Cork Stopper TCA Detection via Headspace Gas Sampling

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Solution Overview

Problem

Current methods for analyzing cork stoppers for 2,4,6-trichloroanisole contamination are time-consuming, destructive, and do not guarantee each cork is free from contamination, making it difficult to ensure the quality of wine bottles.

Innovation Solution

A method involving heating the cork in a sealed container to vaporize 2,4,6-trichloroanisole, followed by direct gas sampling and analysis using gas chromatography, which is non-destructive, faster, and more reliable, allowing for individual cork analysis and automated implementation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If the cork is macerated in a hydroalcoholic solution for TCA migration simulation, then the overall contamination of the batch can be assessed, but the method is time-consuming and destructive, preventing analysis of each individual cork

Engineering Contradiction:
Improvebatch contamination assessmentVSAvoidanalysis speed and individual cork testing capability
Core Design Contradiction:
Measurement precisionVSProductivity

Solution Approach 1:

The invention changes the physical state and extraction parameters by using headspace gas phase extraction instead of liquid maceration. The cork is heated to 40-60°C in a sealed vial, allowing TCA to volatilize and partition into the headspace, where it can be directly injected into GC-MS for analysis. This parameter change enables rapid analysis without destroying the cork structure.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention replaces the mechanical/chemical maceration process with a thermal volatilization and gas phase extraction system. Instead of soaking corks in solution, the method uses controlled heating to vaporize TCA, which then enters the headspace for direct gas chromatography injection. This substitution eliminates the time-consuming maceration step while enabling individual cork analysis.

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

2Productivity

If the cork is heated in a sealed container to vaporize TCA, then rapid and non-destructive analysis of individual corks is enabled, but additional equipment and process steps are required

Engineering Contradiction:
Improveanalysis speed and individual cork testingVSAvoidheating and gas sampling equipment
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The invention makes the GC-MS injection system multi-functional by enabling it to directly accept headspace gas samples from sealed vials without requiring a separate headspace sampler device. The sealed vial with cork can be directly connected to the GC injection port, allowing the existing chromatography system to perform both liquid and gas phase analyses with minimal additional equipment.

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

Solution Approach 2:

The sealed vial system is self-contained, requiring no complex gas sampling apparatus. The TCA volatilizes and accumulates in the headspace of the sealed vial during heating, creating a self-generated gas sample that can be directly injected. The cork itself serves as both the sample and the containment vessel, eliminating the need for separate sampling devices.

Inventive Principle:
Principle #25Self-service

3Measurement precision

If successive steps of heating, adsorption on PDMS bar, and thermal desorption are used, then haloanisole analysis is possible, but the process is complex, long, and expensive with compound losses during adsorption/desorption

Engineering Contradiction:
Improvehaloanisole detection capabilityVSAvoidadsorption/desorption process complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The invention extracts only the essential function of TCA volatilization and headspace accumulation, eliminating the intermediate adsorption/desorption steps. By heating the sealed vial containing the cork, TCA is released and accumulates in the headspace in sufficient concentration for direct GC-MS injection. This extraction approach removes the complex PDMS bar adsorption and thermal desorption equipment while maintaining detection precision.

Inventive Principle:
Principle #2Taking out (Extraction)

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 method provides sensitive and reliable detection of 2,4,6-trichloroanisole with a detection threshold of 0.5 ng/l, enabling the selection of corks free from contamination, ensuring the quality of wine bottles without altering the corks' properties.

Implementation Method 1

heating of the container containing the cap under conditions, in particular of temperature, pressure and duration, allowing vaporization of 2,4,6-trichloroanisole possibly present in the cap

Methodology Applied
Scientific EffectVaporization: Evaporation

Implementation Method 2

injection of the gaseous sample taken into the container (11) directly into an analysis module, and analysis of the gas sample thus taken for the presence of 2,4,6-trichloroanisole

Methodology Applied
Scientific EffectGas chromatography: Chromatography

Data Source

PatentEP2837936B2Method for analysing a cork stopper for the presence of 2,4,6-trichloroanisole and device for implementing same
Publication Date: 2020.11.25 CEVAQOE INVEST
  • EP2837936B2 patent drawingFigure 1~2a
  • EP2837936B2 patent drawingFigure 2b~3

AI summary

The invention relates to a non-destructive method for analyzing a cork stopper for the presence of 2,4,6-trichloroanisole. The method comprises placing the cork in a hermetically sealed container, heating the container under conditions that allow vaporization of any 2,4,6-trichloroanisole present in the cork, collecting a gaseous sample from the atmosphere surrounding the cork in the container, and analyzing the gaseous sample thus collected for the presence of 2,4,6-trichloroanisole. This method allows for the non-destructive selection, within a batch of corks, of those stoppers substantially devoid of 2,4,6-trichloroanisole.