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Extraction: Advanced Methods

Extraction: Advanced Methods

Metal ions can be separated from one another by complexation with organic ligands–the chelating agent– to form uncharged chelates. Here, the chelating agent must contain hydrophobic groups and behave as a weak acid, losing a proton to bind with the metal. Since most organic ligands used in this process are insoluble or undergo oxidation in the aqueous phase, the chelating agent is initially added to the organic phase and extracted into the aqueous phase. The metal-ligand complex is...

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In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy

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Brass wires with different surface wettability used for in-tube solid-phase microextraction.

Yu-Ping Zhang¹, Cong-Cong Luan², Zhen-Yu Lu³

¹College of Chemistry and Materials Engineering, Hunan University of Arts and Science, Changde, 415000, China; College of Chemistry, Zhengzhou University, Zhengzhou 450001, China; Henan Institute of Science and Technology, Xinxiang 453000, China.

Journal of Chromatography. A

|March 26, 2022

Summary

Brass wires were modified for solid-phase microextraction (SPME) fibers. Superhydrophobic wires modified with 2-naphthalenethiol showed the highest estrogen extraction efficiency due to π-π interactions, not just surface wettability.

Keywords:

Brass wire In-tube SPME Superhydrophilic Superhydrophobic

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Area of Science:

Analytical Chemistry
Materials Science

Background:

Metal wires offer a robust alternative to fragile silica fibers for solid-phase microextraction (SPME).
Surface modification of metal wires for SPME is often complex and challenging.

Purpose of the Study:

To develop a facile method for modifying brass wires for in-tube SPME-HPLC online systems.
To investigate the role of surface wettability and chemical modification in the extraction efficiency of estrogens.

Main Methods:

Brass wires were etched using an acidic iron trichloride solution to create micro/nanoscale hierarchical structures, altering surface wettability.
Wires were further modified with n-octadecanethiol (ODT) and 2-naphthalenethiol (NT) to achieve superhydrophobicity.
Characterization involved SEM, EDS, and contact angle measurements.
An online in-tube SPME-HPLC system was constructed and utilized for estrogen extraction.

Main Results:

Chemical etching transformed hydrophobic brass to hydrophilic surfaces.
Modification with ODT and NT resulted in superhydrophobic surfaces.
The superhydrophobic wire modified with NT demonstrated the highest extraction efficiency for six estrogens (enrichment factors 36-350).
Extraction efficiency correlated with π-π interactions between the naphthalene rings of the NT modifier and the benzene rings of estrogens, surpassing the effect of surface wettability.

Conclusions:

A simple and effective method for preparing superhydrophobic brass wires for SPME was developed.
2-Naphthalenethiol-modified brass wires are highly efficient for estrogen extraction in an online SPME-HPLC system.
The enhanced extraction performance is primarily attributed to π-π interactions, highlighting the importance of chemical functionalization beyond surface hydrophobicity.