A method of making solid-phase microextraction probe

An extraction and stainless steel wire technology, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the problems of long production time, sol blockage of pore size, and difficult to accurately control coating thickness, and achieve fast production speed. , good selectivity, good reproducibility

Active Publication Date: 2022-04-12
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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Problems solved by technology

[0004] At present, the commonly used methods for preparing SPME probes using MOFs (ZIFs) as adsorption materials include in-situ hydrothermal synthesis, physical adhesion, sol-gel and adhesive methods. These preparation methods have the disadvantages of long production time and difficult coating thickness. Precise control, or defects such as sol clogged pores

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example

[0055] 1. Carrier pretreatment

[0056] Straightened stainless steel wires with a diameter of 0.15 mm were ultrasonically cleaned with ethanol and deionized water for 10 min to remove any possible contaminants, and then dried in air.

[0057] Two, the preparation of hydroxyl double salt

[0058] 1. In a 20mL vial, add 10mL of deionized water and a magnet, then add 0.406g (5mmol) of zinc oxide, and stir rapidly for 20min to obtain a suspension of zinc oxide, named solution A.

[0059] 2. Weigh 1.098g (5mmol) of zinc acetate dihydrate and dissolve it in 5mL of deionized water to obtain solution B.

[0060] 3. Add solution B to solution A under rapid stirring, and then continue to stir at room temperature for 24 hours to obtain a gel-like viscous liquid, indicating the formation of (Zn,Zn)HDS.

[0061] 3. Electrodeposition of hydroxyl double salt

[0062] In a 10mL small weighing bottle, add an appropriate amount of (Zn, Zn) HDS suspension, use stainless steel wire as the work...

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Abstract

A method for making a solid-phase microextraction probe, comprising the steps of: S1, depositing a hydroxyl double salt on a stainless steel wire by an electrochemical method; S2, depositing the stainless steel wire with a hydroxyl double salt and 2-methylimidazole Reacting with an aqueous solution of surfactant at room temperature, the hydroxyl double salt is converted into ZIF in situ, and a solid-phase microextraction probe with a ZIF‑8 coating is obtained. A solid phase microextraction method, using the solid phase microextraction probe made by the method to carry out solid phase microextraction. The method for manufacturing the SPME probe of the invention is simple and fast, and the prepared coating is compact and uniform, and has good adhesion with the carrier, thereby improving its service life. The SPME probe with ZIF-8 coating produced by the invention can extract polycyclic aromatic hydrocarbons in environmental water samples, has high extraction efficiency, and meets the requirements of trace analysis.

Description

technical field [0001] The invention relates to a solid-phase microextraction technique for chemical analysis and testing, in particular to a method for making a solid-phase microextraction probe. Background technique [0002] Solid Phase Microextraction (Solid Phase Microextraction, SPME) integrates sampling, extraction, concentration and sample injection, and is a new technology for solvent-free sample processing. Compared with traditional sample pretreatment technologies, SPME technology completes extraction, concentration and sample injection under solvent-free conditions, and can be used in conjunction with GC, HPLC and MS to effectively analyze trace organic compounds in samples to Fast qualitative / quantitative analysis. The current commercialized SPME probes are mainly developed and produced by the U.S. Supelco company. The coatings of the commercialized SPME extraction probes mainly include polydimethylsiloxane (PDMS), polyethylene glycol / polydimethylsiloxane ( CAR...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/10C02F1/28C02F101/30
CPCB01D15/10C02F1/28C02F2101/30
Inventor 田园霍新明余泉王晓浩冯喜兰
Owner SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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