Gas Flow Chamber for In-Situ ATR-FTIR Reaction Monitoring

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Solution Overview

Problem

Current methods for monitoring solid-gas and liquid-gas chemical reactions, such as ex-situ analysis, face limitations including breaking mass balances and inability to continuously monitor reaction progress due to time-consuming specimen transfer, necessitating the development of in-situ monitoring techniques.

Innovation Solution

The implementation of a gas flow chamber device and method for in-situ time-dependent ATR-FTIR spectroscopy, allowing for continuous monitoring of solid-gas and liquid-gas reactions by attaching a flow chamber to an infrared spectrometer, supplying a gaseous medium to interact with the specimen, and recording infrared spectra over time, enabling real-time reaction monitoring.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If ex-situ analysis is used to monitor chemical reactions, then specimen can be analyzed by instrumental analysis, but mass balance is broken and continuous monitoring is not possible due to time-consuming transfer

Engineering Contradiction:
Improvereaction progress determinationVSAvoidspecimen transfer time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent combines the reaction environment (flow chamber) with the analytical instrument (ATR-FTIR spectrometer) into an integrated system. The flow chamber is directly attached to the spectrometer, allowing the reaction to occur and be monitored in the same location, thereby eliminating the need for specimen transfer between separate reactor and analysis instrument.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent introduces a gas flow chamber as an intermediary medium that allows reactants to be delivered to the specimen and products to be removed, while simultaneously enabling infrared transmission for spectroscopic analysis. The chamber acts as a bridge between the chemical reaction system and the analytical measurement system.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Measurement precision

If ex-situ analysis is used, then instrumental analysis can be performed, but continuous monitoring of reaction kinetics cannot be achieved

Engineering Contradiction:
Improvechemical composition analysisVSAvoidreaction monitoring efficiency
Core Design Contradiction:
Measurement precisionVSProductivity

Solution Approach 1:

The patent establishes continuous monitoring by maintaining a constant flow of gas through the chamber while continuously recording infrared spectra. The flow chamber allows uninterrupted access of reactants to the specimen and simultaneous continuous detection of product formation, enabling real-time reaction kinetics measurement without interruption.

Inventive Principle:
Principle #20Continuity of useful action

3Productivity

If in-situ monitoring is implemented, then continuous reaction monitoring is possible, but the system complexity increases with flow chamber attachment

Engineering Contradiction:
Improvecontinuous monitoring capabilityVSAvoidflow chamber and spectrometer integration
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The flow chamber is designed to serve multiple functions: it acts as a reaction vessel for chemical reactions, a flow channel for gas transport, an infrared transmission window for spectroscopic analysis, and a sealed environment for controlled atmosphere. This multi-functionality reduces the need for separate components and simplifies the overall system architecture.

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

4Measurement precision

If ATR-FTIR spectroscopy is used for solid-gas reactions, then molecular structure information can be obtained, but the reaction environment must be controlled to prevent mass balance disruption

Engineering Contradiction:
Improvemolecular structure determinationVSAvoidmass balance maintenance
Core Design Contradiction:
Measurement precisionVSReliability

Solution Approach 1:

The system implements feedback control by continuously monitoring the infrared spectra to detect product formation and reactant consumption in real-time. This information can be used to adjust flow rates, temperature, or other parameters to maintain mass balance and ensure reliable reaction monitoring throughout the process.

Inventive Principle:
Principle #23Feedback

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

Enables continuous, real-time monitoring of chemical reactions without disrupting the reaction environment, maintaining mass balance, and providing detailed insights into reaction kinetics and molecular structures through time-dependent infrared spectra analysis.

Implementation Method 1

In the ATR crystal, the infrared electromagnetic radiation is confined, so that only its evanescent field escapes the ATR crystal and penetrates the surrounding medium for a few micrometers

Methodology Applied
Scientific EffectTotal internal reflection: Total Internal Reflection

Implementation Method 2

When the specimen is placed on top of the ATR crystal and pressed to it to make tight contact, the specimen absorbs a fraction of the evanescent field. The non-absorbed part of the IR radiation is reflected inside the ATR crystal

Methodology Applied
Scientific EffectAbsorption of infrared radiation: Absorption (EM radiation)

Data Source

PatentUS20240142374A1Gas Flow Chamber Device and Method of ATR Infrared Spectroscopy for Monitoring Chemical Reactions in Controlled Environments
Publication Date: 2024.05.02 MORGAN STATE UNIVERSITY
  • US20240142374A1 patent drawing
  • US20240142374A1 patent drawing
  • US20240142374A1 patent drawing

AI summary

A gas flow chamber device and method for in-situ time-dependent attenuated total reflectance (ATR) infrared spectroscopy for monitoring solid-gas and liquid-gas chemical reactions in a gaseous flowing medium (gas or vapor) within a controlled environment includes a flow chamber enclosure attached to the infrared spectrometer, such that it covers the specimen on the ATR plate of the infrared spectrometer; a flow chamber inlet port to provide the gaseous flowing medium of desired chemical composition inside the chamber and in contact with the specimen; and a flow chamber outlet port to provide for the exhaust of the gaseous flowing medium from the flow chamber after the gaseous flowing medium has been in contact with the solid or liquid specimen.