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Solid phase micro-extraction stainless steel fiber and preparation method thereof

A technology of stainless steel and stainless steel wire, which is applied in the field of new solid phase microextraction fiber and its preparation, can solve the problems of easy fiber breakage, high cost, and easy bending of fiber, and achieve high enrichment efficiency, simple method and low cost

Inactive Publication Date: 2009-09-16
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Commercial extraction fibers show a series of defects: easy fiber breakage, thermal instability (usually 240-280°C), easy bending of the fiber, easy peeling off of the coating and high price
In this paper, the SPME fiber is composed of aluminum wire with alumina surface, which shows good properties: strong, low cost, good stability, and easy to prepare; however, this fiber only Suitable for analysis of gas samples with humidity less than 25%

Method used

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  • Solid phase micro-extraction stainless steel fiber and preparation method thereof
  • Solid phase micro-extraction stainless steel fiber and preparation method thereof
  • Solid phase micro-extraction stainless steel fiber and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (a) Put the water bath in a well-ventilated fume hood and heat to a constant temperature of 40°C;

[0032] (b) in the polytetrafluoroethylene container, add the hydrofluoric acid of mass concentration 40%, it is put into (a) in the water bath constant temperature;

[0033] (c) A 304 stainless steel wire with a diameter of 300 μm is vertically fixed on the upper end of the polytetrafluoroethylene container in (b), so that about 4 cm of the stainless steel wire is immersed in hydrofluoric acid. React for 10-15 minutes;

[0034] (d) The corroded stainless steel wire is taken out, and the residual hydrofluoric acid on the stainless steel wire is carefully rinsed off with clear water;

[0035] (e) Insert the stainless steel wire in (d) into the gas phase injection port and age at 320° C. for 4 h under the protection of nitrogen to obtain the stainless steel fiber for solid phase microextraction.

[0036] The prepared solid-phase microextraction stainless steel fiber 1 is l...

Embodiment 2

[0038] (a) Put the water bath in a well-ventilated fume hood and heat to a constant temperature of 25°C;

[0039] (b) in the polytetrafluoroethylene container, add the hydrofluoric acid of mass concentration 40%, it is put into (a) in the water bath constant temperature;

[0040] (c) Fix a 304 stainless steel wire with a diameter of 300 μm vertically on the upper end of the polytetrafluoroethylene container in (b), so that about 4 cm (or any length between 3 and 6 cm) of the stainless steel wire is immersed in hydrofluoric acid. Reaction about 1h;

[0041] (d) The corroded stainless steel wire is taken out, and the residual hydrofluoric acid on the stainless steel wire is carefully rinsed off with clear water;

[0042] (e) Pack the stainless steel wire in (d) into a micro-injector to make a solid-phase microextraction device. The prepared solid phase microextraction fiber was inserted into the gas phase injection port and aged at 280°C for 4h under the protection of nitrogen...

Embodiment 3

[0044] The solid-phase microextraction stainless steel fiber that embodiment 2 is made is used for the pre-enrichment of six kinds of EPA-PAHs of naphthalene, acenaphthene, fluorene, phenanthrene, fluoranthene, pyrene in the determination water sample (see appendix figure 2 , the concentration of each analyte is 10ppb), and the sensitivity of the detection limit obtained after the enrichment is 2630-3570 times higher than that before the enrichment. The detection limit is 0.24-0.63ppb. Tested repeatedly, its relative standard deviation is less than 6.0%. After the extraction fiber is used 250 times, the enrichment effect basically does not change.

[0045] GC-FID operating conditions: SE-54 capillary quartz column (30m×0.53mm.×1.0μm), heating program: 180°C for 1.5min, 4°Cmin -1 Raise the temperature to 220°C and keep it for 5min. Injection port temperature: 320°C, detector temperature: 320°C.

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Abstract

The invention relates to a novel solid phase micro-extraction stainless steel fiber and a preparation method thereof, which provides a method for easily and rapidly preparing the solid phase micro-extraction stainless steel fiber with high stability and high reproducibility. The preparation method is as follows: soaking the part of cleaned stainless steel wire into acid for treatment; washing by water; ageing under the protection of nitrogen, obtaining the solid phase micro-extraction stainless steel fiber; mounting the prepared solid phase micro-extraction stainless steel fiber in a microliter syringe, obtaining a simple solid phase micro-extraction device. The method is simple in operation and low in cost. The prepared solid phase micro-extraction stainless steel fiber has excellent extraction performance on all trace amount organic pollutants. Compared with commercial solid phase micro-extraction device, the solid phase micro-extraction device has better mechanical strength and thermal stability, and has low cost and long service life. The extraction fiber has excellent application potential in fields of environmental monitoring, food hygiene and the like.

Description

【Technical field】: [0001] The invention relates to a novel solid-phase microextraction fiber and a preparation method thereof. 【Background technique】: [0002] The solid-phase microextraction technology proposed by Pawliszyn in the 1990s combines sampling, extraction and sample processing. The method is simple, flexible, low-cost, solvent-free, rapid and sensitive. [0003] At present, commercial solid-phase microextraction fibers are mainly based on quartz as the carrier. Coatings mainly include polydimethylsiloxane (PDMS), polyacrylate (PA), polydimethylsiloxane / divinylbenzene (PDMS / DVB), polyethylene glycol / divinylbenzene (PEG / DVB), Carboxen / PDMS, Carbowax / divinylbenzene (CW / DVB) and polyacrylonitrile (PAN). These coatings are fixed on the surface of quartz fibers by physical or chemical methods. [0004] The commercial extraction fiber shows a series of defects: the fiber is easy to break, thermally unstable (usually 240-280°C), the fiber is easy to bend, the coatin...

Claims

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Application Information

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IPC IPC(8): B01D15/08B01J20/28B01J20/32C23F1/00C23F1/28
Inventor 江冬青徐华玲李妍严秀平
Owner NANKAI UNIV
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