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Solid phase microextraction head based on ionic liquid coating and preparation method thereof

A solid-phase micro-extraction head and ionic liquid technology, applied in the field of environmental analytical chemistry, can solve the problems of cumbersome preparation process of the extraction head, low target substance enrichment efficiency, difficult hydrolysis, thermal stability, etc. Low cost and long service life

Inactive Publication Date: 2016-05-18
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ionic liquid [AMIM][BF 4 ] coated on the fused silica fiber matrix, the preparation process of the extraction head is cumbersome, time-consuming (several hours), the preparation cost is high, and the defect that the extraction head is easy to break cannot be avoided, and it is inconvenient to use
In addition, the headspace solid-phase microextraction method is used in the extraction process. In order to improve the extraction efficiency of the target substance, the sample solution needs to be heated to a higher temperature (80°C), and the target substance (especially for high boiling point and strong hydrophobicity) The enrichment efficiency of the target object) is not high, and it is difficult to be popularized in actual analysis
[0004] In recent years, a class of ionic liquids whose anions are tris(perfluoroalkyl)trifluorophosphate [FAP] has been used as a liquid-phase microextraction technique due to its strong hydrophobicity, difficult hydrolysis, and good thermal stability. Extractant, but the application of this type of ionic liquid in solid phase microextraction has not been reported

Method used

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  • Solid phase microextraction head based on ionic liquid coating and preparation method thereof
  • Solid phase microextraction head based on ionic liquid coating and preparation method thereof
  • Solid phase microextraction head based on ionic liquid coating and preparation method thereof

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preparation example Construction

[0027] The present invention also discloses a method for preparing a metal fiber for a solid phase microextraction head as described above, comprising the following steps:

[0028] Step 1, select a section of metal wire with a diameter of 0.3mm as the metal carrier;

[0029]Step 2, insert the metal wire vertically into an ionic liquid, keep it for 3-10 minutes, then lift it out of the liquid surface, and let it stand in the air for 1.0-5.0 minutes; repeat the above coating process until the required coating thickness, The desired metal fibers are thus obtained;

[0030] In step 3, the metal fiber coated with the ionic liquid coating prepared in step 2 is aged at a high temperature under the protection of helium to remove volatile impurities, that is, to obtain the metal fiber of the solid phase microextraction head.

[0031] Preferably, step 1 also includes the steps of roughening, washing and drying the metal wire.

[0032] Preferably, between step 1 and step 2, the step of...

Embodiment 1

[0050] figure 1 A structural diagram of a solid-phase microextraction head coated with a metal carrier ionic liquid is given. In the figure, the rubber stopper 1, stainless steel capillary tube 2, SPME sleeve 3 and metal fiber 4 constitute the body of the extraction head, and the rubber stopper 1 is installed on the The upper end of the stainless steel capillary 2, the SPME casing 3 is set on the stainless steel capillary 2, exposing the two ends of the stainless steel capillary 2, and the metal fiber 4 is fixed to the top of the stainless steel capillary 2, wherein the inner diameter of the stainless steel capillary 2 in this embodiment is about 0.3mm , about 100mm in length; the metal fiber 4 of the extraction head is made of stainless steel wire with a diameter of about 0.15mm (iron wire, platinum wire, titanium wire or nickel wire can also be selected), and the surface is coated with an ionic liquid coating 5, and the ionic liquid coating The thickness of the layer is abou...

Embodiment 2

[0057] The metal fiber of present embodiment experiment is stainless steel wire, and the diameter of stainless steel wire is 0.1mm, and ionic liquid is 1-hexyl-3-methylimidazolium tris(pentafluoroethyl) trifluorophosphate ([HMIM][FAP]) ; During the coating process, insert the stainless steel wire vertically into the ionic liquid, keep it for 10 minutes, then lift it vertically at a constant speed, let it stand in the air for 5 minutes, and repeat the coating until the thickness of the ionic liquid coating is about 80 μm; the aging condition is 250 ° C for 1.5 h. Other structures and manufacturing conditions, steps are the same as in Example 1.

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Abstract

The invention provides a metal fiber for a solid phase microextraction head. The metal fiber for the solid phase microextraction head is composed of a metal wire and an ionic liquid coating with the thickness ranging from 20 micrometers to 80 micrometers or so, wherein the surface of the metal wire is coated with the ionic liquid coating, and negative ions of ionic liquid are tris(pentafluoroethyl)trifluorophosphate ([FAP]) ions. The invention further provides the solid phase microextraction head and preparing methods of the solid phase microextraction head and the metal fiber. The solid phase microextraction head prepared through the physical coating method has a very strong enrichment capacity on organophosphorus ester fire retardants; the preparing method of the solid phase microextraction head is easy and convenient to implement, low in preparing difficulty and low in cost, and materials are convenient to obtain. The solid phase microextraction fiber prepared through the method has the advantages of being high in mechanical strength, good in heat stability, high in enrichment capacity, good in reproducibility, long in service life and the like, can be applied to enrichment analysis of trace components of organophosphorus ester fire retardants in water and has good application potential.

Description

technical field [0001] The invention belongs to the field of environmental analysis chemistry and relates to a solid-phase micro-extraction head based on an ionic liquid coating and a preparation method thereof. Background technique [0002] Organophosphate esters (Organophosphateesters, OPEs) are an important class of flame retardants, which have the advantages of good flame retardant effect, low production cost and simple production process, and are widely used in building materials, home decoration materials, textile products, chemicals and electrical and electronic equipment. However, OPEs and polymer substrates are bound by intermolecular forces rather than chemical bonds, and are gradually released into the environment during use, becoming ubiquitous pollutants in various environmental media. The properties of OPEs are very stable, and the alkyl and aryl phosphates have strong biological effects. In recent years, the environmental pollution of OPEs has become a focus ...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/32C02F1/26C02F101/34
CPCB01J20/02B01J20/22B01J20/28011B01J20/3231C02F1/26C02F2101/34
Inventor 刘景富石凤琼
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI