摘要:
To collect analyte in a supercritical fluid extraction process, the extractant flows to a collection container under pressure. In one embodiment, the collection container contains collection solvent through which the extractant flows to partition analyte. The extractant adds to the liquid and when the collection solvent-extractant mixture rises to a heating zone, the extractant vaporizes selecively since its vapor pressure is higher than the vapor pressure of the collection solvent. When its pressure exceeds a preset valve pressure it is vented so that extractant continually leaves the collection container. After the extraction is complete, the analyte is concentrated in the collection solvent. In another embodiment, the collection vessel includes a solid material on which the analyte collects. It is removed under pressure by a solvent that is concentrated under pressure.
摘要:
To control a solvent composition in a supercritical fluid system, a first pump pumps a first solvent through a first conduit into a mixer and a second pump pumps a second solvent through a second conduit into the mixer. First and second transducers measure the pressure in the first and second conduits and generate first and second signals proportional to the pressures. Each pressure signal is multiplied by a corresponding programmed concentration signal and compared to the programmed pressure in a feedback system to generate an error signal. The error signal is multiplied by concentration signals from a programmer to control the pumping rate of each pump. The pumps pressurize each fluid one at a time at the start of a run. The pressurization process is also used for producing disturbance-free flow as delivery is changed from one pump to another during prolonged runs.
摘要:
An apparatus for supercritical fluid extraction incorporates a removable extraction cartridge which in operation has insignificant pressure difference between its inside and outside walls. In one embodiment, the extractor includes a fraction collector for extractants, an automatic sample changer and an automatic cartridge transfer mechanism which provide completely automated extractions. To automatically perform extraction, valves for the fluids are automatically opened and closed in synchronism with the insertion and removal of the cartridges. These valves force a hard valve element into a softer valve seat with a valve stem that does not rotate significantly under the control of a rotary motor.
摘要:
To avoid deposits on the restrictor that channels extractant into a collector, a heated capillary tube pressure release restrictor, has a thermally insulated outlet end in a collecting trap substantially colder than the capillary tube. The restrictor is heated between the insulation and the capillary tube by Joulean heating. The solvent in the trap is at a pressure of 5 to 200 psi above atmospheric pressure. The thermal resistance of the insulation is selected to reduce the heat added to the extractant to a minimum and yet cause the temperature of the extractant to be in a range within which it is sufficiently hot so it does not freeze when added to the collection solvent but not so hot as to reduce partitioning of the extract and extractant before the extractant leaves the collection solvent. It has a thermal conductivity no greater than 60 BTU's per hour, per square foot, per inch for a one degree Fahrenheit difference.
摘要:
An apparatus for supercritical fluid extraction incorporates a removable extraction cartridge which in operation has insignificant pressure difference between its inside and outside walls. Because of the low pressure difference, the extraction cartridge need not have the strength to withstand significant pressure and can be made out of molded plastic for disposable use as well as stainless steel and/or machined plastic for reusability. The extraction cartridge can be removed and opened for sample access without the use of tools. The outside of the cartridge can be purged after it is installed in a heated high pressure vessel to remove contamination from its exterior. In one embodiment, the extractor includes a fraction collector fr extractants, an automatic sample changer and an automatic cartridge transfer mechanism which provide completely automated extractions.
摘要:
To supply a programmed gradient to a high pressure pump for introduction into a column, a mixer, degasser and accumulator communicates with the high pressure pump to supply fluid thereto, having a volume no more than 150 times the chamber volume of the high pressure pump. The mixer, degasser and accumulator includes temperature sensors which sense when the mixer, degasser and accumulator has been emptied to a level where it cannot respond to a demand for fluid from said high pressure pump and provides a signal to a low pressure pump which responds by cycling to again fill the mixer, degasser and accumulator. Upon receiving a demand signal, the low pressure pump fills by drawing fluid from a plurality of fluid sources to compose the gradient being used at that time, with the pump slowing during valve opening and closing so as to avoid cavitation.
摘要:
Purchase orders for chromatographic columns and sampler tubing are entered into based on estimating usage for a year. An initial partial shipment is made of tagged columns or tubing as the tubing or columns are used. An RFID transmits trigger signals until an order point is reached at which time a new partial shipment is made. This process is repeated until the end of the year.
摘要:
A liquid chromatographic system includes columns, column mounting fixtures to which the columns are mounted, a detector, a collector, a controller and a plurality of RFIDs. A first RFID communicates with the controller and cooperating RFIDs mounted to other components provide information such as the history of components, parameters and the like. They also receive information from sensors relating to the operation of the liquid chromatograph, store the information and transmit it. Moreover, the RFIDs may substitute for hard wiring in many applications and may enable a central computer to control several liquid chromatographic
摘要:
To pump supercritical carbon dioxide into a supercritical extractor without overpressure in the reservoir and to record the volume being delivered, the pumping speed is controlled and the volume pumped is determined from a pressure-related signal used in a feedback circuit. The feedback controls the velocity of pumping in conjunction with programmed values to avoid destructive reverse torque. A cam in the pump controls piston stroke, has a depressurization portion with an initial slope equal to but in the opposite direction of the final slope, rounded transition slopes, increasing linear velocity to the refill portion and constant velocity in the refill portion.
摘要:
A variable-orifice fluid restrictor for use with a supercritical extractor or chromatograph includes an inlet line for fluid at a pressure above its critical pressure, an extended tubular probe having an inner and an outer surface and a proximal and a distal end. The proximal end of the probe is disposed toward the inlet line. The distal end of the probe includes an adjustable orifice means adapted for metering the fluid and having first and second orifice members and an adjusting stem having first and second ends. The adjustable orifice means is adjacent to the outer surface of the probe and the orifice means is adjustable with the adjusting stem. The end of the adjusting stem is located at the distal end of the probe and is adapted for moving the first orifice member with respect to the second orifice member to control the adjustable orifice for varying the restriction of fluid passing through the adjustable orifice.