Electrospray Apparatus for Uniform Polymer Specimen Deposition

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Solution Overview

Problem

MALDI mass spectrometry lacks reproducibility for quantitative analysis of polymers, particularly due to variations in specimen thickness affecting ionization efficiency and pattern consistency, and existing techniques are not applicable to commercialized MALDI-TOF MS equipment.

Innovation Solution

A method using an electrospray apparatus with a main nozzle and auxiliary nozzle, along with a mask to control specimen thickness and a sheath gas for precise deposition on a sample plate, ensuring a thickness deviation of 30% or less, allowing for uniform specimen preparation suitable for commercial MALDI-TOF equipment.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional electrospray method is used for specimen preparation, then the specimen can be deposited on sample plate, but the specimen thickness varies significantly leading to poor reproducibility of MALDI spectrum

Engineering Contradiction:
Improvereproducibility of MALDI spectrumVSAvoidspecimen thickness uniformity
Core Design Contradiction:
ReliabilityVSManufacturing precision

Solution Approach 1:

A mask with a hole of specific diameter (0.5-2.0 mm) is introduced as an intermediary component between the electrospray nozzle and sample plate. This mask mediates the deposition process by restricting the spray area to the center region, thereby controlling specimen thickness uniformity and improving MALDI spectrum reproducibility

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The invention applies local quality by selecting only the center region of the electrospray jet for specimen deposition. The mask with a central hole restricts the spray to the core area where the most uniform and controlled polymer sample is deposited, excluding the periphery where thickness variation is greater

Inventive Principle:
Principle #3Local quality

2Reliability

If matrix is sprayed along with polymer sample from main nozzle, then ionization can occur, but matrix deposits in vicinity of nozzle causing clogging and reduced reliability

Engineering Contradiction:
Improveconsistent ionization and spectrum qualityVSAvoidnozzle clogging from matrix deposition
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The invention segments the electrospray system into two independent nozzles: a main nozzle for polymer sample delivery and an auxiliary nozzle for matrix delivery. This segmentation allows separate control of sample and matrix deposition, preventing matrix clogging of the main nozzle while ensuring consistent ionization

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The auxiliary nozzle acts as an intermediary that delivers matrix to the specimen after the polymer sample has been deposited by the main nozzle. This intermediate step ensures matrix is present for ionization without causing clogging in the primary sample delivery path

Inventive Principle:
Principle #24Intermediary (Mediator)

3Measurement precision

If quantitative analysis is performed on polymer using conventional MALDI, then molecular weight information can be obtained, but the results lack reproducibility across different specimens and analysis spots

Engineering Contradiction:
Improvequantitative accuracy of polymer analysisVSAvoidreproducibility across specimens and spots
Core Design Contradiction:
Measurement precisionVSReliability

Solution Approach 1:

The invention changes the specimen preparation parameters by controlling deposition area through the mask hole diameter (0.5-2.0 mm) and selecting the center region of the electrospray jet. These parameter changes result in specimens with thickness deviation of 30% or less, enabling reproducible quantitative analysis across different specimens and analysis spots

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

The method achieves reproducible MALDI spectra with a relative standard deviation of 30% or less, enabling efficient and quick quantitative analysis of polymers across multiple specimens and analysis spots.

Implementation Method 1

a main nozzle (110) for electrospray of a polymer sample which is a mixed solution of a polymer compound, a matrix and a solvent

Methodology Applied
Scientific EffectElectrospray: Electrohydrodynamics

Implementation Method 2

spraying the solvent from an auxiliary nozzle (120) surrounding the main nozzle (110) and coaxial with the main nozzle (110), so as to prevent the matrix from being deposited in the vicinity of the main nozzle (110)

Methodology Applied
Scientific EffectElectrospray: Electrohydrodynamics

Implementation Method 3

jetting a sheath gas through a sheath gas supply pipe (130) so that the sheath gas guides the polymer sample to be sprayed onto the predetermined position of the sample plate

Methodology Applied
Scientific EffectGas flow guidance: Fluid Spray

Data Source

PatentEP3696529B1Method for quantitative analysis of polymer using maldi mass spectrometry, and method for manufacturing sample for maldi mass spectrometry for quantitative analysis of polymer
Publication Date: 2023.02.22 LG CHEM LTD
  • EP3696529B1 patent drawingFigure 1
  • EP3696529B1 patent drawingFigure 2
  • EP3696529B1 patent drawingFigure 3

AI summary

The present invention provides a method enabling a quantitative analysis of a polymer by MALDI mass spectrometry, and a method for manufacturing a sample for MALDI mass spectrometry for a quantitative analysis of a polymer. To that end, the methods can increase reproducibility of a MALDI spectrum by making uniform the thickness of a sample affecting the pattern in a polymer MALDI spectrum. The sample according to the present invention is applicable also to a commercial MALDI-TOF instrument, and, thus, can quantitatively analyze a polymer in a more efficient and faster manner.