Cryogenic Liquid Analyzer Using Partial Vaporization for Trace Impurities

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Solution Overview

Problem

Current methods for analyzing impurities in cryogenic liquids, such as those used in air separation by cryogenic distillation, face challenges in detecting low levels of contaminants like N2O and CO2, which are below 100 ppb, requiring complex apparatus and significant operating skill, and often result in incomplete or inaccurate determination of impurity types and quantities due to prolonged vaporization processes and lack of precise sampling.

Innovation Solution

An apparatus that involves partial vaporization of a known quantity of cryogenic liquid, allowing impurities to concentrate in the liquid phase, followed by direct analysis of the vaporized phase after overheating to ensure complete vaporization and measurement of contaminant content using conventional analyzers capable of detecting concentrations below 1 ppm, with a controlled cycle time to avoid prolonged accumulation and ensure accurate quantification.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If complex apparatus and prolonged vaporization processes are used to detect low levels of impurities, then measurement precision is improved, but device complexity and operational time increase

Engineering Contradiction:
Improveimpurity detection capabilityVSAvoidapparatus complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The invention changes the concentration parameter by partially vaporizing the liquid oxygen sample, which concentrates the impurities in the remaining liquid phase. This parameter change enables conventional analyzers to detect impurities at levels below 100 ppb without requiring complex specialized apparatus, thus resolving the contradiction between measurement precision and device complexity

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention utilizes the phase transition of oxygen from liquid to vapor during controlled partial vaporization. By exploiting the different vaporization characteristics of oxygen and impurities, the method concentrates impurities in the liquid phase while oxygen vaporizes, enabling detection with standard equipment and reducing both device complexity and operational time

Inventive Principle:
Principle #36Phase transitions

2Measurement precision

If prolonged vaporization processes are used to accumulate sufficient impurities for detection, then measurement precision is improved, but loss of time increases

Engineering Contradiction:
Improveimpurity quantification accuracyVSAvoidanalysis cycle time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The invention applies partial vaporization rather than complete vaporization of the liquid oxygen sample. By vaporizing only a controlled portion (enough to concentrate impurities to detectable levels), the method achieves accurate impurity quantification significantly faster than prolonged complete vaporization processes, thus resolving the contradiction between measurement precision and time loss

Inventive Principle:
Principle #16Partial or excessive action

Solution Approach 2:

The method changes the concentration parameter through controlled partial vaporization, achieving sufficient impurity concentration for accurate detection within a short time frame. This parameter change eliminates the need for prolonged accumulation processes while maintaining measurement precision

Inventive Principle:
Principle #35Parameter changes

3Ease of operation

If conventional analyzers are used for impurity detection, then ease of operation is improved, but measurement precision deteriorates due to detection limits

Engineering Contradiction:
Improveoperational simplicityVSAvoiddetection limit
Core Design Contradiction:
Ease of operationVSMeasurement precision

Solution Approach 1:

The invention changes the concentration parameter by partially vaporizing the liquid oxygen, which concentrates impurities in the remaining liquid phase. This parameter change raises the impurity concentration above the detection limits of conventional analyzers, enabling these simpler devices to achieve the required measurement precision for detecting impurities below 100 ppb

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention creates a local concentrated phase of impurities in the remaining liquid after partial vaporization. This local concentration enables conventional analyzers to detect and measure impurities accurately without requiring complex specialized equipment, thus resolving the contradiction between ease of operation and measurement precision

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

Enables rapid and precise measurement of impurity concentrations below 1 ppm, reducing operational complexity and cycle time, while ensuring accurate determination of contaminant content without the need for prolonged accumulation or external sampling, thereby enhancing operational safety and efficiency in cryogenic distillation systems.

Implementation Method 1

a) a partial vaporization of a determined quantity of this liquid is performed

Methodology Applied
Scientific EffectVaporization: Evaporation

Implementation Method 2

allowing impurities to concentrate in the liquid phase

Methodology Applied
Scientific EffectConcentration:

Implementation Method 3

b) the vaporized phase is then overheated, thus creating a rise in pressure in the vaporization enclosure

Methodology Applied
Scientific EffectOverheating: Superheating

Implementation Method 4

The evolution of the pressure measured in the closed enclosure gives the quantity of matter initially present in the liquid or solid phase

Methodology Applied
Scientific EffectPressure measurement:

Data Source

PatentEP3625536B1Apparatus for treating liquid to be analysed
Publication Date: 2022.11.16 LAIR LIQUIDE SA POUR LETUDE & LEXPLOITATION DES PROCEDES GEORGES CLAUDE
  • EP3625536B1 patent drawingFigure 1

AI summary

An apparatus for analysing the content of at least one contaminant in a liquid cryogen comprising a cylindrical enclosure (E), an annular enclosure (V) arranged around the cylindrical enclosure, means (1, 3, 5) for dividing a flow of liquid cryogen in two, means for delivering a first part (3) of the liquid cryogen to the cylindrical enclosure, means for delivering a second part (5) of the liquid cryogen to the annular enclosure, a pipe (13) connected to the cylindrical enclosure to allow vaporised liquid to pass through, a pipe (6) connected to the annular enclosure to allow vaporised liquid to pass through, a heater (H) for heating the cylindrical enclosure vessel and means (V1) for stopping the delivery of liquid cryogen to the cylindrical enclosure.