Personal Observations

1986 ◽  
Vol 30 ◽  
pp. 29-33
Author(s):  
Ron Jenkins
Keyword(s):  
Transition Period ◽  
Matrix Effects ◽  
Analytical Tool ◽  
X Ray Diffraction ◽  
X Ray ◽  
General Acceptance ◽  
Methods Of Analysis ◽  
The Matrix ◽  
Instrumental Methods

Like most instrumental methods of analysis, X-Ray Fluoresence (XRF) has progressed through the various stages of Innovation, Frustration, Application and Consolidation. My own association with the method dates back to the late 1950's which would correspond to the transition period between the innovation and frustration stages alluded to above. At that time, there were probably less than 500 XRF spectrometers in the whole world and to myself, as a young analyst with a limited background in x-ray diffraction methods, the potential power which the XRF method seemed to offer far outweighed any problems from the ‘matrix effects' that people were starting to talk about. This talk covers my own impressions of the highlights of the 20 year period of frustration and application which were to culminate with the general acceptance of the XRF method, in the mid-1970's, as a versatile and reliable analytical tool.

Detection Confirmation and Determination of Trace Amounts of Selenium by X-Ray Methods

1963 ◽  
Vol 7 ◽  
pp. 542-554
Author(s):  
Frank L. Chan
Keyword(s):  
Matrix Effects ◽  
Hexagonal Structure ◽  
Elemental Selenium ◽  
X Ray Diffraction ◽  
X Ray ◽  
Yellow Color ◽  
The Matrix ◽  
Ray Methods ◽  
Tetravalent State

AbstractRecently, interest in the determination of selenium in trace amounts has been greatly intensified because of the nutritional aspects of this element. It has been reported that selenium in the amount of 13 μg in the form of sodium selenite in 100 g of feed has an effect similar to that of vitamin E. In the field of semiconductors, the detection and determination of trace amounts of selenium in arsenic, antimony, and small single crystals of solid solution of cadmium selenide and sulfide are of considerable importance in semiconductor performance.In the Aerospace Research Laboratories, 4,5 diamino-6-tbiopyi-imidine has been successfully adopted as a reagent for the spectrophotometric determination of selenium. The reaction of 4,5 diamino-6-thiopyrimidine and tetxavalent selenium produces a yellow color with the formation of elemental selenium. It is possible to determine elemental selenium by collecting it in a thin layer. The selenium deposited in this layer may then be determined by an X-ray fluorescence method. A procedure of this nature has the advantage of eliminating the matrix effects commonly encountered in X-ray fluorescence. Furthermore, the slow generation of selenium affords a convenient means of detection and confirmation of this element by the use of X-ray diffraction procedures. By this technique selenium is first converted to its tetravalent state and is then reacted with 4,5 diamino-6-thiopyrimidine. On standing, the selenium is reduced to a red precipitate of elemental selenium which can be dissolved in carbon disulfide. Finally, the selenium can be converted into its hexagonal structure by annealing at 205-207°C.

Quantitative X-ray diffraction and X-ray fluorescence analyses of mixtures – unified and simplified

2018 ◽  
Vol 51 (3) ◽  
pp. 789-795
Author(s):  
Frank H. Chung
Keyword(s):  
Matrix Effects ◽  
Chemical Elements ◽  
Complex Mixture ◽  
Current Approach ◽  
Complex Matrix ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Matrix ◽  
Simplified Procedure ◽  
Xrf Analyses

Owing to the complex matrix effects, the current approach to quantitative X-ray diffraction (XRD) and X-ray fluorescence (XRF) analyses of mixtures requires calibration lines from standards, and is hence tedious and time consuming. New insights reveal that both the matrix effects and the calibration lines can be eliminated mathematically. Any complex mixture can be transformed into a set of simple binary mixtures. One straightforward formula decodes both XRD and XRF. A single XRD or XRF scan quantifies the chemical compounds or chemical elements in any mixture. The unified and simplified procedure reduces by some 80% the laboratory work associated with current practice. Five sets of experimental data are presented to verify its applications. Statistical evaluation of this new procedure gives a precision of ±5% or better, which is normally expected from XRD and XRF analyses.

Characteristics of Ni–Cr–Fe laser clad layers on EA4T steel

2017 ◽  
Vol 31 (16-19) ◽  
pp. 1744031
Author(s):  
Wenjing Chen ◽  
Hui Chen ◽  
Yongjing Wang ◽  
Congchen Li ◽  
Xiaoli Wang
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cladding Layer ◽  
Metallurgical Bonding ◽  
The Matrix ◽  
Feeding Speed ◽  
Upper Bainite ◽  
Scanning Electron

The Ni–Cr–Fe metal powder was deposited on EA4T steel by laser cladding technology. The microstructure and chemical composition of the cladding layer were analyzed by optical microscopy (OM), scanning electron microscopy (SEM) and X-ray diffraction (XRD). The bonding ability between the cladding layer and the matrix was measured. The results showed that the bonding between the cladding layer and the EA4T steel was metallurgical bonding. The microstructure of cladding layer was composed of planar crystals, columnar crystals and dendrite, which consisted of Cr2Ni3, [Formula: see text] phase, M[Formula: see text]C6 and Ni3B phases. When the powder feeding speed reached 4 g/min, the upper bainite occurred in the heat affected zone (HAZ). Moreover, the tensile strength of the joint increased, while the yield strength and the ductility decreased.

Detection of Compositional Fluctuations in High Temperature Exposed Waspaloy

2001 ◽  
Vol 699 ◽  
Author(s):  
Xiaodong Zou ◽  
Tariq Makram ◽  
Rosario A. Gerhardt
Keyword(s):  
Exposure Time ◽  
Structural Integrity ◽  
Thermal Exposure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Gamma Prime ◽  
Distribution Shape ◽  
The Matrix ◽  
Quantitative Stereology ◽  
Nickel Base

AbstractWaspaloy is a nickel base super-alloy used in aircraft engines. When this alloy is placed in service, it is subjected to long term exposure at high temperatures, which can cause the reinforcing gamma prime precipitate population to fluctuate and thus affect its structural integrity. The population fluctuates as a result of coarsening, dissolution or re-precipitation. Samples exposed to 1200° F for times ranging from 0 to 12626 hours were characterized using impedance spectroscopy, microhardness measurements, x-ray diffraction and quantitative stereology. Two important parameters were derived from the impedance measurements: (1) the imaginary admittance peak magnitude (Ymax) and (2) the associated relaxation frequency (fmax). As the distribution, shape and size of the precipitates change with exposure time, these parameters were also found to vary. In addition to the changes in precipitate geometry, lattice constant changes detected by analyzing x-ray diffraction data suggest that there are compositional shifts in the matrix as well as the gamma prime precipitates. Furthermore, the preferred orientation of the precipitates can also be seen to change with exposure time. These changes in composition, size and shape as a function of thermal exposure time are accompanied by changes in the volume fractions of primary and secondary gamma prime particles present. Using effective medium models, it is possible to predict that the measured properties are related to the gamma prime population. The grain boundary carbides do not appear to play any role at the conditions presented.

scholarly journals Влияние режима получения образцов и термообработки на локальную структуру халькогенидного полупроводника Ge-=SUB=-2-=/SUB=-Sb-=SUB=-2-=/SUB=-Te-=SUB=-5-=/SUB=-

2022 ◽  
Vol 56 (3) ◽  
pp. 291
Author(s):  
С.Н. Гарибова ◽  
А.И. Исаев ◽  
С.И. Мехтиева ◽  
С.У. Атаева ◽  
Р.И. Алекперов
Keyword(s):  
Heat Treatment ◽  
Thermal Processing ◽  
Thermal Evaporation ◽  
Amorphous State ◽  
Hexagonal Structure ◽  
Structural Elements ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Matrix ◽  
Close Range

Specifics of "amorphous state - crystal" phase transitions in dependence on the samples obtaining method and thermal processing, as well as changes in the structure and close range order in the arrangement of the atoms of Ge20Sb20.5Te51 chalcogenide semiconductors have been studied by the x-ray diffraction and Raman spectroscopy. It has been shown that Ge20Sb20.5Te51 films obtained by thermal evaporation on an unheated substrate are amorphous; after heat treatment at 220 and 400 °C, transform into a crystalline phase with a cubic and hexagonal structure. The chemical bonds and the main structural elements that form the matrix of the investigated objects, as well as the changes that occur in them during heat treatment, have been determined.

scholarly journals Thermal History of Matrix Forsterite Grains from Murchison Based on High-resolution Tomography

2021 ◽  
Vol 922 (2) ◽  
pp. 256
Author(s):  
Giulia Perotti ◽  
Henning O. Sørensen ◽  
Henning Haack ◽  
Anja C. Andersen ◽  
Dario Ferreira Sanchez ◽  
...  
Keyword(s):  
High Resolution ◽  
Electron Density ◽  
Chemical Compositions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Density Maps ◽  
Thermally Processed ◽  
The Matrix ◽  
History Of ◽  
Chondrule Formation

Abstract Protoplanetary disks are dust- and gas-rich structures surrounding protostars. Depending on the distance from the protostar, this dust is thermally processed to different degrees and accreted to form bodies of varying chemical compositions. The primordial accretion processes occurring in the early protoplanetary disk such as chondrule formation and metal segregation are not well understood. One way to constrain them is to study the morphology and composition of forsteritic grains from the matrix of carbonaceous chondrites. Here, we present high-resolution ptychographic X-ray nanotomography and multimodal chemical microtomography (X-ray diffraction and X-ray fluorescence) to reveal the early history of forsteritic grains extracted from the matrix of the Murchison CM2.5 chondrite. The 3D electron density maps revealed, at unprecedented resolution (64 nm), spherical inclusions containing Fe–Ni, very little silica-rich glass and void caps (i.e., volumes where the electron density is consistent with conditions close to vacuum) trapped in forsterite. The presence of the voids along with the overall composition, petrological textures, and shrinkage calculations is consistent with the grains experiencing one or more heating events with peak temperatures close to the melting point of forsterite (∼2100 K), and subsequently cooled and contracted, in agreement with chondrule-forming conditions.

Machinability and Microstructure of SiC/h-BN Nano-Composites

2008 ◽  
Vol 569 ◽  
pp. 45-48
Author(s):  
Hai Yun Jin ◽  
Guan Jun Qiao ◽  
Zong Ren Peng ◽  
Ji Qiang Gao
Keyword(s):  
Fracture Strength ◽  
Nano Composites ◽  
Weak Interface ◽  
X Ray Diffraction ◽  
X Ray ◽  
Sic Particles ◽  
N2 Atmosphere ◽  
The Matrix ◽  
Better Than

SiC particles coated with nano-BN were synthesized and the machinable SiC/BN ceramic nano-composites were fabricated by Plasma Active Sintering (PAS) in N2 atmosphere. The existing and distribution of h-BN phase were revealed by X-ray diffraction (XRD), and SEM. For the existing of weak interface between h-BN and SiC grains, the machinability of both SiC/BN micro-composites and nano-composites were improved obviously. Because the nano-sized h-BN crystals were homogeneously dispersed around the SiC grains of the matrix, the fracture strength of the nano-composites was better than the SiC/h-BN micro-composite.

Aspects of the structure and composition of baleen, and some effects of exposure to petroleum hydrocarbons

1984 ◽  
Vol 62 (2) ◽  
pp. 193-198 ◽  
Author(s):  
D. J. St. Aubin ◽  
R. H. Stinson ◽  
J. R. Geraci
Keyword(s):  
Petroleum Hydrocarbons ◽  
Trichloroacetic Acid ◽  
Breaking Strength ◽  
X Ray Diffraction ◽  
Balaenoptera Physalus ◽  
Fin Whale ◽  
X Ray ◽  
The Matrix ◽  
Spilled Oil ◽  
Iron And Calcium

The structure and composition of baleen from seven species of whales was studied using tensiometry. X-ray diffraction, and elemental analysis. Baleen was found to be composed principally of amorphous and α-keratin. Hydroxyapatite (bone mineral, Ca10 (PO4)6 OH2) was present in all species. Certain elements, notably manganese, copper, boron, iron, and calcium were more highly concentrated in the fibers than in the matrix of the plate. The breaking strength of baleen plates from fin (Balaenoptera physalus), sei (B. borealis), and grey (Eschrichtius robustus) whales was comparable to that of buffalo horn, in the range of 2−9 × 106 N∙m−2. The stiffness of baleen was somewhat less than that of other keratinized tissues. Treatment with 10% (v/v) trichloroacetic acid for 8 days removed most of the calcium salts, denatured α-keratin, and made fin whale plates stronger and stiffer. Exposure to gasoline for 1.5 h or 14 days, crude oil for 8 days, or tar for 21 days resulted in loss of trace elements from baleen, and inconsistent changes in keratin organization. After tar exposure, fin whale baleen plates were stiffer and stronger. We presume that at sea, baleen would be relatively resistant to damage by spilled oil.

A New X-Ray Diffraction Method for Quantitative Multicomponent Analysis

1973 ◽  
Vol 17 ◽  
pp. 106-115 ◽  
Author(s):  
Frank H. Chung
Keyword(s):  
Calibration Curve ◽  
Fundamental Matrix ◽  
Diffraction Method ◽  
X Ray Diffraction ◽  
Absorption Effect ◽  
Multicomponent Analysis ◽  
X Ray ◽  
Practical Applications ◽  
The Matrix

AbstractA unified matrix-flushing theory and its practical applications for quantitative multicomponent analysis by X-ray diffraction are presented.In this method, a fundamental “matrix-flushing” concept is introduced; the calibration curve procedure is shunted; the matrix (absorption) effect is totally eliminated; all components, crystalline or amorphous, can be determined.

Sb-rich nanoinclusions in an AlGaAsSb metamaterial

MRS Advances ◽  
2019 ◽  
Vol 4 (5-6) ◽  
pp. 277-284
Author(s):  
Nikolay A. Bert ◽  
Vladimir V. Chaldyshev ◽  
Nikolay A. Cherkashin ◽  
Vladimir N. Nevedomskiy ◽  
Valery V. Preobrazhenskii ◽  
...  
Keyword(s):  
Molecular Beam ◽  
Filling Factor ◽  
Local Thermodynamic Equilibrium ◽  
Average Diameter ◽  
Formation Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Self Organized ◽  
Transmission Electron ◽  
The Matrix

ABSTRACTWe studied the microstructure of Al0.28Ga0.72As0.972Sb0.028 metamaterials containing a developed array of AsSb nanoinclusions. The AlGaAsSb films were grown by low-temperature molecular-beam epitaxy followed by high-temperature annealing at 750°C. The process resulted in an array of self-organized AsSb nanonclusions with an average diameter of 15 nm. The volume filling factor was about 0.003. Using transmission electron microscopy and x-ray diffraction we showed that the nanoinclusions have A7-type rhombohedral atomic structure with the following orientation in the matrix (0003)p || {111}m and [-2110]p || 〈220〉m, where p and m indices indicate the AsSb precipitate and AlGaAsSb matrix, correspondingly. The nanoinclusions appeared to be strongly enriched by antimony (more than 90 atomic %), whereas the Sb content in the AlGaAsSb matrix was 2.8 atomic %. The strong enrichment of the inclusion with Sb resulted from the local thermodynamic equilibrium between the solid AlGaAsSb matrix and AsSb inclusions which became liquid at a formation temperature of 750°C.

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