scholarly journals Simultaneous Infrared Spectroscopy, Raman Spectroscopy and Luminescence Sensing: A Multi-Spectroscopic Analyti-cal Platform

Author(s):  
Sarah Klingler ◽  
Julian Hniopek ◽  
Robert Stach ◽  
Michael Schmitt ◽  
Jürgen Popp ◽  
...  

Scientific questions in fields such as catalysis, monitoring of biological processes or environmental chemistry demand for analytical technologies combining orthogonal spectroscopies. Combined spectroscopic concepts facilitate in-situ on-line monitoring of dynamic processes providing for a better understanding of the involved reaction pathways. In the present study, a low-liquid-volume multi-spectroscopic platform was developed based on infrared attenuated total reflection (IR-ATR) spectroscopy combined with Raman spectroscopy and lumines-cence sensing. For demonstrating the measurement capabilities, exemplary analyte systems including water / heavy water and aqueous solutions of ammonium sulfate were analyzed as proof-of-principle studies. It was successfully demonstrated that three optical techniques may be integrated into a single analytical platform with-out interference providing synchronized and complementary datasets by probing the same minute sample vol-ume. In addition, the developed assembly provides a gas-tight lid sealing the headspace above the probed liq-uid for monitoring the concentration of molecular oxygen also in the gas phase via luminescence quenching. Hence, the entire assembly may be operated at inert conditions, as required for example during the analysis of photocatalytic processes.

2003 ◽  
Vol 57 (5) ◽  
pp. 574-579 ◽  
Author(s):  
Hannes Voraberger ◽  
Volker Ribitsch ◽  
Markus Janotta ◽  
Boris Mizaikoff

The presented work applies mid-infrared attenuated total reflection (ATR) spectroscopy to the measurment of hydrogen peroxide in aqueous matrices. The performance of different ATR crystals mounted in flow cells was investigated in the presence of aqueous hydrogen peroxide solutions. Quantitative determination has been achieved by evaluation of specific OH stretching and deformation vibrations with linear correlation between peak areas or peak heights and hydrogen peroxide concentration in the range of 1–10% (weight in water). Important aspects such as chemical stability of the waveguide material and influences of pH and ionic strength on the performance are discussed. Feasibility for the investigation of real world samples is demonstrated by measuring industrial bleaching solutions with known concentrations of hydrogen peroxide fitting well with calibration graphs established with neat hydrogen peroxide solutions. The presented sensor system is capable of determining hydrogen peroxide within complex matrices and clearly corroborates the potential of providing an in situ measurement concept for on-line hydrogen peroxide detection.


2003 ◽  
Vol 75 (9) ◽  
pp. 2166-2171 ◽  
Author(s):  
Nicolae Leopold ◽  
Michael Haberkorn ◽  
Thomas Laurell ◽  
Johan Nilsson ◽  
Josefa R. Baena ◽  
...  

2003 ◽  
Vol 83 (6) ◽  
pp. 668-680 ◽  
Author(s):  
Christopher Cannizzaro ◽  
Martin Rhiel ◽  
Ian Marison ◽  
Urs von Stockar

1996 ◽  
Vol 50 (7) ◽  
pp. 823-828 ◽  
Author(s):  
C. Esen ◽  
T. Kaiser ◽  
G. Schweiger

Raman spectroscopy was used to investigate polymerization reactions in a single micrometer-sized monomer droplet. An Ar+ laser levitated the microparticles and simultaneously excited the Raman scattering. The polymerization reaction was initiated by exposing the monomer droplets to the UV radiation of a mercury arc excitation lamp. The Raman spectrum of the reacting particle was investigated on-line. The results demonstrate that the combination of the technique of optical levitation and Raman spectroscopy allows nondestructive in situ measurements of single particles and is therefore very useful for the study of fundamental processes.


1996 ◽  
Vol 50 (1) ◽  
pp. 109-114 ◽  
Author(s):  
Lisheng Xu ◽  
John R. Schlup

Product quality in composite processing will be improved by dependable methods for monitoring the process. In this paper, the feasibility of using near-infrared attenuated total reflection (NIR ATR) spectroscopy as a sensor for monitoring epoxy resin cure is demonstrated. An ATR crystal serves as a contact sensor, which has several potential advantages over embedded optic fiber techniques previously reported. NIR ATR spectra obtained from several epoxy/amine systems show that both primary amine and epoxy functional groups have well-isolated absorption peaks in the near-infrared region. The utility of NIR ATR spectroscopy for in situ cure monitoring is demonstrated by following the reaction between phenyl glycidyl ether and butylamine at ambient temperature.


2018 ◽  
Vol 72 (9) ◽  
pp. 1396-1403 ◽  
Author(s):  
Brent A. Sperling ◽  
Berc Kalanyan

Silicon wafer-based internal reflection elements (IREs) present many practical advantages over the prisms conventionally used for attenuated total reflection (ATR) spectroscopy in the infrared. We examine two methods of using minimally prepared IREs that have appeared in the literature, edge-coupled (EC) and prism-coupled (PC), in conjunction with a liquid flow cell. Polarization measurements show that radiation entering the PC-IRE becomes depolarized due to stress-induced birefringence, and transmission through the edge of the EC-IRE also affects the polarization state. Quantification of the noise and a calibration using a series of sodium acetate solutions show the sensitivity of the PC-IRE outweighs the lower noise obtainable with the EC-IRE.


Author(s):  
Hans Bettermann ◽  
Peter Fischer

This contribution intends to show how Raman spectroscopy can be used to pursue processes inside PEM fuel cells. For this, two experimental setups have been worked out. At first a microscope objective was inserted into one bipolar plate. This enabled the detection of hydrogen, oxygen, nitrogen, vaporous and liquid water as well as changes in gas compositions and water distribution induced by an artificial pinhole within the MEA. A multiple-fiber Raman spectrometer with seven twin fibers was then developed to refine the look inside fuel cells. This setup permits the simultaneous record of gas compositions, liquid water and water vapor and how those species do change locally during operation. Beside the collection of data for modelling fuel cell processes, the multiple-fiber setup is primarily considered to monitor degradation processes and pre-stages of membrane damages.


Author(s):  
M.A. O’Keefe ◽  
J. Taylor ◽  
D. Owen ◽  
B. Crowley ◽  
K.H. Westmacott ◽  
...  

Remote on-line electron microscopy is rapidly becoming more available as improvements continue to be developed in the software and hardware of interfaces and networks. Scanning electron microscopes have been driven remotely across both wide and local area networks. Initial implementations with transmission electron microscopes have targeted unique facilities like an advanced analytical electron microscope, a biological 3-D IVEM and a HVEM capable of in situ materials science applications. As implementations of on-line transmission electron microscopy become more widespread, it is essential that suitable standards be developed and followed. Two such standards have been proposed for a high-level protocol language for on-line access, and we have proposed a rational graphical user interface. The user interface we present here is based on experience gained with a full-function materials science application providing users of the National Center for Electron Microscopy with remote on-line access to a 1.5MeV Kratos EM-1500 in situ high-voltage transmission electron microscope via existing wide area networks. We have developed and implemented, and are continuing to refine, a set of tools, protocols, and interfaces to run the Kratos EM-1500 on-line for collaborative research. Computer tools for capturing and manipulating real-time video signals are integrated into a standardized user interface that may be used for remote access to any transmission electron microscope equipped with a suitable control computer.


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