bluuebunny/crossref_metadata_2025_split huggingface dataset:
A Commentary on Recent Developments in X-RAY Detectors and Ancillary Instrumentation and Data Extraction Algorithms
Authors: Fiori Charles E. , Swyt Carol R. 
Published: June 2020

When a lithium-drifted silicon, Si(Li), energy dispersive X-ray detector is attached to a scanning electron microscope or a scanning transmission electron microscope, it becomes possible to perform an assay of the elemental composition of a localized region of a specimen. This capability has existed now for almost 20 years. During this time, the quality of the analytical results has slowly improved with the availability of better instrumentation and increased understanding of the physical basis of measurement and matrix effects. During the last few years, the pace in both instrumental development and theoretical understanding has picked up dramatically. What seemed like a maturing and ever more mundane field has now been reinvigorated. We will catalog here and comment on several of the developments which have occurred in x-ray detectors and in the hardware and software used to process the resulting x-ray signals into quantitative information.Although the Si(Li) x-ray spectrometer has dominated the field of x-ray microanalysis for many years, recent developments in intrinsic germanium (IG) detectors have produced spectrometers which, in several important characteristics, rival or exceed those of the Si(Li) spectrometer.
Novel Dry Dispersions for Automated Scanning Electron Microscopy: Energy and Wavelength Dispersive X-RAY Spectrometry (ASEM-EDS/WDS)
Authors: Detter-Hoskin Lisa D. , Wortman Beth G. 
Published: June 2020

In recent years, the need for more precise size and chemical analysis of materials has been stressed since these features can have major effects on product performance. Historically, optical and manual scanning electron microscopy, the latter in combination with energy and wavelength dispersive x-ray spectrometry (SEM-EDS/WDS), have been used in our laboratory to size and identify the chemical composition of materials. In recent years, automated SEM-EDS/VDS methods have been developed and are likewise used for similar measurements, especially where large sets of particle information are desired.The inherent success of ASEM-EDS/WDS critically depends on sample preparation. Particle dispersion criteria include: 1) a smooth substrate, free of defects, 2) a uniform distribution of particles, and 3) proper density of particle loading. Traditionally, particles have been suspended and homogenized in liquid media and then either filtered through membrane filters or aliquots directly dispersed onto highly polished carbon planchets. While wet dispersions are applicable to a wide array of materials, in the case of complex materials, alternative dry dispersion protocols are necessary.
Structure Change of Crystalline Graphite Due to Hydrogen Ion Irradiation Observed by In-Situ Electron Energy Loss Spectroscopy
Authors: Kushita Kouhei , Hojou Kiichi 
Published: June 2020

Carbon materials such as isotropic graphite and C/C composite are widely used for first walls or divertor plates in fusion reactors such as JT-60. In this respect, as well as from fundamental viewpoints, observations of microstructural change in ion-irradiated graphite is important. Although radiation damage in carbon materials has widely been studied, there are few data in this field examined by Electron Energy Loss Spectroscopy. The present paper reports the results of in-situ EELS observation of ion-irradiated crystalline graphite.Specimens used in this experiment were pseudo-monocrystal graphite supplied from Le Carbone Lorraine. Thin films of the graphite suitable for transmission electron microscopy were made by crashing a small portion of the sample in a mortar with npropyl alcohol. The resultant flake-like thin films were scooped up with a micro mesh, and then irradiated with 10 keV ions at an ambient temperature with a flux of 6.3×1013H/cm2s. The apparatus schematically shown in Fig.1 was used for the ion irradiation as well as for electron microscopy and electron energy loss spectroscopy.
High-efficiency x-ray monochromator for measurement of Ca in the TEM
Authors: Sun Songquan , Tormey John McD. , Wittry David B. 
Published: June 2020

A novel miniature wavelength dispersive (WDS) monochromator with a LiF crystal has been developed for use in a transmission electron microscope (JEOL 100CX). Our goal has been to improve on the limited sensitivity available when energy dispersive spectrometry (EDS) is used to measure low concentrations of Ca in biological tissues. This paper presents the calculated performance, design features and experimental results .Limitations of EDS - When EDS is used to measure biological Ca in an electron column instrument, precision is severely limited by counting statistics. In the past, EDS was used by Tormey to quantify Ca in cardiac muscle, employing procedures similar to those used by Shuman and Somlyo. In a typical application, myofibrillar [Ca] increased from 1.4 ± 0.2 to 2.6 ± 0.3 mmol/kg dry wt when going from rest to contracture. This precision (± standard error of mean) was the result of 125 measurements in each condition.
Low-cost system for electron probe microanalysis based on a personal computer
Authors: Foster Margaret C. , Saubermann Albert J. 
Published: June 2020

The development of personal computers increases the options available for electron probe microanalysis. Hardware and software are now available for personal computers which make it feasible to use them to acquire, process, and analyze x-ray spectra. One advantage of a personal computer (PC) based system is the low cost--approximately 20% of the cost of other options. A second advantage is that a system can be developed which is tailored to the needs of the laboratory, so that experimental questions asked of the data can dictate procedures for data acquisition and processing.We have developed a PC-based system for electron probe microanalysis, which we use for data acquisition, processing, and analysis of frozen and freeze-dried biological samples. X-ray spectra may be acquired either for spot analysis or for elemental images. Spectra acquired from large areas of the frozen, hydrated sample are used together with spectra from the freeze-dried specimen to calculate concentrations relative to sample wet weight.
Atrial specific granules: The intracellular calcium store
Authors: Zhong Cisheng , Yu Zhang , Yu Wenqian , Ling Yiping 
Published: June 2020

It is well known that certain organells in cytosol contain high calcium concentration and they are named intracellular Ca stores. These stores regulate the intracellular Ca concentration. The present project aims at exploring whether the release of atrial natriuretic peptide (ANP) from the atrial specific granules(ASG) is dependent on the release of calcium from the ASG. For this purpose, we have to know first whether the ASG contain high Ca concentration. In this work, positive results were obtained by quantitative electron probe x ray microanalysis (EPMA) and Ca-ATPase cytochemical localization.Adult female Sprague Dawley rats were used. The auricle samples were prepared in five different procedures: 1 )preparation of routine ultrathin sections; 2)ethanolic phosphotungstic acid(EPTA) staining ultrathin sections for ASG showing; [1] 3) cytochemical localization of Ca-ATPase ;[2] 4) preparation of ultrathin cryosections of fresh rapid frozen auricles; [3] 5) quantitative EPMA with Link AN10000 and Link Quantem/FLS quantitative analysis software.
Electron-probe x-ray microanalysis studies on the intracellular calcium translocation during the contraction-relaxation cycle in the fish swimbladder muscle
Authors: Suzuki Suechika , Hino Naoki , Sugi Haruo 
Published: June 2020

The swimbladder muscle of a teleost fish,Sebasticus marmoratus, contracts rapidly to produce sounds for communication and contains extremely well developed sarcoplasmic reticulum (SR), providing a material suitable for studying the intracellular Ca translocation during the contraction-relaxation cycle. We examined the change of Ca distribution along the sarcomere at various states of the fibers during the contractionrelaxation cycle in the swimbladder muscle by means of quantitative electron probe X-ray microanalysis of cryosections.The muscle fibers were rapidly frozen at rest, during sustained contraction and at 0.1 and 1.0 sec after the onset of relaxation with a dual-jet liquid propane freezing device. Cryosections (200 nm thick) were cut from the middle portion of the frozen fibers at -110°C on a LKB NOVA cryoultramicrotome, and placed on thin carbon supporting films on Nigrids. Then the cryosections were freeze-dried at 10-6torr and below -80°C. Electron probe X-ray microanalysis was performed on a liquid N2-cooled Be-stage at -130°C in a JEOL 2000FX electron microscope operated at 80 kV and equipped with a Tracor Northern TN5500 energy dispersive X-ray microanalyzer.
Spectroscopy imaging of involvement of sugar residues in adhesion step and interiorization of T. Cruzi heart muscle cells by lectin binding
Authors: Santos Barbosa Helene , Goldenberg Samuel , de Nazareth Mariä , Meirelles L. 
Published: June 2020

The high percentage of adhesion and interiorization of metacyclic trypomastigotes (clone Dm28c) of T. cruzi obtained from TAU3AAG differentiation medium (1) to heart muscle cells (HMC) points out this system as a very suitable to study the involvment of membrane components during the recognition and endocytosis process leading to formation of endocytic vacuole (2).In this report, we used the lectin Ricinus communis (RCA I) and Triticum vulgaris (WGA) as markers of galactosyl and N-acetyl-D-glucosamine or N-acetyl-neuraminic acid residues, respectivily, from host cell for studies of involvment in the attachment and interiorization of parasite. In order to investigate the localization of these sugars residues on the surface of HMC, we incubated the cells in the presence of RCA conjugated with ferritin (50 μg/ml) and WGA with gold particles at 42C for 30 min. The cell cultures were washed, infected T. cruzi, for 2-4 hours, fixed and processed for TEM.
Cryogenic cooling and in situ analysis of fluid inclusions in geological materials with an ultra-thin windowed Si(Li) detector in a SEM
Authors: Griffin Brendon 
Published: June 2020

The determination of fluid compositions in geological processes is an essential but difficult problem. Many techniques have been developed based on the optical microscope. These are indirect analytical techniques, determining fluid composition by analogy. More sophisticated spectroscopic techniques, e.g. laser microprobes, are relatively inaccessible through high capital cost. Scanning electron microscopes [SEM’s] and electron microprobes have been used to identify the non-volatile components by decrepitating near-surface inclusions with an energetic electron beam and then analysing the residual.It is found that application of the cryo-SEM to the study of fluid inclusions with the common availability of windowless and low absorbance windowed Si(Li) detectors is a convenient and low cost technique. Suitable slabs (<1 mm) are frozen and then fractured. No coating is applied, to minimise element interference. The fresh surfaces are inspected using backscattered electron [BSE] imaging and exposed inclusions analysed.Studies of inclusions in quartz, fluorite and sphalerite have determined the presence of carbon dioxide, water and various daughter salts, including halite (NaCl) and hydrophilite (CaCl2).
Electron probe microanalysis of borophosphosilicate coatings
Authors: Willich Peter , Schiffmann Kirsten 
Published: June 2020

Planarization and passivation of integrated circuits by use of borophosphosilicate glass (BPSG) is of considerable technological interest. BPSG is prepared by chemical vapour deposition and electron probe microanalysis (EPMA) offers the possibility of non-destructive characterization in respect of composition and film thickness. Particular difficulties of EPMA are due to the insulating character of BPSG in combination with the demand for analysis of ultra-light elements (B and O). However, EPMA of BPSG also demonstrates the accuracy of recent bulk and thin film data processing when based on refined experimental procedures.Carbon coating is required to carry out reproducible measurements on BPSG. The C-Kα intensity determined on various samples and mineral standards (Table 1) shows a wide variation of the carbon film thickness (10-40 nm), even when a set of samples was simultaneously coated. The film thickness of BPSG is in the range of 0.3-1.5 μm and consequently EPMA has to be performed at a low electron energy (Eo= 4-10 keV) to enable ‘bulk’ quantitative analysis without influence of the silicon substrate.
Application Of Electron Probe Analyses Of Minerals In Discussing The Relationship Between Ductile Deformation And Metamorphism
Authors: Guochuan Fan , Zhongshi Sun 
Published: June 2020

Under influence of ductile shear deformation, granulite facies mineral paragenesis underwent metamorphism and changes in chemical composition. The present paper discusses some changes in chemical composition of garnet in hypers thene_absent felsic gnesiss and of hypersthene in rock in early and late granulite facies undergone increasing ductile shear deformation .In garnet fetsic geniss, band structures were formed because of partial melting and resulted in zoning from massive⟶transitional⟶melanocrate zones in increasing deformed sequence. The electron-probe analyses for garnet in these zones are listed in table 1 . The Table shows that Mno, Cao contents in garnet decrease swiftly from slightly to intensely deformed zones.In slightly and moderately deformed zones, Mgo contents keep unchanged and Feo is slightly lower. In intensely deformed zone, Mgo contents increase, indicating a higher temperature. This is in accord with the general rule that Mgo contents in garnet increase with rising temperature.
Microanalyses Of Structural Defects In Polymer-Derived Ceramic Fibers
Authors: Freeman H. A. , Rabe J. A. 
Published: June 2020

Microanalyses were performed with a Cameca MBX scanning electron microprobe and a JEM 2000FX analytical electron microscope to determine the composition of foreign defect structures found on primary fracture surfaces of ceramic fibers derived from melt-spun Si-N-C-O polymeric precursors. The defects were the critical flaws responsible for deterioration of tensile strength in these fibers after thermal exposure in the range of 1400°C and above. High fiber strength is necessary to provide reinforcement and toughening in structural ceramic composites during high temperature use.Among the defects found were roughly spherical internal nodular flaws which contained Pb (Fig. 1) as well as others (Fig. 2) containing both Pb and Sn. Granular aggregates were also seen in which Fe and Cr were detected. Other nodular surface defects contained Ca, minor Al, and levels of 0 higher than that in the surrounding fiber (Fig. 3) . Extremely fine whisker growths at discrete sites along the length of some fibers were identified as silicon oxynitride by electron diffraction.
In Situ Ion Beam Cleaning in a Cambridge S-200 SEM
Authors: Laabs F.C. 
Published: June 2020

The increased use of the scanning electron microscope as a flexible analytical tool has resulted in applying its use to a variety of problems which utilize signals that originate or are controlled by surface properties, including crystallographic orientation, contamination and structural deformation of the surface layer. This paper describes results and observations of efforts to control and remove that layer by energetic argon ion bombardment.Experimental
A Kratos Mini-Beam I ion gun was attached to a Cambridge Model S-200 scanning electron microscope utilizing the horizontal port normally occupied by an energy dispersive spectrometer (Figure 1). The EDS spectrometer was moved to a position 35 degrees above the port position. This configuration results in the ion gun lying in a plane perpendicular to the electron beam and 45 degrees to the tilt axis, necessitating tilting the sample toward the ion beam during ion bombardment and, importantly, sputtered material is directed away from the EDS detector.
Recent Advances In The Analysis And Interpretation Of C-O-H-N Fluids By Application Of Laser Raman Microspectroscopy
Authors: Dill Pasteris Jill , Seitz Jeffery C. , Wopenka Brigitte , Chou I-Ming 
Published: June 2020

One of the major goals of a geologist is to infer, from his field and laboratory observations, the temperature, pressure, and compositional parameters of the ambient system during rock formation or ore deposition. Because fluids are actively involved in many rock-forming processes, fluid inclusions trapped within minerals are studied as evidence of the pertinent system parameters. Individual minerals may contain several generations of fluid inclusions due to the complex histories of many geological environments. Micro-analytical techniques for the measurement of small quantities of materials in individual inclusions on the order of a few micrometers in diameter therefore are required.The classical technique is microthermometry, which involves monitoring phase changes in an inclusion during controlled cooling and heating on a microscope stage. Given appropriate phase diagrams (not available in many cases) for the chemical system under study, the phase changes at recorded temperatures can be interpreted in terms of a specific fluid composition and density.
Interlaboratory study of the accuracy of airborne asbestos analysis by TEM
Authors: Turner S. , Steel E.B. , Beard M.E. 
Published: June 2020

The determination of the concentration of asbestos in air or water is a goal common to research laboratories conducting environmental and health related studies and to commercial laboratories involved in asbestos abatement projects. The analytical procedure is a multistep process in which 1) particles from a known volume of air or water are deposited onto the surface and/or interior of a filtering media, 2) the particles are transferred to a carbon film suitable for TEM analysis and 3) a known area of the carbon film is systematically traversed and particles of interest identified by use of the TEM. In this work, an interlaboratory study was conducted to determine the accuracy and problems encountered by operators performing the electron microscope analysis.Chrysotile and nonasbestos particles were deposited onto a 37 mm polycarbonate filter from a freon-based solution. Grid sections suitable for electron microscope analysis were prepared from the filter and sent to eighteen commercial laboratories.
Fluidized Catalytic Cracking Catalyst Microstructure as Determined by A Scanning Ion Microprobe
Authors: Lampert J.K. , Koermer G.S. , Macaoy J.M. , Chabala J.M. , Levi-Setti R. 
Published: June 2020

We have used high spatial resolution imaging secondary ion mass spectrometry (SIMS) to differentiate mineralogical phases and to investigate chemical segregations in fluidized catalytic cracking (FCC) catalyst particles. The oil industry relies on heterogeneous catalysis using these catalysts to convert heavy hydrocarbon fractions into high quality gasoline and fuel oil components. Catalyst performance is strongly influenced by catalyst microstructure and composition, with different chemical reactions occurring at specific types of sites within the particle. The zeolitic portions of the particle, where the majority of the oil conversion occurs, can be clearly distinguished from the surrounding silica-alumina matrix in analytical SIMS images.The University of Chicago scanning ion microprobe (SIM) employed in this study has been described previously. For these analyses, the instrument was operated with a 40 keV, 10 pA Ga+ primary ion probe focused to a 30 nm FWHM spot. Elemental SIMS maps were obtained from 10×10 μm2 areas in times not exceeding 524s.
Applications of Time-OF-Flight Secondary Ion Mass Spectrometry (TOF-SIMS)
Authors: Schueler Bruno , Odom Robert W. 
Published: June 2020

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) provides unique capabilities for elemental and molecular compositional analysis of a wide variety of surfaces. This relatively new technique is finding increasing applications in analyses concerned with determining the chemical composition of various polymer surfaces, identifying the composition of organic and inorganic residues on surfaces and the localization of molecular or structurally significant secondary ions signals from biological tissues. TOF-SIMS analyses are typically performed under low primary ion dose (static SIMS) conditions and hence the secondary ions formed often contain significant structural information.This paper will present an overview of current TOF-SIMS instrumentation with particular emphasis on the stigmatic imaging ion microscope developed in the authors’ laboratory. This discussion will be followed by a presentation of several useful applications of the technique for the characterization of polymer surfaces and biological tissues specimens. Particular attention in these applications will focus on how the analytical problem impacts the performance requirements of the mass spectrometer and vice-versa.
The Connective Tissue Matrix of Cartilage as Revealed by Standard Fixation, Ruthenium Staining, High-Pressure Freezing, and Embedding in Water Soluble Media: A Comparison of Methods
Authors: Keene Douglas R. 
Published: June 2020

Proteoglycan is a major component of the cartilage extracellular matrix, and the overall structure of this anionic molecule is highly dependent on the hydrated environment of cartilage. Without specific stabilization, proteoglycans are extracted or collapsed during deydration while processing for electron microscopy. The purpose of these experiments is to determine a method by which the structure of proteoglycans might be stabilized for electron microscopic evaluation.Chick sternal cartilage was prepared for transmission electron microscopy by the following methods and the resultant tissue ultrastructure compared: A) 1.5/1.5% gluteraldehyde/paraformaldehyde and 1% OsO4 fixation, dehydration in ethanol, propylene oxide, and embedding in Spurrs epoxy B) Fixation as in (A) directly followed by infiltration and embedding in Hexamethylol-melamine-methyl-ether (a water soluble embedding medium) trade name “nanoplast” C) Fixation by high pressure freezing followed by freeze substitution in acetone/OsO4 prior to embedding in epon 812. In variations of methods A and B above, ruthenium red (RR, 1500 ppm) or ruthenium hexamine trichloride (RHT, 6000 ppm) were added to the primary and secondary fixatives. All tissue sections were stained in uranyl acetate and lead citrate.
The Contributions Of Analytical Electron Microscopy to the Detection and Quantification of Asbestos in Human Lung Samples
Authors: Roggli Victor L. 
Published: June 2020

Analytical electron microscopy has contributed a great deal to our understanding of asbestosrelated diseases. Exposure to the various forms of asbestos, which include the serpentine form known as chrysotile asbestos, and the amphibole forms referred to as amosite, crocidolite, tremolite, anthophyllite, and actinolite asbestos, has been associated with the development of a number of diseases in man. These include asbestosis (scarring of the lung parenchyma), pleural plaques (scarring of the pleura), malignant mesothelioma of the pleura and peritoneum, and carcinoma of the lung, especially among those who also smoke cigarettes.Analysis of the mineral fiber content of the lung in patients with these various diseases has provided a powerful investigative tool to researchers interested in the relationship between fiber burdens and disease. Such studies have shown that when sufficiently sensitive digestion concentration techniques are employed, some asbestos can be found in lung tissue from virtually every adult in the general population.