Thorough small-angle X-ray scattering analysis of the instability of liquid micro-jets in air

2013 ◽  
Vol 21 (1) ◽  
pp. 193-202 ◽  
Author(s):  
Benedetta Marmiroli ◽  
Fernando Cacho-Nerin ◽  
Barbara Sartori ◽  
Javier Pérez ◽  
Heinz Amenitsch

Liquid jets are of interest, both for their industrial relevance and for scientific applications (more important, in particular for X-rays, after the advent of free-electron lasers that require liquid jets as sample carrier). Instability mechanisms have been described theoretically and by numerical simulation, but confirmed by few experimental techniques. In fact, these are mainly based on cameras, which is limited by the imaging resolution, and on light scattering, which is hindered by absorption, reflection, Mie scattering and multiple scattering due to complex air/liquid interfaces during jet break-up. In this communication it is demonstrated that synchrotron small-angle X-ray scattering (SAXS) can give quantitative information on liquid jet dynamics at the nanoscale, by detecting time-dependent morphology and break-up length. Jets ejected from circular tubes of different diameters (100–450 µm) and speeds (0.7–21 m s−1) have been explored to cover the Rayleigh and first wind-induced regimes. Various solvents (water, ethanol, 2-propanol) and their mixtures have been examined. The determination of the liquid jet behaviour becomes essential, as it provides background data in subsequent studies of chemical and biological reactions using SAXS or X-ray diffraction based on synchrotron radiation and free-electron lasers.

2013 ◽  
Vol 46 (5) ◽  
pp. 1508-1512 ◽  
Author(s):  
Byron Freelon ◽  
Kamlesh Suthar ◽  
Jan Ilavsky

Coupling small-angle X-ray scattering (SAXS) and ultra-small-angle X-ray scattering (USAXS) provides a powerful system of techniques for determining the structural organization of nanostructured materials that exhibit a wide range of characteristic length scales. A new facility that combines high-energy (HE) SAXS and USAXS has been developed at the Advanced Photon Source (APS). The application of X-rays across a range of energies, from 10 to 50 keV, offers opportunities to probe structural behavior at the nano- and microscale. An X-ray setup that can characterize both soft matter or hard matter and high-Zsamples in the solid or solution forms is described. Recent upgrades to the Sector 15ID beamline allow an extension of the X-ray energy range and improved beam intensity. The function and performance of the dedicated USAXS/HE-SAXS ChemMatCARS-APS facility is described.


1984 ◽  
Vol 17 (5) ◽  
pp. 337-343 ◽  
Author(s):  
O. Yoda

A high-resolution small-angle X-ray scattering camera has been built, which has the following features. (i) The point collimation optics employed allows the scattering cross section of the sample to be directly measured without corrections for desmearing. (ii) A small-angle resolution better than 0.5 mrad is achieved with a camera length of 1.6 m. (iii) A high photon flux of 0.9 photons μs−1 is obtained on the sample with the rotating-anode X-ray generator operated at 40 kV–30 mA. (iv) Incident X-rays are monochromated by a bent quartz crystal, which makes the determination of the incident X-ray intensity simple and unambiguous. (v) By rotation of the position-sensitive proportional counter around the direct beam, anisotropic scattering patterns can be observed without adjusting the sample. Details of the design and performance are presented with some applications.


2016 ◽  
Vol 87 (6) ◽  
pp. 063905 ◽  
Author(s):  
I. Steinke ◽  
M. Walther ◽  
F. Lehmkühler ◽  
P. Wochner ◽  
J. Valerio ◽  
...  

1997 ◽  
Vol 30 (1) ◽  
pp. 49-54 ◽  
Author(s):  
J.-M. Dubuisson ◽  
T. Decamps ◽  
P. Vachette

An evacuated, temperature-controlled cell has been built for use on the small-angle X-ray scattering instrument D24 at the synchrotron radiation facility LURE. The sample is placed in a quartz capillary sealed in a stainless-steel holder using a vacuum-tight glue. Several O rings provide a vacuum path upstream and downstream from the cell, so that the X-ray beam only meets the capillary walls and the solution under study between the slits and the beam stop, while the sample is maintained under atmospheric pressure. The cell temperature is controlled via a water circulation through a copper sheath in tight contact with the steel holder. The use of this cell results in a marked reduction of the background, as observed in two series of parallel experiments using a conventional cell and this evacuated cell. The decrease ranges from a factor of 2 at s 1 values larger than 0.008 Å−1 to more than 15 at s = 0.00116 Å−1, where s is the modulus of the scattering vector (s = 2sin θ/λ, 2θ is the scattering angle and λ is the wavelength of the X-rays).


2007 ◽  
Vol 40 (4) ◽  
pp. 791-795 ◽  
Author(s):  
Takeshi Morita ◽  
Yoshitada Tanaka ◽  
Kazuki Ito ◽  
Yoshihiro Takahashi ◽  
Keiko Nishikawa

A novel apparatus has been developed that enables the simultaneous determination of the absorption factor during measurement of small-angle X-ray scattering (SAXS) intensities of a sample. It was designed especially for the use of relatively low-energy X-rays at SAXS beamlines of synchrotron facilities. The X-ray intensity of transmittance is measured by a silicon PIN photodiode, which is implanted in a direct beamstop set in a vacuum chamber. Since the assembly transmits an attenuated direct beam to a detector during the scattering measurement, a zero-angle position can be monitored without additional operation. It was confirmed that the linearity between the signal from the photodiode and the intensity of X-rays is good and the photodiode is applicable for the desired purpose. For a performance test, the absorption factors of a supercritical fluid were measured with a wide density range.


1999 ◽  
Vol 32 (1) ◽  
pp. 113-114 ◽  
Author(s):  
Stephen J. Henderson

While the difference between using heavy and light water as solvents for small-angle neutron scattering experiments is well known, the lesser difference for the case of small-angle X-ray scattering with these same isotopes of water has, as yet, not been reported. This difference for the case of X-rays is discussed and quantified for several familiar materials: polystyrene latexes, proteins and lipids.


2007 ◽  
Vol 40 (2) ◽  
pp. 218-231 ◽  
Author(s):  
Giuseppe Portale ◽  
Alessandro Longo ◽  
Lucio D'Ilario ◽  
Andrea Martinelli ◽  
Ruggero Caminiti ◽  
...  

The use of polychromaticBremsstrahlungX-rays generated by commercial tubes for energy-dispersive small-angle scattering measurements has not been extensively discussed in the literature, mainly because of some difficulties associated with it. If a suitable experimental setup is chosen and concomitant phenomena are taken into account for correcting the observed X-ray patterns, energy-dispersive small-angle X-ray scattering (SAXS) may become an interesting alternative to conventional measurements based on monochromatic beams. Energy-dispersive SAXS experiments carried out on protein solutions, micelles, semicrystalline polymers and catalytic systems are discussed to illustrate the new opportunities offered by this technique as well as its limitations.


2008 ◽  
Vol 41 (1) ◽  
pp. 167-175 ◽  
Author(s):  
Nozomi Ando ◽  
Pascale Chenevier ◽  
Martin Novak ◽  
Mark W. Tate ◽  
Sol M. Gruner

A high-pressure cell for synchrotron small-angle X-ray scattering (SAXS) studies of protein solutions is described. The design was optimized for use at up to 400 MPa in liquid pressure and with 8−12 keV X-rays with particular emphasis on the ease of use. The high-pressure cell was fabricated from corrosion-resistant Inconel 725 (Special Metals Corporation, Huntington, WV, USA) and featured Poulter-type windows [Poulter (1932).Phys. Rev.40, 861–871]. Flat natural diamonds, 500 µm thick, were recycled from diamond anvil cells and were shown to perform well as high-pressure SAXS windows. For a simple and effective method of sample isolation, disposable plastic sample cells with a defined path length and reproducible parasitic scattering were designed. These sample cells enable efficient use of synchrotron time. The cells facilitate rapid and easy sample changes, eliminate the need to clean the cell between sample changes, and reduce the sample volume to as low as 12 µl. The disposable cells can also be used separately from the high-pressure cell for SAXS measurements at ambient pressure and temporary storage of samples. The performance of the apparatus is demonstrated with T4 lysozyme.


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