Liquid chromatography apparatus

• US 4,233,156 A
• Filed: 03/07/1979
• Issued: 11/11/1980
• Est. Priority Date: 03/10/1978
• Status: Expired due to Term

• Current Assignee: Hitachi, Ltd.
• Original Assignee: Hitachi, Ltd.
• Inventors: Ohnuma, Sadabumi, Tsukada, Katsuo
• Primary Examiner(s): Adee, John
• Application Number:
  US06/018,334
• Time in Patent Office: 615 Days
• Field of Search: 210/101, 210/198 C, 210/138, 73/61.1 C
• US Class Current: 210/101
• CPC Class Codes: B01D 15/08 Selective adsorption, e.g. chromatography
• CPC Class Codes: B01D 15/14 relating to the introduction of the feed to the apparatus
• CPC Class Codes: B01D 15/163 Pressure or speed conditioning
• CPC Class Codes: B01D 15/166 Fluid composition conditioning, e.g. gradient
• CPC Class Codes: G01N 2030/326 pumps
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence
• CPC Class Codes: G01N 30/34 of fluid composition, e.g. gradient G01N30/36 takes precedence

Abstract

A plurality of liquid mobile phases stored in a plurality of reservoirs respectively are filled and pumped by a dual pump driven by a stepping motor, through valves complementarily subjected to on-off control by a gradient programmer. The dual pump has two pistons in contact with the periphery of a cam in opposition to each other at 180 degrees, which pistons fill and pump the liquid mobile phases by linear reciprocation along the contour of the cam with the rotation of the cam. The radius of the cam linearly increases in the range from 0 to 180 degrees and linearly decreases in the range from 180 to 360 degrees at the same rate as when it increases. An electric signal is produced from a timing device during a period from the rotational positions of the cam reaches 0 and 180 degrees to a predetermined rotational positions. The liquid mobile phase delivered from the dual pump is supplied to a pressure transducer, and after passing through it, supplied to a column through an injector for injecting a specimen. The components into which the specimen is separated are detected by a detector. When the timing device detects that the cam is positioned in intervals from 0 and 180 degree to a predetermined angle therefrom, the motor control circuit drives the stepping motor at high speed during period from a time which the time derivative of the back pressure signal from the pressure transducer reaches value smaller than a predetermined value to a time it reaches value larger than the predetermined value.

Claims

1. A liquid chromatography apparatus comprising:

at least one reservoir for storing at least one liquid mobile phase;

at least one valve for controlling the liquid mobile phase flowing out of said at least one reservoir;

a reciprocating dual-piston pump including two pistons for filling two chambers with the liquid mobile phase flowing out of said valve and pumping alternately the liquid mobile phase filled in said chambers, one end of each piston being in contact with the periphery of a rotatable cam in opposition to one end of the other piston at 180 degrees, the other end of each piston extending into each of said chambers, each of said pistons being reciprocated linearly along the contour of said cam with the rotation of said cam, thus filling said liquid mobile phase into said chambers and pumping said liquid mobile phase out of said chambers;

an injector for injecting a specimen into the liquid mobile phase passed through said pump;

a column for separating the specimen injected by said injector, into components;

a detector for detecting the components of said specimen separated by said column;

a programmer for controlling the operating time of said at least one valve;

motor means coupled to said cam of said pump for driving said pump through successive cycles of reciprocation;

said cam having a shape such that when the time derivative of displacement of one piston is positive over an angle range, the time derivative of displacement of the other piston is a negative fixed value over substantially the entire angle range that said one piston is positive, and when the time derivative of displacement of said one piston is negative over an angle range, the time derivative of displacement of said other piston is a positive fixed value over substantially the entire angle range that said one piston is negative.

2. A liquid chromatography apparatus according to claim 1, further comprising:

a pressure transducer connected between said reciprocating dual-piston pump and said injector for providing an electric signal proportional to the flow rate of said liquid mobile phase from said pump, and

a motor control circuit for applying to said motor means a control signal for controlling the reciprocating speed of said reciprocating dual pistons in esponse to an electric signal from said pressure transducer.

3. A liquid chromatography apparatus according to claim 2, wherein said motor control circuit includes a circuit for providing a high-speed rotation command to said motor means until the time derivative of the electric signal provided from said pressure transducer reaches a level larger than a predetermined value.

4. A liquid chromatography apparatus according to claim 1, wherein said motor comprises a stepping motor, and

said motor control circuit includes:

a differentiator for differentiating an electric signal from said pressure transducer;

a comparator which produces an output only when the output of said differentiator is reduced below a predetermined output value,

a first AND circuit for calculating a logic product of the outputs of said timing device and said comparator and producing an output when both of said outputs are "high";

a high frequency pulse generator for producing a high frequency pulse for driving said stepping motor at high speed when the output of said first AND circuit is high level;

a variable frequency pulse generator for producing a variable frequency pulse for driving said stepping motor at a steady speed to correspond a predetermined discharge flow rate; and

a switching circuit including

an AND circuit impressed with the output of said first AND circuit and the output of said high frequency pulse generator, and producing to said motor drive circuit an output for driving said stepping motor at high speed when both of the outputs of said first AND circuit and said high frequency pulse generator are "high", and a NAND circuit impressed with the output of said first AND circuit and the output of said variable frequency pulse generator, and applying to said motor drive circuit an output for driving said stepping motor at steady speed in response to the output pulse of said variable frequency pulse generator when the output of said first AND circuit is "low".

5. A liquid chromatography apparatus according to claim 1, 2, 3, or 4 wherein said programmer includes a pulse generator for generating a pulse having an interval equivalent to the time required for at least one valve to operate once, a programmable voltage generator for changing the voltage value in the range from 0 to 100%, a pulse width modulator for changing the pulse width of the pulse generated from said pulse generator in the range from 0 to 100% in response to the output of said programmable voltage regulator, valve operating means for controlling the operation of at least one valve in response to the output of said pulse width modulator.

6. A liquid chromatography apparatus according to claim 1, 2, 3, 4 or 5, further comprising a plurality of valves for controlling each of said liquid mobile phases flowing out of said plurality of said reservoirs, said valve operating means including a circuit for controlling the operation of said plurality of said valves complementarily with each other in response to the output of said pulse width modulator.

7. A liquid chromatography apparatus according to claim 5, further comprising a plurality of valves for controlling each of said liquid mobile phases flowing out of said plurality of said reservoirs, said valve operating means including a circuit for controlling the operation of said plurality of said valves complementarily with each other in response to the output of said pulse width modulator.

8. A liquid chromatography apparatus according to claim 3, wherein said circuit for providing a high-speed rotation command comprises means for sending said command to said motor means when said pressure transducer detects a reduction in back pressure in said column.

9. A liquid chromatography apparatus according to claim 1, wherein said cam has a shape such that its radius increases linearly from 0 to 180 degrees and decreases linearly from 180 to 360 degrees, with the rate of increase of the radius being the same, in absolute value, as the rate of decrease of the radius.

10. A liquid chromatography apparatus comprising:

at least one reservoir for storing at least one liquid mobile phase;

at least one valve for controlling the liquid mobile phase flowing out of said at least one reservoir;

a reciprocating dual-piston pump including two pistons for filling two chambers with the liquid mobile phase flowing out of said valve and pumping alternately the liquid mobile phase filled in said chambers, one end of each piston being in contact with the periphery of a rotatable cam in opposition to one end of the other piston at 180 degrees, the other end of each piston extending into each of said chambers, each of said pistons being reciprocated linearly along the contour of said cam with the rotation of said cam, thus filling said liquid mobile phase into said chambers and pumping said liquid mobile phase out of said chambers;

an injector for injecting a specimen into the liquid mobile phase passed through said pump;

a column for separating the specimen injected by said injector, into components;

a detector for detecting the components of said specimen separated by said column;

a programmer for controlling the operating time of said at least one valve;

motor means coupled to said cam of said pump for driving said pump through successive cycles of reciprocation;

a pressure transducer connected between said reciprocating dual-piston pump and said injector for providing an electric signal proportional to the flow rate of said liquid mobile phase from said pump;

a motor control circuit for applying to said motor means a control signal for controlling the reciprocating speed of said reciprocating dual pistons in response to an electric signal from said pressure transducer, said motor control circuit including a circuit for providing a high-speed rotation command to said motor means until the time derivative of the electric signal provided from the pressure transducer reaches a level larger than a predetermined value; and

a timing device for applying an electric signal to said motor control circuit during a period from the cam rotational positions of 0 and 180 degrees to predetermined cam rotational positions, said motor control circuit including a circuit for issuing a high-speed rotation command to said motor means in response to an electric signal from said timing device until the time derivative of the electric signal produced from said pressure transducer reaches a value larger than a predetermined value;

said cam having a shape such that its radius increases linearly from 0 to 180 degrees and decreases linearly from 180 to 360 degrees, with the rate of increase of the radius being the same, in absolute value, as the rate of decrease of the radius.

11. A liquid chromatography apparatus according to claim 10, wherein said timing circuit includes a chopper adapted to rotate about the same axis as the cam and position detector means working in combination with said chopper to detect the cam positions of 0 and 180 degrees.

12. A liquid chromatography apparatus comprising:

at least one reservoir for storing at least one liquid mobile phase;

at least one valve for controlling the liquid mobile phase flowing out of said at least one reservoir;

a reciprocating dual-piston pump including two pistons for filling two chambers with the liquid mobile phase flowing out of said valve and pumping alternately the liquid mobile phase filled in said chambers, one end of each piston being in contact with the periphery of a rotatable cam in opposition to one end of the other piston at 180 degrees, the other end of each piston extending into each of said chambers, each of said pistons being reciprocated linearly along the contour of said cam with the rotation of said cam, thus filling said liquid mobile phase into said chambers and pumping said liquid mobile phase out of said chambers;

an injector for injecting a specimen into the liquid mobile phase passed through said pump;

a column for separating the specimen injected by said injector, into components;

a detector for detecting the components of said specimen separated by said column;

a programmer for controlling the operating time of said at least one valve; and

motor means coupled to said cam of said pump for driving said pump through successive cycles of reciprocation,

said cam having a shape such that its radius increases linearly from 0 to 180 degrees and decreases linearly from 180 to 360 degrees, with the rate of increase of the radius being the same, in absolute value, as the rate of decrease of the radius.