Isco, Inc.

John N Jones

Robert W Allington

Abolghassem Y Tehrani

Yoossef Tehrani

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.

Chromatographic system

Chromatographic system with mixer

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.

Method of making a frit

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.

Apparatus for reducing tailing in a liquid chromatograph

To accommodate microscale chromatographs, a flow cell has an inlet port, inlet path, light path, outlet path and outlet port, with the inlet and outlet paths being formed continuously around wires of the proper diameters during molding. The wires pass through the mold and against a metal light-path insert during molding and are removed from the plastic after molding to form portions of the inlet and outlet paths. The insert for the light path is formed in two parts, each having a groove in the form of a half cylinder along its center for the light path and having channels on each side. The paths are machined prior to lapping, and after lapping, the light path is coated with a bright metal such as rhodium and then it is burnished for a mirror image with a roughness of less than sixteen RMS micro inches.

Chromatographic flow cell and method of making it

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 2 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.

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Lincoln, NE, United States of America

John N Jones