Polymer additive characterization by capillary supercritical fluid chromatography/Fourier transform infrared microspectrometry

Raynor, Mark W.; Bartle, Keith D.; Davies, I. L.; Williams, Alan; Clifford, Anthony A.; Chalmers, John M.; Cook, Bernard W.

doi:10.1021/ac00156a011

Cited by 92 publications

(14 citation statements)

References 37 publications

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“…Equation ( 1 ) can be used to predict the rate of extraction from spherical particles. If the natural logarithm of this equation is taken, a characteristic time, t,, is defined as I t, = -?r2D ( 5 ) and factorizing the term exp(t/t,) gives the result…”

Section: Diffusion Limited Extractionsmentioning

confidence: 99%

Rate and extent of supercritical fluid extraction of additives from polypropylene: Diffusion, solubility, and matrix effects

Cotton

Bartle

Clifford

et al. 1993

J of Applied Polymer Sci

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SYNOPSISAnalytical extraction of additives from polymers using a supercritical fluid (SFE) is a promising alternative to liquid extraction. Factors affecting SFE with carbon dioxide of Irgafos 168 and Irganox 1010 from commercial polypropylene have been studied, with analysis of extracts by capillary supercritical fluid chromatography (SFC) . A diffusion limited extraction model was investigated by measuring the rate of SFE as a function of pressure, particle size, flow rate, and temperature. The rate of extraction was found to fit the sum of exponential decays; results were also consistent with an extrapolation procedure to obtain the total mass of additive without exhaustive extraction. Derived diffusion coefficients for the additive in polypropylene differed from literature values by approximately two orders of magnitude apparently because of swelling of the polymer by sorbed carbon dioxide. The variation of extraction rate with pressure and flow rate confirmed the solubility limitation of proposed model. The rate of extraction increased between 20 and 140°C, then fell away at higher temperatures with the onset of melting.

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Section: Diffusion Limited Extractionsmentioning

confidence: 99%

Rate and extent of supercritical fluid extraction of additives from polypropylene: Diffusion, solubility, and matrix effects

Cotton

Bartle

Clifford

et al. 1993

J of Applied Polymer Sci

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“…Common mobile phases like carbon dioxide have high transparency in the ultraviolet (UV) and infrared (IR) regions of the electromagnetic spectrum and are also compatible with flame based detectors and mass spectrometry (MS) [ll]. The volatility of the mobile phase also enables SFC to be coupled with Fourier transform infrared spectrometry (FTIR) using a microscope accessory and a solvent elimination interface [12].…”

Section: Discussionmentioning

confidence: 99%

“…The other end of the column was butt-connected as previously described [12], to two fused silica capillaries with tapered restrictors at their ends. One was installed in the FID and the other was used as a transfer line to the solvent elimination interface.…”

Section: Supercritical Fluid Chromatographymentioning

confidence: 99%

Supercritical fluid extraction / capillary supercritical fluid chromatography / Fourier transform infrared microspectrometry of polycyclic aromatic compounds in a coal tar pitch

Raynor

Davies

Bartle

et al. 1988

J. High Resol. Chromatogr.

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The combination of supercritical fluid extraction, high resolution capillary supercritical fluid chromatography, and Fourier transform infrared microspectrometry is described for the separation and identification of polycyclic aromatic hydrocarbons in a coal tar pitch. The variable solvating power of the supercritical fluid was utilized to selectively fractionate the sample. The fluid extract was decompressed through a frit restrictor into the sample cavity of a cooled microvalve injector, where the analytes were deposited and concentrated for subsequent chromatographic analysis. Several of the analytes separated in the chromatograph were collected on a potassium bromide disc at a solvent elimination interface for subsequent infrared analysis involving the use of an infrared microscope accessory. The spectra obtained show the power of this detection technique for distinguishing between isomers.

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“…Supercritical fluid chromatography has also been applied to the determination of polymer additives (Raynor et al 1988;Carrott 1998). The most widely used technique for determination of non-volatile additives is high performance liquid chromatography (HPLC) with UV detection (Lichtenthaler and Ranfelt 1978;Haney and Dark 1980;Schabron and Fenska 1980;Hodgeman 1981;Perlstein 1983;Munteanu et al 1987;Freitag 1988;Caceres et al 1996;Smith and Taylor 2002).…”

Section: Introductionmentioning

confidence: 99%

Determination of Chimassorb 944 in Polypropylene Geotextiles by HPLC-UV

et al. 2011

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This paper reports the development of a method for the determination of Chimassorb 944 (C944), in polypropylene geotextiles, by high performance liquid chromatography with ultraviolet detection. The C944 was removed from the geotextiles by an ultrasonic extraction and then separated in a NH 2 column, followed by UV detection at 244 nm. Analytical validation showed that the method is accurate and precise. The developed methodology was applied for the determination of C944 in geotextiles exposed to artificial UV radiation and to natural weathering. To the best of our knowledge, this is the first method proposed for the determination of C944 in geotextiles.

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Polymer additive characterization by capillary supercritical fluid chromatography/Fourier transform infrared microspectrometry

Cited by 92 publications

References 37 publications

Rate and extent of supercritical fluid extraction of additives from polypropylene: Diffusion, solubility, and matrix effects

Rate and extent of supercritical fluid extraction of additives from polypropylene: Diffusion, solubility, and matrix effects

Supercritical fluid extraction / capillary supercritical fluid chromatography / Fourier transform infrared microspectrometry of polycyclic aromatic compounds in a coal tar pitch

Determination of Chimassorb 944 in Polypropylene Geotextiles by HPLC-UV

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