This finding opens a door to utilising the results of microscopic simulations in continuum theory, something that is likely to be useful in the investigation of a range of biophysical and nano-scale applications and should stimulate further studies in this direction.

Laboratory Evaluation of Ion-Selective Electrodes for Simultaneous Analysis of Macronutrients in Hydroponic Solution

USDA-ARS?s Scientific Manuscript database

Automated sensing of macronutrients in hydroponic solution would allow more efficient management of nutrients for crop growth in closed hydroponic systems. Ion-selective microelectrode technology requires an ion-selective membrane or a solid metal material that responds selectively to one analyte in...

Four-probe measurements with a three-probe scanning tunneling microscope.

PubMed

Salomons, Mark; Martins, Bruno V C; Zikovsky, Janik; Wolkow, Robert A

2014-04-01

We present an ultrahigh vacuum (UHV) three-probe scanning tunneling microscope in which each probe is capable of atomic resolution. A UHV JEOL scanning electron microscope aids in the placement of the probes on the sample. The machine also has a field ion microscope to clean, atomically image, and shape the probe tips. The machine uses bare conductive samples and tips with a homebuilt set of pliers for heating and loading. Automated feedback controlled tip-surface contacts allow for electrical stability and reproducibility while also greatly reducing tip and surface damage due to contact formation. The ability to register inter-tip position by imaging of a single surface feature by multiple tips is demonstrated. Four-probe material characterization is achieved by deploying two tips as fixed current probes and the third tip as a movable voltage probe.

Fast detection of narcotics by single photon ionization mass spectrometry and laser ion mobility spectrometry

NASA Astrophysics Data System (ADS)

Laudien, Robert; Schultze, Rainer; Wieser, Jochen

2010-10-01

In this contribution two analytical devices for the fast detection of security-relevant substances like narcotics and explosives are presented. One system is based on an ion trap mass spectrometer (ITMS) with single photon ionization (SPI). This soft ionization technique, unlike electron impact ionization (EI), reduces unwanted fragment ions in the mass spectra allowing the clear determination of characteristic (usually molecular) ions. Their enrichment in the ion trap and identification by tandem MS investigations (MS/MS) enables the detection of the target substances in complex matrices at low concentrations without time-consuming sample preparation. For SPI an electron beam pumped excimer light source of own fabrication (E-Lux) is used. The SPI-ITMS system was characterized by the analytical study of different drugs like cannabis, heroin, cocaine, amphetamines, and some precursors. Additionally, it was successfully tested on-site in a closed illegal drug laboratory, where low quantities of MDMA could be directly detected in samples from floors, walls and lab equipments. The second analytical system is based on an ion mobility (IM) spectrometer with resonant multiphoton ionization (REMPI). With the frequency quadrupled Nd:YAG laser (266 nm), used for ionization, a selective and sensitive detection of aromatic compounds is possible. By application of suited aromatic dopants, in addition, also non-aromatic polar compounds are accessible by ion molecule reactions like proton transfer or complex formation. Selected drug precursors could be successfully detected with this device as well, qualifying it to a lower-priced alternative or useful supplement of the SPI-ITMS system for security analysis.

Matching the laser wavelength to the absorption properties of matrices increases the ion yield in UV-MALDI mass spectrometry.

PubMed

Wiegelmann, Marcel; Soltwisch, Jens; Jaskolla, Thorsten W; Dreisewerd, Klaus

2013-09-01

A high analytical sensitivity in ultraviolet matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) is only achieved if the laser wavelength corresponds to a high optical absorption of the matrix. Laser fluence and the physicochemical properties of the compounds, e.g., the proton affinity, also influence analytical sensitivity significantly. In combination, these parameters determine the amount of material ejected per laser pulse and the ion yield, i.e., the fraction of ionized biomolecules. Here, we recorded peptide ion signal intensities as a function of these parameters. Three cinnamic acid matrices were investigated: α-cyano-4-hydroxycinnamic acid, α-cyano-4-chlorocinnamic acid, and α-cyano-2,4-difluorocinnamic acid. In addition, 2,5-dihydroxybenzoic acid was used in comparison experiments. Ion signal intensities "per laser shot" and integrated ion signal intensities were acquired over 900 consecutive laser pulses applied on distinct positions on the dried-droplet sample preparations. With respect to laser wavelength, the two standard MALDI wavelengths of 337/355 nm were investigated. Also, 305 or 320 nm was selected to account for the blue-shifted absorption profiles of the halogenated derivatives. Maximal peptide ion intensities were obtained if the laser wavelength fell within the peak of the absorption profile of the compound and for fluences two to three times the corresponding ion detection threshold. The results indicate ways for improving the analytical sensitivity in MALDI-MS, and in particular for MALDI-MS imaging applications where a limited amount of material is available per irradiated pixel.

Low-cost and reagent-free paper-based device to detect chloride ions in serum and sweat.

PubMed

Cinti, Stefano; Fiore, Luca; Massoud, Renato; Cortese, Claudio; Moscone, Danila; Palleschi, Giuseppe; Arduini, Fabiana

2018-03-01

The recent goal of sustainability in analytical chemistry has boosted the development of eco-designed analytical tools to deliver fast and cost-effective analysis with low economic and environmental impact. Due to the recent focus in sustainability, we report the use of low-cost filter paper as a sustainable material to print silver electrodes and to load reagents for a reagent-free electrochemical detection of chloride in biological samples, namely serum and sweat. The electrochemical detection of chloride ions was carried out by exploiting the reaction of the analyte (i.e. chloride) with the silver working electrode. During the oxidation wave in cyclic voltammetry the silver ions are produced, thus they react with chloride ions to form AgCl, while in the reduction wave, the following reaction occurs: AgCl + e - -->Ag + Cl - . These reactions at the electrode surface resulted in anodic/cathodic peaks directly proportional to the chloride ions in solution. Chloride ions were detected with the addition of only 10μL of the sample on the paper-based electrochemical cell, obtaining linearity up to 200mM with a detection limit equal to 1mM and relative standard deviation lower than 10%. The accuracy of the sensor was evaluated in serum and sweat samples, with percentage recoveries between 93 ± 10 and 108 ± 8%. Moreover, the results achieved with the paper-based device were positively compared with those obtained by using the gold standard method (Ion Selective Electrode) adopted in routine clinical analyses. Copyright © 2017 Elsevier B.V. All rights reserved.

Space Plasma Ion Processing of Ilmenite in the Lunar Soil: Insights from In-Situ TEM Ion Irradiation Experiments

NASA Technical Reports Server (NTRS)

Christoffersen, R.; Keller, L. P.

2007-01-01

Space weathering on the moon and asteroids results largely from the alteration of the outer surfaces of regolith grains by the combined effects of solar ion irradiation and other processes that include deposition of impact or sputter-derived vapors. Although no longer considered the sole driver of space weathering, solar ion irradiation remains a key part of the space weathering puzzle, and quantitative data on its effects on regolith minerals are still in short supply. For the lunar regolith, previous transmission electron microscope (TEM) studies performed by ourselves and others have uncovered altered rims on ilmenite (FeTiO3) grains that point to this phase as a unique "witness plate" for unraveling nanoscale space weathering processes. Most notably, the radiation processed portions of these ilmenite rims consistently have a crystalline structure, in contrast to radiation damaged rims on regolith silicates that are characteristically amorphous. While this has tended to support informal designation of ilmenite as a "radiation resistant" regolith mineral, there are to date no experimental data that directly and quantitatively compare ilmenite s response to ion radiation relative to lunar silicates. Such data are needed because the radiation processed rims on ilmenite grains, although crystalline, are microstructurally and chemically complex, and exhibit changes linked to the formation of nanophase Fe metal, a key space weathering process. We report here the first ion radiation processing study of ilmenite performed by in-situ means using the Intermediate Voltage Electron Microscope- Tandem Irradiation facility (IVEM-Tandem) at Argonne National Laboratory. The capability of this facility for performing real time TEM observations of samples concurrent with ion irradiation makes it uniquely suited for studying the dose-dependence of amorphization and other changes in irradiated samples.

Ion yields in UV-MALDI mass spectrometry as a function of excitation laser wavelength and optical and physico-chemical properties of classical and halogen-substituted MALDI matrixes.

PubMed

Soltwisch, Jens; Jaskolla, Thorsten W; Hillenkamp, Franz; Karas, Michael; Dreisewerd, Klaus

2012-08-07

The laser wavelength constitutes a key parameter in ultraviolet-matrix-assisted laser desorption ionization-mass spectrometry (UV-MALDI-MS). Optimal analytical results are only achieved at laser wavelengths that correspond to a high optical absorption of the matrix. In the presented work, the wavelength dependence and the contribution of matrix proton affinity to the MALDI process were investigated. A tunable dye laser was used to examine the wavelength range between 280 and 355 nm. The peptide and matrix ion signals recorded as a function of these irradiation parameters are displayed in the form of heat maps, a data representation that furnishes multidimensional data interpretation. Matrixes with a range of proton affinities from 809 to 866 kJ/mol were investigated. Among those selected are the standard matrixes 2,5-dihydroxybenzoic acid (DHB) and α-cyano-4-hydroxycinnamic acid (HCCA) as well as five halogen-substituted cinnamic acid derivatives, including the recently introduced 4-chloro-α-cyanocinnamic acid (ClCCA) and α-cyano-2,4-difluorocinnamic acid (DiFCCA) matrixes. With the exception of DHB, the highest analyte ion signals were obtained toward the red side of the peak optical absorption in the solid state. A stronger decline of the molecular analyte ion signals generated from the matrixes was consistently observed at the low wavelength side of the peak absorption. This effect is mainly the result of increased fragmentation of both analyte and matrix ions. Optimal use of multiply halogenated matrixes requires adjustment of the excitation wavelength to values below that of the standard MALDI lasers emitting at 355 (Nd:YAG) or 337 nm (N(2) laser). The combined data provide new insights into the UV-MALDI desorption/ionization processes and indicate ways to improve the analytical sensitivity.

Imaging and elemental mapping of biological specimens with a dual-EDS dedicated scanning transmission electron microscope

PubMed Central

Wu, J.S.; Kim, A. M.; Bleher, R.; Myers, B.D.; Marvin, R. G.; Inada, H.; Nakamura, K.; Zhang, X.F.; Roth, E.; Li, S.Y.; Woodruff, T. K.; O'Halloran, T. V.; Dravid, Vinayak P.

2013-01-01

A dedicated analytical scanning transmission electron microscope (STEM) with dual energy dispersive spectroscopy (EDS) detectors has been designed for complementary high performance imaging as well as high sensitivity elemental analysis and mapping of biological structures. The performance of this new design, based on a Hitachi HD-2300A model, was evaluated using a variety of biological specimens. With three imaging detectors, both the surface and internal structure of cells can be examined simultaneously. The whole-cell elemental mapping, especially of heavier metal species that have low cross-section for electron energy loss spectroscopy (EELS), can be faithfully obtained. Optimization of STEM imaging conditions is applied to thick sections as well as thin sections of biological cells under low-dose conditions at room- and cryogenic temperatures. Such multimodal capabilities applied to soft/biological structures usher a new era for analytical studies in biological systems. PMID:23500508

A capillary electrophoresis chip for the analysis of print and film photographic developing agents in commercial processing solutions using indirect fluorescence detection.

PubMed

Sirichai, S; de Mello, A J

2001-01-01

The separation and detection of both print and film developing agents (CD-3 and CD-4) in photographic processing solutions using chip-based capillary electrophoresis is presented. For simultaneous detection of both analytes under identical experimental conditions a buffer pH of 11.9 is used to partially ionise the analytes. Detection is made possible by indirect fluorescence, where the ions of the analytes displace the anionic fluorescing buffer ion to create negative peaks. Under optimal conditions, both analytes can be analyzed within 30 s. The limits of detection for CD-3 and CD-4 are 0.17 mM and 0.39 mM, respectively. The applicability of the method for the analysis of seasoned photographic processing developer solutions is also examined.

Analytical model for the density distribution in the Io plasma torus

NASA Technical Reports Server (NTRS)

Mei, YI; Thorne, Richard M.; Bagenal, Fran

1995-01-01

An analytical model is developed for the diffusive equilibrium plasma density distribution in the Io plasma torus. The model has been employed successfully to follow the ray path of plasma waves in the multi-ion Jovian magnetosphere; it would also be valuable for other studies of the Io torus that require a smooth and continuous description of the plasma density and its gradients. Validity of the analytical treatment requires that the temperature of thermal electrons be much lower than the ion temperature and that superthermal electrons be much less abundant than the thermal electrons; these two conditions are satisfied in the warm outer region of the Io torus from L = 6 to L = 10. The analytical solutions agree well with exact numerical calculations for the most dense portion of the Io torus within 30 deg of the equator.

Porosity characterization for heterogeneous shales using integrated multiscale microscopy

NASA Astrophysics Data System (ADS)

Rassouli, F.; Andrew, M.; Zoback, M. D.

2016-12-01

Pore size distribution analysis plays a critical role in gas storage capacity and fluid transport characterization of shales. Study of the diverse distribution of pore size and structure in such low permeably rocks is withheld by the lack of tools to visualize the microstructural properties of shale rocks. In this paper we try to use multiple techniques to investigate the full pore size range in different sample scales. Modern imaging techniques are combined with routine analytical investigations (x-ray diffraction, thin section analysis and mercury porosimetry) to describe pore size distribution of shale samples from Haynesville formation in East Texas to generate a more holistic understanding of the porosity structure in shales, ranging from standard core plug down to nm scales. Standard 1" diameter core plug samples were first imaged using a Versa 3D x-ray microscope at lower resolutions. Then we pick several regions of interest (ROIs) with various micro-features (such as micro-cracks and high organic matters) in the rock samples to run higher resolution CT scans using a non-destructive interior tomography scans. After this step, we cut the samples and drill 5 mm diameter cores out of the selected ROIs. Then we rescan the samples to measure porosity distribution of the 5 mm cores. We repeat this step for samples with diameter of 1 mm being cut out of the 5 mm cores using a laser cutting machine. After comparing the pore structure and distribution of the samples measured form micro-CT analysis, we move to nano-scale imaging to capture the ultra-fine pores within the shale samples. At this stage, the diameter of the 1 mm samples will be milled down to 70 microns using the laser beam. We scan these samples in a nano-CT Ultra x-ray microscope and calculate the porosity of the samples by image segmentation methods. Finally, we use images collected from focused ion beam scanning electron microscopy (FIB-SEM) to be able to compare the results of porosity measurements from all different imaging techniques. These multi-scale characterization techniques are then compared with traditional analytical techniques such as Mercury Porosimetry.

Live cell imaging at the Munich ion microbeam SNAKE - a status report.

PubMed

Drexler, Guido A; Siebenwirth, Christian; Drexler, Sophie E; Girst, Stefanie; Greubel, Christoph; Dollinger, Günther; Friedl, Anna A

2015-02-18

Ion microbeams are important tools in radiobiological research. Still, the worldwide number of ion microbeam facilities where biological experiments can be performed is limited. Even fewer facilities combine ion microirradiation with live-cell imaging to allow microscopic observation of cellular response reactions starting very fast after irradiation and continuing for many hours. At SNAKE, the ion microbeam facility at the Munich 14 MV tandem accelerator, a large variety of biological experiments are performed on a regular basis. Here, recent developments and ongoing research projects at the ion microbeam SNAKE are presented with specific emphasis on live-cell imaging experiments. An overview of the technical details of the setup is given, including examples of suitable biological samples. By ion beam focusing to submicrometer beam spot size and single ion detection it is possible to target subcellular structures with defined numbers of ions. Focusing of high numbers of ions to single spots allows studying the influence of high local damage density on recruitment of damage response proteins.

Ion Release and Galvanic Corrosion of Different Orthodontic Brackets and Wires in Artificial Saliva.

PubMed

Tahmasbi, Soodeh; Sheikh, Tahereh; Hemmati, Yasamin B

2017-03-01

To investigate the galvanic corrosion of brackets manufactured by four different companies coupled with stainless steel (SS) or nickel-titanium (NiTi) wires in an artificial saliva solution. A total of 24 mandibular central incisor Roth brackets of four different manufacturers (American Orthodontics, Dentaurum, Shinye, ORJ) were used in this experimental study. These brackets were immersed in artificial saliva along with SS or NiTi orthodontic wires (0.016'', round) for 28 days. The electric potential difference of each bracket/ wire coupled with a saturated calomel reference electrode was measured via a voltmeter and recorded constantly. Corrosion rate (CR) was calculated, and release of ions was measured with an atomic absorption spectrometer. Stereomicroscope was used to evaluate all samples. Then, samples with corrosion were further assessed by scanning electron microscope and energy-dispersive X-ray spectroscopy. Two-way analysis of variance was used to analyze data. Among ions evaluated, release of nickel ions from Shinye brackets was significantly higher than that of other brackets. The mean potential difference was significantly lower in specimens containing a couple of Shinye brackets and SS wire compared with other specimens. No significant difference was observed in the mean CR of various groups (p > 0.05). Microscopic evaluation showed corrosion in two samples only: Shinye bracket coupled with SS wire and American Orthodontics bracket coupled with NiTi wire. Shinye brackets coupled with SS wire showed more susceptibility to galvanic corrosion. There were no significant differences among specimens in terms of the CR or released ions except the release of Ni ions, which was higher in Shinye brackets.

Doped δ-bismuth oxides to investigate oxygen ion transport as a metric for condensed phase thermite ignition.

PubMed

Wang, Xizheng; Zhou, Wenbo; DeLisio, Jeffery B; Egan, Garth C; Zachariah, Michael R

2017-05-24

Nanothermites offer high energy density and high burn rates, but are mechanistically only now being understood. One question of interest is how initiation occurs and how the ignition temperature is related to microscopic controlling parameters. In this study, we explored the potential role of oxygen ion transport in Bi 2 O 3 as a controlling mechanism for condensed phase ignition reaction. Seven different doped δ-Bi 2 O 3 were synthesized by aerosol spray pyrolysis. The ignition temperatures of Al/doped Bi 2 O 3 , C/doped Bi 2 O 3 and Ta/doped Bi 2 O 3 were measured by temperature-jump/time-of-flight mass spectrometer coupled with a high-speed camera respectively. These results were then correlated to the corresponding oxygen ion conductivity (directly proportional to ion diffusivity) for these doped Bi 2 O 3 measured by impedance spectroscopy. We find that ignition of thermite with doped Bi 2 O 3 as oxidizer occurs at a critical oxygen ion conductivity (∼0.06 S cm -1 ) of doped Bi 2 O 3 in the condensed-phase so long as the aluminum is in a molten state. These results suggest that oxygen ion transport limits the condensed state Bi 2 O 3 oxidized thermite ignition. We also find that the larger oxygen vacancy concentration and the smaller metal-oxide bond energy in doped Bi 2 O 3 , the lower the ignition temperature. The latter suggests that we can consider the possibility of manipulating microscopic properties within a crystal, to tune the resultant energetic properties.

Method of forming aperture plate for electron microscope

NASA Technical Reports Server (NTRS)

Heinemann, K. (Inventor)

1974-01-01

An electron microscope is described with an electron source a condenser lens having either a circular aperture for focusing a solid cone of electrons onto a specimen or an annular aperture for focusing a hollow cone of electrons onto the specimen. It also has objective lens with an annular objective aperture, for focusing electrons passing through the specimen onto an image plane. A method of making the annular objective aperture using electron imaging, electrolytic deposition and ion etching techniques is included.

Estimation of changes in nickel and chromium content in nickel-titanium and stainless steel orthodontic wires used during orthodontic treatment: An analytical and scanning electron microscopic study

PubMed Central

Kararia, Vandana; Jain, Pradeep; Chaudhary, Seema; Kararia, Nitin

2015-01-01

Introduction: The biocompatibility of orthodontic dental alloys has been investigated over the past 20 years, but the results have been inconclusive. The study compares standard 3 M Unitek nickel-titanium (NiTi) and stainless steel archwires with locally available JJ orthodontics wires. Scanning electron microscope (SEM) study of surface changes and complexometric titration to study compositional change was performed. Materials and Methods: Ten archwires each of group 1–3 M 0.016” NiTi, group 2-JJ 0.016” NiTi, group 3–3 M 0.019” *0.025” SS and group 4-JJ SS contributed a 10 mm piece of wire for analysis prior to insertion in the patient and 6 weeks post insertion. SEM images were recorded at ×2000, ×4000 and ×6000 magnification. The same samples were subjected to complexiometric titration using ethylenediaminetetraacetic acid to gauge the actual change in the composition. Observations and Results: The SEM images of all the archwires showed marked changes with deep scratches and grooves and dark pitting corrosion areas post intraoral use. 3M wires showed an uniform criss-cross pattern in as received wires indicating a coating which was absent after intraoral use. There was a significant release of Nickel and Chromium from both group 3 and 4. Group 2 wires released ions significantly more than group 1 (P = 0.0). Conclusion: Extensive and stringent trials are required before certifying any product to be used in Orthodontics. PMID:25684911

Ion acceleration in shell cylinders irradiated by a short intense laser pulse

DOE Office of Scientific and Technical Information (OSTI.GOV)

Andreev, A.; ELI-ALPS, Szeged; Platonov, K.

The interaction of a short high intensity laser pulse with homo and heterogeneous shell cylinders has been analyzed using particle-in-cell simulations and analytical modeling. We show that the shell cylinder is proficient of accelerating and focusing ions in a narrow region. In the case of shell cylinder, the ion energy exceeds the ion energy for a flat target of the same thickness. The constructed model enables the evaluation of the ion energy and the number of ions in the focusing region.

Fiber optic sensors for corrosion detection

NASA Technical Reports Server (NTRS)

Smith, Alphonso C.

1993-01-01

The development of fiber optic sensors for the detection of a variety of material parameters has grown tremendously over the past several years. Additionally, the potential for analytical applications of fiber optic sensors have become more widely used. New pH sensors have also been developed using fiber optic techniques to detect fluorescence characteristics from immobilized fluorogenic reagent chemicals. The primary purpose of this research was to investigate the feasibility of using fiber optic sensors to detect the presence of Al(sup 3+) ions made in the process of environmental corrosion of aluminum materials. The Al(sup 3+) ions plus a variety of other type of metal ions can be detected using analytical techniques along with fiber optic sensors.

An analytic expression for the sheath criterion in magnetized plasmas with multi-charged ion species

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hatami, M. M., E-mail: m-hatami@kntu.ac.ir

2015-04-15

The generalized Bohm criterion in magnetized multi-component plasmas consisting of multi-charged positive and negative ion species and electrons is analytically investigated by using the hydrodynamic model. It is assumed that the electrons and negative ion density distributions are the Boltzmann distribution with different temperatures and the positive ions enter into the sheath region obliquely. Our results show that the positive and negative ion temperatures, the orientation of the applied magnetic field and the charge number of positive and negative ions strongly affect the Bohm criterion in these multi-component plasmas. To determine the validity of our derived generalized Bohm criterion, itmore » reduced to some familiar physical condition and it is shown that monotonically reduction of the positive ion density distribution leading to the sheath formation occurs only when entrance velocity of ion into the sheath satisfies the obtained Bohm criterion. Also, as a practical application of the obtained Bohm criterion, effects of the ionic temperature and concentration as well as magnetic field on the behavior of the charged particle density distributions and so the sheath thickness of a magnetized plasma consisting of electrons and singly charged positive and negative ion species are studied numerically.« less

Three modified activated carbons by different ligands for the solid phase extraction of copper and lead.

PubMed

Ghaedi, M; Ahmadi, F; Tavakoli, Z; Montazerozohori, M; Khanmohammadi, A; Soylak, M

2008-04-15

In the presented work, 5,5-diphenylimidazolidine-2,4-dione (phenytoin) (DFTD), 5,5-diphenylimidazolidine-2-thione-,4-one (thiophenytoin) (DFID) and 2-(4'-methoxy-benzylidenimine) thiophenole (MBIP) modified activated carbons have been used for the solid phase extraction of copper and lead ions prior to their flame atomic absorption spectrometric determinations. The influences of the various analytical parameters including pH, amounts of reagent, sample volume and eluent type, etc. on the recovery efficiencies of copper and lead ions were investigated. The influences of alkaline, earth alkaline and some transition metals on the adsorption of the analytes were also examined. The detection limits by three sigma for analyte ions were 0.65 and 0.42 microg L(-1) using activated carbon modified with DFID; 0.52 and 0.37 microg L(-1) using activated carbon modified with DFTD and 0.46 and 0.31 microg L(-1) using activated carbon modified with MBIP for Pb(II) and Cu(II), respectively. The procedure was applied to the determination of analytes in natural waters, soil, and blood samples with satisfactory results (recoveries greater than 95%, R.S.D.'s lower than 4%).

Isotope-ratio-monitoring gas chromatography-mass spectrometry: methods for isotopic calibration

NASA Technical Reports Server (NTRS)

Merritt, D. A.; Brand, W. A.; Hayes, J. M.

1994-01-01

In trial analyses of a series of n-alkanes, precise determinations of 13C contents were based on isotopic standards introduced by five different techniques and results were compared. Specifically, organic-compound standards were coinjected with the analytes and carried through chromatography and combustion with them; or CO2 was supplied from a conventional inlet and mixed with the analyte in the ion source, or CO2 was supplied from an auxiliary mixing volume and transmitted to the source without interruption of the analyte stream. Additionally, two techniques were investigated in which the analyte stream was diverted and CO2 standards were placed on a near-zero background. All methods provided accurate results. Where applicable, methods not involving interruption of the analyte stream provided the highest performance (sigma = 0.00006 at.% 13C or 0.06% for 250 pmol C as CO2 reaching the ion source), but great care was required. Techniques involving diversion of the analyte stream were immune to interference from coeluting sample components and still provided high precision (0.0001 < or = sigma < or = 0.0002 at.% or 0.1 < or = sigma < or = 0.2%).

Simultaneous extraction and preconcentration of uranium and thorium in aqueous samples by new modified mesoporous silica prior to inductively coupled plasma optical emission spectrometry determination.

PubMed

Yousefi, Seyed Reza; Ahmadi, Seyed Javad; Shemirani, Farzaneh; Jamali, Mohammad Reza; Salavati-Niasari, Masoud

2009-11-15

A new synthesized modified mesoporous silica (MCM-41) using 5-nitro-2-furaldehyde (fural) was applied as an effective sorbent for the solid phase extraction of uranium(VI) and thorium(IV) ions from aqueous solution for the measurement by inductively coupled plasma optical emission spectrometry (ICP OES). The influences of some analytical parameters on the quantitative recoveries of the analyte ions were investigated in batch method. Under optimal conditions, the analyte ions were sorbed by the sorbent at pH 5.5 and then eluted with 1.0 mL of 1.0 mol L(-1) HNO(3). The preconcentration factor was 100 for a 100mL sample volume. The limits of detection (LOD) obtained for uranium(VI) and thorium(IV) were 0.3 microg L(-1). The maximum sorption capacity of the modified MCM-41 was found to be 47 and 49 mg g(-1) for uranium(VI) and thorium(IV), respectively. The sorbent exhibited good stability, reusability, high adsorption capacity and fast rate of equilibrium for sorption/desorption of uranium and thorium ions. The applicability of the synthesized sorbent was examined using CRM and real water samples.

A study of density effects in plasmas using analytical approximations for the self-consistent potential

NASA Astrophysics Data System (ADS)

Poirier, M.

2015-06-01

Density effects in ionized matter require particular attention since they modify energies, wavefunctions and transition rates with respect to the isolated-ion situation. The approach chosen in this paper is based on the ion-sphere model involving a Thomas-Fermi-like description for free electrons, the bound electrons being described by a full quantum mechanical formalism. This permits to deal with plasmas out of thermal local equilibrium, assuming only a Maxwell distribution for free electrons. For H-like ions, such a theory provides simple and rather accurate analytical approximations for the potential created by free electrons. Emphasis is put on the plasma potential rather than on the electron density, since the energies and wavefunctions depend directly on this potential. Beyond the uniform electron gas model, temperature effects may be analyzed. In the case of H-like ions, this formalism provides analytical perturbative expressions for the energies, wavefunctions and transition rates. Explicit expressions are given in the case of maximum orbital quantum number, and compare satisfactorily with results from a direct integration of the radial Schrödinger equation. Some formulas for lower orbital quantum numbers are also proposed.

Mass Spectrometry Parameters Optimization for the 46 Multiclass Pesticides Determination in Strawberries with Gas Chromatography Ion-Trap Tandem Mass Spectrometry

NASA Astrophysics Data System (ADS)

Fernandes, Virgínia C.; Vera, Jose L.; Domingues, Valentina F.; Silva, Luís M. S.; Mateus, Nuno; Delerue-Matos, Cristina

2012-12-01

Multiclass analysis method was optimized in order to analyze pesticides traces by gas chromatography with ion-trap and tandem mass spectrometry (GC-MS/MS). The influence of some analytical parameters on pesticide signal response was explored. Five ion trap mass spectrometry (IT-MS) operating parameters, including isolation time (IT), excitation voltage (EV), excitation time (ET), maximum excitation energy or " q" value (q), and isolation mass window (IMW) were numerically tested in order to maximize the instrument analytical signal response. For this, multiple linear regression was used in data analysis to evaluate the influence of the five parameters on the analytical response in the ion trap mass spectrometer and to predict its response. The assessment of the five parameters based on the regression equations substantially increased the sensitivity of IT-MS/MS in the MS/MS mode. The results obtained show that for most of the pesticides, these parameters have a strong influence on both signal response and detection limit. Using the optimized method, a multiclass pesticide analysis was performed for 46 pesticides in a strawberry matrix. Levels higher than the limit established for strawberries by the European Union were found in some samples.

Minimizing analyte electrolysis in electrospray ionization mass spectrometry using a redox buffer coated emitter electrode

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peintler-Krivan, Emese; Van Berkel, Gary J; Kertesz, Vilmos

2010-01-01

An emitter electrode with an electroactive poly(pyrrole) (PPy) polymer film coating was constructed for use in electrospray ionization mass spectrometry (ESI-MS). The PPy film acted as a surface-attached redox buffer limiting the interfacial potential of the emitter electrode. While extensive oxidation of selected analytes (reserpine and amodiaquine) was observed in positive ion mode ESI using a bare metal (gold) emitter electrode, the oxidation was suppressed for these same analytes when using the PPy-coated electrode. A semi-quantitative relationship between the rate of oxidation observed and the interfacial potential of the emitter electrode was shown. The redox buffer capacity, and therefore themore » lifetime of the redox buffering effect, correlated with the oxidation potential of the analyte and with the magnitude of the film charge capacity. Online reduction of the PPy polymer layer using negative ion mode ESI between analyte injections was shown to successfully restore the redox buffering capacity of the polymer film to its initial state.« less

Synthesis of nanoscale copper nitride thin film and modification of the surface under high electronic excitation.

PubMed

Ghosh, S; Tripathi, A; Ganesan, V; Avasthi, D K

2008-05-01

Nanoscale (approximately 90 nm) Copper nitride (Cu3N) films are deposited on borosilicate glass and Si substrates by RF sputtering technique in the reactive environment of nitrogen gas. These films are irradiated with 200 MeV Au15+ ions from Pelletron accelerator in order to modify the surface by high electronic energy deposition of heavy ions. Due to irradiation (i) at incident ion fluence of 1 x 10(12) ions/cm2 enhancement of grains, (ii) at 5 x 10912) ions/cm2 mass transport on the films surface, (iii) at 2 x 10(13) ions/cm2 line-like features on Cu3N/glass and nanometallic structures on Cu3N/Si surface are observed. The surface morphology is examined by atomic force microscope (AFM). All results are explained on the basis of a thermal spike model of ion-solid interaction.

Adhesive bonding of ion beam textured metals and fluoropolymers

NASA Technical Reports Server (NTRS)

Mirtich, M. J.; Sovey, J. S.

1978-01-01

An electron bombardment argon ion source was used to ion etch various metals and fluoropolymers. The metal and fluoropolymers were exposed to (0.5 to 1.0) keV Ar ions at ion current densities of (0.2 to 1.5) mA/sq cm for various exposure times. The resulting surface texture is in the form of needles or spires whose vertical dimensions may range from tenths to hundreds of micrometers, depending on the selection of beam energy, ion current density, and etch time. The bonding of textured surfaces is accomplished by ion beam texturing mating pieces of either metals or fluoropolymers and applying a bonding agent which wets in and around the microscopic cone-like structures. After bonding, both tensile and shear strength measurements were made on the samples. Also tested, for comparison's sake, were untextured and chemically etched fluoropolymers. The results of these measurements are presented.

Adhesive bonding of ion beam textured metals and fluoropolymers

NASA Technical Reports Server (NTRS)

Mirtich, M. J.; Sovey, J. S.

1978-01-01

An electron-bombardment argon ion source was used to ion-etch various metals and fluoropolymers. The metal and fluoropolymers were exposed to (0.5 to 1.0)-keV Ar ions at ion current densities of 0.2 to 1.5 mA/sq cm for various exposure times. The resulting surface texture is in the form of needles or spires whose vertical dimensions may range from tenths to hundreds of micrometers, depending on the selection of beam energy, ion current density, and etch time. The bonding of textured surfaces is accomplished by ion-beam texturing mating pieces of either metals or fluoropolymers and applying a bonding agent which wets in and around the microscopic conelike structures. After bonding, both tensile and shear strength measurements were made on the samples. Also tested, for comparison's sake, were untextured and chemically etched fluoropolymers. The results of these measurements are presented in this paper.

Simulation of Galactic Cosmic Rays and Dose-Rate Effects in RITRACKS

NASA Technical Reports Server (NTRS)

Plante, Ianik; Ponomarev, Artem; Slaba, Tony; Blattnig, Steve; Hada, Megumi

2017-01-01

The NASA Space Radiation Laboratory (NSRL) facility has been used successfully for many years to generate ion beams for radiation research experiments by NASA investigators. Recently, modifications were made to the beam lines to allow rapid switching between different types of ions and energies, with the aim to simulate the Galactic Cosmic Rays (GCR) environment. As this will be a focus of space radiation research for upcoming years, the stochastic radiation track structure code RITRACKS (Relativistic Ion Tracks) was modified to simulate beams of various ion types and energies during time intervals specified by the user at the microscopic and nanoscopic scales. For example, particle distributions of a mixed 344.1-MeV protons (18.04 cGy) and 950-MeV/n iron (5.64 cGy) beam behind a 20 g/cm(exp 2) aluminum followed by a 10 g/cm(exp 2) polyethylene shield as calculated by the code GEANT4 were used as an input field in RITRACKS. Similarly, modifications were also made to simulate a realistic radiation environment in a spacecraft exposed to GCR by sampling the ion types and energies from particle spectra pre-calculated by the code HZETRN. The newly implemented features allows RITRACKS to generate time-dependent differential and cumulative 3D dose voxel maps. These new capabilities of RITRACKS will be used to investigate dose-rate effects and synergistic interactions of various types of radiations for many end points at the microscopic and nanoscopic scales such as DNA damage and chromosome aberrations.

The electrocatalytic reduction of nitrate in water on Pd/Sn-modified activated carbon fiber electrode.

PubMed

Wang, Ying; Qu, Jiuhui; Wu, Rongcheng; Lei, Pengju

2006-03-01

The Pd/Sn-modified activated carbon fiber (ACF) electrodes were successfully prepared by the impregnation of Pd2+ and Sn2+ ions onto ACF, and their electrocatalytic reduction capacity for nitrate ions in water was evaluated in a batch experiment. The electrode was characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), X-ray photoelectron spectrum (XPS) and temperature programmed reduction (TPR). The capacity for nitrate reduction depending on Sn content on the electrode and the pH of electrolyte was discussed at length. The results showed that at an applied current density of 1.11 mA cm(-2), nitrate ions in water (solution volume: 400 mL) were reduced from 110 to 3.4 mg L(-1) after 240 min with consecutive change of intermediate nitrite. Ammonium ions and nitrogen were formed as the main final products. The amount of other possible gaseous products (including NO and N2O) was trace. With the increase of Sn content on the Pd/Sn-modified ACF electrode, the activity for nitrate reduction went up to reach a maximum (at Pd/Sn = 4) and then decreased, while the selectivity to N2 was depressed. Higher pH value of electrolyte exhibited more suppression effect on the reduction of nitrite than that of nitrate. However, no significant influence on the final ammonia formation was observed. Additionally, Cu ion in water was found to cover the active sites of the electrode to make the electrode deactivated.

Design and performance of a Near Ultra High Vacuum Helium Ion Microscope

NASA Astrophysics Data System (ADS)

Poelsema, Bene; van Gastel, Raoul; Hlawacek, Gregor; Zandvliet, Harold J. W.

2012-02-01

The advent of He Ion Microscopy (HIM) as a new nanoscopic technique to image materials has enabled a new look at materials that is based on the interaction of swift light ions with matter. Initial HIM instruments have demonstrated high-resolution imaging, combined with great surface sensitivity, the ability to neutralize charge very efficiently, and with enhanced materials contrast when ion induced secondary electrons are used for imaging. To achieve ultimate performance, the chamber vacuum of the existing platform may be improved. For instance, carbon deposits due to beam interaction are readily seen due to the surface sensitivity of the technique. At high current densities the sharply focused beam may very efficiently decompose residual hydrocarbons. Not only can this obscure a clear view of the sample, thereby negating the benefits of the small spot size, it also limits the available acquisition time. This has proven extremely useful for nanopatterning for sensors, and other device fabrication applications at the sub-10nm level. However, it is undesirable when the instrument is used for materials characterization. We will discuss the basic considerations that went into the design of a Near-UHV He Ion Microscope [1]. First applications that the instrument was used for will be highlighted and its impact in surface physics and other research areas that require increased imaging sensitivity will be discussed. [4pt] [1] R.van Gastel et al, Microscopy and Microanalysis 17, 928-929 (2011)

Quantitative SIMS Imaging of Agar-Based Microbial Communities.

PubMed

Dunham, Sage J B; Ellis, Joseph F; Baig, Nameera F; Morales-Soto, Nydia; Cao, Tianyuan; Shrout, Joshua D; Bohn, Paul W; Sweedler, Jonathan V

2018-05-01

After several decades of widespread use for mapping elemental ions and small molecular fragments in surface science, secondary ion mass spectrometry (SIMS) has emerged as a powerful analytical tool for molecular imaging in biology. Biomolecular SIMS imaging has primarily been used as a qualitative technique; although the distribution of a single analyte can be accurately determined, it is difficult to map the absolute quantity of a compound or even to compare the relative abundance of one molecular species to that of another. We describe a method for quantitative SIMS imaging of small molecules in agar-based microbial communities. The microbes are cultivated on a thin film of agar, dried under nitrogen, and imaged directly with SIMS. By use of optical microscopy, we show that the area of the agar is reduced by 26 ± 2% (standard deviation) during dehydration, but the overall biofilm morphology and analyte distribution are largely retained. We detail a quantitative imaging methodology, in which the ion intensity of each analyte is (1) normalized to an external quadratic regression curve, (2) corrected for isomeric interference, and (3) filtered for sample-specific noise and lower and upper limits of quantitation. The end result is a two-dimensional surface density image for each analyte. The sample preparation and quantitation methods are validated by quantitatively imaging four alkyl-quinolone and alkyl-quinoline N-oxide signaling molecules (including Pseudomonas quinolone signal) in Pseudomonas aeruginosa colony biofilms. We show that the relative surface densities of the target biomolecules are substantially different from values inferred through direct intensity comparison and that the developed methodologies can be used to quantitatively compare as many ions as there are available standards.

The effect of pre-evaporation on ion distributions in inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Liu, Shulan; Beauchemin, Diane

2006-02-01

The connecting tube (2 or 5-mm i. d., 11-cm long) between the spray chamber and the torch was heated (to 400 °C) to investigate the effect of pre-evaporation on the distribution of ions in inductively coupled plasma mass spectrometry (ICP-MS). Axial and radial profiles of analyte ions (Al +, V +, Cr +, Ni +, Zn +, Mn +, Zn +, As +, Se +, Mo +, Cd +, Sb +, La +, Pb +) in 1% HNO 3 as well as some polyatomic ions (LaO +, ArO +, ArN +, CO 2+) were simultaneously obtained on a time-of-flight ICP-MS instrument. Upon heating the connecting tube, the optimal axial position of all elements shifted closer to the load coil. Without the heated tube, 3.5 mm was the compromise axial position for multielemental analysis, which was optimal for 6 analytes. With the heated tube, this position became 1.5 mm, which was then optimal for 9 of the 14 analytes. Furthermore, the radial profiles, which were wide with a plateau in their middle without heating, became significantly narrower and Gaussian-like with a heated tube. This narrowing, which was most important for the 5-mm tube, slightly (by a factor of two at the most) yet significantly (at the 95% confidence level) improved the sensitivity of all elements but Mn upon optimisation of the axial position for compromise multi-element analysis. Furthermore, a concurrent decrease in the standard deviation of the blank was significant at the 95% confidence level for 9 of the 14 analytes. For most of the analytes, this translated into a two-fold to up to an order of magnitude improvement in detection limit, which is commensurate with a reduction of noise resulting from the smaller droplets entering the plasma after traversing the pre-evaporation tube.

Scanning ion imaging - a potent tool in SIMS U -Pb zircon geochronology

NASA Astrophysics Data System (ADS)

Whitehouse, M. J.; Fedo, C.; Kusiak, M.; Nemchin, A.

2012-12-01

The application of high spatial resolution (< 15-20 μm lateral) U-Pb data obtained by sec-ondary ion mass spectrometers (SIMS) coupled with textural information from scanning electron microscope (SEM) based cathodoluminescence (CL) and/or back-scattered elec-tron (BSE) characterisation, has revolutionised geochronology over the past 25 years, re-vealing complexities of crustal evolution from zoned zircons. In addition to ge-ochronology, such studies now commonly form the basis of broader investigations using O- and Hf- isotopes and trace elements obtained from the same growth zone as age, circumventing ambiguities commonly present in bulk-rock isotope studies. The choice of analytical beam diameter is often made to maximise the precision of data obtained from a given area of analysis within an identifiable growth zone. In cases where zircons yield poorly constrained internal structures in SEM, high spatial resolution spot analyses may yield uninterpretable and/or meaningless mixed ages by inadvertent sampling across regions with real age differences. Scanning ion imaging (SII) has the potential to generate accurate and precise geochrono-logical data with a spatial resolution down to ca. 2 μm, much higher than that of a normal spot analysis. SII acquisition utilises a rastered primary beam to image an area of the sample with a spatial resolution dependent on the selected primary beam diameter. On the Cameca ims1270/80 instruments, the primary beam scanning is coupled with the dynamic transfer optical system (DTOS) which deflects the secondary ions back on to the ion optical axis of the instrument regardless of where in the raster illuminated area the ions originated. This feature allows retention of a high field magnification (= high transmission) mode and the ability to operate the mass spectrometer at high mass resolution without any compromise in the quality of the peak shape. Secondary ions may be detected either in a sequential (peak hopping) mono-collection mode or simultaneous multicollection mode using low-noise pulse counting electron multipliers. Regardless of the detection mode, data are acquired over sufficient cycles to generate usable counting statistics from selected sub-areas of the image. In two case studies from southern west Greenland and Antarctica, Pb-isotope maps gen-erated using SII reveal considerable complexities of internal structure, age and isotope systematics that were not predictable from CL imaging of the grains (Fig. 1). Fig. 1. Scanning ion images of the 207Pb/206Pb ratio in zircons from (a) W. Greenland and (b) Antarctica (inset shows rastered area of grain corresponding to the image).

Insights into the activation mechanism of calcium ions on the sericite surface: A combined experimental and computational study

NASA Astrophysics Data System (ADS)

Hu, Yuehua; He, Jianyong; Zhang, Chenhu; Zhang, Chenyang; Sun, Wei; Zhao, Dongbo; Chen, Pan; Han, Haisheng; Gao, Zhiyong; Liu, Runqing; Wang, Li

2018-01-01

The adsorption behaviors and the activation mechanism of calcium ions (Ca2+) on sericite surface have been investigated by Zeta potential measurements, Fourier transform infrared spectroscopy (FT-IR), Micro-flotation tests and First principle calculations. Zeta potential tests results show that the sericite surface potential increases due to the adsorption of calcium ions on the surface. Micro-flotation tests demonstrate that sericite recovery remarkably rise by 10% due to the calcium ions activation on sericite surface. However, the characteristic adsorption bands of calcium oleate do not appear in the FT-IR spectrum, suggesting that oleate ions just physically adsorb on the sericite surface. The first principle calculations based on the density functional theory (DFT) further reveals the microscopic adsorption mechanism of calcium ions on the sericite surface before and after hydration.

SPM observation of slow highly charged ion induced nanodots on highly orientated pyrolytic graphite

NASA Astrophysics Data System (ADS)

Mitsuda, Y.; Nakamura, B. E. O'Rourke1 N.; Kanai, Y.; Ohtani, S.; Yamazaki, Y.

2007-03-01

We have observed nanodots on a highly orientated pyrolytic graphite (HOPG) surface produced by highly charged ion impacts using a scanning tunneling microscope. Previous measurements have con.rmed the dominant role of the potential energy or the incident ion charge state on the size and height of the observed nanodots. The present results extend these previous measurements to much lower kinetic energy. It appears that there is no observable influence on the lateral size of the nanodots due to the incident ion kinetic energy down to approximately 200 eV. In contrast some slight reduction in the nanodot height was observed as the kinetic energy was reduced.

Use of high-resolution mass spectrometry to investigate a metabolite interference during liquid chromatography/tandem mass spectrometric quantification of a small molecule in toxicokinetic study samples.

PubMed

Furlong, Michael; Bessire, Andrew; Song, Wei; Huntington, Christopher; Groeber, Elizabeth

2010-07-15

During routine liquid chromatography/tandem mass spectrometric (LC/MS/MS) bioanalysis of a small molecule analyte in rat serum samples from a toxicokinetic study, an unexpected interfering peak was observed in the extracted ion chromatogram of the internal standard. No interfering peaks were observed in the extracted ion chromatogram of the analyte. The dose-dependent peak area response and peak area response versus time profiles of the interfering peak suggested that it might have been related to a metabolite of the dosed compound. Further investigation using high-resolution mass spectrometry led to unequivocal identification of the interfering peak as an N-desmethyl metabolite of the parent analyte. High-resolution mass spectrometry (HRMS) was also used to demonstrate that the interfering response of the metabolite in the multiple reaction monitoring (MRM) channel of the internal standard was due to an isobaric relationship between the (13)C-isotope of the metabolite and the internal standard (i.e., common precursor ion mass), coupled with a metabolite product ion with identical mass to the product ion used in the MRM transition of the internal standard. These results emphasize (1) the need to carefully evaluate internal standard candidates with regard to potential interferences from metabolites during LC/MS/MS method development, validation and bioanalysis of small molecule analytes in biological matrices; (2) the value of HRMS as a tool to investigate unexpected interferences encountered during LC/MS/MS analysis of small molecules in biological matrices; and (3) the potential for interference regardless of choice of IS and therefore the importance of conducting assay robustness on incurred in vitro or in vivo study samples. Copyright 2010 John Wiley & Sons, Ltd.

Impact desolvation of electrosprayed microdroplets--a new ionization method for mass spectrometry of large biomolecules.

PubMed

Aksyonov, S A; Williams, P

2001-01-01

Impact desolvation of electrosprayed microdroplets (IDEM) is a new method for producing gas-phase ions of large biomolecules. Analytes are dissolved in an electrolyte solution which is electrosprayed in vacuum, producing highly charged micron and sub-micron sized droplets (microdroplets). These microdroplets are accelerated through potential differences approximately 5 - 10 kV to velocities of several km/s and allowed to impact a target surface. The energetic impacts vaporize the droplets and release desolvated gas-phase ions of the analyte molecules. Oligonucleotides (2- to 12-mer) and peptides (bradykinin, neurotensin) yield singly and doubly charged molecular ions with no detectable fragmentation. Because the extent of multiple charging is significantly less than in atmospheric pressure electrospray ionization, and the method produces ions largely free of adducts from solutions of high ionic strength, IDEM has some promise as a method for coupling to liquid chromatographic techniques and for mixture analysis. Ions are produced in vacuum at a flat equipotential surface, potentially allowing efficient ion extraction. Copyright 2001 John Wiley & Sons, Ltd.

Collision-Induced Dissociation Study of the Adduct Ions Produced in NO3−-Free Area of Atmospheric Pressure Negative Corona Discharges under Ambient Air Conditions

PubMed Central

Sekimoto, Kanako; Matsuda, Natsuki; Takayama, Mitsuo

2013-01-01

Collision-induced dissociation (CID) experiments of adducts [M+R]− with negative atmospheric ions R− (O2−, HCO3− and COO−(COOH)) produced in NO3−-free discharge area in atmospheric pressure corona discharge ionization (APCDI) method were performed using aliphatic and aromatic compounds M. The [M+R]− adducts for individual R− fragmented to form deprotonated analytes [M−H]− as well as the specific product ions which also occurred in the CID of [M−H]−, independent of analytes with several different functional groups. The results obtained suggested that the specific product ions formed in the CID of [M+R]−, as well as CID of [M−H]−, are generated due to further fragmentation of the product ions [M−H]−. It was concluded, therefore, that CID of [M+R]− formed in NO3−-free discharge area can indirectly lead to the formation of the product ions originating from [M−H]−. PMID:24860710

Matrix-enhanced secondary ion mass spectrometry: The Alchemist's solution?

NASA Astrophysics Data System (ADS)

Delcorte, Arnaud

2006-07-01

Because of the requirements of large molecule characterization and high-lateral resolution SIMS imaging, the possibility of improving molecular ion yields by the use of specific sample preparation procedures has recently generated a renewed interest in the static SIMS community. In comparison with polyatomic projectiles, however, signal enhancement by a matrix might appear to some as the alchemist's versus the scientist's solution to the current problems of organic SIMS. In this contribution, I would like to discuss critically the pros and cons of matrix-enhanced SIMS procedures, in the new framework that includes polyatomic ion bombardment. This discussion is based on a short review of the experimental and theoretical developments achieved in the last decade with respect to the three following approaches: (i) blending the analyte with a low-molecular weight organic matrix (MALDI-type preparation procedure); (ii) mixing alkali/noble metal salts with the analyte; (iii) evaporating a noble metal layer on the analyte sample surface (organic molecules, polymers).

Sample displacement chromatography as a method for purification of proteins and peptides from complex mixtures

PubMed Central

Gajdosik, Martina Srajer; Clifton, James; Josic, Djuro

2012-01-01

Sample displacement chromatography (SDC) in reversed-phase and ion-exchange modes was introduced approximately twenty years ago. This method takes advantage of relative binding affinities of components in a sample mixture. During loading, there is a competition among different sample components for the sorption on the surface of the stationary phase. SDC was first used for the preparative purification of proteins. Later, it was demonstrated that this kind of chromatography can also be performed in ion-exchange, affinity and hydrophobic-interaction mode. It has also been shown that SDC can be performed on monoliths and membrane-based supports in both analytical and preparative scale. Recently, SDC in ion-exchange and hydrophobic interaction mode was also employed successfully for the removal of trace proteins from monoclonal antibody preparations and for the enrichment of low abundance proteins from human plasma. In this review, the principals of SDC are introduced, and the potential for separation of proteins and peptides in micro-analytical, analytical and preparative scale is discussed. PMID:22520159

Self-organized fluorescent nanosensors for ratiometric Pb2+ detection.

PubMed

Arduini, Maria; Mancin, Fabrizio; Tecilla, Paolo; Tonellato, Umberto

2007-07-31

Silica nanoparticles (60 nm diameter) doped with fluorescent dyes and functionalized on the surface with thiol groups have been proved to be efficient fluorescent chemosensors for Pb2+ ions. The particles can detect a 1 microM metal ion concentration with a good selectivity, suffering only interference from Cu2+ ions. Analyte binding sites are provided by the simple grafting of the thiol groups on the nanoparticles. Once bound to the particles surface, the Pb2+ ions quench the emission of the reporting dyes embedded. Sensor performances can be improved by taking advantage of the ease of production of multishell silica particles. On one hand, signaling units can be concentrated in the external shells, allowing a closer interaction with the surface-bound analyte. On the other, a second dye can be buried in the particle core, far enough from the surface to be unaffected by the Pb2+ ions, thus producing a reference signal. In this way, a ratiometric system is easily prepared by simple self-organization of the particle components.

Preparation, characterization and antibacterial properties against E. coli K88 of chitosan nanoparticle loaded copper ions

NASA Astrophysics Data System (ADS)

Du, Wen-Li; Xu, Ying-Lei; Xu, Zi-Rong; Fan, Cheng-Li

2008-02-01

The present study was conducted to prepare and characterize chitosan nanoparticle loaded copper ions, and evaluate their antibacterial activity. Chitosan nanoparticles were prepared based on ionotropic gelation, and then the copper ions were loaded. The particle size, zeta potential and morphology were determined. Antibacterial activity was evaluated against E. coli K88 by determination of the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) in vitro. Results showed that the antibacterial activity was significantly enhanced by the loading of copper ions compared to those of chitosan nanoparticles and copper ions. The MIC and MBC of chitosan nanoparticle loaded copper ions were 21 times and 42 times lower than those of copper ions, respectively. To confirm the antibacterial mechanism, morphological changes of E. coli K88 treated by chitosan nanoparticle loaded copper ions were dynamically observed with an atomic force microscope (AFM). It was found that chitosan nanoparticle loaded copper ions killed E. coli K88 through damage to the cell membrane.

Electrostatic Propulsion Beam Divergence Effects on Spacecraft Surfaces. Volume 2, Addendum 1: Ion Time-of-flight Determinations of Doubly to Singly Ionized Mercury Ion Ratios from a Mercury Electron Bombardment Discharge

NASA Technical Reports Server (NTRS)

Sellen, J. M., Jr.; Kemp, R. F.; Hall, D. F.

1973-01-01

The analysis of ion exhaust beam current flow for multiply charged ion species and the application to propellant utilization for the thruster are discussed. The ion engine in use in the experiments is a twenty centimeter diameter electromagnet electron bombardment engine. The experimental technique to determine the multiply charged ion abundance ratios using ion time of flight is described. An analytical treatment of the discharge action in producing various ion species has been carried out.

Analytical probabilistic modeling of RBE-weighted dose for ion therapy.

PubMed

Wieser, H P; Hennig, P; Wahl, N; Bangert, M

2017-11-10

Particle therapy is especially prone to uncertainties. This issue is usually addressed with uncertainty quantification and minimization techniques based on scenario sampling. For proton therapy, however, it was recently shown that it is also possible to use closed-form computations based on analytical probabilistic modeling (APM) for this purpose. APM yields unique features compared to sampling-based approaches, motivating further research in this context. This paper demonstrates the application of APM for intensity-modulated carbon ion therapy to quantify the influence of setup and range uncertainties on the RBE-weighted dose. In particular, we derive analytical forms for the nonlinear computations of the expectation value and variance of the RBE-weighted dose by propagating linearly correlated Gaussian input uncertainties through a pencil beam dose calculation algorithm. Both exact and approximation formulas are presented for the expectation value and variance of the RBE-weighted dose and are subsequently studied in-depth for a one-dimensional carbon ion spread-out Bragg peak. With V and B being the number of voxels and pencil beams, respectively, the proposed approximations induce only a marginal loss of accuracy while lowering the computational complexity from order [Formula: see text] to [Formula: see text] for the expectation value and from [Formula: see text] to [Formula: see text] for the variance of the RBE-weighted dose. Moreover, we evaluated the approximated calculation of the expectation value and standard deviation of the RBE-weighted dose in combination with a probabilistic effect-based optimization on three patient cases considering carbon ions as radiation modality against sampled references. The resulting global γ-pass rates (2 mm,2%) are [Formula: see text]99.15% for the expectation value and [Formula: see text]94.95% for the standard deviation of the RBE-weighted dose, respectively. We applied the derived analytical model to carbon ion treatment planning, although the concept is in general applicable to other ion species considering a variable RBE.

Analytical probabilistic modeling of RBE-weighted dose for ion therapy

NASA Astrophysics Data System (ADS)

Wieser, H. P.; Hennig, P.; Wahl, N.; Bangert, M.

2017-12-01

Particle therapy is especially prone to uncertainties. This issue is usually addressed with uncertainty quantification and minimization techniques based on scenario sampling. For proton therapy, however, it was recently shown that it is also possible to use closed-form computations based on analytical probabilistic modeling (APM) for this purpose. APM yields unique features compared to sampling-based approaches, motivating further research in this context. This paper demonstrates the application of APM for intensity-modulated carbon ion therapy to quantify the influence of setup and range uncertainties on the RBE-weighted dose. In particular, we derive analytical forms for the nonlinear computations of the expectation value and variance of the RBE-weighted dose by propagating linearly correlated Gaussian input uncertainties through a pencil beam dose calculation algorithm. Both exact and approximation formulas are presented for the expectation value and variance of the RBE-weighted dose and are subsequently studied in-depth for a one-dimensional carbon ion spread-out Bragg peak. With V and B being the number of voxels and pencil beams, respectively, the proposed approximations induce only a marginal loss of accuracy while lowering the computational complexity from order O(V × B^2) to O(V × B) for the expectation value and from O(V × B^4) to O(V × B^2) for the variance of the RBE-weighted dose. Moreover, we evaluated the approximated calculation of the expectation value and standard deviation of the RBE-weighted dose in combination with a probabilistic effect-based optimization on three patient cases considering carbon ions as radiation modality against sampled references. The resulting global γ-pass rates (2 mm,2%) are > 99.15% for the expectation value and > 94.95% for the standard deviation of the RBE-weighted dose, respectively. We applied the derived analytical model to carbon ion treatment planning, although the concept is in general applicable to other ion species considering a variable RBE.

Experimental and analytical evaluation of ion thruster/spacecraft interactions

NASA Technical Reports Server (NTRS)

Carruth, M. R., Jr. (Editor)

1981-01-01

Studies were conducted to both identify the environment produced by ion thrusters and to assess the interaction of this environment on a typical spacecraft and typical science instruments. Spacecraft charging and the charge exchange that accompanies it is discussed in detail. Electromagnetic interference was characterized for ion engines. The electromagnetic compatibility of ion thrusters with spacecraft instruments was determined. The effects of ion thruster plumes on spacecraft were studied with particular emphasis on external surface currents.

Graphene Nanoribbons Fabricated by Helium Ion microscope

NASA Astrophysics Data System (ADS)

Pickard, D.; Oezyilmaz, B.; Thong, J.; Loh, K. P.; Viswanathan, V.; Zhongkai, A.; Mathew, S.; Kundu, T.; Park, C.; Yi, Z.; Xu, X.; Zhang, K.; Tat, T. C.; Wang, H.; Venkatesan, T.; Botton, G.; Couillard, M.

2010-03-01

Graphene, a monolayer graphitic lattice of carbon atoms has tremendous promise for a variety of applications on account of the zero mass of electrons, high mobility and the sensitivity of transport to perturbations at the interface. Patterning graphene is an obvious challenge and mesoscopic devices based on graphene require high spatial resolution patterning that will induce as little damage as possible. We use a helium ion microscope with its 0.4nm spot size beam to directly write patterns on free standing graphene films. TEM images of the patterns reveal holes as small as 4 nm and ribbons with line widths as narrow as 3 nm. The images show recovery of the graphene lattice at a distance of about a nm from the patterned edge. The linewidths of the ribbon can be varied considerably in a controllable fashion over ribbon lengths of the order of microns. . .

In vitro assessments on bacterial adhesion and corrosion performance of TiN coating on Ti6Al4V titanium alloy synthesized by multi-arc ion plating

NASA Astrophysics Data System (ADS)

Lin, Naiming; Huang, Xiaobo; Zhang, Xiangyu; Fan, Ailan; Qin, Lin; Tang, Bin

2012-07-01

TiN coating was synthesized on Ti6Al4V titanium alloy surface by multi-arc ion plating (MIP) technique. Surface morphology, cross sectional microstructure, elemental distributions and phase compositions of the obtained coating were analyzed by means of scanning electron microscope (SEM), optical microscope (OM), glow discharge optical emission spectroscope (GDOES) and X-ray diffraction (XRD). Bacterial adhesion and corrosion performance of Ti6Al4V and the TiN coating were assessed via in vitro bacterial adhesion tests and corrosion experiments, respectively. The results indicated that continuous and compact coating which was built up by pure TiN with a typical columnar crystal structure has reached a thickness of 1.5 μm. This TiN coating could significantly reduce the bacterial adhesion and enhance the corrosion resistance of Ti6Al4V substrate.

Field populations of native Indian honey bees from pesticide intensive agricultural landscape show signs of impaired olfaction

NASA Astrophysics Data System (ADS)

Chakrabarti, Priyadarshini; Rana, Santanu; Bandopadhyay, Sreejata; Naik, Dattatraya G.; Sarkar, Sagartirtha; Basu, Parthiba

2015-07-01

Little information is available regarding the adverse effects of pesticides on natural honey bee populations. This study highlights the detrimental effects of pesticides on honey bee olfaction through behavioural studies, scanning electron microscopic imaging of antennal sensillae and confocal microscopic studies of honey bee brains for calcium ions on Apis cerana, a native Indian honey bee species. There was a significant decrease in proboscis extension response and biologically active free calcium ions and adverse changes in antennal sensillae in pesticide exposed field honey bee populations compared to morphometrically similar honey bees sampled from low/no pesticide sites. Controlled laboratory experiments corroborated these findings. This study reports for the first time the changes in antennal sensillae, expression of Calpain 1(an important calcium binding protein) and resting state free calcium in brains of honey bees exposed to pesticide stress.

Field populations of native Indian honey bees from pesticide intensive agricultural landscape show signs of impaired olfaction

PubMed Central

Chakrabarti, Priyadarshini; Rana, Santanu; Bandopadhyay, Sreejata; Naik, Dattatraya G.; Sarkar, Sagartirtha; Basu, Parthiba

2015-01-01

Little information is available regarding the adverse effects of pesticides on natural honey bee populations. This study highlights the detrimental effects of pesticides on honey bee olfaction through behavioural studies, scanning electron microscopic imaging of antennal sensillae and confocal microscopic studies of honey bee brains for calcium ions on Apis cerana, a native Indian honey bee species. There was a significant decrease in proboscis extension response and biologically active free calcium ions and adverse changes in antennal sensillae in pesticide exposed field honey bee populations compared to morphometrically similar honey bees sampled from low/no pesticide sites. Controlled laboratory experiments corroborated these findings. This study reports for the first time the changes in antennal sensillae, expression of Calpain 1(an important calcium binding protein) and resting state free calcium in brains of honey bees exposed to pesticide stress. PMID:26212690

Method of making an ion beam sputter-etched ventricular catheter for hydrocephalus shunt

NASA Technical Reports Server (NTRS)

Banks, B. A. (Inventor)

1984-01-01

The centricular catheter comprises a multiplicity of inlet microtubules. Each microtubule has both a large opening at its inlet end and a multiplicity of microscopic openings along its lateral surfaces. The microtubules are perforated by an ion beam sputter etch technique. The holes are etched in each microtubule by directing an ion beam through an electro formed mesh mask producing perforations having diameters ranging from about 14 microns to about 150 microns. This structure assures a reliable means for shunting cerebrospinal fluid from the cerebral ventricles to selected areas of the body.

Ion beams in radiotherapy - from tracks to treatment planning

NASA Astrophysics Data System (ADS)

Krämer, M.; Scifoni, E.; Wälzlein, C.; Durante, M.

2012-07-01

Several dozen clinical sites around the world apply beams of fast light ions for radiotherapeutical purposes. Thus there is a vested interest in the various physical and radiobiological processes governing the interaction of ion beams with matter, specifically living systems. We discuss the various modelling steps which lead from basic interactions to the application in actual patient treatment planning. The nano- and microscopic scale is covered by sample calculations with our TRAX code. On the macroscopic scale we feature the TRiP98 treatment planning system, which was clinically used in GSI's radiotherapy pilot project.

Influence of ligand chemistry on silver nanoparticles for colorimetric detection of Cr3+ and Hg2+ ions

NASA Astrophysics Data System (ADS)

Kailasa, Suresh Kumar; Chandel, Madhurya; Mehta, Vaibhavkumar N.; Park, Tae Jung

2018-04-01

In this work, we describe the role of ligand chemistry on the surfaces of silver nanoparticles (Ag NPs) for tuning their analytical applications. The citrate and melamine (MA) molecules were used as ligands for the surface modification of Ag NPs. The addition of Cr3+ ion in citrate-Ag NPs (Cit-Ag NPs) and of Hg2+ ion in melamine-Ag NPs (MA-Ag NPs) cause Ag NPs aggregation, and are accompanied by a color change and a red-shift. The resulting distinctly visual readouts are favorable for colorimetric detection of Cr3+ and Hg2+ ions. Under optimal conditions, the linear ranges are observed in the concentration ranges of 1.0-50.0 and of 10.0-100.0 μM, and with detection limit of 0.52 and 1.80 μM for Cr3+ and Hg2+ ions. The simultaneous detection of Cr3+ and Hg2+ ion is driven by the changing the ligand chemistry on the surfaces of Ag NPs that allows to tune their specific interactions with target analytes. Finally, the functionalized Ag NPs were successfully applied to detect Cr3+ and Hg2+ ions in water samples with satisfactory recoveries.

Tunable Ionization Modes of a Flowing Atmospheric-Pressure Afterglow (FAPA) Ambient Ionization Source.

PubMed

Badal, Sunil P; Michalak, Shawn D; Chan, George C-Y; You, Yi; Shelley, Jacob T

2016-04-05

Plasma-based ambient desorption/ionization sources are versatile in that they enable direct ionization of gaseous samples as well as desorption/ionization of analytes from liquid and solid samples. However, ionization matrix effects, caused by competitive ionization processes, can worsen sensitivity or even inhibit detection all together. The present study is focused on expanding the analytical capabilities of the flowing atmospheric-pressure afterglow (FAPA) source by exploring additional types of ionization chemistry. Specifically, it was found that the abundance and type of reagent ions produced by the FAPA source and, thus, the corresponding ionization pathways of analytes, can be altered by changing the source working conditions. High abundance of proton-transfer reagent ions was observed with relatively high gas flow rates and low discharge currents. Conversely, charge-transfer reagent species were most abundant at low gas flows and high discharge currents. A rather nonpolar model analyte, biphenyl, was found to significantly change ionization pathway based on source operating parameters. Different analyte ions (e.g., MH(+) via proton-transfer and M(+.) via charge-transfer) were formed under unique operating parameters demonstrating two different operating regimes. These tunable ionization modes of the FAPA were used to enable or enhance detection of analytes which traditionally exhibit low-sensitivity in plasma-based ADI-MS analyses. In one example, 2,2'-dichloroquaterphenyl was detected under charge-transfer FAPA conditions, which were difficult or impossible to detect with proton-transfer FAPA or direct analysis in real-time (DART). Overall, this unique mode of operation increases the number and range of detectable analytes and has the potential to lessen ionization matrix effects in ADI-MS analyses.

Fast 2D fluid-analytical simulation of ion energy distributions and electromagnetic effects in multi-frequency capacitive discharges

NASA Astrophysics Data System (ADS)

Kawamura, E.; Lieberman, M. A.; Graves, D. B.

2014-12-01

A fast 2D axisymmetric fluid-analytical plasma reactor model using the finite elements simulation tool COMSOL is interfaced with a 1D particle-in-cell (PIC) code to study ion energy distributions (IEDs) in multi-frequency capacitive argon discharges. A bulk fluid plasma model, which solves the time-dependent plasma fluid equations for the ion continuity and electron energy balance, is coupled with an analytical sheath model, which solves for the sheath parameters. The time-independent Helmholtz equation is used to solve for the fields and a gas flow model solves for the steady-state pressure, temperature and velocity of the neutrals. The results of the fluid-analytical model are used as inputs to a PIC simulation of the sheath region of the discharge to obtain the IEDs at the target electrode. Each 2D fluid-analytical-PIC simulation on a moderate 2.2 GHz CPU workstation with 8 GB of memory took about 15-20 min. The multi-frequency 2D fluid-analytical model was compared to 1D PIC simulations of a symmetric parallel-plate discharge, showing good agreement. We also conducted fluid-analytical simulations of a multi-frequency argon capacitively coupled plasma (CCP) with a typical asymmetric reactor geometry at 2/60/162 MHz. The low frequency 2 MHz power controlled the sheath width and sheath voltage while the high frequencies controlled the plasma production. A standing wave was observable at the highest frequency of 162 MHz. We noticed that adding 2 MHz power to a 60 MHz discharge or 162 MHz to a dual frequency 2 MHz/60 MHz discharge can enhance the plasma uniformity. We found that multiple frequencies were not only useful for controlling IEDs but also plasma uniformity in CCP reactors.

Ion Mobility Derived Collision Cross Sections to Support Metabolomics Applications

PubMed Central

2015-01-01

Metabolomics is a rapidly evolving analytical approach in life and health sciences. The structural elucidation of the metabolites of interest remains a major analytical challenge in the metabolomics workflow. Here, we investigate the use of ion mobility as a tool to aid metabolite identification. Ion mobility allows for the measurement of the rotationally averaged collision cross-section (CCS), which gives information about the ionic shape of a molecule in the gas phase. We measured the CCSs of 125 common metabolites using traveling-wave ion mobility-mass spectrometry (TW-IM-MS). CCS measurements were highly reproducible on instruments located in three independent laboratories (RSD < 5% for 99%). We also determined the reproducibility of CCS measurements in various biological matrixes including urine, plasma, platelets, and red blood cells using ultra performance liquid chromatography (UPLC) coupled with TW-IM-MS. The mean RSD was < 2% for 97% of the CCS values, compared to 80% of retention times. Finally, as proof of concept, we used UPLC–TW-IM-MS to compare the cellular metabolome of epithelial and mesenchymal cells, an in vitro model used to study cancer development. Experimentally determined and computationally derived CCS values were used as orthogonal analytical parameters in combination with retention time and accurate mass information to confirm the identity of key metabolites potentially involved in cancer. Thus, our results indicate that adding CCS data to searchable databases and to routine metabolomics workflows will increase the identification confidence compared to traditional analytical approaches. PMID:24640936

Four-probe measurements with a three-probe scanning tunneling microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Salomons, Mark; Martins, Bruno V. C.; Zikovsky, Janik

2014-04-15

We present an ultrahigh vacuum (UHV) three-probe scanning tunneling microscope in which each probe is capable of atomic resolution. A UHV JEOL scanning electron microscope aids in the placement of the probes on the sample. The machine also has a field ion microscope to clean, atomically image, and shape the probe tips. The machine uses bare conductive samples and tips with a homebuilt set of pliers for heating and loading. Automated feedback controlled tip-surface contacts allow for electrical stability and reproducibility while also greatly reducing tip and surface damage due to contact formation. The ability to register inter-tip position bymore » imaging of a single surface feature by multiple tips is demonstrated. Four-probe material characterization is achieved by deploying two tips as fixed current probes and the third tip as a movable voltage probe.« less

Brightness measurement of an electron impact gas ion source for proton beam writing applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, N.; Santhana Raman, P.; Department of Electrical and Computer Engineering, National University of Singapore, Singapore 117583

We are developing a high brightness nano-aperture electron impact gas ion source, which can create ion beams from a miniature ionization chamber with relatively small virtual source sizes, typically around 100 nm. A prototype source of this kind was designed and successively micro-fabricated using integrated circuit technology. Experiments to measure source brightness were performed inside a field emission scanning electron microscope. The total output current was measured to be between 200 and 300 pA. The highest estimated reduced brightness was found to be comparable to the injecting focused electron beam reduced brightness. This translates into an ion reduced brightness thatmore » is significantly better than that of conventional radio frequency ion sources, currently used in single-ended MeV accelerators.« less

Brightness measurement of an electron impact gas ion source for proton beam writing applications.

PubMed

Liu, N; Xu, X; Pang, R; Raman, P Santhana; Khursheed, A; van Kan, J A

2016-02-01

We are developing a high brightness nano-aperture electron impact gas ion source, which can create ion beams from a miniature ionization chamber with relatively small virtual source sizes, typically around 100 nm. A prototype source of this kind was designed and successively micro-fabricated using integrated circuit technology. Experiments to measure source brightness were performed inside a field emission scanning electron microscope. The total output current was measured to be between 200 and 300 pA. The highest estimated reduced brightness was found to be comparable to the injecting focused electron beam reduced brightness. This translates into an ion reduced brightness that is significantly better than that of conventional radio frequency ion sources, currently used in single-ended MeV accelerators.

Analysis with electron microscope of multielement samples using pure element standards

DOEpatents

King, Wayne E.

1987-01-01

A method and modified analytical electron microscope for determining the concentration of elements in a multielement sample by exposing samples with differing thicknesses for each element to a beam of electrons, simultaneously measuring the electron dosage and x-ray intensities for each sample of element to determine a "K.sub.AB " value to be used in the equation ##EQU1## where I is intensity and C is concentration for elements A and B, and exposing the multielement sample to determine the concentrations of the elements in the sample.

Formation of Pyrylium from Aromatic Systems with a Helium:Oxygen Flowing Atmospheric Pressure Afterglow (FAPA) Plasma Source

NASA Astrophysics Data System (ADS)

Badal, Sunil P.; Ratcliff, Tyree D.; You, Yi; Breneman, Curt M.; Shelley, Jacob T.

2017-06-01

The effects of oxygen addition on a helium-based flowing atmospheric pressure afterglow (FAPA) ionization source are explored. Small amounts of oxygen doped into the helium discharge gas resulted in an increase in abundance of protonated water clusters by at least three times. A corresponding increase in protonated analyte signal was also observed for small polar analytes, such as methanol and acetone. Meanwhile, most other reagent ions (e.g., O2 +·, NO+, etc.) significantly decrease in abundance with even 0.1% v/v oxygen in the discharge gas. Interestingly, when analytes that contained aromatic constituents were subjected to a He:O2-FAPA, a unique (M + 3)+ ion resulted, while molecular or protonated molecular ions were rarely detected. Exact-mass measurements revealed that these (M + 3)+ ions correspond to (M - CH + O)+, with the most likely structure being pyrylium. Presence of pyrylium-based ions was further confirmed by tandem mass spectrometry of the (M + 3)+ ion compared with that of a commercially available salt. Lastly, rapid and efficient production of pyrylium in the gas phase was used to convert benzene into pyridine. Though this pyrylium-formation reaction has not been shown before, the reaction is rapid and efficient. Potential reactant species, which could lead to pyrylium formation, were determined from reagent-ion mass spectra. Thermodynamic evaluation of reaction pathways was aided by calculation of the formation enthalpy for pyrylium, which was found to be 689.8 kJ/mol. Based on these results, we propose that this reaction is initiated by ionized ozone (O3 +·), proceeds similarly to ozonolysis, and results in the neutral loss of the stable CHO2 · radical. [Figure not available: see fulltext.

Formation of Pyrylium from Aromatic Systems with a Helium:Oxygen Flowing Atmospheric Pressure Afterglow (FAPA) Plasma Source.

PubMed

Badal, Sunil P; Ratcliff, Tyree D; You, Yi; Breneman, Curt M; Shelley, Jacob T

2017-06-01

The effects of oxygen addition on a helium-based flowing atmospheric pressure afterglow (FAPA) ionization source are explored. Small amounts of oxygen doped into the helium discharge gas resulted in an increase in abundance of protonated water clusters by at least three times. A corresponding increase in protonated analyte signal was also observed for small polar analytes, such as methanol and acetone. Meanwhile, most other reagent ions (e.g., O 2 +· , NO + , etc.) significantly decrease in abundance with even 0.1% v/v oxygen in the discharge gas. Interestingly, when analytes that contained aromatic constituents were subjected to a He:O 2 -FAPA, a unique (M + 3) + ion resulted, while molecular or protonated molecular ions were rarely detected. Exact-mass measurements revealed that these (M + 3) + ions correspond to (M - CH + O) + , with the most likely structure being pyrylium. Presence of pyrylium-based ions was further confirmed by tandem mass spectrometry of the (M + 3) + ion compared with that of a commercially available salt. Lastly, rapid and efficient production of pyrylium in the gas phase was used to convert benzene into pyridine. Though this pyrylium-formation reaction has not been shown before, the reaction is rapid and efficient. Potential reactant species, which could lead to pyrylium formation, were determined from reagent-ion mass spectra. Thermodynamic evaluation of reaction pathways was aided by calculation of the formation enthalpy for pyrylium, which was found to be 689.8 kJ/mol. Based on these results, we propose that this reaction is initiated by ionized ozone (O 3 +· ), proceeds similarly to ozonolysis, and results in the neutral loss of the stable CHO 2 · radical. Graphical Abstract ᅟ.

Development of a selective and sensitive flotation method for determination of trace amounts of cobalt, nickel, copper and iron in environmental samples.

PubMed

Karimi, H; Ghaedi, M; Shokrollahi, A; Rajabi, H R; Soylak, M; Karami, B

2008-02-28

A simple, selective and rapid flotation method for the separation-preconcentration of trace amounts of cobalt, nickel, iron and copper ions using phenyl 2-pyridyl ketone oxime (PPKO) has been developed prior to their flame atomic absorption spectrometric determinations. The influence of pH, amount of PPKO as collector, type and amount of eluting agent, type and amount of surfactant as floating agent and ionic strength was evaluated on the recoveries of analytes. The influences of the concomitant ions on the recoveries of the analyte ions were also examined. The enrichment factor was 93. The detection limits based on 3 sigma for Cu, Ni, Co and Fe were 0.7, 0.7, 0.8, and 0.7 ng mL(-1), respectively. The method has been successfully applied for determination of trace amounts of ions in various real samples.

A Robust Analytical Approach for the Identification of Specific Protein Carbonylation Sites: Metal-Catalyzed Oxidations of Human Serum Albumin

PubMed Central

Ugur, Zafer; Gronert, Scott

2017-01-01

The formation of protein carbonyls in the metal-catalyzed oxidation of human serum albumin (HSA) is characterized using a new analytical approach that involves tagging the modification site with multiple hydrazide reagents. Protein carbonyl formation at lysine and arginine residues was catalyzed with copper and iron ions, and the resulting oxidation patterns in HSA are contrasted. A total of 18 modification sites were identified with iron ion catalysis and 14 with copper ion catalysis. However, with the more stringent requirement of identification with at least two tagging reagents, the number of validated modification sites drops to 10 for iron and 9 for copper. Of the 14 total validated sites, there were only five in common for the two metal ions. The results illustrate the value of using multiple tagging agents and highlight the selective and specific nature of metal-catalyzed protein oxidations. PMID:28303033

Interpretation of plasma impurity deposition probes. Analytic approximation

NASA Astrophysics Data System (ADS)

Stangeby, P. C.

1987-10-01

Insertion of a probe into the plasma induces a high speed flow of the hydrogenic plasma to the probe which, by friction, accelerates the impurity ions to velocities approaching the hydrogenic ion acoustic speed, i.e., higher than the impurity ion thermal speed. A simple analytic theory based on this effect provides a relation between impurity fluxes to the probe Γimp and the undisturbed impurity ion density nimp, with the hydrogenic temperature and density as input parameters. Probe size also influences the collection process and large probes are found to attract a higher flux density than small probes in the same plasma. The quantity actually measured, cimp, the impurity atom surface density (m-2) net-deposited on the probe, is related to Γimp and thus to nimp by taking into account the partial removal of deposited material caused by sputtering and the redeposition process.

Differentiation of regioisomeric aromatic ketocarboxylic acids by atmospheric pressure chemical ionization CAD tandem mass spectrometry in a linear quadrupole ion trap mass spectrometer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Amundson, Lucas M.; Owen, Ben C.; Gallardo, Vanessa A.

2011-01-01

Positive-mode atmospheric pressure chemical ionization tandem mass spectrometry (APCI-MS n ) was tested for the differentiation of regioisomeric aromatic ketocarboxylic acids. Each analyte forms exclusively an abundant protonated molecule upon ionization via positive-mode APCI in a commercial linear quadrupole ion trap (LQIT) mass spectrometer. Energy-resolved collision-activated dissociation (CAD) experiments carried out on the protonated analytes revealed fragmentation patterns that varied based on the location of the functional groups. Unambiguous differentiation between the regioisomers was achieved in each case by observing different fragmentation patterns, different relative abundances of ion-molecule reaction products, or different relative abundances of fragment ions formed at differentmore » collision energies. The mechanisms of some of the reactions were examined by H/D exchange reactions and molecular orbital calculations.« less

Adiabatic model of field reversal by fast ions in an axisymmetric open trap

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tsidulko, Yu. A., E-mail: tsidulko@mail.ru

2016-06-15

A model of field reversal by fast ions has been developed under the assumption of preservation of fast-ion adiabatic invariants. Analytical solutions obtained in the approximation of a narrow fast-ion layer and numerical solutions to the evolutionary problem are presented. The solutions demonstrate the process of formation of a field reversed configuration with parameters close to those of the planned experiment.

Rapid detection and identification of N-acetyl-L-cysteine thioethers using constant neutral loss and theoretical multiple reaction monitoring combined with enhanced product-ion scans on a linear ion trap mass spectrometer.

PubMed

Scholz, Karoline; Dekant, Wolfgang; Völkel, Wolfgang; Pähler, Axel

2005-12-01

A sensitive and specific liquid chromatography-mass spectrometry (LC-MS) method based on the combination of constant neutral loss scans (CNL) with product ion scans was developed on a linear ion trap. The method is applicable for the detection and identification of analytes with identical chemical substructures (such as conjugates of xenobiotics formed in biological systems) which give common CNLs. A specific CNL was observed for thioethers of N-acetyl-L-cysteine (mercapturic acids, MA) by LC-MS/MS. MS and HPLC parameters were optimized with 16 MAs available as reference compounds. All of these provided a CNL of 129 Da in the negative-ion mode. To assess sensitivity, a multiple reaction monitoring (MRM) mode with 251 theoretical transitions using the CNL of 129 Da combined with a product ion scan (IDA thMRM) was compared with CNL combined with a product ion scan (IDA CNL). An information-dependent acquisition (IDA) uses a survey scan such as MRM (multiple reaction monitoring) to generate "informations" and starting a second acquisition experiment such as a product ion scan using these "informations." Th-MRM means calculated transitions and not transitions generated from an available standard in the tuning mode. The product ion spectra provide additional information on the chemical structure of the unknown analytes. All MA standards were spiked in low concentrations to rat urines and were detected with both methods with LODs ranging from 60 pmol/mL to 1.63 nmol/mL with IDA thMRM. The expected product ion spectra were observed in urine. Application of this screening method to biological samples indicated the presence of a number of MAs in urine of unexposed rats, and resulted in the identification of 1,4-dihydroxynonene mercapturic acid as one of these MAs by negative and positive product ion spectra. These results show that the developed methods have a high potential to serve as both a prescreen to detect unknown MAs and to identify these analytes in complex matrix.

Procurement of novel microanalysis equipment for construction materials.

DOT National Transportation Integrated Search

2012-02-01

The equipment procured (i.e. an Orbis micro X-ray Fluorescence (MXRF) and an APSEX personal Scanning Electron Microscope (PSEM)) is part of the next generation of micro analytical equipment. These tools have the ability to make large volumes of...

Microstructural evolution and micromechanical properties of gamma-irradiated Au ball bonds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yusoff, Wan Yusmawati Wan, E-mail: yusmawati@upnm.edu.my; Ismail, Roslina, E-mail: roslina.ismail@ukm.my; Jalar, Azman, E-mail: azmn@ukm.my

2014-07-01

The effect of gamma radiation on the mechanical and structural properties of gold ball bonds was investigated. Gold wires from thermosonic wire bonding were exposed to gamma rays from a Cobalt-60 source at a low dose (5 Gy). The load–depth curve of nanoindentation for the irradiated gold wire bond has an apparent staircase shape during loading compared to the as-received sample. The hardness of the specimens calculated from the nanoindentation shows an increase in value from 0.91 to 1.09 GPa for specimens after exposure. The reduced elastic modulus for irradiated specimens significantly increased as well, with values from 75.18 tomore » 98.55 GPa. The change in intrinsic properties due to gamma radiation was investigated using dual-focused ion beam and high-resolution transmission electron microscope analysis. The dual-focused ion beam and high-resolution transmission electron microscope images confirmed the changes in grain structure and the presence of dislocations. The scanning electron microscope micrographs of focused ion beam cross sections showed that the grain structure of the gold became elongated and smaller after exposure to gamma rays. Meanwhile, high-resolution transmission electron microscopy provided evidence that gamma radiation induced dislocation of the atomic arrangement. - Highlights: • Nanoindentation technique provides a detailed characterisation of Au ball bond. • P–h curve of irradiated Au ball bond shows an apparent pop-in event. • Hardness and reduced modulus increased after exposure. • Elongated and smaller grain structure in irradiated specimens • Prevalent presence of dislocations in the atomic arrangement.« less

Comparative Study of the Energetics of Ion Permeation in Kv1.2 and KcsA Potassium Channels

PubMed Central

Baştuğ, Turgut; Kuyucak, Serdar

2011-01-01

Biological ion channels rely on a multi-ion transport mechanism for fast yet selective permeation of ions. The crystal structure of the KcsA potassium channel provided the first microscopic picture of this process. A similar mechanism is assumed to operate in all potassium channels, but the validity of this assumption has not been well investigated. Here, we examine the energetics of ion permeation in Shaker Kv1.2 and KcsA channels, which exemplify the six-transmembrane voltage-gated and two-transmembrane inward-rectifier channels. We study the feasibility of binding a third ion to the filter and the concerted motion of ions in the channel by constructing the potential of mean force for K+ ions in various configurations. For both channels, we find that a pair of K+ ions can move almost freely within the filter, but a relatively large free-energy barrier hinders the K+ ion from stepping outside the filter. We discuss the effect of the CMAP dihedral energy correction that was recently incorporated into the CHARMM force field on ion permeation dynamics. PMID:21281577

Fast screening of analytes for chemical reactions by reactive low-temperature plasma ionization mass spectrometry.

PubMed

Zhang, Wei; Huang, Guangming

2015-11-15

Approaches for analyte screening have been used to aid in the fine-tuning of chemical reactions. Herein, we present a simple and straightforward analyte screening method for chemical reactions via reactive low-temperature plasma ionization mass spectrometry (reactive LTP-MS). Solution-phase reagents deposited on sample substrates were desorbed into the vapor phase by action of the LTP and by thermal desorption. Treated with LTP, both reagents reacted through a vapor phase ion/molecule reaction to generate the product. Finally, protonated reagents and products were identified by LTP-MS. Reaction products from imine formation reaction, Eschweiler-Clarke methylation and the Eberlin reaction were detected via reactive LTP-MS. Products from the imine formation reaction with reagents substituted with different functional groups (26 out of 28 trials) were successfully screened in a time of 30 s each. Besides, two short-lived reactive intermediates of Eschweiler-Clarke methylation were also detected. LTP in this study serves both as an ambient ionization source for analyte identification (including reagents, intermediates and products) and as a means to produce reagent ions to assist gas-phase ion/molecule reactions. The present reactive LTP-MS method enables fast screening for several analytes from several chemical reactions, which possesses good reagent compatibility and the potential to perform high-throughput analyte screening. In addition, with the detection of various reactive intermediates (intermediates I and II of Eschweiler-Clarke methylation), the present method would also contribute to revealing and elucidating reaction mechanisms. Copyright © 2015 John Wiley & Sons, Ltd.

Means and method of detection in chemical separation procedures

DOEpatents

Yeung, Edward S.; Koutny, Lance B.; Hogan, Barry L.; Cheung, Chan K.; Ma, Yinfa

1993-03-09

A means and method for indirect detection of constituent components of a mixture separated in a chemical separation process. Fluorescing ions are distributed across the area in which separation of the mixture will occur to provide a generally uniform background fluorescence intensity. For example, the mixture is comprised of one or more charged analytes which displace fluorescing ions where its constituent components separate to. Fluorescing ions of the same charge as the charged analyte components cause a displacement. The displacement results in the location of the separated components having a reduced fluorescence intensity to the remainder of the background. Detection of the lower fluorescence intensity areas can be visually, by photographic means and methods, or by automated laser scanning.

Means and method of detection in chemical separation procedures

DOEpatents

Yeung, E.S.; Koutny, L.B.; Hogan, B.L.; Cheung, C.K.; Yinfa Ma.

1993-03-09

A means and method are described for indirect detection of constituent components of a mixture separated in a chemical separation process. Fluorescing ions are distributed across the area in which separation of the mixture will occur to provide a generally uniform background fluorescence intensity. For example, the mixture is comprised of one or more charged analytes which displace fluorescing ions where its constituent components separate to. Fluorescing ions of the same charge as the charged analyte components cause a displacement. The displacement results in the location of the separated components having a reduced fluorescence intensity to the remainder of the background. Detection of the lower fluorescence intensity areas can be visually, by photographic means and methods, or by automated laser scanning.

Study of a rare-gas transverse fast discharge

NASA Technical Reports Server (NTRS)

Chubb, D. L.; Michels, C. J.

1979-01-01

An experimental and analytical study of a Blumlein-type transverse fast discharge operating with He and Xe are presented. An electro-optical voltage probe was used to measure the discharge voltage, and the measured voltages were in agreement with the computed voltages. The analytical model was used to predict the dependence of the discharge efficiency for producing metastables and ions on the important plasma and external circuit parameters. In He the ion efficiency is greater than the metastable efficiency, while in Xe it is the opposite; the He ion efficiencies are much larger than in Xe, while Xe metastable efficiencies are much larger than in He. These differences between Xe and He are accounted by the large dissociative recombination rate of Xe compared with He.

Highly charged ion secondary ion mass spectroscopy

DOEpatents

Hamza, Alex V.; Schenkel, Thomas; Barnes, Alan V.; Schneider, Dieter H.

2001-01-01

A secondary ion mass spectrometer using slow, highly charged ions produced in an electron beam ion trap permits ultra-sensitive surface analysis and high spatial resolution simultaneously. The spectrometer comprises an ion source producing a primary ion beam of highly charged ions that are directed at a target surface, a mass analyzer, and a microchannel plate detector of secondary ions that are sputtered from the target surface after interaction with the primary beam. The unusually high secondary ion yield permits the use of coincidence counting, in which the secondary ion stops are detected in coincidence with a particular secondary ion. The association of specific molecular species can be correlated. The unique multiple secondary nature of the highly charged ion interaction enables this new analytical technique.

Nanophotonic production, modulation and switching of ions by silicon microcolumn arrays

DOEpatents

Vertes, Akos; Walker, Bennett N.

2013-09-10

The production and use of silicon microcolumn arrays that harvest light from a laser pulse to produce ions are described. The systems of the present invention seem to behave like a quasi-periodic antenna array with ion yields that show profound dependence on the plane of laser light polarization and the angle of incidence. By providing photonic ion sources, this enables enhanced control of ion production on a micro/nano scale and direct integration with miniaturized analytical devices.

Nanophotonic production, modulation and switching of ions by silicon microcolumn arrays

DOEpatents

Vertes, Akos; Walker, Bennett N

2015-04-07

The production and use of silicon microcolumn arrays that harvest light from a laser pulse to produce ions are described. The systems of the present invention seem to behave like a quasi-periodic antenna array with ion yields that show profound dependence on the plane of laser light polarization and the angle of incidence. By providing photonic ion sources, this enables enhanced control of ion production on a micro/nano scale and direct integration with miniaturized analytical devices.

Nanophotonic production, modulation and switching of ions by silicon microcolumn arrays

DOEpatents

Vertes, Akos [Reston, VA; Walker, Bennett N [Washington, DC

2012-02-07

The production and use of silicon microcolumn arrays that harvest light from a laser pulse to produce ions are described. The systems of the present invention seem to behave like a quasi-periodic antenna array with ion yields that show profound dependence on the plane of laser light polarization and the angle of incidence. By providing photonic ion sources, this enables enhanced control of ion production on a micro/nano scale and direct integration with miniaturized analytical devices.

Electromagnetic tornadoes in space. Ion conics along auroral field lines generated by lower hybrid waves and electromagnetic turbulence in the ion-cyclotron range of frequencies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chang, T.; Crew, G.B.; Retterer, J.M.

1988-01-01

The exotic phenomenon of energetic ion-conic formation by plasma waves in the magnetosphere is considered. Two particular transverse heating mechanisms are reviewed in detail: lower-hybrid energization of ions in the boundary layer of the plasma sheet, and electromagnetic ion cyclotron resonance heating in the central region of the plasma sheet. Mean particle calculations, plasma simulations, and analytical treatments of the heating processes are described.

General Unknown Screening by Ion Trap LC/MS/MS

DTIC Science & Technology

2010-04-01

Subtitle 5 . Report Date April 2010 General Unknown Screening by Ion Trap LC/MS/MS 6 . Performing Organization Code 7. Author(s) 8... 5 Table 1: Analytical Data for Each of the...359 Compounds in the LC/MS/MS Library . . . . . . . . . . . 6 1 General Unknown ScreeninG by ion Trap lc/MS/MS INTrOduCTION The Federal Aviation

Analysis of nine food additives in red wine by ion-suppression reversed-phase high-performance liquid chromatography using trifluoroacetic acid and ammonium acetate as ion-suppressors.

PubMed

Zhao, Yong-Gang; Chen, Xiao-Hong; Yao, Shan-Shan; Pan, Sheng-Dong; Li, Xiao-Ping; Jin, Mi-Cong

2012-01-01

A reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for the simultaneous determination of nine food additives, i.e., acesulfame, saccharin, caffeine, aspartame, benzoic acid, sorbic acid, stevioside, dehydroacetic acid and neotame in red wine. The effects of ion-suppressors, i.e., trifluoroacetic acid (TFA) and ammonium acetate (AmAc) on retention behavior of nine food additives in RP-HPLC separation were discussed in detail. The relationships between retention factors of solutes and volume percent of ion-suppressors in the mobile-phase systems of acetonitrile-TFA aqueous solution and acetonitrile-TFA-AmAc aqueous solution were quantitatively established, respectively. The results showed that the ion suppressors had not only an ion suppression effect, but also an organic modification effect on the acidic analytes. The baseline separation of nine food additives was completed by a gradient elution with acetonitrile-TFA(0.01%, v/v)-AmAc(2.5 mmol L(-1)) aqueous solution as the mobile phase. The recoveries were between 80.2 - 99.5% for all analytes with RSDs in the range of 1.5 - 8.9%. The linearities were in the range of 0.2 - 100.0 mg L(-1) with determination coefficients (r(2)) higher than 0.9991 for all analytes. The limits of quantification (LOQs) were between 0.53 - 0.99 mg L(-1). The applicability of the proposed method to detect and quantify food additives has been demonstrated in the analysis of 30 real samples.

A role for ion implantation in quantum computing

NASA Astrophysics Data System (ADS)

Jamieson, David N.; Prawer, Steven; Andrienko, Igor; Brett, David A.; Millar, Victoria

2001-04-01

We propose to create arrays of phosphorus atoms in silicon for quantum computing using ion implantation. Since the implantation of the ions is essentially random, the yield of usefully spaced atoms is low and therefore some method of registering the passage of a single ion is required. This can be accomplished by implantation of the ions through a thin surface layer consisting of resist. Changes to the chemical and/or electrical properties of the resist will be used to mark the site of the buried ion. For chemical changes, the latent damage will be developed and the atomic force microscope (AFM) used to image the changes in topography. Alternatively, changes in electrical properties (which obviate the need for post-irradiation chemical etching) will be used to register the passage of the ion using scanning tunneling microscopy (STM), the surface current imaging mode of the AFM. We address the central issue of the contrast created by the passage of a single ion through resist layers of PMMA and C 60.

Ion beam analysis in cultural heritage studies: Milestones and perspectives

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dran, Jean-Claude; Calligaro, Thomas

2013-07-18

For three decades, ion beam analysis (IBA) in external mode was considered as the best choice for the characterisation of cultural heritage materials, as it combines excellent analytical performance and non-invasive character. However, in recent years, other analytical techniques arose as serious competitors, such as those based on synchrotron radiation (X-ray absorption, fluorescence or diffraction) or those using portable instruments (XRF, micro-Raman). It is shown that nevertheless IBA remains unmatched thanks to two unique features, namely the analysis of light elements and the high-resolution 3D chemical imaging.

Analytical application of solid contact ion-selective electrodes for determination of copper and nitrate in various food products and drinking water.

PubMed

Wardak, Cecylia; Grabarczyk, Malgorzata

2016-08-02

A simple, fast and cheap method for monitoring copper and nitrate in drinking water and food products using newly developed solid contact ion-selective electrodes is proposed. Determination of copper and nitrate was performed by application of multiple standard additions technique. The reliability of the obtained results was assessed by comparing them using the anodic stripping voltammetry or spectrophotometry for the same samples. In each case, satisfactory agreement of the results was obtained, which confirms the analytical usefulness of the constructed electrodes.

Passive Films, Surface Structure and Stress Corrosion and Crevice Corrosion Susceptibility.

DTIC Science & Technology

1980-08-01

with pure titanium ( 4 ], it is of interest to pursue the effects on titanium -palladium alloys, to evaluate their susceptibility to stress corrosion...cracking due to hydrogen embrittlement with the field ion microscope, and to compare the results with those previously obtained with pure titanium [ 4 ...characterized as 99.99+ percent pure, and was used in the previous field ion microscopy study of titanium [ 4 ], where it was found that strain annealing titanium

Formation of 4H-closely packed structure in thin films of metastable nanocrystalline Co 13Cu 87 alloy

NASA Astrophysics Data System (ADS)

Khalyapin, D. L.; Kim, J.; Stolyar, S. V.; Turpanov, I. A.; Kim, P. D.; Kim, I.

2003-11-01

The crystal structure of the thin films of metastable Co 13Cu 87 alloy prepared by magnetron sputtering was investigated by transmission electron microscope. As-deposited films have a nanocrystal structure with an fcc lattice. As a result of the prolonged ion polishing with a beam of Ar ions with the energy of 4.7 keV, the four-layer 4H dhcp structure was formed.

Determination of the accuracy for targeted irradiations of cellular substructures at SNAKE

NASA Astrophysics Data System (ADS)

Siebenwirth, C.; Greubel, C.; Drexler, S. E.; Girst, S.; Reindl, J.; Walsh, D. W. M.; Dollinger, G.; Friedl, A. A.; Schmid, T. E.; Drexler, G. A.

2015-04-01

In the last 10 years the ion microbeam SNAKE, installed at the Munich 14 MV tandem accelerator, has been successfully used for radiobiological experiments by utilizing pattern irradiation without targeting single cells. Now for targeted irradiation of cellular substructures a precise irradiation device was added to the live cell irradiation setup at SNAKE. It combines a sub-micrometer single ion irradiation facility with a high resolution optical fluorescence microscope. Most systematic errors can be reduced or avoided by using the same light path in the microscope for beam spot verification as well as for and target recognition. In addition online observation of the induced cellular responses is possible. The optical microscope and the beam delivering system are controlled by an in-house developed software which integrates the open-source image analysis software, CellProfiler, for semi-automatic target recognition. In this work the targeting accuracy was determined by irradiation of a cross pattern with 55 MeV carbon ions on nucleoli in U2OS and HeLa cells stably expressing a GFP-tagged repair protein MDC1. For target recognition, nuclei were stained with Draq5 and nucleoli were stained with Syto80 or Syto83. The damage response was determined by live-cell imaging of MDC1-GFP accumulation directly after irradiation. No systematic displacement and a random distribution of about 0.7 μm (SD) in x-direction and 0.8 μm (SD) in y-direction were observed. An independent analysis after immunofluorescence staining of the DNA damage marker yH2AX yielded similar results. With this performance a target with a size similar to that of nucleoli (i.e. a diameter of about 3 μm) is hit with a probability of more than 80%, which enables the investigation of the radiation response of cellular subcompartments after targeted ion irradiation in the future.

IBiSA_Tools: A Computational Toolkit for Ion-Binding State Analysis in Molecular Dynamics Trajectories of Ion Channels.

PubMed

Kasahara, Kota; Kinoshita, Kengo

2016-01-01

Ion conduction mechanisms of ion channels are a long-standing conundrum. Although the molecular dynamics (MD) method has been extensively used to simulate ion conduction dynamics at the atomic level, analysis and interpretation of MD results are not straightforward due to complexity of the dynamics. In our previous reports, we proposed an analytical method called ion-binding state analysis to scrutinize and summarize ion conduction mechanisms by taking advantage of a variety of analytical protocols, e.g., the complex network analysis, sequence alignment, and hierarchical clustering. This approach effectively revealed the ion conduction mechanisms and their dependence on the conditions, i.e., ion concentration and membrane voltage. Here, we present an easy-to-use computational toolkit for ion-binding state analysis, called IBiSA_tools. This toolkit consists of a C++ program and a series of Python and R scripts. From the trajectory file of MD simulations and a structure file, users can generate several images and statistics of ion conduction processes. A complex network named ion-binding state graph is generated in a standard graph format (graph modeling language; GML), which can be visualized by standard network analyzers such as Cytoscape. As a tutorial, a trajectory of a 50 ns MD simulation of the Kv1.2 channel is also distributed with the toolkit. Users can trace the entire process of ion-binding state analysis step by step. The novel method for analysis of ion conduction mechanisms of ion channels can be easily used by means of IBiSA_tools. This software is distributed under an open source license at the following URL: http://www.ritsumei.ac.jp/~ktkshr/ibisa_tools/.

Nitrogen implantation with a scanning electron microscope.

PubMed

Becker, S; Raatz, N; Jankuhn, St; John, R; Meijer, J

2018-01-08

Established techniques for ion implantation rely on technically advanced and costly machines like particle accelerators that only few research groups possess. We report here about a new and surprisingly simple ion implantation method that is based upon a widespread laboratory instrument: The scanning electron microscope. We show that it can be utilized to ionize atoms and molecules from the restgas by collisions with electrons of the beam and subsequently accelerate and implant them into an insulating sample by the effect of a potential building up at the sample surface. Our method is demonstrated by the implantation of nitrogen ions into diamond and their subsequent conversion to nitrogen vacancy centres which can be easily measured by fluorescence confocal microscopy. To provide evidence that the observed centres are truly generated in the way we describe, we supplied a 98% isotopically enriched 15 N gas to the chamber, whose natural abundance is very low. By employing the method of optically detected magnetic resonance, we were thus able to verify that the investigated centres are actually created from the 15 N isotopes. We also show that this method is compatible with lithography techniques using e-beam resist, as demonstrated by the implantation of lines using PMMA.

High fluence swift heavy ion structure modification of the SiO2/Si interface and gate insulator in 65 nm MOSFETs

NASA Astrophysics Data System (ADS)

Ma, Yao; Gao, Bo; Gong, Min; Willis, Maureen; Yang, Zhimei; Guan, Mingyue; Li, Yun

2017-04-01

In this work, a study of the structure modification, induced by high fluence swift heavy ion radiation, of the SiO2/Si structures and gate oxide interface in commercial 65 nm MOSFETs is performed. A key and novel point in this study is the specific use of the transmission electron microscopy (TEM) technique instead of the conventional atomic force microscope (AFM) or scanning electron microscope (SEM) techniques which are typically performed following the chemical etching of the sample to observe the changes in the structure. Using this method we show that after radiation, the appearance of a clearly visible thin layer between the SiO2 and Si is observed presenting as a variation in the TEM intensity at the interface of the two materials. Through measuring the EDX line scans we reveal that the Si:O ratio changed and that this change can be attributed to the migration of the Si towards interface after the Si-O bond is destroyed by the swift heavy ions. For the 65 nm MOSFET sample, the silicon substrate, the SiON insulator and the poly-silicon gate interfaces become blurred under the same irradiation conditions.

Ion irradiation synthesis of Ag-Au bimetallic nanospheroids in SiO2 glass substrate with tunable surface plasmon resonance frequency

NASA Astrophysics Data System (ADS)

Meng, Xuan; Shibayama, Tamaki; Yu, Ruixuan; Takayanagi, Shinya; Watanabe, Seiichi

2013-08-01

Ag-Au bimetallic nanospheroids with tunable localized surface plasmon resonance (LSPR) were synthesized by 100 keV Ar-ion irradiation of 30 nm Ag-Au bimetallic films deposited on SiO2 glass substrates. A shift of the LSPR peaks toward shorter wavelengths was observed up to an irradiation fluence of 1.0 × 1017 cm-2, and then shifted toward the longer wavelength because of the increase of fragment volume under ion irradiation. Further control of LSPR frequency over a wider range was realized by modifying the chemical components. The resulting LSPR frequencies lie between that of the pure components, and an approximate linear shift of the LSPR toward the longer wavelength with the Au concentration was achieved, which is in good agreement with the theoretical calculations based on Gans theory. In addition, the surface morphology and compositions were examined with a scanning electron microscope equipped with an energy dispersive spectrometer, and microstructural characterizations were performed using a transmission electron microscope. The formation of isolated photosensitive Ag-Au nanospheroids with a FCC structure partially embedded in the SiO2 substrate was confirmed, which has a potential application in solid-state devices.

Surface modifications of crystal-ion-sliced LiNbO3 thin films by low energy ion irradiations

NASA Astrophysics Data System (ADS)

Bai, Xiaoyuan; Shuai, Yao; Gong, Chaoguan; Wu, Chuangui; Luo, Wenbo; Böttger, Roman; Zhou, Shengqiang; Zhang, Wanli

2018-03-01

Single crystalline 128°Y-cut LiNbO3 thin films with a thickness of 670 nm are fabricated onto Si substrates by means of crystal ion slicing (CIS) technique, adhesive wafer bonding using BCB as the medium layer to alleviate the large thermal coefficient mismatch between LiNbO3 and Si, and the X-ray diffraction pattern indicates the exfoliated thin films have good crystalline quality. The LiNbO3 thin films are modified by low energy Ar+ irradiation, and the surface roughness of the films is decreased from 8.7 nm to 3.4 nm. The sputtering of the Ar+ irradiation is studied by scanning electron microscope, atomic force microscope and X-ray photoelectron spectroscopy, and the results show that an amorphous layer exists at the surface of the exfoliated film, which can be quickly removed by Ar+ irradiation. A two-stage etching mechanism by Ar+ irradiation is demonstrated, which not only establishes a new non-contact surface polishing method for the CIS-fabricated single crystalline thin films, but also is potentially useful to remove the residue damage layer produced during the CIS process.

Impact of Ion Bombardment on the Structure and Magnetic Properties of Fe78Si13B9 Amorphous Alloy

NASA Astrophysics Data System (ADS)

Wu, Yingwei; Peng, Kun

2018-06-01

Amorphous Fe78Si13B9 alloy ribbons were bombarded by ion beams with different incident angles ( θ ). The evolution of the microstructure and magnetic properties of ribbons caused by ion beam bombardment was investigated by x-ray diffraction, transmission electron microscope and vibrating sample magnetometer analysis. Low-incident-angle bombardment led to atomic migration in the short range, and high-incident-angle bombardment resulted in the crystallization of amorphous alloys. Ion bombardment induces magnetic anisotropy and affects magnetic properties. The effective magnetic anisotropy was determined by applying the law of approach to saturation, and it increased with the increase of the ion bombardment angle. The introduction of effective magnetic anisotropy will reduce the permeability and increase the relaxation frequency. Excellent high-frequency magnetic properties can be obtained by selecting suitable ion bombardment parameters.

Molecular dynamics and dynamic Monte-Carlo simulation of irradiation damage with focused ion beams

NASA Astrophysics Data System (ADS)

Ohya, Kaoru

2017-03-01

The focused ion beam (FIB) has become an important tool for micro- and nanostructuring of samples such as milling, deposition and imaging. However, this leads to damage of the surface on the nanometer scale from implanted projectile ions and recoiled material atoms. It is therefore important to investigate each kind of damage quantitatively. We present a dynamic Monte-Carlo (MC) simulation code to simulate the morphological and compositional changes of a multilayered sample under ion irradiation and a molecular dynamics (MD) simulation code to simulate dose-dependent changes in the backscattering-ion (BSI)/secondary-electron (SE) yields of a crystalline sample. Recent progress in the codes for research to simulate the surface morphology and Mo/Si layers intermixing in an EUV lithography mask irradiated with FIBs, and the crystalline orientation effect on BSI and SE yields relating to the channeling contrast in scanning ion microscopes, is also presented.

Application of air ions for bacterial de-colonization in air filters contaminated by aerosolized bacteria.

PubMed

Kim, Yang Seon; Yoon, Ki Young; Park, Jae Hong; Hwang, Jungho

2011-01-15

We aerosolized the Escherichia coli (E. coli) and Staphylococcus epidermidis (S. epidermidis) bacteria and collected them on membrane filters. Then we generated air ions by applying a high voltage to a carbon fiber tip and applied them to the contaminated filters. The antibacterial efficiency was not significantly affected by the bacteria being Gram-positive or Gram-negative, however, negative ions showed a lower antibacterial efficiency than positive ions to both E. coli and S. epidermidis, even though the concentration of negative air ions was much higher than that of positive air ions. With a field emission scanning electron microscope (FE-SEM) images and fluorescence microscopy images using a LIVE/DEAD BacLight Bacterial Viability Kit, electrostatic disruption of the bacteria was found to be the dominant antibacterial effect. Copyright © 2010 Elsevier B.V. All rights reserved.

The effects on γ-LiAlO2 induced by nuclear energy losses during Ga ions implantation

NASA Astrophysics Data System (ADS)

Zhang, Jing; Song, Hong-Lian; Qiao, Mei; Yu, Xiao-Fei; Wang, Tie-Jun; Wang, Xue-Lin

2017-09-01

To explore the evolution of γ-LiAlO2 under ion irradiation at low energy, we implanted Ga ions of 30, 80 and 150 keV at fluences of 1 × 1014 and 1 × 1015 ions/cm2 in z-cut γ-LiAlO2 samples, respectively. The implantation resulted in damage regions dominated by nuclear energy losses at depth of 232 Å, 514 Å, and 911 Å beneath the surface, respectively, which was simulated by the Stopping and Range of Ions in Matter program. The irradiated γ-LiAlO2 were characterized with atomic force microscope, Raman spectroscopy, X-ray diffraction and Rutherford backscattering in a channeling mode for morphology evolution, structure information and damage profiles. The interesting and partly abnormal results showed the various behaviors in modification of surface by Ga ions implantation.

Monte Carlo simulations of nanoscale focused neon ion beam sputtering.

PubMed

Timilsina, Rajendra; Rack, Philip D

2013-12-13

A Monte Carlo simulation is developed to model the physical sputtering of aluminum and tungsten emulating nanoscale focused helium and neon ion beam etching from the gas field ion microscope. Neon beams with different beam energies (0.5-30 keV) and a constant beam diameter (Gaussian with full-width-at-half-maximum of 1 nm) were simulated to elucidate the nanostructure evolution during the physical sputtering of nanoscale high aspect ratio features. The aspect ratio and sputter yield vary with the ion species and beam energy for a constant beam diameter and are related to the distribution of the nuclear energy loss. Neon ions have a larger sputter yield than the helium ions due to their larger mass and consequently larger nuclear energy loss relative to helium. Quantitative information such as the sputtering yields, the energy-dependent aspect ratios and resolution-limiting effects are discussed.

Ion-induced electron emission microscopy

DOEpatents

Doyle, Barney L.; Vizkelethy, Gyorgy; Weller, Robert A.

2001-01-01

An ion beam analysis system that creates multidimensional maps of the effects of high energy ions from an unfocussed source upon a sample by correlating the exact entry point of an ion into a sample by projection imaging of the secondary electrons emitted at that point with a signal from a detector that measures the interaction of that ion within the sample. The emitted secondary electrons are collected in a strong electric field perpendicular to the sample surface and (optionally) projected and refocused by the electron lenses found in a photon emission electron microscope, amplified by microchannel plates and then their exact position is sensed by a very sensitive X Y position detector. Position signals from this secondary electron detector are then correlated in time with nuclear, atomic or electrical effects, including the malfunction of digital circuits, detected within the sample that were caused by the individual ion that created these secondary electrons in the fit place.

Fast and Adaptive Auto-focusing Microscope

NASA Astrophysics Data System (ADS)

Obara, Takeshi; Igarashi, Yasunobu; Hashimoto, Koichi

Optical microscopes are widely used in biological and medical researches. By using the microscope, we can observe cellular movements including intracellular ions and molecules tagged with fluorescent dyes at a high magnification. However, a freely motile cell easily escapes from a 3D field of view of the typical microscope. Therefore, we propose a novel auto-focusing algorithm and develop a auto-focusing and tracking microscope. XYZ positions of a microscopic stage are feedback controlled to focus and track the cell automatically. A bright-field image is used to estimate a cellular position. XY centroids are used to estimate XY positions of the tracked cell. To estimate Z position, we use a diffraction pattern around the cell membrane. This estimation method is so-called Depth from Diffraction (DFDi). However, this method is not robust for individual differences between cells because the diffraction pattern depends on each cellular shape. Therefore, in this study, we propose a real-time correction of DFDi by using 2D Laplacian of an intracellular area as a goodness of the focus. To evaluate the performance of our developed algorithm and microscope, we auto-focus and track a freely moving paramecium. In this experimental result, the paramecium is auto-focused and kept inside the scope of the microscope during 45s. The evaluated focal error is within 5µm, while a length and a thickness of the paramecium are about 200µm and 50µm, respectively.

Quality-assurance results for routine water analysis in US Geological Survey laboratories, water year 1991

USGS Publications Warehouse

Maloney, T.J.; Ludtke, A.S.; Krizman, T.L.

1994-01-01

The US. Geological Survey operates a quality- assurance program based on the analyses of reference samples for the National Water Quality Laboratory in Arvada, Colorado, and the Quality of Water Service Unit in Ocala, Florida. Reference samples containing selected inorganic, nutrient, and low ionic-strength constituents are prepared and disguised as routine samples. The program goal is to determine precision and bias for as many analytical methods offered by the participating laboratories as possible. The samples typically are submitted at a rate of approximately 5 percent of the annual environmental sample load for each constituent. The samples are distributed to the laboratories throughout the year. Analytical data for these reference samples reflect the quality of environmental sample data produced by the laboratories because the samples are processed in the same manner for all steps from sample login through data release. The results are stored permanently in the National Water Data Storage and Retrieval System. During water year 1991, 86 analytical procedures were evaluated at the National Water Quality Laboratory and 37 analytical procedures were evaluated at the Quality of Water Service Unit. An overall evaluation of the inorganic (major ion and trace metal) constituent data for water year 1991 indicated analytical imprecision in the National Water Quality Laboratory for 5 of 67 analytical procedures: aluminum (whole-water recoverable, atomic emission spectrometric, direct-current plasma); calcium (atomic emission spectrometric, direct); fluoride (ion-exchange chromatographic); iron (whole-water recoverable, atomic absorption spectrometric, direct); and sulfate (ion-exchange chromatographic). The results for 11 of 67 analytical procedures had positive or negative bias during water year 1991. Analytical imprecision was indicated in the determination of two of the five National Water Quality Laboratory nutrient constituents: orthophosphate as phosphorus and phosphorus. A negative or positive bias condition was indicated in three of five nutrient constituents. There was acceptable precision and no indication of bias for the 14 low ionic-strength analytical procedures tested in the National Water Quality Laboratory program and for the 32 inorganic and 5 nutrient analytical procedures tested in the Quality of Water Service Unit during water year 1991.

Transmission electron microscope studies of extraterrestrial materials

NASA Technical Reports Server (NTRS)

Keller, Lindsay P.

1995-01-01

Transmission Electron Microscopy, X-Ray spectrometry and electron-energy-loss spectroscopy are used to analyse carbon in interplanetary dust particles. Optical micrographs are shown depicting cross sections of the dust particles embedded in sulphur. Selected-area electron diffraction patterns are shown. Transmission Electron Microscope specimens of lunar soil were prepared using two methods: ion-milling and ultramicrotomy. A combination of high resolution TEM imaging and electron diffraction is used to characterize the opaque assemblages. The opaque assemblages analyzed in this study are dominated by ilmenite with lesser rutile and spinel exsolutions, and traces of Fe metal.

Nonlinear ion dynamics in Hall thruster plasma source by ion transit-time instability

NASA Astrophysics Data System (ADS)

Lim, Youbong; Choe, Wonho; Mazouffre, Stéphane; Park, Jae Sun; Kim, Holak; Seon, Jongho; Garrigues, L.

2017-03-01

High-energy tail formation in an ion energy distribution function (IEDF) is explained in a Hall thruster plasma with the stationary crossed electric and magnetic fields whose discharge current is oscillated at the ion transit-time scale with a frequency of 360 kHz. Among ions in different charge states, singly charged Xe ions (Xe+) have an IEDF that is significantly broadened and shifted toward the high-energy side, which contributes to tail formation in the entire IEDF. Analytical and numerical investigations confirm that the IEDF tail is due to nonlinear ion dynamics in the ion transit-time oscillation.

10 CFR 830.3 - Definitions.

Code of Federal Regulations, 2014 CFR

2014-01-01

... research and experimental and analytical laboratory activities, electron microscopes, and X-ray machines... research, test, and power reactors, and critical and pulsed assemblies and any assembly that is designed to... covering a topic such as: quality assurance; maintenance of safety systems; personnel training; conduct of...

A fluorescent chemosensor for Hg(2+) and Cd(2+) ions in aqueous medium under physiological pH and its applications in imaging living cells.

PubMed

Maity, Shubhra B; Banerjee, Saikat; Sunwoo, Kyoung; Kim, Jong Seung; Bharadwaj, Parimal K

2015-04-20

A new BODIPY derivative with 2,2'-(ethane-1,2-diylbis(oxy))bis(N,N-bis(pyridine-2-ylmethyl)aniline unit as the metal receptor has been designed and synthesized. The dye selectively detects either Cd(2+) or Hg(2+) ions in the presence of hosts of other biologically important and environmentally relevant metal ions in aqueous medium at physiological pH. Binding of metal ions causes a change in the emission behavior of the dye from weakly fluorescent to highly fluorescent. Confocal microscopic experiments validate that the dye can be used to identify changes in either Hg(2+) or Cd(2+) levels in living cells.

Inactivation of individual Bacillus subtilis spores in dependence on their distance to single cosmic heavy ions.

PubMed

Facius, R; Reitz, G; Schafer, M

1994-10-01

For radiobiological experiments in space, designed to investigate biological effects of the heavy ions of the cosmic radiation field, a mandatory requirement is the possibility to spatially correlate the observed biological response of individual test organisms to the passage of single heavy ions. Among several undertakings towards this goal, the BIOSTACK experiments in the Apollo missions achieved the highest precision and therefore the most detailed information on this question. Spores of Bacillus subtilis as a highly radiation resistant and microscopically small test organism yielded these quantitative results. This paper will focus on experimental and procedural details, which must be included for an interpretation and a discussion of these findings in comparison to control experiments with accelerated heavy ions.

Imaging of dynamic ion signaling during root gravitropism.

PubMed

Monshausen, Gabriele B

2015-01-01

Gravitropic signaling is a complex process that requires the coordinated action of multiple cell types and tissues. Ca(2+) and pH signaling are key components of gravitropic signaling cascades and can serve as useful markers to dissect the molecular machinery mediating plant gravitropism. To monitor dynamic ion signaling, imaging approaches combining fluorescent ion sensors and confocal fluorescence microscopy are employed, which allow the visualization of pH and Ca(2+) changes at the level of entire tissues, while also providing high spatiotemporal resolution. Here, I describe procedures to prepare Arabidopsis seedlings for live cell imaging and to convert a microscope for vertical stage fluorescence microscopy. With this imaging system, ion signaling can be monitored during all phases of the root gravitropic response.

Neuromorphic Data Microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Naegle, John H.; Suppona, Roger A.; Aimone, James Bradley

In 2016, Lewis Rhodes Labs, (LRL), shipped the first commercially viable Neuromorphic Processing Unit, (NPU), branded as a Neuromorphic Data Microscope (NDM). This product leverages architectural mechanisms derived from the sensory cortex of the human brain to efficiently implement pattern matching. LRL and Sandia National Labs have optimized this product for streaming analytics, and demonstrated a 1,000x power per operation reduction in an FPGA format. When reduced to an ASIC, the efficiency will improve to 1,000,000x. Additionally, the neuromorphic nature of the device gives it powerful computational attributes that are counterintuitive to those schooled in traditional von Neumann architectures. Themore » Neuromorphic Data Microscope is the first of a broad class of brain-inspired, time domain processors that will profoundly alter the functionality and economics of data processing.« less

PtyNAMi: ptychographic nano-analytical microscope at PETRA III: interferometrically tracking positions for 3D x-ray scanning microscopy using a ball-lens retroreflector

NASA Astrophysics Data System (ADS)

Schroer, Christian G.; Seyrich, Martin; Kahnt, Maik; Botta, Stephan; Döhrmann, Ralph; Falkenberg, Gerald; Garrevoet, Jan; Lyubomirskiy, Mikhail; Scholz, Maria; Schropp, Andreas; Wittwer, Felix

2017-09-01

In recent years, ptychography has revolutionized x-ray microscopy in that it is able to overcome the diffraction limit of x-ray optics, pushing the spatial resolution limit down to a few nanometers. However, due to the weak interaction of x rays with matter, the detection of small features inside a sample requires a high coherent fluence on the sample, a high degree of mechanical stability, and a low background signal from the x-ray microscope. The x-ray scanning microscope PtyNAMi at PETRA III is designed for high-spatial-resolution 3D imaging with high sensitivity. The design concept is presented with a special focus on real-time metrology of the sample position during tomographic scanning microscopy.

Monoenergetic ion acceleration and Rayleigh-Taylor instability of the composite target irradiated by the laser pulse

NASA Astrophysics Data System (ADS)

Khudik, Vladimir; Yi, S. Austin; Shvets, Gennady

2012-10-01

Acceleration of ions in the two-specie composite target irradiated by a circularly polarized laser pulse is studied analytically and via particle-in-cell (PIC) simulations. A self-consistent analytical model of the composite target is developed. In this model, target parameters are stationary in the center of mass of the system: heavy and light ions are completely separated from each other and form two layers, while electrons are bouncing in the potential well formed by the laser ponderomotive and electrostatic potentials. They are distributed in the direction of acceleration by the Boltzmann law and over velocities by the Maxwell-Juttner law. The laser pulse interacts directly only with electrons in a thin sheath layer, and these electrons transfer the laser pressure to the target ions. In the fluid approximation it is shown, the composite target is still susceptible to the Rayleigh-Taylor instability [1]. Using PIC simulations we found the growth rate of initially seeded perturbations as a function of their wavenumber for different composite target parameters and compare it with analytical results. Useful scaling laws between this rate and laser pulse pressure and target parameters are discussed.[4pt] [1] T.P. Yu, A. Pukhov, G. Shvets, M. Chen, T. H. Ratliff, S. A. Yi, and V. Khudik, Phys. Plasmas, 18, 043110 (2011).

Experimental and analytical investigation of a modified ring cusp NSTAR engine

NASA Technical Reports Server (NTRS)

Sengupta, Anita

2005-01-01

A series of experimental measurements on a modified laboratory NSTAR engine were used to validate a zero dimensional analytical discharge performance model of a ring cusp ion thruster. The model predicts the discharge performance of a ring cusp NSTAR thruster as a function the magnetic field configuration, thruster geometry, and throttle level. Analytical formalisms for electron and ion confinement are used to predict the ionization efficiency for a given thruster design. Explicit determination of discharge loss and volume averaged plasma parameters are also obtained. The model was used to predict the performance of the nominal and modified three and four ring cusp 30-cm ion thruster configurations operating at the full power (2.3 kW) NSTAR throttle level. Experimental measurements of the modified engine configuration discharge loss compare well with the predicted value for propellant utilizations from 80 to 95%. The theory, as validated by experiment, indicates that increasing the magnetic strength of the minimum closed reduces maxwellian electron diffusion and electrostatically confines the ion population and subsequent loss to the anode wall. The theory also indicates that increasing the cusp strength and minimizing the cusp area improves primary electron confinement increasing the probability of an ionization collision prior to loss at the cusp.

Development of analytically capable time-of-flight mass spectrometer with continuous ion introduction

NASA Astrophysics Data System (ADS)

Hárs, György; Dobos, Gábor

2010-03-01

The present article describes the results and findings explored in the course of the development of the analytically capable prototype of continuous time-of-flight (CTOF) mass spectrometer. Currently marketed pulsed TOF (PTOF) instruments use ion introduction with a 10 ns or so pulse width, followed by a waiting period roughly 100 μs. Accordingly, the sample is under excitation in 10-4 part of the total measuring time. This very low duty cycle severely limits the sensitivity of the PTOF method. A possible approach to deal with this problem is to use linear sinusoidal dual modulation technique (CTOF) as described in this article. This way the sensitivity of the method is increased, due to the 50% duty cycle of the excitation. All other types of TOF spectrometer use secondary electron multiplier (SEM) for detection, which unfortunately discriminates in amplification in favor of the lighter ions. This discrimination effect is especially undesirable in a mass spectrometric method, which targets high mass range. In CTOF method, SEM is replaced with Faraday cup detector, thus eliminating the mass discrimination effect. Omitting SEM is made possible by the high ion intensity and the very slow ion detection with some hundred hertz detection bandwidth. The electrometer electronics of the Faraday cup detector operates with amplification 1010 V/A. The primary ion beam is highly monoenergetic due to the construction of the ion gun, which made possible to omit any electrostatic mirror configuration for bunching the ions. The measurement is controlled by a personal computer and the intelligent signal generator Type Tabor WW 2571, which uses the direct digital synthesis technique for making arbitrary wave forms. The data are collected by a Labjack interface board, and the fast Fourier transformation is performed by the software. Noble gas mixture has been used to test the analytical capabilities of the prototype setup. Measurement presented proves the results of the mathematical calculations as well as the future potentiality for use in chemical analysis of gaseous mixtures.

Microscopic Theory of Supercapacitors

NASA Astrophysics Data System (ADS)

Skinner, Brian Joseph

As new energy technologies are designed and implemented, there is a rising demand for improved energy storage devices. At present the most promising class of these devices is the electric double-layer capacitor (EDLC), also known as the supercapacitor. A number of recently created supercapacitors have been shown to produce remarkably large capacitance, but the microscopic mechanisms that underlie their operation remain largely mysterious. In this thesis we present an analytical, microscopic-level theory of supercapacitors, and we explain how such large capacitance can result. Specifically, we focus on four types of devices that have been shown to produce large capacitance. The first is a capacitor composed of a clean, low-temperature two-dimensional electron gas adjacent to a metal gate electrode. Recent experiments have shown that such a device can produce capacitance as much as 40% larger than that of a conventional plane capacitor. We show that this enhanced capacitance can be understood as the result of positional correlations between electrons and screening by the gate electrode in the form of image charges. Thus, the enhancement of the capacitance can be understood primarily as a classical, electrostatic phenomenon. Accounting for the quantum mechanical properties of the electron gas provides corrections to the classical theory, and these are discussed. We also present a detailed numerical calculation of the capacitance of the system based on a calculation of the system's ground state energy using the variational principle. The variational technique that we develop is broadly applicable, and we use it here to make an accurate comparison to experiment and to discuss quantitatively the behavior of the electrons' correlation function. The second device discussed in this thesis is a simple EDLC composed of an ionic liquid between two metal electrodes. We adopt a simple description of the ionic liquid and show that for realistic parameter values the capacitance can be as much as three times larger than that of a plane capacitor with thickness equal to the ion diameter. As in the previous system, this large capacitance is the result of image charge formation in the metal electrode and positional correlations between discrete ions that comprise the electric double-layer. We show that the maximum capacitance scales with the temperature to the power -1/3, and that at moderately large voltage the capacitance also decays as the inverse one third power of voltage. These results are confirmed by a Monte Carlo simulation. The third type of device we consider is that of a porous supercapacitor, where the electrode is made from a conducting material with a dense arrangement of narrow, planar pores into which ionic liquid can enter when a voltage is applied. In this case we show that when the electrode is metallic the narrow pores aggressively screen the interaction between neighboring ions in a pore, leading to an interaction energy between ions that decays exponentially. This exponential interaction between ions allows the capacitance to be nearly an order of magnitude larger than what is predicted by mean-field theories. This result is confirmed by a Monte Carlo simulation. We also present a theory for the capacitance when the electrode is not a perfect metal, but has a finite electronic screening radius. When this screening radius is larger than the distance between pores, ions begin to interact across multiple pores and the capacitance is determined by the Yukawa-like interaction of a three-dimensional, correlated arrangement of ions. Finally, we consider the case of supercapacitor electrodes made from a stack of graphene sheets with randomly-inserted "spacer" molecules. For such devices, experiments have produced very large capacitance despite the small density of states of the electrode material, which would seem to imply poor screening of the ionic charge. We show that these large capacitance values can be understood as the result of collective entrance of ions into the graphene stack (GS) and the renormalization of the ionic charge produced by nonlinear screening. The collective behavior of ions results from the strong elastic energy associated with intercalated ions deforming the GS, which creates an effective attraction between them. The result is the formation of "disks" of charge that enter the electrode collectively and have their charge renormalized by the strong, nonlinear screening of the surrounding graphene layers. This renormalization leads to a capacitance that at small voltages increases linearly with voltage and is enhanced over mean-field predictions by a large factor proportional to the number of ions within the disk to the power 9/4. At large voltages, the capacitance is dictated by the physics of graphite intercalation compounds and is proportional to the voltage raised to the power -4/5. We also examine theoretically the case where the effective fine structure constant of the GS is a small parameter, and we uncover a wealth of scaling regimes.

Focused analyte spray emission apparatus and process for mass spectrometric analysis

DOEpatents

Roach, Patrick J [Kennewick, WA; Laskin, Julia [Richland, WA; Laskin, Alexander [Richland, WA

2012-01-17

An apparatus and process are disclosed that deliver an analyte deposited on a substrate to a mass spectrometer that provides for trace analysis of complex organic analytes. Analytes are probed using a small droplet of solvent that is formed at the junction between two capillaries. A supply capillary maintains the droplet of solvent on the substrate; a collection capillary collects analyte desorbed from the surface and emits analyte ions as a focused spray to the inlet of a mass spectrometer for analysis. The invention enables efficient separation of desorption and ionization events, providing enhanced control over transport and ionization of the analyte.

Helium ion beam induced electron emission from insulating silicon nitride films under charging conditions

NASA Astrophysics Data System (ADS)

Petrov, Yu. V.; Anikeva, A. E.; Vyvenko, O. F.

2018-06-01

Secondary electron emission from thin silicon nitride films of different thicknesses on silicon excited by helium ions with energies from 15 to 35 keV was investigated in the helium ion microscope. Secondary electron yield measured with Everhart-Thornley detector decreased with the irradiation time because of the charging of insulating films tending to zero or reaching a non-zero value for relatively thick or thin films, respectively. The finiteness of secondary electron yield value, which was found to be proportional to electronic energy losses of the helium ion in silicon substrate, can be explained by the electron emission excited from the substrate by the helium ions. The method of measurement of secondary electron energy distribution from insulators was suggested, and secondary electron energy distribution from silicon nitride was obtained.

Electromagnetic tornadoes in space

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chang, T.; Crew, G.B.; Retterer, J.M.

1988-01-01

The exotic phenomenon of energetic-ion conic formation by plasma waves in the magnetosphere is considered. Two particular transverse heating mechanisms are reviewed in detail; lower-hybrid energization of ions in the boundary layer of the plasma sheet and electromagnetic ion cyclotron resonance heating in the central region of the plasma sheet. Mean particle calculations, plasma simulations and analytical treatments of the heating processes are described.

Molecular Structures and Momentum Transfer Cross Sections: The Influence of the Analyte Charge Distribution.

PubMed

Young, Meggie N; Bleiholder, Christian

2017-04-01

Structure elucidation by ion mobility spectrometry-mass spectrometry methods is based on the comparison of an experimentally measured momentum transfer cross-section to cross-sections calculated for model structures. Thus, it is imperative that the calculated cross-section must be accurate. However, it is not fully understood how important it is to accurately model the charge distribution of an analyte ion when calculating momentum transfer cross-sections. Here, we calculate and compare momentum transfer cross-sections for carbon clusters that differ in mass, charge state, and mode of charge distribution, and vary temperature and polarizability of the buffer gas. Our data indicate that the detailed distribution of the ion charge density is intimately linked to the contribution of glancing collisions to the momentum transfer cross-section. The data suggest that analyte ions with molecular mass ~3 kDa or momentum transfer cross-section 400-500 Å 2 would be significantly influenced by the charge distribution in nitrogen buffer gas. Our data further suggest that accurate structure elucidation on the basis of IMS-MS data measured in nitrogen buffer gas must account for the molecular charge distribution even for systems as large as C 960 (~12 kDa) when localized charges are present and/or measurements are conducted under cryogenic temperatures. Finally, our data underscore that accurate structure elucidation is unlikely if ion mobility data recorded in one buffer gas is converted into other buffer gases when electronic properties of the buffer gases differ. Graphical Abstract ᅟ.

Capillary ion chromatography with on-column focusing for ultra-trace analysis of methanesulfonate and inorganic anions in limited volume Antarctic ice core samples.

PubMed

Rodriguez, Estrella Sanz; Poynter, Sam; Curran, Mark; Haddad, Paul R; Shellie, Robert A; Nesterenko, Pavel N; Paull, Brett

2015-08-28

Preservation of ionic species within Antarctic ice yields a unique proxy record of the Earth's climate history. Studies have been focused until now on two proxies: the ionic components of sea salt aerosol and methanesulfonic acid. Measurement of the all of the major ionic species in ice core samples is typically carried out by ion chromatography. Former methods, whilst providing suitable detection limits, have been based upon off-column preconcentration techniques, requiring larger sample volumes, with potential for sample contamination and/or carryover. Here, a new capillary ion chromatography based analytical method has been developed for quantitative analysis of limited volume Antarctic ice core samples. The developed analytical protocol applies capillary ion chromatography (with suppressed conductivity detection) and direct on-column sample injection and focusing, thus eliminating the requirement for off-column sample preconcentration. This limits the total sample volume needed to 300μL per analysis, allowing for triplicate sample analysis with <1mL of sample. This new approach provides a reliable and robust analytical method for the simultaneous determination of organic and inorganic anions, including fluoride, methanesulfonate, chloride, sulfate and nitrate anions. Application to composite ice-core samples is demonstrated, with coupling of the capillary ion chromatograph to high resolution mass spectrometry used to confirm the presence and purity of the observed methanesulfonate peak. Copyright © 2015 Elsevier B.V. All rights reserved.

Generalization of the Child-Langmuir law to the alternate extraction of positive and negative ions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lafleur, T., E-mail: trevor.lafleur@lpp.polytechnique.fr; ONERA-The French Aerospace Lab, 91120 Palaiseau; Aanesland, A.

Using a combined analytical and simulation approach, we investigate positive and negative ion extraction between two electrodes from an ion-ion plasma source. With a square voltage waveform applied to the electrodes, we obtain approximate analytical solutions for the time-averaged extracted current densities, which are given simply by: J{sub p}{sup ac}=[α−fL√((M{sub p})/(q{sub p}V{sub 0}) )]J{sub p}{sup dc}, and J{sub n}{sup ac}=[(1−α)−fL√((M{sub n})/(q{sub n}V{sub 0}) )]J{sub n}{sup dc}, where J{sup ac} is the time-averaged current density, α is the square waveform duty cycle, f is the frequency, L is the electrode gap length, M is the ion mass, q is the ionmore » charge, V{sub 0} is the applied voltage amplitude, J{sup dc} is the dc extracted current density, and the subscripts p and n refer to positive and negative ions, respectively. In particular, if J{sup dc} is the dc space-charge limited current density, then these equations describe the square waveform generalization of the Child-Langmuir law.« less

Quantum tunneling recombination in a system of randomly distributed trapped electrons and positive ions.

PubMed

Pagonis, Vasilis; Kulp, Christopher; Chaney, Charity-Grace; Tachiya, M

2017-09-13

During the past 10 years, quantum tunneling has been established as one of the dominant mechanisms for recombination in random distributions of electrons and positive ions, and in many dosimetric materials. Specifically quantum tunneling has been shown to be closely associated with two important effects in luminescence materials, namely long term afterglow luminescence and anomalous fading. Two of the common assumptions of quantum tunneling models based on random distributions of electrons and positive ions are: (a) An electron tunnels from a donor to the nearest acceptor, and (b) the concentration of electrons is much lower than that of positive ions at all times during the tunneling process. This paper presents theoretical studies for arbitrary relative concentrations of electrons and positive ions in the solid. Two new differential equations are derived which describe the loss of charge in the solid by tunneling, and they are solved analytically. The analytical solution compares well with the results of Monte Carlo simulations carried out in a random distribution of electrons and positive ions. Possible experimental implications of the model are discussed for tunneling phenomena in long term afterglow signals, and also for anomalous fading studies in feldspars and apatite samples.

Miniature GC-Minicell Ion Mobility Spectrometer (IMS) for In Situ Measurements in Astrobiology Planetary Missions

NASA Technical Reports Server (NTRS)

Kojiro, Daniel R.; Stimac, Robert M.; Kaye, William J.; Holland, Paul M.; Takeuchi, Norishige

2006-01-01

Astrobiology flight experiments require highly sensitive instrumentation for in situ analysis of volatile chemical species and minerals present in the atmospheres and surfaces of planets, moons, and asteroids. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. The use of land rovers and balloon aero-rovers place additional emphasis on miniaturization of the analytical instrumentation. In addition, smaller instruments, using tiny amounts of consumables, allow the use of more instrumentation and/or ionger mission life for stationary landers/laboratories. The miniCometary Ice and Dust Experiment (miniCIDEX), which combined Gas Chromatography (GC) with helium Ion Mobility Spectrometry (IMS), was capable of providing the wide range of analytical information required for Astrobiology missions. The IMS used here was based on the PCP model 111 IMS. A similar system, the Titan Ice and Dust Experiment (TIDE), was proposed as part of the Titan Orbiter Aerorover Mission (TOAM). Newer GC systems employing Micro Electro- Mechanical System (MEMS) based technology have greatly reduced both the size and resource requirements for space GCs. These smaller GCs, as well as the continuing miniaturization of Astrobiology analytical instruments in general, has highlighted the need for smaller, dry helium IMS systems. We describe here the development of a miniature, MEMS GC-IMS system (MEMS GC developed by Thorleaf Research Inc.), employing the MiniCell Ion Mobility Spectrometer (IMS), from Ion Applications Inc., developed through NASA's Astrobiology Science and Technology Instrument Development (ASTID) Program and NASA s Small Business Innovative Research (SBIR) Program.

Analyte preconcentration in nanofluidic channels with nonuniform zeta potential

NASA Astrophysics Data System (ADS)

Eden, A.; McCallum, C.; Storey, B. D.; Pennathur, S.; Meinhart, C. D.

2017-12-01

It is well known that charged analytes in the presence of nonuniform electric fields concentrate at locations where the relevant driving forces balance, and a wide range of ionic stacking and focusing methods are commonly employed to leverage these physical mechanisms in order to improve signal levels in biosensing applications. In particular, nanofluidic channels with spatially varying conductivity distributions have been shown to provide increased preconcentration of charged analytes due to the existence of a finite electric double layer (EDL), in which electrostatic attraction and repulsion from charged surfaces produce nonuniform transverse ion distributions. In this work, we use numerical simulations to show that one can achieve greater levels of sample accumulation by using field-effect control via wall-embedded electrodes to tailor the surface potential heterogeneity in a nanochannel with overlapped EDLs. In addition to previously demonstrated stacking and focusing mechanisms, we find that the coupling between two-dimensional ion distributions and the axial electric field under overlapped EDL conditions can generate an ion concentration polarization interface in the middle of the channel. Under an applied electric field, this interface can be used to concentrate sample ions between two stationary regions of different surface potential and charge density. Our numerical model uses the Poisson-Nernst-Planck system of equations coupled with the Stokes equation to demonstrate the phenomenon, and we discuss in detail the driving forces behind the predicted sample enhancement. The numerical velocity and salt concentration profiles exhibit good agreement with analytical results from a simplified one-dimensional area-averaged model for several limiting cases, and we show predicted amplification ratios of up to 105.

Direct evidence of ionic fluxes across ion-selective membranes: a scanning electrochemical microscopic and potentiometric study.

PubMed

Gyurcsányi, R E; Pergel, E; Nagy, R; Kapui, I; Lan, B T; Tóth, K; Bitter, I; Lindner, E

2001-05-01

Scanning electrochemical microscopy (SECM) supplemented with potentiometric measurements was used to follow the time-dependent buildup of a steady-state diffusion layer at the aqueous-phase boundary of lead ion-selective electrodes (ISEs). Differential pulse voltammetry is adapted to SECM for probing the local concentration profiles at the sample side of solvent polymeric membranes. Major factors affecting the membrane transport-related surface concentrations were identified from SECM data and the potentiometric transients obtained under different experimental conditions (inner filling solution composition, membrane thickness, surface pretreatment). The amperometrically determined surface concentrations correlated well with the lower detection limits of the lead ion-selective electrodes.

Electronegative plasma diagnostic by laser photo-detachment combined with negatively biased Langmuir probe

NASA Astrophysics Data System (ADS)

Oudini, N.; Sirse, N.; Taccogna, F.; Ellingboe, A. R.; Bendib, A.

2018-05-01

We propose a new technique for diagnosing negative ion properties using Langmuir probe assisted pulsed laser photo-detachment. While the classical technique uses a laser pulse to convert negative ions into electron-atom pairs and a positively biased Langmuir probe tracking the change of electron saturation current, the proposed method uses a negatively biased Langmuir probe to track the temporal evolution of positive ion current. The negative bias aims to avoid the parasitic electron current inherent to probe tip surface ablation. In this work, we show through analytical and numerical approaches that, by knowing electron temperature and performing photo-detachment at two different laser wavelengths, it is possible to deduce plasma electronegativity (ratio of negative ion to electron densities) α, and anisothermicity (ratio of electron to negative ion temperatures) γ-. We present an analytical model that links the change in the collected positive ion current to plasma electronegativity and anisothermicity. Particle-In-Cell simulation is used as a numerical experiment covering a wide range of α and γ- to test the new analysis technique. The new technique is sensitive to α in the range 0.5 < α < 10 and yields γ- for large α, where negative ion flux affects the probe sheath behavior, typically α > 1.

Constraining the sensitivity of iodide adduct chemical ionization mass spectrometry to multifunctional organic molecules using the collision limit and thermodynamic stability of iodide ion adducts

DOE PAGES

Lopez-Hilfiker, Felipe D.; Iyer, Siddarth; Mohr, Claudia; ...

2016-04-06

The sensitivity of a chemical ionization mass spectrometer (ions formed per number density of analytes) is fundamentally limited by the collision frequency between reagent ions and analytes, known as the collision limit, the ion–molecule reaction time, and the transmission efficiency of product ions to the detector. We use the response of a time-of-flight chemical ionization mass spectrometer (ToF-CIMS) to N 2O 5, known to react with iodide at the collision limit, to constrain the combined effects of ion–molecule reaction time, which is strongly influenced by mixing and ion losses in the ion–molecule reaction drift tube. A mass spectrometric voltage scanningmore » procedure elucidates the relative binding energies of the ion adducts, which influence the transmission efficiency of molecular ions through the electric fields within the vacuum chamber. Together, this information provides a critical constraint on the sensitivity of a ToF-CIMS towards a wide suite of routinely detected multifunctional organic molecules for which no calibration standards exist. Lastly, we describe the scanning procedure and collision limit determination, and we show results from the application of these constraints to the measurement of organic aerosol composition at two different field locations.« less

Modeling of steady-state convective cooling of cylindrical Li-ion cells

NASA Astrophysics Data System (ADS)

Shah, K.; Drake, S. J.; Wetz, D. A.; Ostanek, J. K.; Miller, S. P.; Heinzel, J. M.; Jain, A.

2014-07-01

While Lithium-ion batteries have the potential to serve as an excellent means of energy storage, they suffer from several operational safety concerns. Temperature excursion beyond a specified limit for a Lithium-ion battery triggers a sequence of decomposition and release, which can preclude thermal runaway events and catastrophic failure. To optimize liquid or air-based convective cooling approaches, it is important to accurately model the thermal response of Lithium-ion cells to convective cooling, particularly in high-rate discharge applications where significant heat generation is expected. This paper presents closed-form analytical solutions for the steady-state temperature profile in a convectively cooled cylindrical Lithium-ion cell. These models account for the strongly anisotropic thermal conductivity of cylindrical Lithium-ion batteries due to the spirally wound electrode assembly. Model results are in excellent agreement with experimentally measured temperature rise in a thermal test cell. Results indicate that improvements in radial thermal conductivity and axial convective heat transfer coefficient may result in significant peak temperature reduction. Battery sizing optimization using the analytical model is discussed, indicating the dependence of thermal performance of the cell on its size and aspect ratio. Results presented in this paper may aid in accurate thermal design and thermal management of Lithium-ion batteries.

Analytical model of radiation-induced precipitation at the surface of dilute binary alloy

NASA Astrophysics Data System (ADS)

Pechenkin, V. A.; Stepanov, I. A.; Konobeev, Yu. V.

2002-12-01

Growth of precipitate layer at the foil surface of an undersaturated binary alloy under uniform irradiation is treated analytically. Analytical expressions for the layer growth rate, layer thickness limit and final component concentrations in the matrix are derived for coherent and incoherent precipitate-matrix interfaces. It is shown that the high temperature limit of radiation-induced precipitation is the same for both types of interfaces, whereas layer thickness limits are different. A parabolic law of the layer growth predicted for both types of interfaces is in agreement with experimental data on γ '-phase precipitation at the surface of Ni-Si dilute alloys under ion irradiation. Effect of sputtering on the precipitation rate and on the low temperature limit of precipitation under ion irradiation is discussed.

SYSTEMATIC SCANNING ELECTRON MICROSCOPY TECHNIQUE FOR EVALUATING COMBINED BIOLOIGCAL/GRANULAR ACTIVATED CARBON TREATMENT PROCESSES

EPA Science Inventory

A systematic scanning election microscope analytical technique has been developed to examine granular activated carbon used a a medium for biomass attachment in liquid waste treatment. The procedure allows for the objective monitoring, comparing, and trouble shooting of combined ...

Ion Dynamics Model for Collisionless Radio Frequency Sheaths

NASA Technical Reports Server (NTRS)

Bose, Deepak; Govindan, T.R.; Meyyappan, M.

2000-01-01

Full scale reactor model based on fluid equations is widely used to analyze high density plasma reactors. It is well known that the submillimeter scale sheath in front of a biased electrode supporting the wafer is difficult to resolve in numerical simulations, and the common practice is to use results for electric field from some form of analytical sheath model as boundary conditions for full scale reactor simulation. There are several sheath models in the literature ranging from Child's law to a recent unified sheath model [P. A. Miller and M. E. Riley, J. Appl. Phys. 82, 3689 (1997)l. In the present work, the cold ion fluid equations in the radio frequency sheath are solved numerically to show that the spatiotemporal variation of ion flux inside the sheath, commonly ignored in analytical models, is important in determining the electric field and ion energy at the electrode. Consequently, a semianalytical model that includes the spatiotemporal variation of ion flux is developed for use as boundary condition in reactor simulations. This semianalytical model is shown to yield results for sheath properties in close agreement with numerical solutions.