Headspace Analysis for TCA Detection in Cork Stoppers

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Solution Overview

Problem

Current methods for detecting 2,4,6-trichloroanisole (TCA) in cork stoppers are invasive, destructive, or inefficient, failing to fully prevent its transmission to wine and are costly, especially when trying to achieve low concentration detection within parts per trillion ranges, which is crucial for maintaining wine quality.

Innovation Solution

A non-invasive and non-destructive method using a closed conditioning system with high-speed chromatography for detecting TCA in cork stoppers, allowing for concentration ranges of ng/L without separation techniques like chromatography, enabling categorization and separation of cork stoppers based on established acceptance levels, and analyzing 1,000 to 10,000 stoppers per hour.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If conventional detection methods are used to detect TCA in cork stoppers, then detection capability is achieved, but the methods are invasive and destructive to the cork stoppers

Engineering Contradiction:
Improvedetection capabilityVSAvoiddamage to cork stoppers
Core Design Contradiction:
Measurement precisionVSObject-affected harmful factors

Solution Approach 1:

The patent introduces a headspace as an intermediary medium that contains the volatile compounds emitted by the cork stopper. Instead of directly analyzing the cork material, the system detects TCA in the headspace gas phase, which serves as a mediator between the cork and the detection system, thereby avoiding direct contact and damage to the cork stopper.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent replaces destructive mechanical extraction methods with a non-invasive gas phase detection system. Volatile compounds naturally evaporate into the headspace, and this gas phase sample is then analyzed using chemical sensors or mass spectrometry, substituting mechanical destruction with a chemical/physical detection approach.

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

2Measurement precision

If conventional detection methods are used to achieve low concentration detection of TCA, then detection sensitivity is improved, but energy consumption increases and analysis time extends

Engineering Contradiction:
Improvedetection sensitivityVSAvoidenergy consumption
Core Design Contradiction:
Measurement precisionVSUse of energy by moving object

Solution Approach 1:

The patent performs preliminary concentration of volatile compounds in the closed headspace before detection. By sealing the cork stopper in a closed container and allowing volatiles to accumulate over time, the system pre-concentrates the analyte, thereby reducing the energy required during the actual detection phase and enabling sensitive detection without excessive energy input.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent utilizes the phase transition of volatile compounds from liquid/solid bound state in the cork to gas phase in the headspace. This natural evaporation process concentrates the volatiles in the gas phase, enabling sensitive detection without requiring high-energy extraction procedures.

Inventive Principle:
Principle #36Phase transitions

3Measurement precision

If conventional detection methods are used, then TCA detection is achieved, but productivity is low and cannot meet industrial production rhythms

Engineering Contradiction:
Improvedetection accuracyVSAvoidanalysis speed
Core Design Contradiction:
Measurement precisionVSProductivity

Solution Approach 1:

The patent enables continuous analysis by processing multiple cork stoppers sequentially in the same headspace system. After one cork is analyzed, the headspace is quickly cleared and the next cork is introduced, maintaining continuous operation without lengthy reset periods, thereby matching industrial production rhythms of 1,000-10,000 stoppers per hour.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent extracts only the volatile compound information from the cork stopper by analyzing the headspace, leaving the cork stopper intact and ready for immediate use or further processing. This selective extraction of information without physical removal or destruction of the cork enables rapid sequential analysis.

Inventive Principle:
Principle #2Taking out (Extraction)

4Measurement precision

If conventional detection methods are used, then TCA presence is detected, but cost increases especially for low concentration detection

Engineering Contradiction:
Improvelow concentration detectionVSAvoiddetection cost
Core Design Contradiction:
Measurement precisionVSEase of manufacture

Solution Approach 1:

The patent employs disposable or easily replaceable chemical sensors or sorbent traps that capture volatiles from the headspace. These low-cost consumable elements can be replaced frequently without requiring expensive, complex instrumentation, thereby enabling low concentration detection at reduced cost.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The patent changes the detection parameter from analyzing bulk cork material to detecting volatile compounds in the gas phase. This parameter change enables the use of more sensitive, lower-cost detection methods such as chemical sensors or simple mass spectrometry rather than requiring expensive, complex chromatographic analysis of solid cork material.

Inventive Principle:
Principle #35Parameter changes

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 effectively reduces energy consumption, ensures 100% control of TCA contamination levels under sensorial detection limits, and maintains the integrity of cork stoppers, addressing the industry's need for rapid, reliable analysis compatible with industrial production rhythms.

Implementation Method 1

The trap (4), which concentrates the volatile compounds for analysis by adsorption

Methodology Applied
Scientific EffectAdsorption: Adsorption

Implementation Method 2

The trap (4) is heated to a temperature within the range of 80°C to 300°C for a period of time of 10 to 60 seconds, depending on the trap's material characteristics, for desorption of the volatile compounds

Methodology Applied
Scientific EffectThermal desorption: Desorption

Implementation Method 3

a) the cork stoppers are separately or jointly taken to the incubation chamber (1) wherein an incubation period begins

Methodology Applied
Scientific EffectVaporization: Evaporation

Data Source

PatentEP3165918B1Method of detecting volatile components emitted from cork stoppers using headspace analysis and thermal desorption
Publication Date: 2021.03.10 CORK SUPPLY PORTUGAL
  • EP3165918B1 patent drawingFigure 1a~1d
  • EP3165918B1 patent drawingFigure 2a~2b
  • EP3165918B1 patent drawingFigure 3

AI summary

A method for detecting a volatile analyte for categorization and separation of cork stoppers depending on the concentration of the said analyte, with the detection being carried out in concentrations within the range of ng/L (parts per trillion), in a concentrated gas over the cork stoppers, confined to a closed conditioning system. In the said method, the cork stoppers are separately or jointly led to an incubation chamber (1); air or nitrogen is injected into the incubation chamber (1), dragging the gas enriched in the cork's volatile compounds and carrying it to the concentration system which is provided with a trap (4), the latter being meanwhile heated for desorption of the volatile compounds; these are led by the dragging gas towards a detection system (6) which registers a signal related to the presence of the analyte, this signal being used for purposes of classification of the cork stopper or groups of cork stoppers; finally, a software receives the signal and compares it with the established minimum threshold, taking a decision of approval or rejection. An installation for the operation of the said method is also described.