Capillary Chromatography Packing for Low Pressure Loss

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Solution Overview

Problem

Chromatographic columns with porous stationary phases face high pressure loss and low productivity due to the characteristics of fine particle packings, limiting their industrial application, and existing solutions like multi-capillary fillings lack optimal operating conditions and characterized products.

Innovation Solution

A composite packing is proposed, comprising capillary conduits with a porous secondary material, such as organic or mineral gel, on the interior walls, allowing a mobile phase to flow continuously between upstream and downstream faces, with the secondary material's thickness between 0.05 and 0.5 times the conduit diameter, and a cumulative volume greater than 15% of the total packing volume, enabling efficient chromatographic separation at high elution rates.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If porous packing consisting of fine particles is used, then chromatographic separation is achieved, but pressure drop increases and productivity decreases

Engineering Contradiction:
Improvechromatographic separationVSAvoidproductivity
Core Design Contradiction:
Measurement precisionVSProductivity

Solution Approach 1:

The packing is segmented into multiple capillary conduits (each 10-500 μm in diameter) containing stationary phase, arranged in parallel within the column. This segmentation reduces the pressure drop while maintaining separation efficiency by distributing the flow across multiple channels with optimized dimensions.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The stationary phase is implemented as a porous material with controlled porosity (30-80%) and pore size (0.1-10 μm) coating the inner walls of capillary conduits. This porous structure provides high surface area for separation while allowing optimized mobile phase flow, reducing pressure drop compared to dense fine particle packings.

Inventive Principle:
Principle #31Porous materials

2Measurement precision

If porous packing consisting of fine particles is used, then chromatographic separation is achieved, but pressure drop increases

Engineering Contradiction:
Improvechromatographic separationVSAvoidpressure drop
Core Design Contradiction:
Measurement precisionVSStress or pressure

Solution Approach 1:

The packing is segmented into multiple capillary conduits (each 10-500 μm in diameter) containing stationary phase, arranged in parallel within the column. This segmentation reduces the pressure drop while maintaining separation efficiency by distributing the flow across multiple channels with optimized dimensions.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The parameters of the capillary conduits (diameter 10-500 μm, length 1-100 cm) and stationary phase (porosity 30-80%, pore size 0.1-10 μm) are optimized to achieve low pressure drop (1-50 bar) while maintaining chromatographic separation performance.

Inventive Principle:
Principle #35Parameter changes

3Productivity

If multi-capillary packing is used, then productivity is improved, but optimal operating conditions are not established

Engineering Contradiction:
ImproveproductivityVSAvoidoptimal operating conditions
Core Design Contradiction:
ProductivityVSEase of operation

Solution Approach 1:

The parameters of the capillary conduits (diameter 10-500 μm, length 1-100 cm) and stationary phase (porosity 30-80%, pore size 0.1-10 μm) are optimized to achieve low pressure drop (1-50 bar) while maintaining chromatographic separation performance.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention provides characterized products with defined properties that enable optimization of operating parameters (flow rate, temperature, mobile phase composition) to achieve optimal productivity and separation efficiency, establishing feedback loops for process optimization.

Inventive Principle:
Principle #23Feedback

4Productivity

If high elution rate is used, then productivity is increased, but separation efficiency may decrease

Engineering Contradiction:
ImproveproductivityVSAvoidseparation efficiency
Core Design Contradiction:
ProductivityVSMeasurement precision

Solution Approach 1:

The parameters of the capillary conduits (diameter 10-500 μm, length 1-100 cm) and stationary phase (porosity 30-80%, pore size 0.1-10 μm) are optimized to achieve low pressure drop (1-50 bar) while maintaining chromatographic separation performance.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The system allows dynamic adjustment of operating conditions (elution rate, mobile phase composition, temperature) to optimize the balance between productivity and separation efficiency, with the porous stationary phase maintaining performance across a wide range of flow rates.

Inventive Principle:
Principle #15Dynamics

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 configuration significantly reduces pressure losses, increases productivity, and allows for high mobile phase flow rates while maintaining efficiency, enabling preparative chromatography with short cycle times and high throughput, making it suitable for industrial-scale separations.

Implementation Method 1

The invention relates to a chromatographic column containing a porous stationary phase

Methodology Applied
Scientific EffectChromatography: Chromatography

Implementation Method 2

the walls separating the channels are made porous

Methodology Applied
Scientific EffectAdsorption: Adsorption

Implementation Method 3

a gaseous, liquid or supercritical mobile phase containing separate species is circulated through a packing comprising a stationary phase

Methodology Applied
Scientific EffectDiffusion: Diffusion

Implementation Method 4

the thickness of the secondary material defines, inside the pipe, at least one tubular channel empty of solid material, the channel being open in order to allow the mobile phase to enter and extending continuously between the upstream and downstream faces

Methodology Applied
Scientific EffectPressure gradient: Pressure Gradient

Data Source

PatentEP3694622B1Chromatography method
Publication Date: 2024.12.18 PARMENTIER FRANCOIS
  • EP3694622B1 patent drawingFigure 1~2
  • EP3694622B1 patent drawingFigure 3~4
  • EP3694622B1 patent drawingFigure 5

AI summary

Method for exchanging materials, wherein a gaseous, liquid or supercritical mobile phase containing species to be separated is circulated through a packing comprising a stationary phase, the method being characterised in that: - the packing comprises a plurality of capillary ducts formed in at least one first material, the ducts passing through the packing between an upstream face through which the mobile phase enters the packing and a downstream face through which the mobile phase leaves the packing, - each duct comprises, on at least one portion of the inner wall thereof, at least one secondary material consisting of an organic gel or porous mineral, - the thickness of the secondary material defines, inside the duct, at least one empty tubular channel of solid material, the channel being open so as to allow the mobile phase to enter and extending continuously between the upstream and downstream faces of the capillary duct - the secondary material has a thickness between 0.05 times and 0.5 times the diameter of the channel - the method is carried out with a velocity of the mobile phase between 5.0 times and 50 times the speed of the optimum mobile phase defined by the minimum of the Van Deemter curve of the majority separating compound under the method conditions - the cumulative volume of the capillary ducts is more than 15% of the total packing volume.