Measurement of the solubility of metal complexes in supercritical carbon dioxide using a UV–vis spectrometer

Haruki, Masashi; Kobayashi, Fumiya; Kishimoto, Kazuya; Kihara, Sorin; Takishima, Shigeki

doi:10.1016/j.fluid.2009.03.010

Cited by 29 publications

(20 citation statements)

References 14 publications

(27 reference statements)

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“…Despite the great potential of organometallic complexes for a variety of applications in organic synthesis, removal of toxic metal compounds, and processing of advanced functional materials as catalysts or precursors, the available solubility data of the organometallic complex in sc CO 2 [17][18][19][20] are obviously fewer than those of other compounds in sc CO 2 .…”

Section: Introductionmentioning

confidence: 99%

Solubility determination of organometallic complexes in supercritical carbon dioxide by chromatographic impulse response method

Kong

Sone

Sako

et al. 2011

Fluid Phase Equilibria

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The solubilities of organometallic complexes in supercritical CO 2 were determined from retention factors measured by the chromatographic impulse response (CIR) method, in which a solute was pulse-injected into a supercritical CO 2 flowing in a polymer coated open capillary column, and the response curve, i.e. time change of solute concentration, was monitored at the exit of the column. The retention factor and binary diffusion coefficient were simultaneously obtained as two parameters so that the fitting error between response curves of solute species measured and calculated was minimized. The validities of the method and the apparatus employed in this study were verified by determining the solubilities of naphthalene, which have extensively been reported in the literature. Then, the solubilities of organometallic complexes such as ferrocene and cobalt (III) acetylacetonate in supercritical CO 2 were determined. The data determined in this study were in good agreement with the literature data. The solubilities were also correlated with the Chrastil equation including the three adjustable parameters.

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Section: Introductionmentioning

confidence: 99%

Solubility determination of organometallic complexes in supercritical carbon dioxide by chromatographic impulse response method

Kong

Sone

Sako

et al. 2011

Fluid Phase Equilibria

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“…The spectra shapes of anthracene in supercritical carbon dioxide, hexane, acetone and toluene are almost identical although a peak shift of about 8 nm was observed between supercritical carbon dioxide and the two organic solvents. A calibration curve was prepared using acetone and hexane according to Haruki et al (2009Haruki et al ( , 2010Haruki et al ( , 2011aHaruki et al ( , 2011bHaruki et al ( , 2013. The calibration curve was obtained using the average absorbance in the entire peak wavelength to reduce the significant spectral shift due to a change in fluid density (Inomata et al, 1993;Rice et al, 1995).…”

Section: Determination Methods Of the Concentration Of Anthracene In Smentioning

confidence: 99%

Effects of Solution Concentrations on Crystal Growth of Anthracene Thin Films on Silicon by Rapid Expansion of Supercritical Solutions (RESS) Using Carbon Dioxide

Fujii

Takahashi

Uchida

2015

J. Chem. Eng. Japan / JCEJ

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We report on an investigation to the e ects of supercritical solution concentrations on the crystal morphology, crystallinity, growth rate, and number density of anthracene grains in thin lms on silicon substrates by rapid expansion of supercritical solutions (RESS) using carbon dioxide to examine the crystal growth mechanism of anthracene thin lms. (molar fraction; a threshold concentration) with a change in morphology of grains from dendritic to island-like. Although the number densities of island-like and dendritic grains increased almost linearly with the solution concentration, the trend in the number density of grains also changed at the threshold concentration, with the change in morphology from dendritic to island-like grains. The crystal growth of grains deposited on the substrate was dominant and most of the given supersaturation was consumed for the crystal growth of grains at solution concentrations lower than the threshold concentration. At solution concentrations higher than the threshold concentration, the crystal nucleation on the substrate was dominant and most of the given supersaturation was consumed for the crystal nucleation of grains, followed by the crystal growth of the grains.

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“…The solubility of Co(acac) 3 in scCO 2 at 70 C and 20 MPa was 5 Â 10 À5 mole fraction. [24] A stainless steel screen was placed in the middle of the vessel to separate the RFA substrate and the stirring bar. The system was sealed and heated to 70 C using a circulating heater/cooler (Cole Parmer, Model 12108-15).…”

Section: Cobalt Loading On Rfas By Scdmentioning

confidence: 99%

Supercritical Deposition Coupled with Ammonia Treatment: A New Route to Co‐Promoted N‐Doped Carbon Aerogels with High Oxygen Reduction Reaction Activity

et al. 2019

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A new highly active family of Co‐promoted N‐doped carbon aerogel catalysts is prepared by a supercritical CO2‐assisted technique combined with NH3 treatment. The active sites are created during the complex transformation of an organic aerogel to a carbon aerogel in the presence of cobalt by NH3 as the source of nitrogen and pyrolysis medium. The mass activity for oxygen reduction reaction (ORR) is highest for the catalyst pyrolyzed at 800 °C. The catalyst displays similar activity for ORR as a commercial Pt/C catalyst. Moreover, the catalyst exhibits nearly double the mass activity of N‐doped carbon aerogel pyrolyzed at the same temperature. The nature of the active sites for ORR is also investigated by selectively adding or removing various species (i.e., Co–Nx and Co–O) via post acid–base treatments. After removing the Co species from the catalyst, the same activity as the parent catalyst is achieved suggesting that the Co species in the catalyst are spectators in ORR catalysis and they serve only to promote the formation of catalytically active graphitic N sites during pyrolysis in NH3. A strong correlation is found between the relative distribution of graphitic N species and the mass activity.

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Measurement of the solubility of metal complexes in supercritical carbon dioxide using a UV–vis spectrometer

Cited by 29 publications

References 14 publications

Solubility determination of organometallic complexes in supercritical carbon dioxide by chromatographic impulse response method

Solubility determination of organometallic complexes in supercritical carbon dioxide by chromatographic impulse response method

Effects of Solution Concentrations on Crystal Growth of Anthracene Thin Films on Silicon by Rapid Expansion of Supercritical Solutions (RESS) Using Carbon Dioxide

Supercritical Deposition Coupled with Ammonia Treatment: A New Route to Co‐Promoted N‐Doped Carbon Aerogels with High Oxygen Reduction Reaction Activity

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