scholarly journals Dynamic range multiwavelength particle characterization using analytical ultracentrifugation

Nanoscale ◽  
2016 ◽  
Vol 8 (14) ◽  
pp. 7484-7495 ◽  
Author(s):  
Johannes Walter ◽  
Wolfgang Peukert
Keyword(s):  
Dynamic Range ◽  
Analytical Ultracentrifugation ◽  
Particle Characterization

Insight into protein–protein interactions from analytical ultracentrifugation

2010 ◽  
Vol 38 (4) ◽  
pp. 901-907 ◽  
Author(s):  
Stephen E. Harding ◽  
Arthur J. Rowe
Keyword(s):  
Protein Interactions ◽  
Dynamic Range ◽  
Analytical Ultracentrifugation ◽  
Dissociation Constants ◽  
Interaction Strength ◽  
Sedimentation Equilibrium ◽  
Solution Technique ◽  
Protein Protein Interactions ◽  
Self Association ◽  
Made In

Analytical ultracentrifugation is a free solution technique with no supplementary immobilization, columns or membranes required, and can be used to study self-association and hetero-interactions, stoichiometry, reversibility and interaction strength across a very large dynamic range (dissociation constants from 10−12 M to 10−1 M). In the present paper, we review some of the advances that have been made in the two different types of sedimentation experiment – sedimentation equilibrium and sedimentation velocity – for the analysis of protein–protein interactions and indicate how major complications such as thermodynamic and hydrodynamic non-ideality can be dealt with.

The Nature of Rapidly Extracted Phycocyanin from the Blue-Green Alga Plectonema Boryanum

1971 ◽  
Vol 29 ◽  
pp. 366-367
Author(s):  
M. Kessel ◽  
R. MacColl
Keyword(s):  
Self Assembly ◽  
Analytical Ultracentrifugation ◽  
Uranyl Acetate ◽  
The Self ◽  
Major Protein ◽  
Subunit Structure ◽  
Blue Green Alga ◽  
Thin Sections ◽  
Blue Green Algae ◽  
Cacodylate Buffer

The major protein of the blue-green algae is the biliprotein, C-phycocyanin (Amax = 620 nm), which is presumed to exist in the cell in the form of distinct aggregates called phycobilisomes. The self-assembly of C-phycocyanin from monomer to hexamer has been extensively studied, but the proposed next step in the assembly of a phycobilisome, the formation of 19s subunits, is completely unknown. We have used electron microscopy and analytical ultracentrifugation in combination with a method for rapid and gentle extraction of phycocyanin to study its subunit structure and assembly.To establish the existence of phycobilisomes, cells of P. boryanum in the log phase of growth, growing at a light intensity of 200 foot candles, were fixed in 2% glutaraldehyde in 0.1M cacodylate buffer, pH 7.0, for 3 hours at 4°C. The cells were post-fixed in 1% OsO4 in the same buffer overnight. Material was stained for 1 hour in uranyl acetate (1%), dehydrated and embedded in araldite and examined in thin sections.

Particle characterization of CVD tungsten metallization for 64 MBIT DRAM

1991 ◽  
Vol 49 ◽  
pp. 896-897
Author(s):  
Marylyn Bennett-Lilley ◽  
Thomas T.H. Fu ◽  
David D. Yin ◽  
R. Allen Bowling
Keyword(s):  
Chemical Vapor ◽  
Device Performance ◽  
Particle Characterization ◽  
Particle Generation ◽  
Tungsten Hexafluoride ◽  
Homogeneous Particle ◽  
Multiple Levels ◽  
Circuit Density ◽  
Sources Of Contamination

Chemical Vapor Deposition (CVD) tungsten metallization is used to increase VLSI device performance due to its low resistivity, and improved reliability over other metallization schemes. Because of its conformal nature as a blanket film, CVD-W has been adapted to multiple levels of metal which increases circuit density. It has been used to fabricate 16 MBIT DRAM technology in a manufacturing environment, and is the metallization for 64 MBIT DRAM technology currently under development. In this work, we investigate some sources of contamination. One possible source of contamination is impurities in the feed tungsten hexafluoride (WF6) gas. Another is particle generation from the various reactor components. Another generation source is homogeneous particle generation of particles from the WF6 gas itself. The purpose of this work is to investigate and analyze CVD-W process-generated particles, and establish a particle characterization methodology.

Slow-Scan CCD Observation of Backscattering Patterns in SEM

1992 ◽  
Vol 50 (2) ◽  
pp. 1308-1309
Author(s):  
F. Ouyang ◽  
D. A. Ray ◽  
O. L. Krivanek
Keyword(s):  
Electron Beam ◽  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Dynamic Range ◽  
High Sensitivity ◽  
Lens System ◽  
Wide Dynamic Range ◽  
Peltier Cooler ◽  
Diffraction Patterns ◽  
Scanning Electron

Electron backscattering Kikuchi diffraction patterns (BKDP) reveal useful information about the structure and orientation of crystals under study. With the well focused electron beam in a scanning electron microscope (SEM), one can use BKDP as a microanalysis tool. BKDPs have been recorded in SEMs using a phosphor screen coupled to an intensified TV camera through a lens system, and by photographic negatives. With the development of fiber-optically coupled slow scan CCD (SSC) cameras for electron beam imaging, one can take advantage of their high sensitivity and wide dynamic range for observing BKDP in SEM.We have used the Gatan 690 SSC camera to observe backscattering patterns in a JEOL JSM-840A SEM. The CCD sensor has an active area of 13.25 mm × 8.83 mm and 576 × 384 pixels. The camera head, which consists of a single crystal YAG scintillator fiber optically coupled to the CCD chip, is located inside the SEM specimen chamber. The whole camera head is cooled to about -30°C by a Peltier cooler, which permits long integration times (up to 100 seconds).

Quantitative energy-filtered electron diffraction

1994 ◽  
Vol 52 ◽  
pp. 992-993
Author(s):  
R. Vincent
Keyword(s):  
Electron Diffraction ◽  
Inelastic Scattering ◽  
Dynamic Range ◽  
Electron Optics ◽  
Surface Layers ◽  
High Brightness ◽  
Inclined Surfaces ◽  
Perfect Symmetry ◽  
Amorphous Surface ◽  
The Ideal

Microanalysis and diffraction on a sub-nanometre scale have become practical in modern TEMs due to the high brightness of field emission sources combined with the short mean free paths associated with both elastic and inelastic scattering of incident electrons by the specimen. However, development of electron diffraction as a quantitative discipline has been limited by the absence of any generalised theory for dynamical inelastic scattering. These problems have been simplified by recent innovations, principally the introduction of spectrometers such as the Gatan imaging filter (GIF) and the Zeiss omega filter, which remove the inelastic electrons, combined with annual improvements in the speed of computer workstations and the availability of solid-state detectors with high resolution, sensitivity and dynamic range.Comparison of experimental data with dynamical calculations imposes stringent requirements on the specimen and the electron optics, even when the inelastic component has been removed. For example, no experimental CBED pattern ever has perfect symmetry, departures from the ideal being attributable to residual strain, thickness averaging, inclined surfaces, incomplete cells and amorphous surface layers.

Direct measurement of electron-diffraction-pattern intensities using an energy loss spectrometer

1989 ◽  
Vol 47 ◽  
pp. 668-669
Author(s):  
A. G. Jackson ◽  
M. Rowe
Keyword(s):  
Thermal Effects ◽  
Dynamic Range ◽  
Scattering Amplitude ◽  
Dynamical Theory ◽  
Site Symmetry ◽  
Proof Of Concept ◽  
Parallel Acquisition ◽  
Kinematic Approximation ◽  
Speed Up ◽  
Structure Calculations

Diffraction intensities from intermetallic compounds are, in the kinematic approximation, proportional to the scattering amplitude from the element doing the scattering. More detailed calculations have shown that site symmetry and occupation by various atom species also affects the intensity in a diffracted beam. [1] Hence, by measuring the intensities of beams, or their ratios, the occupancy can be estimated. Measurement of the intensity values also allows structure calculations to be made to determine the spatial distribution of the potentials doing the scattering. Thermal effects are also present as a background contribution. Inelastic effects such as loss or absorption/excitation complicate the intensity behavior, and dynamical theory is required to estimate the intensity value.The dynamic range of currents in diffracted beams can be 104or 105:1. Hence, detection of such information requires a means for collecting the intensity over a signal-to-noise range beyond that obtainable with a single film plate, which has a S/N of about 103:1. Although such a collection system is not available currently, a simple system consisting of instrumentation on an existing STEM can be used as a proof of concept which has a S/N of about 255:1, limited by the 8 bit pixel attributes used in the electronics. Use of 24 bit pixel attributes would easily allowthe desired noise range to be attained in the processing instrumentation. The S/N of the scintillator used by the photoelectron sensor is about 106 to 1, well beyond the S/N goal. The trade-off that must be made is the time for acquiring the signal, since the pattern can be obtained in seconds using film plates, compared to 10 to 20 minutes for a pattern to be acquired using the digital scan. Parallel acquisition would, of course, speed up this process immensely.

Development of imaging plate for a TEM and its characteristics

1989 ◽  
Vol 47 ◽  
pp. 100-101
Author(s):  
N. Mori ◽  
T. Oikawa ◽  
Y. Harada ◽  
J. Miyahara ◽  
T. Matsuo
Keyword(s):  
Dynamic Range ◽  
Protective Layer ◽  
High Sensitivity ◽  
Imaging Plate ◽  
Phosphor Layer ◽  
Imaging Device ◽  
X Ray Imaging ◽  
New Type ◽  
Basic Characteristics ◽  
Reading System

The Imaging Plate (IP) is a new type imaging device, which was developed for diagnostic x ray imaging. We have reported that usage of the IP for a TEM has many merits; those are high sensitivity, wide dynamic range, and good linearity. However in the previous report the reading system was prototype drum-type-scanner, and IP was also experimentally made, which phosphor layer was 50μm thick with no protective layer. So special care was needed to handle them, and they were used only to make sure the basic characteristics. In this article we report the result of newly developed reading, printing system and high resolution IP for practical use. We mainly discuss the characteristics of the IP here. (Precise performance concerned with the reader and other system are reported in the other article.)Fig.1 shows the schematic cross section of the IP. The IP consists of three parts; protective layer, phosphor layer and support.

Slow-scan CCD cameras and low-dose High-Resolution Electron Microscopy: Direct and quantitative

1994 ◽  
Vol 52 ◽  
pp. 412-413
Author(s):  
M. Pan
Keyword(s):  
Electron Microscopy ◽  
High Resolution ◽  
Structural Damage ◽  
Low Dose ◽  
Dynamic Range ◽  
High Resolution Electron Microscopy ◽  
Operating Conditions ◽  
Digital Data ◽  
Ccd Cameras ◽  
Resolution Electron

It has been known for many years that materials such as zeolites, polymers, and biological specimens have crystalline structures that are vulnerable to electron beam irradiation. This radiation damage severely restrains the use of high resolution electron microscopy (HREM). As a result, structural characterization of these materials using HREM techniques becomes difficult and challenging. The emergence of slow-scan CCD cameras in recent years has made it possible to record high resolution (∽2Å) structural images with low beam intensity before any apparent structural damage occurs. Among the many ideal properties of slow-scan CCD cameras, the low readout noise and digital recording allow for low-dose HREM to be carried out in an efficient and quantitative way. For example, the image quality (or resolution) can be readily evaluated on-line at the microscope and this information can then be used to optimize the operating conditions, thus ensuring that high quality images are recorded. Since slow-scan CCD cameras output (undistorted) digital data within the large dynamic range (103-104), they are ideal for quantitative electron diffraction and microscopy.

Quantitative Electron Microscope with imaging plate

1994 ◽  
Vol 52 ◽  
pp. 408-409
Author(s):  
D. Shindo
Keyword(s):  
Electron Microscope ◽  
Dynamic Range ◽  
Processing System ◽  
Digital Data ◽  
Imaging Plate ◽  
Crystal Thickness ◽  
X Ray Diffraction ◽  
Resolution Electron ◽  
Electron Intensity ◽  
Diffraction Patterns

Imaging plate has good properties, i.e., a wide dynamic range and good linearity for the electron intensity. Thus the digital data (2048x1536 pixels, 4096 gray levels in log scale) obtained with the imaging plate can be used for quantification in electron microscopy. By using the image processing system (PIXsysTEM) combined with a main frame (ACOS3900), quantitative analysis of electron diffraction patterns and high-resolution electron microscope (HREM) images has been successfully carried out.In the analysis of HREM images observed with the imaging plate, quantitative comparison between observed intensity and calculated intensity can be carried out by taking into account the experimental parameters such as crystal thickness and defocus value. An example of HREM images of quenched Tl2Ba2Cu1Oy (Tc = 70K) observed with the imaging plate is shown in Figs. 1(b) - (d) comparing with a structure model proposed by x-ray diffraction study of Fig. 1 (a). The image was observed with a JEM-4000EX electron microscope (Cs =1.0 mm).

Precise on-line Measurement of Lattice Vectors

1990 ◽  
Vol 48 (1) ◽  
pp. 530-531
Author(s):  
W.J. de Ruijter ◽  
Sharma Renu
Keyword(s):  
Electron Microscope ◽  
Measurement Errors ◽  
Dynamic Range ◽  
Structural Information ◽  
Statistical Parameter ◽  
Systematic Errors ◽  
Geometric Distortion ◽  
Crystal Silicon ◽  
Camera System ◽  
On Line

Established methods for measurement of lattice spacings and angles of crystalline materials include x-ray diffraction, microdiffraction and HREM imaging. Structural information from HREM images is normally obtained off-line with the traveling table microscope or by the optical diffractogram technique. We present a new method for precise measurement of lattice vectors from HREM images using an on-line computer connected to the electron microscope. It has already been established that an image of crystalline material can be represented by a finite number of sinusoids. The amplitude and the phase of these sinusoids are affected by the microscope transfer characteristics, which are strongly influenced by the settings of defocus, astigmatism and beam alignment. However, the frequency of each sinusoid is solely a function of overall magnification and periodicities present in the specimen. After proper calibration of the overall magnification, lattice vectors can be measured unambiguously from HREM images.Measurement of lattice vectors is a statistical parameter estimation problem which is similar to amplitude, phase and frequency estimation of sinusoids in 1-dimensional signals as encountered, for example, in radar, sonar and telecommunications. It is important to properly model the observations, the systematic errors and the non-systematic errors. The observations are modelled as a sum of (2-dimensional) sinusoids. In the present study the components of the frequency vector of the sinusoids are the only parameters of interest. Non-systematic errors in recorded electron images are described as white Gaussian noise. The most important systematic error is geometric distortion. Lattice vectors are measured using a two step procedure. First a coarse search is obtained using a Fast Fourier Transform on an image section of interest. Prior to Fourier transformation the image section is multiplied with a window, which gradually falls off to zero at the edges. The user indicates interactively the periodicities of interest by selecting spots in the digital diffractogram. A fine search for each selected frequency is implemented using a bilinear interpolation, which is dependent on the window function. It is possible to refine the estimation even further using a non-linear least squares estimation. The first two steps provide the proper starting values for the numerical minimization (e.g. Gauss-Newton). This third step increases the precision with 30% to the highest theoretically attainable (Cramer and Rao Lower Bound). In the present studies we use a Gatan 622 TV camera attached to the JEM 4000EX electron microscope. Image analysis is implemented on a Micro VAX II computer equipped with a powerful array processor and real time image processing hardware. The typical precision, as defined by the standard deviation of the distribution of measurement errors, is found to be <0.003Å measured on single crystal silicon and <0.02Å measured on small (10-30Å) specimen areas. These values are ×10 times larger than predicted by theory. Furthermore, the measured precision is observed to be independent on signal-to-noise ratio (determined by the number of averaged TV frames). Obviously, the precision is restricted by geometric distortion mainly caused by the TV camera. For this reason, we are replacing the Gatan 622 TV camera with a modern high-grade CCD-based camera system. Such a system not only has negligible geometric distortion, but also high dynamic range (>10,000) and high resolution (1024x1024 pixels). The geometric distortion of the projector lenses can be measured, and corrected through re-sampling of the digitized image.

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