scholarly journals Development of a sticker sealed microfluidic device for in situ analytical measurements using synchrotron radiation

Author(s):  
ITAMAR NECKEL ◽  
Lucas F. de Castro ◽  
Flavia Callefo ◽  
Verônica Teixeira ◽  
Angelo Gobbi ◽  
...  

Abstract Shedding synchrotron light on microfluidic systems, exploring several contrasts in situ operando at the nanoscale, like X-ray fluorescence, diffraction, luminescence, and absorption, has the potential to reveal new properties and functionalities of materials across diverse areas, such as green energy, photonics, and nanomedicine. In this work, we present the micro-fabrication and characterization of a multifunctional polyester/glass sealed microfluidic device well-suited to combine with analytical X-ray techniques. The device consists of smooth microchannels patterned on glass, where three gold electrodes are deposited into the channels to serve in situ electrochemistry analysis or standard electrical measurements. It has been efficiently sealed through an ultraviolet-sensitive sticker-like layer based on a polyester film, and The burst pressure determined by pumping water through the microchannel(up to 0.22 MPa). Overall, the device has demonstrated exquisite chemical resistance to organic solvents, and its efficiency in the presence of biological samples (proteins) is remarkable. The device potentialities, and its high transparency to X-rays, have been demonstrated by taking advantage of the X-ray nanoprobe Carnaúba/Sirius/LNLS, by obtaining 2D X-ray nanofluorescence maps on the microchannel filled with water and after an electrochemical nucleation reaction. To wrap up, the microfluidic device characterized here has the potential to be employed in standard laboratory experiments as well as in situ and in vivo analytical experiments using a wide electromagnetic window, from infrared to X-rays, which could serve experiments in many branches of science.

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Itamar T. Neckel ◽  
Lucas F. de Castro ◽  
Flavia Callefo ◽  
Verônica C. Teixeira ◽  
Angelo L. Gobbi ◽  
...  

AbstractShedding synchrotron light on microfluidic systems, exploring several contrasts in situ/operando at the nanoscale, like X-ray fluorescence, diffraction, luminescence, and absorption, has the potential to reveal new properties and functionalities of materials across diverse areas, such as green energy, photonics, and nanomedicine. In this work, we present the micro-fabrication and characterization of a multifunctional polyester/glass sealed microfluidic device well-suited to combine with analytical X-ray techniques. The device consists of smooth microchannels patterned on glass, where three gold electrodes are deposited into the channels to serve in situ electrochemistry analysis or standard electrical measurements. It has been efficiently sealed through an ultraviolet-sensitive sticker-like layer based on a polyester film, and The burst pressure determined by pumping water through the microchannel(up to 0.22 MPa). Overall, the device has demonstrated exquisite chemical resistance to organic solvents, and its efficiency in the presence of biological samples (proteins) is remarkable. The device potentialities, and its high transparency to X-rays, have been demonstrated by taking advantage of the X-ray nanoprobe Carnaúba/Sirius/LNLS, by obtaining 2D X-ray nanofluorescence maps on the microchannel filled with water and after an electrochemical nucleation reaction. To wrap up, the microfluidic device characterized here has the potential to be employed in standard laboratory experiments as well as in in situ and in vivo analytical experiments using a wide electromagnetic window, from infrared to X-rays, which could serve experiments in many branches of science.


2014 ◽  
Vol 47 (6) ◽  
pp. 2078-2080 ◽  
Author(s):  
Monika Witala ◽  
Jun Han ◽  
Andreas Menzel ◽  
Kim Nygård

It is shown that small-angle X-ray scattering from binary liquid mixtures close to the critical point of demixing can be used forin situcharacterization of beam-induced heating of liquid samples. For demonstration purposes, the proposed approach is applied on a well studied critical mixture of water and 2,6-lutidine. Given a typical incident X-ray flux at a third-generation synchrotron light source and using a 1.5 mm-diameter glass capillary as sample container, a beam-induced local temperature increase of 0.45 ± 0.10 K is observed.


2000 ◽  
Vol 07 (04) ◽  
pp. 437-446 ◽  
Author(s):  
G. RENAUD

The application of X-rays to the structural characterization of surfaces and interfaces, in situ and in UHV, is discussed on selected examples. Grazing incidence X-ray diffraction is not only a very powerful technique for quantitatively investigating the atomic structure of surfaces and interfaces, but is also very useful for providing information on the interfacial registry for coherent interfaces or on the strain deformation, island and grain sizes for incoherent epilayers.


2021 ◽  
Vol 28 (2) ◽  
pp. 461-471
Author(s):  
Michael A. Chen ◽  
Benjamin D. Kocar

The study of in situ microscale biogeochemical processes represents a major challenge in the environmental sciences. The combination of microfluidic devices with X-ray fluorescence microprobe spectroscopy may address this need, but typical materials used in these devices attenuate the X-rays needed to analyze key elements of interest, such as Fe or As. In this work, a method is presented for fabricating an etched silicon microfluidic device that is sealed with a 30 µm thin glass window that is sufficiently transparent for X-ray fluorescence microprobe spectroscopy. The capabilities of these devices for X-ray microprobe spectroscopy are demonstrated using an Fe (hydr)oxide solid that is loaded with As and then infused with sulfide, on beamline 4-BM at NSLS-II, resulting in time-variant Fe precipitation reactions and As sorption. Key results include in situ X-ray fluorescence time-series maps of Fe, As and a Br flow tracer, as well as spot XANES at both the Fe K edge and As K edge. Additionally, multiple energy mapping is used to examine the spatial speciation of As over time. The results of this work clearly demonstrate the capabilities of this novel microfluidic system that can be analyzed using X-ray fluorescence microprobe spectroscopy and can be made to study a wide range of complex microscale geochemical systems.


Author(s):  
H. Ade

Many of the transmission x-ray microscopy developments since the late seventies, including the ones at the National Synchrotron Light Source (NSLS), were driven primarily by the potential of x-ray microscopy to image wet and unstained biological samples with low radiation dose. High image contrast between an aqueous environment and carbon based materials can be achieved with photon energies between the carbon and oxygen K absorption edges (290-540 eV). This contrast is based on differences in cross section of the elements oxygen and carbon in this energy range. Going beyond this "elemental" sensitivity, Ade et al. recently demonstrated how chemical (valence) sensitivity can be achieved via the X-ray Absorption Near Edge Structure (XANES) at the carbon K edge. In addition, linear dichroism microscopy can exploit the dependence of x-ray absorption resonances on the bond orientation relative to the linearly polarized x rays. For an application of the latter technique see A.P. Smith et al.


2009 ◽  
Vol 5 (S263) ◽  
pp. 145-146
Author(s):  
Sergio Pilling ◽  
Diana P. P. Andrade ◽  
Alvaro C. Neto ◽  
Roberto Rittner ◽  
Arnaldo N. de Brito

AbstractIn this work, we investigate the possible effects produced by soft X-rays (and secondary electrons) on Titan aerosol analogs in an attempt to simulate some prebiotic photochemistry. The experiments have been performed inside a high vacuum chamber coupled to the soft X-ray spectroscopy beamline at the Brazilian Synchrotron Light Source (LNLS). In-situ sample analysis were performed by a Fourier transform infrared spectrometer. The infrared spectra have presented several organic molecules, including nitriles and aromatic CN compounds. After the irradiation, the brownish-orange organic residue was analyzed ex-situ by gas chromatographic technique revealing the presence of adenine (C5H5N5), one of the constituents of the DNA molecule.


2017 ◽  
Vol 32 (S2) ◽  
pp. S22-S27 ◽  
Author(s):  
Dubravka Šišak Jung ◽  
Tilman Donath ◽  
Oxana Magdysyuk ◽  
Jozef Bednarcik

Characterization of semi and noncrystalline materials, monitoring structural phase transitions in situ, and obtaining structural information together with spatial distribution of the investigated material are only a few applications that hugely benefitted from the combination of high-energy X-rays and modern algorithms for data processing. This work examines the possibility of advancing these applications by shortening the data acquisition and improving the data quality by using the new high-energy PILATUS3 CdTe detector.


Author(s):  
Avril V. Somlyo ◽  
Andrew P. Somlyo

Electron probe x ray microanalysis [EPMA] provides quantitative information within a single spectrum about elements of biological interest with atomic number of 11 or greater. Therefore, the transport of ions and their accompanying co and counter ions across organelle membranes can be studied in situ by sampling within and adjacent to the intracellular organelle of interest under resting and stimulated conditions.EPMA is based on the fact that the ionization of atoms by fast electrons generates x rays having energies characteristic of the excited atoms. The interaction of incident fast electrons with atomic nuclei generates a background of continuum x rays. Elemental quantitation of ultra thin sections with EPMA is generally based on the linear relationship between elemental concentrations and the ratio of the number of characteristic/continuum. The use of this principle, together with the appropriate standards for calibration, has been the most successful approach for quantitative biological EPMA. The spatial resolution of EPMA at present is better than 10 nm and the practical limit of sensitivity for detecting calcium, (albeit with high electron dose), is approximately 0.3 mmol/kg dry wt. Two modes of data collection are utilized: fixed probe analysis of a region of interest or a scanning probe mode, where an x ray spectrum is collected at each picture point, to obtain quantitative elemental x ray maps. To preserve the morphology and the in vivo distribution of diffusible elements, we prepare specimens by rapid freezing in sub cooled Freon or, more recently with a Lifecell CF100 metal are mirror device; thin sections cut at -130 °C to -160 °C on a Reichert cryoultramicrotome. Msec time resolution of physiological are events can be achieved by freeze trapping.


MRS Bulletin ◽  
2004 ◽  
Vol 29 (3) ◽  
pp. 170-176 ◽  
Author(s):  
Gene E. Ice ◽  
Bennett C. Larson

AbstractIn this article, the authors describe the principle and application of differential-aperture x-ray microscopy (DAXM). This recently developed scanning x-ray microprobe technique uses a confocal or traveling pinhole camera approach to determine the crystal structure, crystallographic orientation, and elastic and plastic strain tensors within bulk materials. The penetrating properties of x-rays make the technique applicable to optically opaque as well as transparent materials, and it is nondestructive; this provides for in situ, submicrometer-resolution characterization of local crystal structure and for measurements of microstructure evolution on mesoscopic length scales from tenths to hundreds of micrometers. Examples are presented that illustrate the use of DAXM to study grain and subgrain morphology, grain-boundary types and networks, and local intra- and intergranular elastic and plastic deformation. Information of this type now provides a direct link between the actual structure and evolution in materials and increasingly powerful computer simulations and multiscale modeling of materials microstructure and evolution.


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