Chain-length dependent growth dynamics of n-alkanes on silica investigated by energy-dispersive x-ray reflectivity in situ and in real-time

2012 ◽  
Vol 136 (20) ◽  
pp. 204709 ◽  
Author(s):  
C. Weber ◽  
C. Frank ◽  
S. Bommel ◽  
T. Rukat ◽  
W. Leitenberger ◽  
...  
Nanoscale ◽  
2021 ◽  
Author(s):  
Helena Fridman ◽  
Michael Volokh ◽  
Taleb Mokari

Nanocrystal growth dynamics are investigated by a novel approach: real-time observation of nanocrystals in growth solutions using lab-scale in situ X-ray diffraction. The method reveals the evolution of crystal phase, size, shape, and composition.


1996 ◽  
Vol 8 (8) ◽  
pp. 2102-2108 ◽  
Author(s):  
R. J. Francis ◽  
S. J. Price ◽  
J. S. O. Evans ◽  
S. O'Brie ◽  
D. O'Hare ◽  
...  

Minerals ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 426
Author(s):  
Behrooz Abbasi ◽  
Xiaoliang Wang ◽  
Judith C. Chow ◽  
John G. Watson ◽  
Bijan Peik ◽  
...  

Respirable coal mine dust (RCMD) exposure is associated with black lung and silicosis diseases in underground miners. Although only RCMD mass and silica concentrations are regulated, it is possible that particle size, surface area, and other chemical constituents also contribute to its adverse health effects. This review summarizes measurement technologies for RCMD mass concentrations, morphology, size distributions, and chemical compositions, with examples from published efforts where these methods have been applied. Some state-of-the-art technologies presented in this paper have not been certified as intrinsically safe, and caution should be exerted for their use in explosive environments. RCMD mass concentrations are most often obtained by filter sampling followed by gravimetric analysis, but recent requirements for real-time monitoring by continuous personal dust monitors (CPDM) enable quicker exposure risk assessments. Emerging low-cost photometers provide an opportunity for a wider deployment of real-time exposure assessment. Particle size distributions can be determined by microscopy, cascade impactors, aerodynamic spectrometers, optical particle counters, and electrical mobility analyzers, each with unique advantages and limitations. Different filter media are required to collect integrated samples over working shifts for comprehensive chemical analysis. Teflon membrane filters are used for mass by gravimetry, elements by energy dispersive X-ray fluorescence, rare-earth elements by inductively coupled plasma-mass spectrometry and mineralogy by X-ray diffraction. Quartz fiber filters are analyzed for organic, elemental, and brown carbon by thermal/optical methods and non-polar organics by thermal desorption-gas chromatography-mass spectrometry. Polycarbonate-membrane filters are analyzed for morphology and elements by scanning electron microscopy (SEM) with energy dispersive X-ray, and quartz content by Fourier-transform infrared spectroscopy and Raman spectroscopy.


2018 ◽  
Vol 9 (23) ◽  
pp. 6750-6754 ◽  
Author(s):  
Alessandro Greco ◽  
Alexander Hinderhofer ◽  
M. Ibrahim Dar ◽  
Neha Arora ◽  
Jan Hagenlocher ◽  
...  

2020 ◽  
Vol 61 (6) ◽  
Author(s):  
C E Schrank ◽  
K Gioseffi ◽  
T Blach ◽  
O Gaede ◽  
A Hawley ◽  
...  

Abstract We present a review of a unique non-destructive method for the real-time monitoring of phase transformations and nano-pore evolution in dehydrating rocks: transmission small- and wide-angle synchrotron X-ray scattering (SAXS/WAXS). It is shown how SAXS/WAXS can be applied to investigating rock samples dehydrated in a purpose-built loading cell that allows the coeval application of high temperature, axial confinement, and fluid pressure or flow to the specimen. Because synchrotron sources deliver extremely bright monochromatic X-rays across a wide energy spectrum, they enable the in situ examination of confined rock samples with thicknesses of ≤ 1 mm at a time resolution of order seconds. Hence, fast kinetics with reaction completion times of about hundreds of seconds can be tracked. With beam sizes of order tens to hundreds of micrometres, it is possible to monitor multiple interrogation points in a sample with a lateral extent of a few centimetres, thus resolving potential lateral spatial effects during dehydration and enlarging sample statistics significantly. Therefore, the SAXS/WAXS method offers the opportunity to acquire data on a striking range of length scales: for rock samples with thicknesses of ≤ 10-3 m and widths of 10-2 m, a lateral interrogation-point spacing of ≥ 10-5 m can be achieved. Within each irradiated interrogation-point volume, information concerning pores with sizes between 10-9 and 10-7 m and the crystal lattice on the scale of 10-10 m is acquired in real time. This article presents a summary of the physical principles underpinning transmission X-ray scattering with the aim of providing a guide for the design and interpretation of time-resolved SAXS/WAXS experiments. It is elucidated (1) when and how SAXS data can be used to analyse total porosity, internal surface area, and pore-size distributions in rocks on length scales from ∼1 to 300 nm; (2) how WAXS can be employed to track lattice transformations in situ; and (3) which limitations and complicating factors should be considered during experimental design, data analysis, and interpretation. To illustrate the key capabilities of the SAXS/WAXS method, we present a series of dehydration experiments on a well-studied natural gypsum rock: Volterra alabaster. Our results demonstrate that SAXS/WAXS is excellently suited for the in situ tracking of dehydration kinetics and the associated evolution of nano-pores. The phase transformation from gypsum to bassanite is correlated directly with nano-void growth on length scales between 1 and 11 nm for the first time. A comparison of the SAXS/WAXS kinetic results with literature data emphasises the need for future dehydration experiments on rock specimens because of the impact of rock fabric and the generally heterogeneous and transient nature of dehydration reactions in nature. It is anticipated that the SAXS/WAXS method combined with in situ loading cells will constitute an invaluable tool in the ongoing quest for understanding dehydration and other mineral replacement reactions in rocks quantitatively.


2009 ◽  
Vol 105 (9) ◽  
pp. 093505 ◽  
Author(s):  
M. Croft ◽  
V. Shukla ◽  
E. K. Akdoğan ◽  
N. Jisrawi ◽  
Z. Zhong ◽  
...  

1995 ◽  
Vol 10 (3) ◽  
pp. 173-177 ◽  
Author(s):  
P. Ballirano ◽  
A. Maras ◽  
R. Caminiti ◽  
C. Sadun

New powder X-ray data for cancrinite [ideally Na8Si6Al6O24 (CO3)2·2 H2O] are reported along with in-situ real-time thermal processes recorded using energy dispersive X-ray diffractometry (EDXD). A completely anhydrous phase is obtained after heating the sample up to 600 °C and quickly cooling it to room temperature, as shown by means of both Rietveld analysis and IR spectroscopy. The anhydrous phase does not show any tendency to re-acquire molecular water. During the heating process, at around 450 °C, a peak splitting is observed, possibly due to a reversible phase transition.


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