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System for measuring the solubility of solid compounds in supercritical fluids
| Details |
Inventors: Pauchon, Veronique; Jose, Jacques; Behar, Emmanuel;
Assignee: Institut Francais du Petrole (Rueil-Malmaison, FR)
Primary Examiner: Raevis; Robert
Assistant Examiner:
Attorney, Agent or Firm: Antonelli, Terry, Stout & Kraus, LLP
A system for measuring the solubility of various solid organic compounds in supercritical fluids such as methane or carbon dioxide for example, and for studying the equilibrium between the solid phase and the supercritical phase in a wide pressure and temperature range is disclosed. The system comprises four functional units E1, E2, E3, E4. Unit E1 delivers a supercritical fluid (methane, CO.sub.2, etc.), unit E2 comprises a sampling cell containing the compound to be solubilized, where the pressurized gas from unit E1 saturates on contact therewith, unit E3 is intended for sampling and bringing the sample into solution, and unit E4 is intended to receive the saturated fluid and to analyze it. The system allows dynamic solubilization to be performed with on-line or off-line analysis of the sample. The system can be applied for production of very pure compounds isolated from mixtures of heavy hydrocarbons for example or from alloys, or in the agribusiness for isolation of flavors. |
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DETAILED DESCRIPTION A system according to the invention measures the solubility of solid compounds in supercritical fluids and notably in carbon dioxide or methane.
It comprises a fluid delivery device delivering fluid in a supercritical state at a constant pressure, a saturation cell wherein the fluid saturates the compound to be dissolved and a saturated fluid reception device is connected to the saturation cell by means of a multi-way valve.
The fluid delivery device comprises a pump including a pressure regulator (which may be a concentration gradient type pump for example) associated with complementary pressure and a temperature regulator.
According to an embodiment, these complementary pressure and temperature regulators comprise a filter, a device which establishes a leak rate and a gas surge capacity, and a pump associated with a constant-temperature bath.
According to another embodiment, a saturation cell is provided with a strainer of controlled porosity.
According to another embodiment, a fluid flow control comprises a constant-pressure chamber connected to the saturation cell by means of the multi-way valve.
The constant-pressure chamber comprises for example a volume of mercury and mercury expansion device.
According to another embodiment, the saturation cell, the constant-pressure chamber and the multi-way valve are placed in a thermostatically-controlled enclosure.
The system preferably comprises a device suited for sampling and for bringing the sample into solution, coupled by a multi-way valve to an analysis device which includes a chromatographic column and a detector such as a spectrophotometer operating in the ultraviolet range.
The system preferably comprises a device which generates a pressure drop in order to control the pressure in an analysis device.
The saturation cell comprises for example an elongate chamber arranged vertically and circuits communicating the delivery device with the upper part of the chamber.
The analysis devices used are for example a liquid phase chromatograph or a spectrophotometer operating in the ultraviolet
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MEMS 
