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Solid phase micro-extraction device and method for preparing fibre extraction head thereof

A technology of extraction device and extraction head, which is applied in the direction of ion exchange treatment device, ion exchange regeneration, ion exchange, etc., to achieve the effects of simple structure, easy production and high enrichment multiple.

Inactive Publication Date: 2009-08-05
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The special properties of metal-organic porous frameworks determine that it can be used as an excellent solid-phase microextraction material, but so far there is no method to achieve in-situ growth of metal-organic porous frameworks on metal surfaces, and it cannot be applied to solid-phase microextraction. extraction

Method used

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  • Solid phase micro-extraction device and method for preparing fibre extraction head thereof
  • Solid phase micro-extraction device and method for preparing fibre extraction head thereof
  • Solid phase micro-extraction device and method for preparing fibre extraction head thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1. Preparation of fiber extraction head with metal organic porous framework material MOF-199 on the surface

[0028] First, the pretreatment of metal fibers:

[0029] Put a 1.5-4.0cm long part of a metal fiber with an outer diameter of 0.05-0.3mm and a total length of 3.0-8.0cm in aqua regia, and corrode it at room temperature for 20-60 minutes, and control the outer diameter of the metal fiber to 0.05-8.0cm by controlling the corrosion time. 0.20mm, put the other end of the metal fiber (about 1.5-44.0cm) in HF, corrode at room temperature for 20-40 minutes until the surface of this metal fiber turns black, rinse with pure water and dry.

[0030] Second, in situ preparation of metal-organic porous framework materials on the surface of metal fibers:

[0031] 0.437g Cu 2 (NO 3 ) 2 3H 2 O was dissolved in 6mL of pure water, 0.640g of trimesic acid was dissolved in 18mL of absolute ethanol, ultrasonically dissolved for 10min and then mixed, the mixed solution ...

Embodiment 2

[0032] Example 2, the preparation of the fiber extraction head whose surface is the metal organic porous framework material MOF-5

[0033] First, the pretreatment of metal fibers:

[0034] Put a 1.5-4.0cm long part of a metal fiber with an outer diameter of 0.05-0.3mm and a total length of 3.0-8.0cm in aqua regia, and corrode it at room temperature for 20-60 minutes, and control the outer diameter of the metal fiber to 0.05-8.0cm by controlling the corrosion time. 0.20mm, put the other end of the metal fiber (about 1.5-4.0cm) in HF, corrode at room temperature for 20-40 minutes until the surface of this metal fiber turns black, rinse with pure water and dry.

[0035] Second, in situ preparation of metal-organic porous framework materials on the surface of metal fibers:

[0036] 0.580g Zn(NO 3 ) 2 6H 2 O, 0.160g terephthalic acid, dissolved in 20mL N, N-dimethylformamide, ultrasonically dissolved for 10min, put the solution in a 35mL polytetrafluoroethylene reactor, put th...

Embodiment 3

[0037] Example 3, the surface is the preparation of the fiber extraction head of metal organic porous framework material Zn (BDC) (dabco)

[0038]First, the pretreatment of metal fibers:

[0039] Put the 1.54.0cm long part of a metal fiber with an outer diameter of 0.05-0.3mm and a total length of 3.0-8.0cm in aqua regia, and corrode it at room temperature for 20-60 minutes, and control the outer diameter of the metal fiber to 0.05-0.20 by controlling the corrosion time. mm, put the other end of the metal fiber (about 1.5-4.0cm) in HF, corrode at room temperature for 20-40 minutes until the surface of this metal fiber turns black, rinse with pure water and dry.

[0040] Second, in situ preparation of metal-organic porous framework materials on the surface of metal fibers:

[0041] 0.50g Zn(NO 3 ) 2 6H 2 O, 0.280g terephthalic acid, 0.094g triethylenediamine were dissolved in 20mL N,N-dimethylformamide, and after ultrasonic dissolution for 10min, the solution was placed in...

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Abstract

The invention relates to a solid phase micro-extraction device and a method for preparing a fiber extraction head thereof. The solid phase micro-extraction device comprises a micro sample injector, the inside of a sample injector push rod is provided with a stainless steel capillary pipe, and the lower end of the sample injector push rod is inserted with the fiber extraction head. The preparation method for the fiber extraction head comprises: corroding one end of a metal fiber into aqua regia, while corroding the other end in HF; dissolving metal salt and organic ligand in a solvent in a hot water reaction kettle to obtain a reaction mixed liquor; and immerging the one end of the metal fiber corroded by the HF after pretreatment into the reaction mixed liquor, and controlling the temperature to between 50 and 220 DEG C and the time to between 6 and 90 hours to prepare the solid phase micro-extraction head of which the surface is grown with metal organic porous skeleton materials in situ. The solid phase micro-extraction device has the advantages of difficult damage of extracted fibers, high temperature resistance, low cost, good extraction performance, capability of replacing the extraction head, and large adsorption capacity. The method can grow porous skeleton materials with different structures on the extraction head aiming at different compounds so as to design high-selectivity enrichment to a target object, and has wide application prospect in the aspect of analytical chemistry.

Description

【Technical field】: [0001] The invention relates to the assembly of a solid-phase microextraction device and the preparation of fibers thereof. The fiber is a novel solid-phase microextraction fiber with metal-organic porous framework materials grown on the surface in situ. 【Background technique】: [0002] Solid-phase microextraction technology is a new technology for sample pretreatment. This method has the advantages of less solvent consumption, high sensitivity, and easy automation. Generally, the fused silica fiber is hidden in the needle, and when necessary, the injector push rod can be pushed to make the quartz fiber protrude from the needle. This kind of extraction head is to coat the stationary phase coating on the quartz fiber as the extraction fiber. These stationary phase coatings mainly include polydimethylsiloxane (PDMS), polyacrylate (PA), carbon molecular sieve / ethylene phenylene (CW / DVB) or carbon molecular sieve / molecular template resin (CW / TPR), polyethylen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/08
Inventor 严秀平崔晓燕李妍
Owner NANKAI UNIV
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