Monolith Separation Column Sealing for High-Pressure Flow Control

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Solution Overview

Problem

Conventional high performance liquid chromatography methods using monolith columns face issues with degradation of separation performance due to solvent flow rate and chemical component elution at high pressures, leading to increased analysis time and mobile phase consumption.

Innovation Solution

A monolith type separation column design featuring a cylindrically formed porous monolith rod with a coating material on its outer circumference, a support member, and a rod fixing material packed into the gap between the coating and support member, with the upper end face sealed to manage solvent flow and prevent leakage, allowing for reduced solvent flow rates and maintaining high separation performance.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If the liquid flow velocity is increased to reduce the analysis time, then the productivity is improved, but the consumption of the mobile phase increases

Engineering Contradiction:
Improveanalysis timeVSAvoidmobile phase consumption
Core Design Contradiction:
ProductivityVSQuantity of substance

Solution Approach 1:

The patent uses a monolith porous material with controlled pore size and distribution to enable high flow velocities while maintaining efficient separation. The porous structure provides large surface area for separation while allowing rapid solvent flow, thus reducing analysis time without proportionally increasing mobile phase consumption.

Inventive Principle:
Principle #31Porous materials

Solution Approach 2:

The patent optimizes parameters including pore size (0.1-10 μm), porosity (30-70%), and monolith rod diameter (0.5-5 mm) to achieve the best balance between flow rate and separation performance. By carefully controlling these parameters, the system achieves fast analysis with reduced mobile phase consumption compared to conventional columns.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If a monolith rod with diameter of 4 mm or 4.6 mm is used to increase porosity, then the productivity is improved, but the consumption of the mobile phase increases

Engineering Contradiction:
Improveseparation efficiencyVSAvoidmobile phase consumption
Core Design Contradiction:
ProductivityVSQuantity of substance

Solution Approach 1:

The patent applies different properties to different parts of the column system. The monolith rod has high porosity and large pore size for fast flow, while the outer coating layer provides sealing and structural support. This local differentiation allows the column to achieve high productivity with reduced mobile phase consumption by optimizing each component's function.

Inventive Principle:
Principle #3Local quality

Solution Approach 2:

The patent creates a composite structure combining the monolith porous rod with an outer coating material. The monolith provides high porosity and fast flow paths, while the coating material provides structural integrity and sealing. This composite approach enables reduced mobile phase consumption while maintaining high separation efficiency.

Inventive Principle:
Principle #40Composite materials

3Manufacturing precision

If heating is applied to improve contact between column unit and monolithic adsorbent, then the manufacturing precision is improved, but the separation performance degrades due to removal of octadecylsilyl group

Engineering Contradiction:
Improvecontact between column unit and adsorbentVSAvoidseparation performance
Core Design Contradiction:
Manufacturing precisionVSReliability

Solution Approach 1:

The patent carefully controls the heating temperature parameter during manufacturing to be below the threshold that causes decomposition of the octadecylsilyl group. By optimizing the heating temperature and duration, the patent achieves sufficient contact between components while preserving the chemical integrity of the stationary phase, thus avoiding degradation of separation performance.

Inventive Principle:
Principle #35Parameter changes

4Productivity

If the monolithic molding is made thinner to reduce solvent flow rate, then the productivity is improved, but the separation performance degrades due to significant heating influence

Engineering Contradiction:
Improvesolvent flow rateVSAvoidseparation performance
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent uses a porous monolith structure that provides high surface area and efficient separation even in thin configurations. The porous network maintains structural integrity and thermal stability, allowing thin columns to achieve low flow rates without compromising separation performance through excessive heating effects.

Inventive Principle:
Principle #31Porous materials

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 design reduces solvent flow rates, prevents chemical component elution, and minimizes leakage at high pressures, thereby reducing analysis time while maintaining high separation performance and reducing mobile phase consumption.

Implementation Method 1

the monolith column has an integrated structure of a three-dimensional network skeleton and relevant void (flow path, macro pores, and through pores)... enables a column to have a large porosity and accordingly a nonincreasing flow resistance

Methodology Applied
Scientific EffectPorosity: Porosity

Implementation Method 2

a resin coating material is provided on the outer circumferential surface of the porous material in order to prevent leakage of a mobile phase from the side face of the column

Methodology Applied
Scientific EffectPhysical containment: Physical Containment

Implementation Method 3

a rod fixing material fitted or packed into a gap between the coating material and the support member; the upper end face of the rod fixing material is sealed... prevent leakage at high pressure

Methodology Applied
Scientific EffectPressure sealing: Physical Containment

Data Source

PatentUS7811451B2Separation column and liquid chromatograph using the same
Publication Date: 2010.10.12 HITACHI HIGH TECH CORP
  • US7811451B2 patent drawing
  • US7811451B2 patent drawing
  • US7811451B2 patent drawing

AI summary

The flow rate of a solvent is reduced as a separation column and the separation performance is improved even under high-pressure conditions. There is provided a separation column including a monolith rod into which a sample and a mobile phase flow, the separation column comprising: a coating material coated on the outer circumference of a monolith rod; a support member into which the monolith rod coated with the coating material is inserted, and a rod fixing material fitted into or filled a gap between the coating material and the support member; wherein the upper end face of the rod fixing material is sealed, the upper end face being the inflow-side end when the separation column is assembled.