scholarly journals Airborne nanoparticle collection efficiency of a TEM grid-equipped sampling system

Author(s):  
Maiqi Xiang ◽  
Martin Morgeneyer ◽  
Olivier Aguerre-Chariol ◽  
Florian Philippe ◽  
Christophe Bressot
2019 ◽  
Vol 12 (2) ◽  
pp. 1141-1154 ◽  
Author(s):  
Kazuki Kamezaki ◽  
Shohei Hattori ◽  
Enno Bahlmann ◽  
Naohiro Yoshida

Abstract. Knowledge related to sulfur isotope ratios of carbonyl sulfide (OCS or COS), the most abundant atmospheric sulfur species, remains scarce. An earlier method developed for sulfur isotopic analysis for OCS using S+ fragmentation by an isotope ratio mass spectrometer is inapplicable for ambient air samples because of the large samples required (approx. 500 L of 500 pmol mol−1 OCS). To overcome this difficulty, herein we present a new sampling system for collecting approximately 10 nmol of OCS from ambient air coupled with a purification system. Salient system features are (i) accommodation of samples up to 500 L (approx. 10 nmol) of air at 5 L min−1; (ii) portability of adsorption tubes (1∕4 in. (0.64 cm) outer diameter, 17.5 cm length, approximately 1.4 cm3 volume) for preserving the OCS amount and δ34S(OCS) values at −80 ∘C for up to 90 days and 14 days; and (iii) purification OCS from other compounds such as CO2. We tested the OCS collection efficiency of the systems and sulfur isotopic fractionation during sampling. Results show precision (1σ) of δ34S(OCS) values as 0.4 ‰ for overall procedures during measurements for atmospheric samples. Additionally, this report presents diurnal variation of δ34S(OCS) values collected from ambient air at the Suzukakedai campus of the Tokyo Institute of Technology located in Yokohama, Japan. The observed OCS concentrations and δ34S(OCS) values were, respectively, 447–520 pmol mol−1 and from 10.4 ‰ to 10.7 ‰ with a lack of diurnal variation. The observed δ34S(OCS) values in ambient air differed greatly from previously reported values of δ34S(OCS) = (4.9±0.3) ‰ for compressed air collected at Kawasaki, Japan, presumably because of degradation of OCS in cylinders and collection processes for that sample. The difference of atmospheric δ34S(OCS) values between 10.5 ‰ in Japan (this study) and ∼13 ‰ recently reported in Israel or the Canary Islands indicates that spatial and temporal variation of δ34S(OCS) values is expected due to a link between anthropogenic activities and OCS cycles. The system presented herein is useful for application of δ34S(OCS) for investigation of OCS sources and sinks in the troposphere to elucidate its cycle.


2018 ◽  
Author(s):  
Kazuki Kamezaki ◽  
Shohei Hattori ◽  
Enno Bahlmann ◽  
Naohiro Yoshida

Abstract. Knowledge related to sulfur isotopic composition of carbonyl sulphide (OCS or COS), the most abundant atmospheric sulfur species, remains scarce. Earlier method developed for sulfur isotopic analysis for OCS using S+ fragmentation is inapplicable for ambient air samples because of the large samples required (approx. 500 L of 500 pmol mol−1 OCS). To overcome this difficulty, herein we present a new sampling system for collecting approx. 10 nmol of OCS from ambient air coupled with a purification system. Salient system features are (i) accommodation of samples up to 500 L (= approx. 10 nmol) of air at 5 L min−1, (ii) portability of 7 inch tubes (approx. 1 cm3) for preserving samples, and (iii) purification OCS from other compounds such as CO2. We tested the OCS collection efficiency of the systems and sulfur isotopic fractionation during sampling. Results show precision (1σ) of δ33S(OCS), δ34S(OCS), and Δ33S(OCS) values, respectively, as 0.4 ‰, 0.2 ‰, and 0.4 ‰. Additionally, this report presents diurnal variation of δ34S(OCS) values collected from ambient air at Suzukakedai campus of Tokyo Institute of Technology located in Yokohama, Japan. The observed OCS concentrations and δ34S(OCS) values were, respectively, 447–520 pmol mol−1 and from 10.4 ‰ to 10.7 ‰. No significant difference was found between values obtained during the day and night. The observed δ34S(OCS) values in ambient air differed greatly from previously reported values ((4.9 ± 0.3) ‰) for compressed air collected at Kawasaki, Japan, presumably because of sampling conditions and collection processes for that sample. Consequently, previous values of δ34S(OCS) = (4.9 ± 0.3) ‰ were not representative samples for a global signal. When considering (10.5 ± 0.4) ‰ is postulated as the global signal of δ34S(OCS), this revised δ34S(OCS) value is consistent with previous estimation based on terrestrial and oceanic sulfur sources. The δ34S(OCS) value explains the reported δ34S(OCS) values for background stratospheric sulfate. The system presented herein is useful for application of δ34S(OCS) for investigation of OCS sources and sinks in the troposphere to elucidate its cycle and its contribution to background stratospheric sulfate.


Author(s):  
H. Rose

The scanning transmission electron microscope offers the possibility of utilizing inelastically scattered electrons. Use of these electrons in addition to the elastically scattered electrons should reduce the scanning time (dose) Which is necessary to keep the quantum noise below a certain level. Hence it should lower the radiation damage. For high resolution, Where the collection efficiency of elastically scattered electrons is small, the use of Inelastically scattered electrons should become more and more favorable because they can all be detected by means of a spectrometer. Unfortunately, the Inelastic scattering Is a non-localized interaction due to the electron-electron correlation, occurring predominantly at the circumference of the atomic electron cloud.


Author(s):  
P.E. Batson

Use of the STEM to obtain precise electronic information has been hampered by the lack of energy loss analysis capable of a resolution and accuracy comparable to the 0.3eV energy width of the Field Emission Source. Recent work by Park, et. al. and earlier by Crewe, et. al. have promised magnetic sector devices that are capable of about 0.75eV resolution at collection angles (about 15mR) which are great enough to allow efficient use of the STEM probe current. These devices are also capable of 0.3eV resolution at smaller collection angles (4-5mR). The problem that arises, however, lies in the fact that, even with the collection efficiency approaching 1.0, several minutes of collection time are necessary for a good definition of a typical core loss or electronic transition. This is a result of the relatively small total beam current (1-10nA) that is available in the dedicated STEM. During this acquisition time, the STEM acceleration voltage may fluctuate by as much as 0.5-1.0V.


Author(s):  
J. R. Michael

X-ray microanalysis in the analytical electron microscope (AEM) refers to a technique by which chemical composition can be determined on spatial scales of less than 10 nm. There are many factors that influence the quality of x-ray microanalysis. The minimum probe size with sufficient current for microanalysis that can be generated determines the ultimate spatial resolution of each individual microanalysis. However, it is also necessary to collect efficiently the x-rays generated. Modern high brightness field emission gun equipped AEMs can now generate probes that are less than 1 nm in diameter with high probe currents. Improving the x-ray collection solid angle of the solid state energy dispersive spectrometer (EDS) results in more efficient collection of x-ray generated by the interaction of the electron probe with the specimen, thus reducing the minimum detectability limit. The combination of decreased interaction volume due to smaller electron probe size and the increased collection efficiency due to larger solid angle of x-ray collection should enhance our ability to study interfacial segregation.


Author(s):  
P. E. Batson

In recent years,instrumentation for electron energy loss spectroscopy (EELS) has been steadily improved to increase energy resolution and collection efficiency. At present 0.40eV at 10mR collection half angle is available with commercial magnetic sectors (e.g. Gatan, Inc. and VG Microscopes, Ltd.), and 70meV at 10mR has been demonstrated by use of a Wien filter within a large deceleration field. When these high resolution spectrometers are coupled to the modern small electron probe instrument, we obtain a tool which promises to reveal local changes in bandstructure and bonding near defects and interfaces in heterogeneous materials.Unfortunately, typical electron sources have intrinsic energy widths which limit attainable spectroscopic resolution in the absence of some monochromation system. For instance, the W thermal emitter has a half width of about 1eV.


Author(s):  
A. Buczkowski ◽  
Z. J. Radzimski ◽  
J. C. Russ ◽  
G. A. Rozgonyi

If a thickness of a semiconductor is smaller than the penetration depth of the electron beam, e.g. in silicon on insulator (SOI) structures, only a small portion of incident electrons energy , which is lost in a superficial silicon layer separated by the oxide from the substrate, contributes to the electron beam induced current (EBIC). Because the energy loss distribution of primary beam is not uniform and varies with beam energy, it is not straightforward to predict the optimum conditions for using this technique. Moreover, the energy losses in an ohmic or Schottky contact complicate this prediction. None of the existing theories, which are based on an assumption of a point-like region of electron beam generation, can be used satisfactorily on SOI structures. We have used a Monte Carlo technique which provide a simulation of the electron beam interactions with thin multilayer structures. The EBIC current was calculated using a simple one dimensional geometry, i.e. depletion layer separating electron- hole pairs spreads out to infinity in x- and y-direction. A point-type generation function with location being an actual location of an incident electron energy loss event has been assumed. A collection efficiency of electron-hole pairs was assumed to be 100% for carriers generated within the depletion layer, and inversely proportional to the exponential function of depth with the effective diffusion length as a parameter outside this layer. A series of simulations were performed for various thicknesses of superficial silicon layer. The geometries used for simulations were chosen to match the "real" samples used in the experimental part of this work. The theoretical data presented in Fig. 1 show how significandy the gain decreases with a decrease in superficial layer thickness in comparison with bulk material. Moreover, there is an optimum beam energy at which the gain reaches its maximum value for particular silicon thickness.


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