System and method for rapid chromatography with fluid temperature and mobile phase composition control
First Claim
1. A liquid chromatography system for characterizing a sample, the system comprising a chromatographic column comprising an inlet port for receiving a mobile phase and the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the chromatographic column, a detector in fluid communication with the effluent port of the chromatographic column for detecting a property of at least one of the sample components, an injection port for injecting the sample into the mobile phase, a fluid distribution system for controlling a composition and a temperature of the mobile phase, the fluid distribution system comprising:
- (i) a primary mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, the primary mixing zone being in fluid communication with the inlet port of the chromatographic column, (ii) a first secondary mixing zone adapted to mix a first secondary feed and a second secondary feed to form the first primary feed, the first secondary mixing zone being in fluid communication with the primary mixing zone, and (iii) a second secondary mixing zone adapted to mix a third secondary feed and a fourth secondary feed to form the second primary feed, the second secondary mixing zone being in fluid communication with the primary mixing zone, and a control system for controlling the composition and the temperature of the mobile phase by using one or more control protocols selected from the group consisting of;
(a) varying relative flow rates of the secondary feeds supplied to the first secondary mixing zone, (b) varying relative flow rates of the secondary feeds supplied to the second secondary mixing zone, (c) varying relative flow rates of the first primary feed and the second primary feed supplied to the primary mixing zone, and (d) combinations thereof.
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Abstract
The invention relates to liquid chromatography techniques for rapidly characterizing samples, such as polymer solutions, emulsions and dispersions, and to devices for implementing such techniques. The system includes a design that provides the ability to perform chromatographic separations by using mobile phase composition gradients and temperature gradients during separations. The invention accomplishes this by providing mixing zones for a plurality of fluids as well as heated and chilled feeds feeding the fluids to the mixing zones. Additionally, the system provides the ability to analyze separated components with a detector and/or collect separated fractions into vessels of a fraction collector for further separation and/or analysis.
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Citations
32 Claims
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1. A liquid chromatography system for characterizing a sample, the system comprising a chromatographic column comprising an inlet port for receiving a mobile phase and the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the chromatographic column, a detector in fluid communication with the effluent port of the chromatographic column for detecting a property of at least one of the sample components, an injection port for injecting the sample into the mobile phase, a fluid distribution system for controlling a composition and a temperature of the mobile phase, the fluid distribution system comprising:
- (i) a primary mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, the primary mixing zone being in fluid communication with the inlet port of the chromatographic column, (ii) a first secondary mixing zone adapted to mix a first secondary feed and a second secondary feed to form the first primary feed, the first secondary mixing zone being in fluid communication with the primary mixing zone, and (iii) a second secondary mixing zone adapted to mix a third secondary feed and a fourth secondary feed to form the second primary feed, the second secondary mixing zone being in fluid communication with the primary mixing zone, and a control system for controlling the composition and the temperature of the mobile phase by using one or more control protocols selected from the group consisting of;
(a) varying relative flow rates of the secondary feeds supplied to the first secondary mixing zone, (b) varying relative flow rates of the secondary feeds supplied to the second secondary mixing zone, (c) varying relative flow rates of the first primary feed and the second primary feed supplied to the primary mixing zone, and (d) combinations thereof. - View Dependent Claims (2, 3, 4, 5)
- (i) a primary mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, the primary mixing zone being in fluid communication with the inlet port of the chromatographic column, (ii) a first secondary mixing zone adapted to mix a first secondary feed and a second secondary feed to form the first primary feed, the first secondary mixing zone being in fluid communication with the primary mixing zone, and (iii) a second secondary mixing zone adapted to mix a third secondary feed and a fourth secondary feed to form the second primary feed, the second secondary mixing zone being in fluid communication with the primary mixing zone, and a control system for controlling the composition and the temperature of the mobile phase by using one or more control protocols selected from the group consisting of;
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6. A liquid chromatography system for characterizing a sample, the system comprising a chromatographic column comprising an inlet port for receiving a mobile phase and the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the chromatographic column, a detector in selective fluid communication with the effluent port of the chromatographic column for detecting a property of at least one of the sample components, a fraction collector in selective fluid communication with the effluent port of the column, an injection port for injecting the sample into the mobile phase, a fluid distribution system for controlling a composition and a temperature of the mobile phase, the fluid distribution system comprising:
- (i) a primary mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, the primary mixing zone being in fluid communication with the inlet port of the chromatographic column, (ii) a first secondary mixing zone adapted to mix a first secondary feed and a second secondary feed to form the first primary feed, the first secondary mixing zone being in fluid communication with the primary mixing zone, and (iii) a second secondary mixing zone adapted to mix a third secondary feed and a fourth secondary feed to form the second primary feed, the second secondary mixing zone being in fluid communication with the primary mixing zone, and a control system for controlling the composition and the temperature of the mobile phase by using one or more control protocols selected from the group consisting of;
(a) varying relative flow rates of the secondary feeds supplied to the first secondary mixing zone, (b) varying relative flow rates of the secondary feeds and supplied to the second secondary mixing zone, (c) varying relative flow rates of the first primary feed and the second primary feed supplied to the primary mixing zone, and (d) combinations thereof. - View Dependent Claims (7, 8, 9, 10)
- (i) a primary mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, the primary mixing zone being in fluid communication with the inlet port of the chromatographic column, (ii) a first secondary mixing zone adapted to mix a first secondary feed and a second secondary feed to form the first primary feed, the first secondary mixing zone being in fluid communication with the primary mixing zone, and (iii) a second secondary mixing zone adapted to mix a third secondary feed and a fourth secondary feed to form the second primary feed, the second secondary mixing zone being in fluid communication with the primary mixing zone, and a control system for controlling the composition and the temperature of the mobile phase by using one or more control protocols selected from the group consisting of;
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11. A liquid chromatography system for characterizing a sample, the system comprising a first chromatographic column comprising an inlet port for receiving a mobile phase and the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the first chromatographic column, a second chromatographic column comprising an inlet port for receiving the mobile phase comprising the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the second chromatographic column, a detector in selective fluid communication with the effluent port of the first and second chromatographic columns for detecting a property of at least one of the sample components, a first injection port for injecting the sample into the mobile, phase, the first injection port in selective fluid communication with the inlet port of the first chromatographic column, a second injection port for injecting the sample into the mobile phase, the second injection port in selective fluid communication with the inlet port of the second chromatographic column, a fluid distribution system for controlling a composition and a temperature of the mobile phase, the fluid distribution system comprising:
- (i) a first primary mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, the primary mixing zone being in fluid communication with the inlet port of the first chromatographic column, (ii) a second primary mixing zone adapted to mix the first pry feed and the second primary feed to form the mobile phase, the second primary mixing zone being in fluid communication with the inlet port of the second chromatographic column, (iii) a first secondary mixing zone adapted to mix a first secondary feed and a second secondary feed to form the first primary feed, the first secondary mixing zone being in selective fluid communication with the first and second primary mixing zones, (iii) a second secondary mixing zone adapted to mix a third secondary feed and a fourth secondary feed to form the second primary feed, the second secondary mixing zone being in selective fluid communication with the first and second primary mixing zones, and (iv) a valve located between and in fluid communication with the first and second secondary mixing zones and the first and second primary mixing zones, and being adapted to direct the flow of the first and second primary feeds from the first and second secondary mixing zones to the first primary mixing zone, the second primary mixing zone, or both, and a control system for controlling the composition and the temperature of the mobile phase by using one or more control protocols selected from the group consisting of;
(a) varying relative flow rates of the secondary feeds supplied to the first secondary mixing zone, (b) varying relative flow rates of the secondary feeds supplied to the second secondary mixing zone, (c) varying relative flow rates of the first primary feed and the second primary feed supplied to the first primary mixing zone, (d) varying relative flow rates of the first primary feed and the second primary feed supplied to the second primary mixing zone, and (e) combinations thereof. - View Dependent Claims (12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26)
- (i) a first primary mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, the primary mixing zone being in fluid communication with the inlet port of the first chromatographic column, (ii) a second primary mixing zone adapted to mix the first pry feed and the second primary feed to form the mobile phase, the second primary mixing zone being in fluid communication with the inlet port of the second chromatographic column, (iii) a first secondary mixing zone adapted to mix a first secondary feed and a second secondary feed to form the first primary feed, the first secondary mixing zone being in selective fluid communication with the first and second primary mixing zones, (iii) a second secondary mixing zone adapted to mix a third secondary feed and a fourth secondary feed to form the second primary feed, the second secondary mixing zone being in selective fluid communication with the first and second primary mixing zones, and (iv) a valve located between and in fluid communication with the first and second secondary mixing zones and the first and second primary mixing zones, and being adapted to direct the flow of the first and second primary feeds from the first and second secondary mixing zones to the first primary mixing zone, the second primary mixing zone, or both, and a control system for controlling the composition and the temperature of the mobile phase by using one or more control protocols selected from the group consisting of;
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27. A liquid chromatography system for characterizing a sample, the system comprising a chromatographic column comprising an inlet port for receiving a mobile phase and the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the column, a detector in communication with the effluent port of the chromatographic column for detecting a property of at least one of the sample components, an injection valve proximately coupled to the inlet port of the chromatographic column, for injecting the sample with the mobile phase into the chromatographic column, the injection valve comprising:
- a primary mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, an injection port adapted for injecting the sample into the injection valve, and an outlet adapted for providing a flow path from the injection valve to the chromatographic column, wherein the outlet of the injection valve and the inlet port of the chromatographic column are proximately coupled, and a control system for controlling the temperature and the composition of the mobile phase by varying relative flow rates of the first primary feed and the second primary feed supplied to the primary mixing zone.
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28. A liquid chromatography system for characterizing a sample, the system comprising a chromatographic column comprising an inlet port for receiving a mobile phase comprising the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the column, a detector in selective communication with the effluent port of the chromatographic column for detecting a property of at least one of the sample components, a fraction collector in selective fluid communication with the effluent port of the column, an injection valve proximately coupled to the inlet port of the chromatographic column, for injecting the sample with the mobile phase into the chromatographic column, the injection valve comprising:
- a primary mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, an injection port adapted for injecting the sample into the injection valve, and an outlet adapted for providing a flow path from the injection valve to the chromatographic column, wherein the outlet of the injection valve and the inlet port of the chromatographic column are proximately coupled, and a control system for controlling the temperature and the composition of the mobile phase by varying relative flow rates of the fist primary feed and the second primary feed supplied to the primary mixing zone.
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29. A liquid chromatography system for characterizing a sample, the system comprising:
- a chromatographic column comprising an inlet port for receiving a mobile phase and the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the column, a fraction collector in fluid communication with the effluent port of the chromatographic column for collecting the separated components of the sample in separate vessels, an injection port in selective fluid communication with the inlet port of the chromatographic column for injecting the sample into the mobile phase, a mixing zone adaptable for mixing a first primary feed and a second primary feed to form the mobile phase, and in fluid communication with the inlet port of the chromatographic column, a first line for delivering the first primary feed to the mixing zone, a first temperature control element in thermal communication with the first line for maintaining the first line at a first temperature, a second line for delivering the second primary feed to the mixing zone, a second temperature control element in thermal communication with the second line for maintaining the second line at a second temperature different from the first temperature, and a control system for controlling the composition and the temperature of the mobile phase by using one or more control protocols selected from the group consisting of;
(a) varying relative flow rates of one or more of the feeds, (b) varying the temperatures of the first and second lines, and (c) combinations thereof.
- a chromatographic column comprising an inlet port for receiving a mobile phase and the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the column, a fraction collector in fluid communication with the effluent port of the chromatographic column for collecting the separated components of the sample in separate vessels, an injection port in selective fluid communication with the inlet port of the chromatographic column for injecting the sample into the mobile phase, a mixing zone adaptable for mixing a first primary feed and a second primary feed to form the mobile phase, and in fluid communication with the inlet port of the chromatographic column, a first line for delivering the first primary feed to the mixing zone, a first temperature control element in thermal communication with the first line for maintaining the first line at a first temperature, a second line for delivering the second primary feed to the mixing zone, a second temperature control element in thermal communication with the second line for maintaining the second line at a second temperature different from the first temperature, and a control system for controlling the composition and the temperature of the mobile phase by using one or more control protocols selected from the group consisting of;
- 30. A liquid chromatography system for characterizing a sample, the system comprising a chromatographic column located in an ambient temperature environment, the column comprising an inlet port for receiving a mobile phase and the sample, and an effluent port for discharging the mobile phase and separated components of the sample from the chromatographic column, the chromatographic column adapted to be heated or cooled internally by the mobile phase in the absence of any heating chamber, a detector in fluid communication with the effluent port of the chromatographic column for detecting a property of at least one of the sample components, an injection port in selective fluid communication with the inlet port of the chromatographic column for injecting the sample into the mobile phase, a mixing zone adapted to mix a first primary feed and a second primary feed to form the mobile phase, and a control system for controlling a composition and a temperature of the mobile phase by varying the relative flow rates of one or more of the feeds.
Specification