Cryo Trap Temperature Gradient for Volatile Compound Trapping

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Solution Overview

Problem

Existing methods for analyzing volatile organic compounds in gas chromatography, such as thermal desorption, suffer from sample degradation due to abrupt temperature changes and the need for flash heating, which limits their effectiveness in capturing natural patterns of volatile compound release.

Innovation Solution

A novel thermal desorption system with a cryo trap that utilizes a temperature gradient and low thermal mass, integrated with a split/splitless injector, eliminates the need for flash heating and reduces aerosol formation by maintaining a gradual temperature change, allowing for more efficient trapping and focusing of volatile compounds.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If a cryo trap is evenly cooled to -78°C or lower to trap volatile compounds, then trapping efficiency is improved, but aerosol formation occurs at the interface where warm desorption gas is abruptly cooled

Engineering Contradiction:
Improvetrapping efficiencyVSAvoidaerosol formation
Core Design Contradiction:
Measurement precisionVSObject-generated harmful factors

Solution Approach 1:

The cryo trap is designed with a temperature gradient where the distal end (facing the desorption oven) is maintained at a higher temperature than the proximal end. This spatial variation in temperature quality prevents abrupt cooling at the interface, thereby reducing aerosol formation while maintaining effective trapping at the colder proximal end

Inventive Principle:
Principle #3Local quality

2Manufacturing precision

If the cryo trap is flash heated to 200°C or higher to eliminate chromatographic peak broadening, then peak sharpness is improved, but sample degradation occurs due to the combination of high temperature and active sites

Engineering Contradiction:
Improvechromatographic peak sharpnessVSAvoidsample degradation
Core Design Contradiction:
Manufacturing precisionVSObject-generated harmful factors

Solution Approach 1:

The cryo trap employs a temperature gradient during operation, with the distal end exposed to higher temperatures from the desorption oven and the proximal end remaining colder. This spatial temperature differentiation allows the trap to function effectively without requiring uniform flash heating to 200°C or higher, thereby preventing thermal degradation of labile compounds while still achieving sharp chromatographic peaks

Inventive Principle:
Principle #3Local quality

Solution Approach 2:

The system dynamically manages temperature distribution within the cryo trap, transitioning from a static uniform cooling approach to a dynamic temperature gradient that adapts to the desorption process. This dynamic temperature control eliminates the need for aggressive flash heating by maintaining optimal temperature conditions throughout the trapping and injection process

Inventive Principle:
Principle #15Dynamics

3Productivity

If the desorption oven is set to high temperatures above 150°C to ensure complete desorption of volatile compounds, then desorption efficiency is improved, but thermo labile compounds such as germacrene and pregeijerene degrade

Engineering Contradiction:
Improvedesorption efficiencyVSAvoidcompound degradation
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

The cryo trap's temperature gradient design allows the distal end to be exposed to higher desorption temperatures while the proximal end remains at lower temperatures. This spatial differentiation enables complete desorption of volatile compounds from the filter at the hot end, while the cold end protects thermo labile compounds from degradation during the subsequent trapping and injection process

Inventive Principle:
Principle #3Local quality

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 approach minimizes sample degradation and peak broadening, enabling the capture of dynamic and short-lived volatile compound patterns without the need for solvent extraction, thereby improving the accuracy and reliability of gas chromatography results.

Implementation Method 1

utilizes a temperature gradient for more efficient trapping as well as focusing of volatile compounds

Methodology Applied
Scientific EffectTemperature gradient: Temperature Gradient

Implementation Method 2

the volatile compounds will be retained

Methodology Applied
Scientific EffectCondensation: Condensation

Implementation Method 3

the filter 16 containing the sample is placed in a specifically designed oven where the volatile compounds are released from the filter 16 by elevated temperature

Methodology Applied
Scientific EffectThermal desorption: Desorption

Implementation Method 4

by elevated temperature

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 5

cold with liquid CO2 or sometimes liquid N2, where the volatile compounds will be retained

Methodology Applied
Scientific EffectCryogenic cooling: Cryogenics

Implementation Method 6

The trap therefore either has to be sufficiently long to trap aerosol droplets

Methodology Applied
Scientific EffectCooling: Cooling

Data Source

PatentUS10078071B2Technique for thermal desorption analyses of thermo labile volatile compounds
Publication Date: 2018.09.18 THE GOVERNMENT OF THE UNITED STATES OF AMERICA AS REPRESENTED BY THE SECRETARY DEPARTMENT OF HEALTH & HUMAN SERVICES
  • US10078071B2 patent drawing
  • US10078071B2 patent drawing
  • US10078071B2 patent drawing

AI summary

Herein is described an apparatus for adaptation to existing GC/MS systems, utilizing a splitless injector as the desorption oven with a liquid CO2 cooled low thermal mass cryo trap that eliminates the need for flash heating of volatile compounds.