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Method for manufacturing capillary filled column plunger by using photonic crystal fiber and application

A technology of photonic crystal fiber and capillary, which is applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc. It can solve the problems of poor repeatability, long preparation time, poor controllability of pore structure, etc.

Inactive Publication Date: 2021-05-21
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional plunger preparation methods mainly include silica gel filler sintering method, sol-gel method, and on-column in-situ polymerization method. These methods generally have disadvantages such as long preparation time, numerous steps, poor repeatability, and poor controllability of pore structure (Document 3 Ma Jiping. Journal of Analysis and Testing. 2008.27.42-44)

Method used

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  • Method for manufacturing capillary filled column plunger by using photonic crystal fiber and application
  • Method for manufacturing capillary filled column plunger by using photonic crystal fiber and application
  • Method for manufacturing capillary filled column plunger by using photonic crystal fiber and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1 Using photonic crystal fiber as the plunger to prepare a capillary packed column

[0022] 1) Cut the photonic crystal fiber-1 (outer diameter 125μm, cladding layer 10um, containing 126 air holes with a diameter of 3.2μm) into a length of 1cm, soak in 2mL of toluene solution for 10min, make the outer wall of the fiber cladding layer Swell, then carefully remove the fiber with tweezers and remove the coating;

[0023] 2), apply the potting glue (Dow Corning PDMS-184 glue, USA) evenly on the outer wall of the optical fiber, and then insert it into a 30cm empty capillary (outer diameter 360μm, inner diameter 150μm);

[0024] 4) Put the capillary tube with the optical fiber plunger into an oven at 80°C for 2 hours, so that the epoxy resin glue can be fully cured before use;

[0025] 4), use the homogenization method to fill the capillary column with 3 μm C18 silica gel as the filler. The length of the plunger is 1 cm, and the length of the packing is 25 cm for ch...

Embodiment 2

[0026] Example 2 Using photonic crystal fiber as plunger to prepare capillary packed column

[0027] 1) Cut the photonic crystal fiber-2 (outer diameter 125μm, cladding layer 10um, containing 126 air holes with a diameter of 2.6μm) into a length of 1cm, soak in 2mL of toluene solution for 10min, make the outer wall of the fiber cladding layer Swell, then carefully remove the fiber with tweezers and remove the coating;

[0028] 2), apply the potting glue (Dow Corning PDMS-184 glue, USA) evenly on the outer wall of the optical fiber, and then insert it into a 30cm empty capillary (outer diameter 360μm, inner diameter 150μm);

[0029] 4) Put the capillary tube with the optical fiber plunger into an oven at 80°C for 2 hours, so that the epoxy resin glue can be fully cured before use;

[0030] 4), use the homogenization method to fill the capillary column with 3 μm C18 silica gel as the filler. The length of the plunger is 1 cm, and the length of the packing is 25 cm for chromato...

Embodiment 3

[0031] Example 3 Using porous organic monolithic column as plunger to prepare capillary packed column

[0032] 1), activate the inner wall of an empty capillary (outer diameter 360 μm, inner diameter 150 μm). The UV-transparent capillary was rinsed with 0.1mol / L NaOH aqueous solution (1h), deionized water (0.5h), 0.1mol / L HCl aqueous solution (4h), deionized water (0.5h) and methanol (0.5h) in turn, and then in Dry under nitrogen flow;

[0033] 2) The inner wall of the empty capillary (outer diameter 360 μm, inner diameter 150 μm) is vinyl functionalized. The methanol solution (1:1, v / v) of γ-(methacryloyloxy)propyltrimethoxysilane (γ-MAPS) was injected into the capillary. After the solution was filled, both ends of the capillary were sealed with silica gel sheets. Incubate and put it in a 50°C water bath for 12h; finally rinse the capillary with methanol (1h), and dry it under nitrogen flow;

[0034] 3), to prepare a prepolymer solution. Pipette 170 μL of n-butanol and 13...

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Abstract

The invention relates to a method for manfacturing capillary filled column plunger by using microstructured photonic fiber,MSF with an axial porous microstructure. The method comprises steps: removing a sheath protective layer of the photonic crystal fiber with a certain length, crosslinking the optical fiber with the protective layer removed in the inner wall of the capillary tube by using a pouring sealant as an adhesive, and curing for use. The method has the advantages of few steps, simple operation, good repeatability, controllable plunger length and less time consumption, and the preparation process can be completed within several hours. A prepared plunger matrix is fused silicon dioxide, is not easy to swell in an organic reagent and has very good mechanical stability and thermal stability, and the method can be used for preparing double-end plungers at two ends of a capillary tube, so that filler backflushing during pressure relief after analysis is completed is prevented, and the service life of a packed column is prolonged.

Description

technical field [0001] The invention relates to a method for preparing a capillary filled plunger by using a photonic crystal fiber (MSF) as a raw material. The optical fiber is glued to the inner wall of the capillary and can be used as a plunger after curing. Background technique [0002] Capillary Liquid Chromatography (cLC) is a highly efficient and rapid separation and analysis method using capillary chromatographic columns as analytical columns, which has developed rapidly in recent years. This method has the incomparable advantages of conventional liquid chromatography, such as low consumption of mobile phase, stationary phase and analytical samples, low environmental pollution, easy to be combined with detection methods such as mass spectrometry, etc. It is especially suitable for the separation of rare or precious samples analyze. These advantages make it an important means of "micro-scale" separation and analysis, and it has been widely used in the fields of envi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22G01N30/60
CPCB01D15/22G01N30/6004G01N30/6078
Inventor 欧俊杰马淑娟王妍叶明亮
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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