Determining the Solubility of Organic Compounds in Supercritical Carbon Dioxide Using Supercritical Fluid Chromatography Directly Interfaced to Supercritical Fluid Solubility Apparatus

Abstract

The solubilities of benzoin and 3,3′,4,4′-benzophenonetetracarboxylic dianhydride in supercritical fluid carbon dioxide have been measured using static supercritical fluid solubility apparatus directly interfaced to supercritical fluid chromatography (SFC). The method involves increasing the pressure of supercritical fluid carbon dioxide in controlled steps to produce a series of saturated sample solutions that are sequentially analyzed by online SFC. The system requires minimal manual sample manipulation stages and facilitates a self-validation check procedure. Solubility data for benzoin was determined at 308 and 318 K through the pressure range of 12–24 MPa using 2 MPa steps. Solubility data for 3,3′,4,4′-benzophenonetetracarboxylic dianhydride was determined at 328 and 343 K through the pressure range 15–27.5 MPa using 2.5 MPa steps. The Mendéz-Santiago and Teja model has been successfully applied to correlate all sets of experimental solubility data.

Solubility Measurements of Chloramphenicol in Supercritical Fluid CO2 Using Static Solubility Apparatus Interfaced with Online Supercritical Fluid Chromatography

“…The AARD values obtained for chloramphenicol using eq 4 are within the range previously obtained for several other compounds whose SSV−SFC solubility results were successfully correlated using only the MST model. 8,9,20,29 The results are also in general agreement with the AARD values reported by a large number of other workers who have conducted SF-CO 2 solubility studies using a wide variety of different methods. 32,33…”

“…The semiempirical density-based model developed by Meńdez-Santiago and Teja 19 in an equation simplified by Hansen et al 28 has been previously successfully applied to correlate SSV−SFC experimental solubility data obtained for a range of compounds including: nifedipine and quinine, 8 PAHs, 9 caffeine, 20 and benzoin and 3,3′,4,4′-benzophenonetetracarboxylic dianhydride. 29 Therefore, the utility of the modified MST model was further evaluated by its application to the SSV−SFC solubility results measured for chloramphenicol. The modified MST equation is 23 Standard uncertainties u are: u(T) = 0.3 K, u(P) = 0.1 MPa; relative standard uncertainty, u r (y) = 0.08. where P is the pressure in MPa, P 0 is equal to 1.0 MPa, y is the mole fraction solubility of the chloramphenicol, ρ is the density of CO 2 in kg m −3 , and T is temperature in K. Using the MST model, the solubility of chloramphenicol is calculated using multiple linear regression to optimize parameters A, B, and C, which are independent of temperature.…”

Solute Diffusion into Polymer Swollen by Supercritical CO2 by High-Pressure Electron Paramagnetic Resonance Spectroscopy and Chromatography

“…The distribution coefficient of TEMPONE between the scCO 2 and polymer measurement was carried out using a custom-built system, described in [ 79 ], which included a high-pressure autoclave (stainless steel, total internal volume 150 mL, effective volume 143 mL, Figure 1 ), a sampling device (6-port valve Valco C6W equipped with a 10 µL dosing loop, VICI AG International, Schenkon, Switzerland), and a supercritical fluid chromatograph (Acquity UPC2 with a diode array spectrophotometric detector, Waters, Milford, MA, USA). General principles are described in [ 80 , 81 ].…”

Adsorption of N,N,N′,N′-Tetraoctyl Diglycolamide on Hypercrosslinked Polysterene from a Supercritical Carbon Dioxide Medium

“…We have earlier [ 31 ] proposed a static approach to sorption analysis in SC media based on on-line supercritical fluid chromatography (SFC). A similar approach was applied in several works to determine the substance solubility in SCF [ 32 , 33 , 34 , 35 ] and distribution coefficients in the liquid-SCF system [ 36 , 37 , 38 , 39 , 40 ], and to control chemical reactions [ 41 , 42 ]. It allows fast quantitative analysis of the considered system components without depressurization or special sample preparation.…”