Thermally Modulated Variable Restrictor for Chromatography Split Ratio

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Solution Overview

Problem

Chromatography systems with fixed restrictors face challenges in maintaining a constant split ratio during gradient separations due to changes in mobile phase density or composition, leading to non-linearity and inaccurate quantitation of peaks.

Innovation Solution

A thermally modulated variable restrictor is introduced to dynamically adjust the split ratio by controlling the temperature of the mobile phase stream, ensuring a constant split ratio throughout the chromatographic run by adjusting the heat exchange between the restrictor and the mobile phase.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of operation

If a fixed restrictor is used to split the mobile phase flow, then the system structure is simple and easy to operate, but the split ratio changes during gradient separations due to viscosity changes, leading to non-linearity and inaccurate quantitation

Engineering Contradiction:
Improveease of operationVSAvoidquantitation accuracy
Core Design Contradiction:
Ease of operationVSManufacturing precision

Solution Approach 1:

The patent applies a variable restrictor instead of a fixed restrictor, allowing the restriction to dynamically adjust during the chromatographic run. The restrictor's opening size changes in response to mobile phase conditions (viscosity, density, flow rate) to maintain a constant split ratio despite gradient changes, thereby resolving the contradiction between operational simplicity and quantitation accuracy.

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The patent changes the physical parameters of the restrictor (opening size, restriction value) in response to changing mobile phase conditions. By monitoring parameters such as viscosity, density, or flow rate and adjusting the restrictor accordingly, the system maintains accurate split ratio control throughout gradient separations, eliminating the non-linearity problem while preserving ease of operation through automated control.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If the mobile phase density or composition is changed during gradient separations to improve peak capacity, then the separation performance is improved, but the viscosity changes cause the flow rate through the fixed restrictor to change, altering the split ratio

Engineering Contradiction:
Improvepeak capacityVSAvoidsplit ratio stability
Core Design Contradiction:
ProductivityVSStability of the object's composition

Solution Approach 1:

The patent implements a feedback control mechanism where the system monitors mobile phase conditions (density, viscosity, composition) during gradient separations and uses this information to adjust the variable restrictor. This feedback loop ensures that the split ratio remains stable despite changes in mobile phase properties, allowing gradient separations to maintain both high peak capacity and accurate quantitation.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The variable restrictor dynamically adapts its restriction value in response to changing mobile phase composition and density during gradient separations. This dynamic adjustment compensates for viscosity changes, maintaining a constant split ratio while allowing the gradient to proceed and improve peak capacity, thus resolving the contradiction between separation performance and split ratio stability.

Inventive Principle:
Principle #15Dynamics

3Manufacturing precision

If a thermally modulated variable restrictor is used to maintain constant split ratio, then the quantitation accuracy is improved, but the device complexity increases due to temperature control mechanisms

Engineering Contradiction:
Improvequantitation accuracyVSAvoiddevice complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent replaces complex mechanical adjustment mechanisms with thermal modulation. By using temperature control to change the restrictor's physical properties (viscosity, density, opening size), the system achieves variable restriction with simpler control electronics rather than complex mechanical actuators, thereby reducing overall device complexity while maintaining high quantitation accuracy.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent utilizes thermal effects and phase transitions in the mobile phase or restrictor material to control flow restriction. By modulating temperature, the system changes the physical state or properties of the mobile phase/restrictor, achieving variable split ratio control through thermal means rather than complex mechanical systems, thus improving accuracy while managing device complexity.

Inventive Principle:
Principle #36Phase transitions

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This solution maintains a consistent split ratio, preventing analyte precipitation and ensuring accurate quantitation of all peaks by maintaining an appreciable mobile phase density and optimizing the flow rate to the detector, even with changes in system pressure and mobile phase composition.

Implementation Method 1

a temperature element in thermal communication with said first mobile phase stream to exchange heat therewith

Methodology Applied
Scientific EffectHeat exchange: Heat Exchanger

Implementation Method 2

Thermally modulated variable restrictor... dynamically adjusts a temperature setting of said temperature element... to adjust the heat exchange

Methodology Applied
Scientific EffectThermal modulation: Temperature Gradient

Data Source

PatentUS10006890B2Thermally modulated variable restrictor for normalization of dynamic split ratios
Publication Date: 2018.06.26 WATERS TECHNOLOGY CORP
  • US10006890B2 patent drawing
  • US10006890B2 patent drawing
  • US10006890B2 patent drawing

AI summary

A chromatography system includes a separation column that separates a sample carried by a compressible mobile phase flow into analytes and a splitter in fluidic communication with the separation column to receive and divide the compressible mobile phase flow into first and second mobile phase streams in accordance with a split ratio. A thermally modulated variable restrictor is coupled between the splitter and a detector. The restrictor receives the first mobile phase stream from the splitter and has a temperature element in thermal communication with the first mobile phase stream to exchange heat therewith. A controller, in communication with the restrictor, dynamically adjusts a temperature setting of the temperature element of the restrictor to adjust the heat exchange between the thermally modulated variable restrictor and the first mobile phase stream in order to keep the split ratio constant throughout a chromatographic run.