scholarly journals Identification of cinnabar existing in different objects using portable coupled XRF-XRD, laboratory-type XRD and micro-Raman spectroscopy: comparison of the techniques

2021 ◽  
Vol 3 (12) ◽  
Author(s):  
Jingyi Shen ◽  
Yijia Shen

Abstract Cinnabar (α-HgS) is a common mineral used in various fields. The identification of cinnabar can be achieved by classic mineralogical methods and instrumental methods. X-ray diffraction (XRD) is the most reliable instrumental method for identifying material phases, but the sampling process and the immovable instrument limit its wider application in the cultural heritage field. The occurrence of Assing S. p. A. Surface Monitor, a portable system integrating X-ray fluorescence (XRF) and XRD, provides researchers with a new solution. Raw mineral, polished gemstone, pigment powder and Chinese ink stick claimed to be composed of cinnabar were measured by the system as well as laboratory-type XRD and micro-Raman techniques in this study. The qualitative XRF results were applied to determining the elements existing in the samples and thus defining the range of possible phases. Patterns obtained were compared carefully with the characteristic lines to determine the most likely phases, while the pattern appearances were compared in order to recognize the different states of cinnabar and generalize the experience for identifying cinnabar by the system. The Raman spectra obtained were compared and analyzed in order to learn the best parameters and determine the real composition of each sample. The results indicate that the XRF detector is sensitive enough to distinguish cinnabar from another red pigment, minium (Pb3O4), without destructive preparation provided that the desired phases occupy a major content in the sample, while the laser micro-Raman is even better in application range and measurement speed but correct analysis of the spectra is highly dependent on experience and literatures. The portable coupled XRF-XRD system and the micro-Raman provide researchers with convenient and efficient options to preliminarily identify minerals like cinnabar, which is significantly meaningful to several research fields including mineralogy, heritage science, material science, etc. Article highlights Two efficient and non-destructive methods for the preliminary identification of minerals like cinnabar were developed. The optimum instrument parameters for the effective measurement of different cinnabar samples were given in detail. The study provides useful data for various fields including analytical science, material science, heritage science, etc.

Author(s):  
S.J.B. Reed

Characteristic fluorescenceThe theory of characteristic fluorescence corrections was first developed by Castaing. The same approach, with an improved expression for the relative primary x-ray intensities of the exciting and excited elements, was used by Reed, who also introduced some simplifications, which may be summarized as follows (with reference to K-K fluorescence, i.e. K radiation of element ‘B’ exciting K radiation of ‘A’):1.The exciting radiation is assumed to be monochromatic, consisting of the Kα line only (neglecting the Kβ line).2.Various parameters are lumped together in a single tabulated function J(A), which is assumed to be independent of B.3.For calculating the absorption of the emerging fluorescent radiation, the depth distribution of the primary radiation B is represented by a simple exponential.These approximations may no longer be justifiable given the much greater computing power now available. For example, the contribution of the Kβ line can easily be calculated separately.


Author(s):  
John A. Hunt ◽  
Richard D. Leapman ◽  
David B. Williams

Interactive MASI involves controlling the raster of a STEM or SEM probe to areas predefined byan integration mask which is formed by image processing, drawing or selecting regions manually. EELS, x-ray, or other spectra are then acquired while the probe is scanning over the areas defined by the integration mask. The technique has several advantages: (1) Low-dose spectra can be acquired by averaging the dose over a great many similar features. (2) MASI can eliminate the risks of spatial under- or over-sampling of multiple, complicated, and irregularly shaped objects. (3) MASI is an extremely rapid and convenient way to record spectra for routine analysis. The technique is performed as follows:Acquire reference imageOptionally blank beam for beam-sensitive specimensUse image processor to select integration mask from reference imageCalculate scanning path for probeUnblank probe (if blanked)Correct for specimen drift since reference image acquisition


2007 ◽  
Vol 17 (2) ◽  
pp. 351-354 ◽  
Author(s):  
S. Friedrich ◽  
O.B. Drury ◽  
Shaopang Yuan ◽  
P. Szupryczynski ◽  
M.A. Spurrier ◽  
...  

2017 ◽  
Vol 24 (6) ◽  
pp. 1113-1119 ◽  
Author(s):  
E. Nazaretski ◽  
H. Yan ◽  
K. Lauer ◽  
N. Bouet ◽  
X. Huang ◽  
...  

A hard X-ray scanning microscope installed at the Hard X-ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ∼15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature of a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.


2018 ◽  
Vol 167 ◽  
pp. 03001 ◽  
Author(s):  
Przemyslaw Wachulak ◽  
Alfio Torrisi ◽  
Mesfin Ayele ◽  
Andrzej Bartnik ◽  
Joanna Czwartos ◽  
...  

In this work we present three experimental, compact desk-top imaging systems: SXR and EUV full field microscopes and the SXR contact microscope. The systems are based on laser-plasma EUV and SXR sources based on a double stream gas puff target. The EUV and SXR full field microscopes, operating at 13.8 nm and 2.88 nm wavelengths are capable of imaging nanostructures with a sub-50 nm spatial resolution and short (seconds) exposure times. The SXR contact microscope operates in the “water-window” spectral range and produces an imprint of the internal structure of the imaged sample in a thin layer of SXR sensitive photoresist. Applications of such desk-top EUV and SXR microscopes, mostly for biological samples (CT26 fibroblast cells and Keratinocytes) are also presented. Details about the sources, the microscopes as well as the imaging results for various objects will be presented and discussed. The development of such compact imaging systems may be important to the new research related to biological, material science and nanotechnology applications.


1981 ◽  
Vol 21 (4) ◽  
pp. 470-476
Author(s):  
R. V. Vedrinskii ◽  
S. A. Prosandeev ◽  
V. V. Krivitskii ◽  
A. N. Pavlov

2021 ◽  
Author(s):  
Mingshan Qin ◽  
Juan Gao ◽  
Dongwei Wei ◽  
Liuan Li ◽  
Cun Li ◽  
...  

Abstract Because of their unique surface area and adjustable pore size, Metal-Organic Frameworks(MOFs) have been widely used in lots of research fields, such as catalysis, energy storage, sensing, separation. In this paper, as for the Knoevenagel reaction, UiO66 and other UiO series MOFs were synthesized and modified. UiO66 nanoparticles were prepared by one-pot method. 2-aminopyridine, 3-aminopyridine and 4-aminopyridine were used to prepare UiO66-2Py, UiO66-3Py and UiO66-4Py nanoparticles. UiO66-2Py, UiO66-3Py and UiO66-4Py nanoparticles were modified by activated arginine, lysine and glycine to synthesize UiO66-2Py-Arg, UiO66-3Py-Lys and UiO66-4Py-Gly. Finally, the obtained samples were used for the Knoevenagel catalytic condensation reactions of benzaldehyde and ethyl cyanoacetate. In this process, the prepared samples and their intermediates were characterized by infrared spectroscopy (IR) and X-ray diffraction(XRD), which showed that the modification of UiO66 was successful. UiO66-3Py-Lys and UiO66-4Py-Gly showed high catalytic activity in the supernatant determined by fluorescence spectrophotometer, and UiO66-4Py-Gly showed the best catalytic effects at the volume of 0.4mL benzaldehyde.


1975 ◽  
Vol 68 ◽  
pp. 425-426
Author(s):  
H. S. Hudson ◽  
T. W. Jones ◽  
R. P. Lin

SummaryIn many small solar flares the ∼10–100 keV electrons accelerated during the flash phase contain the bulk of the total flare energy output. In large flares, such as those in the period 1972, August 2–7, the flash phase electrons are present in substantially greater numbers. These electrons can explosively heat the chromosphere-lower corona and eject flare material. The ejected matter can produce a shock wave which will then accelerate nucleons and electrons to relativistic energies. We analyze energetic particle, radio, X-ray, gamma ray and interplanetary shock observations of the 1972 August flares to obtain quantitative estimates of the energy contained in each facet of these large flares. In general these observations are consistent with the above hypothesis. In particular: (1)From the X-ray emission (van Beek et al., 1973) the energy contained in >25 keV electrons is calculated to be 2 × 1032 erg for the 1972, August 4 event. Since the lower energy cutoff to the electron spectrum is known to be below 25 keV and possibly below 10 keV, the electrons contain enough energy to produce the following interplanetary shock wave, which has by far the bulk of the energy dissipated in the flare. Similar numbers are obtained for the large August 7 flare event.(2)From the γ-ray emission (Chupp et al., 1973) the energy in protons dumped at the same level of the atmosphere, assuming a thick target situation, is at least a factor of three smaller than the electrons. Moreover the γ-ray emission indicates that the bulk of the protons are accelerated at least several minutes after the electrons. Thus it is more likely that the electrons are responsible for the flare optical (Hα and white light) emissions which occur in the chromosphere.(3)Approximately 5% of the electrons and 99% of the protons escape into the interplanetary medium to be observed by spacecraft. This situation is consistent with the hypothesis of shock acceleration of the protons high in the solar corona.(4)The four most intense X-ray bursts observed during the period July 31–August 11 are the only bursts followed by an interplanetary shock wave and a new injection of energetic protons into the interplanetary medium.


1989 ◽  
Vol 134 ◽  
pp. 492-493
Author(s):  
G. De Zotti ◽  
M. Persic ◽  
A. Franceschini ◽  
L. Danese ◽  
G.G.C. Palumbo ◽  
...  

Studies of the HEAO–1 A2 all–sky survey data have established that the level of anisotropy of the extragalactic X–ray background (XRB) is relatively low: –The cell–to–cell XRB intensity variations can be entirely accounted for by Poisson fluctuations in the space distribution of known classes of sources; the 90% confidence upper limit to any additional contribution on a scale of 26 square degrees is 2.3% (Shafer and Fabian 1983).–No significant correlations of XRB intensity fluctuations appear to be present; the formal 90% confidence upper limit on the amplitude of autocorrelations, relative to the mean background intensity, for an angular scale of 3° is Γ(3°) ≤ 1.9 × 10−2 (Persic et al. 1988).


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