Nondispersive Infrared Gas Analyzer for Vapor Density Measurements of a Carbonyl-Containing Organometallic Cobalt Precursor

2017 ◽  
Vol 71 (12) ◽  
pp. 2632-2642 ◽  
Author(s):  
James E. Maslar ◽  
William A. Kimes ◽  
Brent A. Sperling ◽  
Ravindra K. Kanjolia
Keyword(s):  
Bandpass Filter ◽  
Sampling Rate ◽  
Signal Averaging ◽  
Gas Analyzer ◽  
Vapor Density ◽  
Flow Conditions ◽  
Ft Ir ◽  
Infrared Gas Analyzer ◽  
Ft Ir Spectroscopy

A nondispersive infrared (NDIR) gas analyzer was demonstrated for measuring the vapor-phase density of the carbonyl-containing organometallic cobalt precurso μ2-η2-(tBu-acetylene) dicobalthexacarbonyl (CCTBA). This sensor was based on direct absorption by CCTBA vapor in the C≡O stretching spectral region and utilized a stable, broadband IR filament source, an optical chopper to modulate the source, a bandpass filter for wavelength isolation, and an InSb detector. The optical system was calibrated by selecting a calibration factor to convert CCTBA absorbance to a partial pressure that, when used to calculate CCTBA flow rate and CCTBA mass removed from the ampoule, resulted in an optically determined mass that was nominally equal to a gravimetrically-determined mass. In situ Fourier transform infrared (FT-IR) spectroscopy was performed simultaneously with the NDIR gas analyzer measurements under selected conditions in order to characterize potential spectroscopic interferences. Interference due to CO evolution from CCTBA was found to be small under the flow conditions employed here. A CCTBA minimum detectable molecular density as low as ≈3 × 1013 cm−3 was calculated (with no signal averaging and for a sampling rate of 200 Hz). While this NDIR gas analyzer was specifically tested for CCTBA, it is suitable for characterizing the vapor delivery of a range of carbonyl-containing precursors.

scholarly journals Monitoring the Interfacial Polymerization of Piperazine and Trimesoyl Chloride with Hydrophilic Interlayer or Macromolecular Additive by in-situ FT-IR Spectroscopy

2019 ◽  
Author(s):  
Xi Yang
Keyword(s):  
Ir Spectroscopy ◽  
Reaction Rate ◽  
Interfacial Polymerization ◽  
Reaction System ◽  
Reaction Rates ◽  
Water Permeation ◽  
Ft Ir ◽  
Trimesoyl Chloride ◽  
Ft Ir Spectroscopy

The interfacial polymerization (IP) of piperazine (PIP) and trimesoyl chloride (TMC) has been extensively utilized to synthesize the nanofiltration (NF) membrane. However, it is still a huge challenge to monitor the IP reaction, because of the fast reaction rate and the formed ultra-thin film. Herein, two effective strategies are applied to reduce the IP reaction rate: (1) the introduction of hydrophilic interlayers between the porous substrate and the formed polyamide layer; (2) the addition of macromolecular additives in the aqueous solution of PIP. As a result, in-situ FT-IR spectroscopy was firstly used to monitor the IP reaction of PIP/TMC reaction system, with hydrophilic interlayers or macromolecular additives. Moreover, we study the formed polyamide layer growth on the substrate, in a real-time manner. The in-situ FT-IR experimental results confirm that the IP reaction rates are effectively suppressed and the formed polyamide thickness reduces from 138±24 nm to 46±2 nm. Furthermore, the optimized NF membrane with excellent performance are consequently obtained, which include the boosted water permeation flux about 141~238 (L·m2·h/MPa) and superior salt rejection of Na2SO4 > 98.4%.

Ethylene polymerization on a SiH4-modified Phillips catalyst: detection of in situ produced α-olefins by operando FT-IR spectroscopy

2012 ◽  
Vol 14 (7) ◽  
pp. 2239 ◽  
Author(s):  
Caterina Barzan ◽  
Elena Groppo ◽  
Elsje Alessandra Quadrelli ◽  
Vincent Monteil ◽  
Silvia Bordiga
Keyword(s):  
Ir Spectroscopy ◽  
Ethylene Polymerization ◽  
Phillips Catalyst ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

scholarly journals In Situ IR Characterization of CO Interacting with Rh Nanoparticles Obtained by Calcination and Reduction of Hydrotalcite-Type Precursors

2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
F. Basile ◽  
I. Bersani ◽  
P. Del Gallo ◽  
S. Fiorilli ◽  
G. Fornasari ◽  
...  
Keyword(s):  
Crystal Size ◽  
Liquid Nitrogen Temperature ◽  
Transmission Electron ◽  
In Situ Ir ◽  
Ft Ir ◽  
Co Disproportionation ◽  
Ft Ir Spectroscopy

Supported Rh nanoparticles obtained by reduction in hydrogen of severely calcined Rh/Mg/Al hydrotalcite-type (HT) phases have been characterized by FT-IR spectroscopy of adsorbed CO [both at room temperature (r.t.) and nominal liquid nitrogen temperature] and Transmission Electron Microscopy (TEM). The effect of reducing temperature has been investigated, showing that Rh crystal size increases from 1.4 nm to 1.8 nm when the reduction temperature increases from 750°C to 950°C. The crystal growth favours the formation of bridged CO species and linear monocarbonyl species with respect to gem-dicarbonyl species; when CO adsorbs at r.t., CO disproportionation occurs on Rh and it accompanies the formation of RhI(CO)2. The role of interlayer anions in the HT precursors to affect the properties of the final materials has been also investigated considering samples prepared from silicate-instead of carbonate-containing precursors. In this case, formation of RhI(CO)2 and CO disproportionation do not occur, and this evidence is discussed in terms of support effect.

In Situ Studies of Coatings on Metal Wires by FT-IR External Reflectance Spectroscopy

1987 ◽  
Vol 41 (7) ◽  
pp. 1172-1175 ◽  
Author(s):  
Gi Xue ◽  
Shi-Ying Liu ◽  
Yi Jin ◽  
Shan-Geng Jiang
Keyword(s):  
Diffuse Reflectance ◽  
Collection Efficiency ◽  
Scattered Light ◽  
Attenuated Total Reflection ◽  
Light Collection ◽  
Wire Sample ◽  
Ft Ir ◽  
Metal Wires ◽  
Ft Ir Spectroscopy

Diffuse reflectance FT-IR spectroscopy was originally developed for particulate samples dispersed in KBr powders. Now, by using ellipsoid mirrors for scattered light collection, we have taken advantage of the collection efficiency of diffuse reflectance optics and have extended their use to an in situ study of coatings on metal wires and of the broken surface of a reinforcement wire as well. The result is that spectra of coatings on wire show good overall agreement with external reflection spectra of thin films. The technique we have developed has an advantage over infrared attenuated total reflection (ATR), in that there is no optical contact problem between the wire sample and ATR crystal.

The effect of high external pressure on the structure and stability of MOF α-Mg3(HCOO)6 probed by in situ Raman and FT-IR spectroscopy

2015 ◽  
Vol 3 (22) ◽  
pp. 11976-11984 ◽  
Author(s):  
Haiyan Mao ◽  
Jun Xu ◽  
Yue Hu ◽  
Yining Huang ◽  
Yang Song
Keyword(s):  
High Pressure ◽  
Ir Spectroscopy ◽  
Vibrational Spectroscopy ◽  
External Pressure ◽  
Structural Transitions ◽  
In Situ Raman ◽  
Ft Ir ◽  
High Pressure Study ◽  
Ft Ir Spectroscopy

A first high-pressure study on MOF α-Mg3(HCOO)6 probed by in situ vibrational spectroscopy revealed strongly contrasting host-dependent structural transitions and stabilities.

Mechanistic Study of Silsesquioxane Synthesis by Mass Spectrometry and in Situ ATR FT-IR Spectroscopy

2003 ◽  
Vol 107 (42) ◽  
pp. 8885-8892 ◽  
Author(s):  
Paolo P. Pescarmona ◽  
Maria E. Raimondi ◽  
John Tetteh ◽  
Ben McKay ◽  
Thomas Maschmeyer
Keyword(s):  
Mass Spectrometry ◽  
Ir Spectroscopy ◽  
Mechanistic Study ◽  
Ft Ir ◽  
Ft Ir Spectroscopy
Sign in / Sign up

Export Citation Format

Share Document