Decentralized Sample Vessel Heating for Chromatography Automation

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Solution Overview

Problem

Current sample preparation methods for analytical chromatography lack automation and reproducibility in thermal treatment and chemical reaction processes, leading to inefficiencies in sample handling and analysis.

Innovation Solution

A device featuring a sample vessel with an integrated heating element allows for rapid thermal treatment and optional chemical reactions within the vessel, decoupled from the chromatography system, enabling automated and reproducible sample preparation through a decentralized vial-based interface that supports pyrolysis and dissolution of samples for subsequent analysis.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Extent of automation

If sample preparation is performed manually in traditional chromatography systems, then flexibility in handling different samples is maintained, but automation and reproducibility are reduced

Engineering Contradiction:
Improveautomation of sample preparationVSAvoidcomplexity of sample preparation system
Core Design Contradiction:
Extent of automationVSDevice complexity

Solution Approach 1:

The sample preparation system is segmented into independent modular units: a sample vessel module containing the test substance, a heating module with heating element, a reaction module for chemical reactions, and a chromatography module. Each module can be independently controlled and optimized, enabling automation while maintaining flexibility for different sample types and preparation methods.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The sample vessel is designed as a multi-functional component that serves multiple purposes: it contains the test substance, provides a controlled environment for thermal treatment via integrated heating, facilitates chemical reactions through reagent addition, and interfaces with the chromatography system. This universal design reduces the need for multiple specialized devices, automating various preparation steps within a single integrated system.

Inventive Principle:
Principle #6Universality (Multi-functionality)

2Manufacturing precision

If thermal treatment and chemical reactions are integrated within the sample vessel, then reproducibility of sample preparation is improved, but the risk of contamination to the chromatography system increases

Engineering Contradiction:
Improvereproducibility of sample preparationVSAvoidcontamination risk to chromatography system
Core Design Contradiction:
Manufacturing precisionVSObject-affected harmful factors

Solution Approach 1:

The thermal treatment and chemical reaction processes are extracted from the chromatography system and performed in a separate, dedicated sample vessel module. This physical separation ensures that any contamination generated during high-temperature pyrolysis or chemical reactions remains confined to the sample preparation module and does not affect the sensitive chromatography components, while still achieving reproducible sample preparation through controlled conditions in the isolated module.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The sample vessel acts as an intermediary component between the sample introduction and the chromatography system. It provides a controlled environment for thermal and chemical processing, then transfers only the prepared sample (via injection through a membrane) to the chromatography system. This intermediary function protects the chromatography system from contamination while enabling reproducible sample preparation through standardized vessel design and controlled processing conditions.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Productivity

If rapid thermal treatment is applied to achieve complete decomposition, then analysis time is reduced, but energy consumption and risk of unwanted reactions increase

Engineering Contradiction:
Improvesample throughputVSAvoidenergy consumption for thermal treatment
Core Design Contradiction:
ProductivityVSUse of energy by moving object

Solution Approach 1:

The heating process is made dynamic and adaptive through programmable temperature profiles that can be adjusted based on the specific sample type and desired decomposition extent. The heating element can apply rapid high-temperature treatment for complete decomposition when needed, or use gentler, lower-energy profiles for samples requiring milder conditions. This dynamic control optimizes the balance between processing speed (productivity) and energy consumption, allowing the system to adapt to different analytical requirements without wasting energy on unnecessary high-temperature treatment.

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 solution enhances the automation and reproducibility of sample preparation, preventing contamination of chromatography systems and allowing for efficient thermal treatment and chemical analysis of samples, improving the precision and throughput of analytical processes.

Implementation Method 1

The sample is heated for a very short time to a temperature that enables a thermo-chemical reaction of the sample. The pyrolysis is generally carried out at temperatures between 500°C and 1400°C.

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 2

A pyrolytic decomposition is carried out in the sample vessel. Thermal degradation (pyrolysis, thermolysis) of semi-solid and solid samples prior to chemical analysis of the resulting degradation products is today an extensively used sample preparation method

Methodology Applied
Scientific EffectPyrolysis: Pyrolysis

Implementation Method 3

The sample vessel is provided with a self-sealing membrane. In order to take samples from this gas space, a sampling device is pierced through the membrane.

Methodology Applied
Scientific EffectElasticity: Elasticity

Data Source

PatentEP2577284B1Apparatus for preparing a sample
Publication Date: 2019.10.02 GERSTEL SYSTEMTECHNIK GMBH & CO KG
  • EP2577284B1 patent drawingFigure 1A~2B
  • EP2577284B1 patent drawingFigure 3
  • EP2577284B1 patent drawingFigure 4A~4B

AI summary

The invention relates to a system for carrying out a sample preparation for an analysis apparatus, in particular a chromatograph, comprising a sample vessel (1), which can be closed by a self-sealing cover and has a sample compartment (31) for receiving a substance to be examined, further comprising a holder, which has a heating wire coil (13) and into which the sample vessel (1) with the sample compartment (31) can be inserted for heating the substance to be examined, and further comprising a power supply for the heating wire coil (13) which is based on a constant current source and is controlled proportionally by pulse width modulation.