Supercritical Fluid Chromatography Using Chiller and Pressure Equalizing Vessel

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Solution Overview

Problem

Traditional flash chromatography systems face challenges in achieving high performance at higher solvent flow stream pressures while using disposable plastic cartridges, which are typically unsuitable for medium pressure applications due to limitations in mechanical behavior and cavitation effects, leading to inconsistent pump performance and the need for expensive high-pressure columns.

Innovation Solution

A supercritical fluid chromatography system incorporating a chiller to subcool liquefied carbon dioxide, a pressure equalizing vessel to balance pressures within chromatography columns, and a cyclonic separator to handle high pressures, enabling the use of standard HPLC pumps and off-the-shelf cartridges in high-pressure applications.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If traditional flash chromatography uses higher pressure systems to improve performance, then chromatography performance is improved, but disposable plastic cartridges become unusable due to mechanical behavior limitations and cavitation effects

Engineering Contradiction:
Improvechromatography performanceVSAvoidcartridge usability
Core Design Contradiction:
ReliabilityVSAdaptability or versatility

Solution Approach 1:

The patent changes the physical state of the mobile phase from liquid to supercritical fluid and operates at temperatures below the critical temperature of CO2 (31.1°C), allowing the use of disposable plastic cartridges at pressures up to 1500 psi. This parameter change resolves the contradiction by enabling high-pressure operation with cartridges that would otherwise fail due to cavitation and mechanical limitations.

Inventive Principle:
Principle #35Parameter changes

2Ease of operation

If traditional flash chromatography uses disposable plastic cartridges, then ease of operation is improved, but the system cannot achieve high performance at higher pressures due to mechanical behavior limitations

Engineering Contradiction:
Improvecartridge disposal convenienceVSAvoidpump performance consistency
Core Design Contradiction:
Ease of operationVSReliability

Solution Approach 1:

By operating below the critical temperature of CO2 and using a chiller to maintain temperatures of 2°C to 5°C, the system eliminates cavitation effects that cause inconsistent pump performance. This allows disposable plastic cartridges to be used at higher pressures (up to 1500 psi) while maintaining reliable and repeatable mass flow rates, resolving the contradiction between ease of operation and reliability.

Inventive Principle:
Principle #35Parameter changes

3Ease of operation

If traditional flash chromatography uses organic solvents, then ease of operation is improved, but loss of substance increases due to large amounts of solvent consumption

Engineering Contradiction:
Improvesolvent handling simplicityVSAvoidorganic solvent consumption
Core Design Contradiction:
Ease of operationVSLoss of substance

Solution Approach 1:

The patent changes the mobile phase from traditional organic solvents to supercritical carbon dioxide, which can be easily handled as a gas at ambient conditions. CO2 is pumped as a liquid at operating conditions but expands to a gas after the column, allowing for minimal solvent consumption and easy disposal. This resolves the contradiction by maintaining ease of operation while dramatically reducing solvent loss.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The system uses CO2 as a recyclable mobile phase that can be easily recovered and reused. After expansion to gas phase, the CO2 can be collected and re-liquefied for repeated use, significantly reducing the loss of substance compared to traditional organic solvents that are consumed and disposed of after a single use.

Inventive Principle:
Principle #34Discarding and recovering

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

The system allows for efficient and repeatable mass flow rates of supercritical fluids, reducing the need for organic solvents and enabling the use of disposable cartridges in high-pressure environments, thereby improving chromatography performance and reducing operational costs.

Implementation Method 1

a chiller to subcool liquefied carbon dioxide

Methodology Applied
Scientific EffectSubcooling: Supercooling

Implementation Method 2

a pressure equalizing vessel to balance pressures within chromatography columns

Methodology Applied
Scientific EffectPressure equalization: Pascal's Law

Implementation Method 3

a cyclonic separator to handle high pressures

Methodology Applied
Scientific EffectCyclonic separation: Cyclone Separation

Implementation Method 4

Systems and methods for supercritical fluid chromatography

Methodology Applied
Scientific EffectSupercritical fluid extraction: Supercritical Fluid Extraction

Data Source

PatentUS10765968B2Systems and methods for supercritical fluid chromatography
Publication Date: 2020.09.08 SUPERCRITICAL FLUID TECH
  • US10765968B2 patent drawing
  • US10765968B2 patent drawing
  • US10765968B2 patent drawing

AI summary

Provided is a supercritical fluid chromatography method, system, and components comprising such a system wherein a non-polar solvent may replace a portion or all of a polar solvent for the purpose of separating or extracting desired sample molecules from a combined sample/solvent stream. The method and system are designed to eliminate or reduce the amount of polar solvent necessary for chromatographic separation and/or extraction of desired samples to less than or equal to twenty percent polar solvent within the total volume concentration of the total solvents used, and the technique may include one or more of a supercritical fluid chiller, a supercritical fluid pressure-equalizing vessel, and a supercritical fluid cyclonic separator. The supercritical fluid chiller and the use of the chiller allow efficient and consistent pumping of liquid-phase gases employing off-the-shelf HPLC pumps in the supercritical chromatography system using liquid-phase gas mobile phase. The pressure equalizing vessel allows the use of off the shelf HPLC column cartridges in the supercritical chromatography system. The cyclonic separator efficiently and effectively allows for separation of sample molecules from a liquid phase or gas phase stream of a supercritical fluid. The technique may further incorporate the use of one or more disposable cartridges containing silica gel or other suitable medium for use as a chromatographic separation column. The technique may also utilize an open loop cooling circuit using fluids with a positive Joule-Thompson coefficient.