Flow control system for liquid chromatographs

• US 4,137,011 A
• Filed: 06/14/1977
• Issued: 01/30/1979
• Est. Priority Date: 06/14/1977
• Status: Expired due to Term

• Current Assignee: Thermo Instrument Systems, Inc. (Thermo Fisher Scientific Incorporated)
• Original Assignee: Spectra-Physics Incorporated (MKS Instruments Incorporated)
• Inventors: Rock, John V.
• Primary Examiner(s): Garrett, Robert E.
• Assistant Examiner(s): Look, Edward
• Application Number:
  US05/806,591
• Time in Patent Office: 595 Days
• Field of Search: 417/1-5, 417/18, 417/22, 417/42-45, 417/53, 73/23.1
• US Class Current: 417/22
• CPC Class Codes: F04B 11/0058 with piston speed control
• CPC Class Codes: F04B 2203/0209 Rotational speed
• CPC Class Codes: F04B 49/20 by changing the driving speed
• CPC Class Codes: G01N 30/34 of fluid composition, e.g. gradient G01N30/36 takes precedence
• CPC Class Codes: G05D 7/0688 by combined action on throttling means and flow sources G05D7/0694 takes precedence

Abstract

A flow control system including a pump for delivering a carrier containing isocratic or gradient controlled elution solvents under pressure to a liquid chromatographic column at a substantially constant selected controlled flow rate.

Claims

1. In a liquid chromatograph system having a motor driven pump for supplying a carrier containing isocratic or gradient controlled elution solvents and for delivering the carrier to an LC column under pressure, a method of flow control of the pump output comprising the steps of measuring pump output pressure over at least one cycle of pump operation at constant pump motor speed to develop a pressure reference level for a given carrier;

subsequently varying the speed drive of the pump motor to maintain the output pressure equal to the pressure reference level;

measuring the pattern of pump motor speed during a cycle of operation;

storing said pattern in a memory to provide a pump motor speed reference, measuring the actual pump motor speed during operation of the system;

comparing the pump motor speed reference and actual pump motor speed to obtain a difference signal in speed caused by changes in system variables;

continually changing the pressure reference level applied to the pump in response to the difference signal.

2. A method of flow control for liquid chromatographs as in claim 1 in which the pump motor is driven with a pulse stepping motor the speed of which varies as a function of the frequency of pulses delivered thereto, and further in which the motor speed pattern is measured in discrete time intervals, the average pump motor speed over each interval being stored as a pulse count for that interval, and further in which the comparing step is carried out by comparing the actual counted pulses C of one interval of operation to the number of reference pulses S stored in memory for that interval to derive said difference signal, applying this difference signal to change the pressure reference level in the next successive interval to modify the demand pressure applied therein, continuing the foregoing steps during each successive interval of the operation of the pump.

3. In a liquid chromatograph system having an LC column for receiving a sample to be analyzed in a liquid carrier delivered under pressure to the column, a motor driven pump for supplying said carrier containing isocratic or gradient controlled elution solvents, means for controlling the flow of the pump output comprising means for measuring pump output pressure over at least one cycle of pump operation at constant pump motor speed to develop a pressure reference level for a given carrier;

means for varying the speed drive of the pump motor to maintain the output pressure equal to the pressure reference level;

means for measuring the pattern of pump motor speed during a cycle of operation and for storing said pattern in a memory to provide a pump motor speed reference, means for measuring the actual pump motor speed during operation of the system;

means for comparing the pump motor speed reference and actual pump motor speed to obtain a difference signal in speed caused by changes in system variables;

means responsive to said difference signal for continually changing the pressure reference level applied to the pump in response thereto to maintain flow constant.

4. Apparatus as in claim 3 in which the pump motor includes a pulse stepping motor the speed of which varies as a function of the frequency of pulses delivered thereto, and further in which the means for measuring motor speed pattern operates over discreet time intervals, the average pump motor speed over each interval being stored as a pulse count for that interval, and further in which the means for comparing the actual counted pulses C of one interval of operation to the number of reference pulses S stored in memory for that interval to derive said difference signal, and in which the means responsive to said difference signal changes the pressure reference level in the next successive interval to modify the demand pressure applied therein.

5. In a liquid chromatograph system means forming an LC column, reservoir means for supplying carrier components at low pressure, a single pump system for taking said carrier components at said low pressure and for delivering the same to said LC column at a high pressure, operative means at said low pressure for selecting isocratic or gradient elution proportions of said carrier components and for supplying the same to said single pump system, means for controlling the flow of the pump output comprising means for measuring pump output pressure over at least one cycle of pump operation at constant pump motor speed to develop a pressure reference level for a given carrier;

means for varying the speed drive of the pump motor to maintain the output pressure equal to the pressure reference level;

means for measuring the pattern of pump motor speed during a cycle of operation and for storing said pattern in a memory to provide a pump motor speed reference, means for measuring the actual pump motor speed during operation of the system;

means for comparing the pump motor speed reference and actual pump motor speed to obtain a difference signal in speed caused by changes in system variables;

means responsive to said difference signal for continually changing the pressure reference level applied to the pump in response thereto to maintain flow constant.

6. A liquid chromatography system as in claim 5 in which said pump system includes a piston operated multiple chamber reciprocating pump.