摘要:
To reduce tailing, the frit at the outlet to the liquid chromatographic column has a diameter substantially equal to that of the inside diameter of the outlet end of the column and less than two millimeters. It is held directly against the packing of the column within a cylindrical member having a shoulder with a central aperture at least the size of the diameter of the frit and cylindrical walls which are fastened to resist force in the direction of the axis of the column from its inlet to its outlet. A gasket seals the cylindrical holder against the column wall. The frit is formed of gold-plated nickel spheres sintered together at a temperature lower than the gold-nickel eutectic temperature of 950 degrees Celsius but above the phase-immiscibility temperature of 720 degrees Celsius. The size and shape of the frit is selected to reduce tailing by causing the flow path from the column to be uniform.
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. The distal end of the probe is inside the collector and the adjusting stem extends outside of the collector.
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.
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.
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.
摘要:
To prevent the solvents forming a gradient from mixing at the wrong place and to provide for accurate composition at start of the gradient in spite of solvent pressure variations, a microliquid or supercritical fluid chromatograph includes a combined mixer and pressure detector in which equal pressures of the two solvents in the gradient are detected by displacement of a ferromagnetic poppet in the mixing chamber. The poppet serves as a stop for the final solvent until the pressures are substantially equal and then its movement is detected by a circuit related to a linear variable differential transformer. The signal energizes a circuit which drives one of the sensing coils to drive the poppet during the gradient to provide mixing.
摘要:
To prevent the solvents forming a gradient from mixing at the wrong place and to provide for accurate composition at start of the gradient in spite of solvent pressure variations, a microliquid or supercritical fluid chromatograph includes a combined mixer and pressure detector in which equal pressures of the two solvents in the gradient are detected by displacement of a ferromagnetic poppet in the mixing chamber. The poppet serves as a stop for the final solvent until the pressures are substantially equal and then its movement is detected by a circuit related to a linear variable differential transformer. The signal energizes a circuit which drives one of the sensing coils to drive the poppet during the gradient to provide mixing.
摘要:
To reduce tailing, the frit at the outlet to the liquid chromatographic column has a diameter substantially equal to that of the inside diameter of the outlet end of the column and less than two millimeters. It is held directly against the packing of the column within a cylindrical member having a shoulder with a central aperture at least the size of the diameter of the frit and cylindrical walls which are fastened to resist force in the direction of the axis of the column from its inlet to its outlet. A gasket seals the cylindrical holder against the column wall. The frit is formed of gold-plated nickel spheres sintered together at temperature lower than the gold-nickel eutectic temperature of 950 degrees Celsius but above the phase-immiscibility temperature of 720 degrees Celsius. The size and shape of the frit is selected to reduce tailing by causing the flow path from the column to be uniform.
摘要:
To prevent the solvents forming a gradient from mixing at the wrong place and to provide for accurate composition at start of the gradient in spite of solvent pressure variations, a microliquid or supercritical fluid chromatograph includes a combined mixer and pressure detector in which equal pressures of the two solvents in the gradient are detected by displacement of a ferromagnetic poppet in the mixing chamber. The poppet serves as a stop for the final solvent until the pressures are substantially equal and then its movement is detected by a circuit related to a linear variable differential transformer. The signal energizes a circuit which drives one of the sensing coils to drive the poppet during the gradient to provide mixing.