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Method for rapidly preparing solid-phase microextraction fiber coating

A technology for extracting fibers and coatings, which is applied in the fields of analytical chemistry and environmental analysis. It can solve the problems of easy shedding, short service life, and low output, and achieve the effects of uniform coating, advanced thinking, and simple coating

Active Publication Date: 2014-03-12
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation methods of carbon nanosheets as functional adsorption coating mainly include: physical adsorption method, chemical bonding method, etc., but there are the following defects: the coating prepared based on the principle of physical adsorption is not firm, easy to fall off, and has a short service life; The coating prepared by the method is stable, but the preparation cycle is long and the output is low, which is not suitable for popularization and application

Method used

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  • Method for rapidly preparing solid-phase microextraction fiber coating
  • Method for rapidly preparing solid-phase microextraction fiber coating
  • Method for rapidly preparing solid-phase microextraction fiber coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) Take a certain amount of rubber monomer PDMS monomer and match the curing agent used at the same time according to the volume ratio of 10:1 and mix evenly to obtain a viscous carrier coating (that is, polydimethylsiloxane). Put it into a vacuum drying oven, evacuate until no bubbles escape, and take it out for use;

[0032] 2) Take a solid-phase microextraction fiber stainless steel needle with a diameter of 250 μm, insert it into a stainless steel tube with an inner diameter of 320 μm, burn it on an alcohol lamp for a few seconds, and then insert it directly into the vacuum-degassed viscous carrier coating obtained in the above step 1), Take it out after 1 second, remove the sleeve, and get a 35 μm thick adhesive carrier coating; then insert it into the graphene solid powder of the coating material, and then insert the sleeve stainless steel tube with an inner diameter of 400 μm, pump it back and forth several times to homogenize Graphene coating to obtain a functio...

Embodiment 2

[0037] The prepared graphene-based SPME was compared with commercial SPME using the following scheme:

[0038] 1) Use commercial SPME with 100 μm thick PDMS to extract the volatiles from the cow beetle at room temperature for 2 minutes, then analyze the volatiles in GC-MS at 280°C for 1 minute, and then perform GC separation and MS detection. The results are shown in Figure 6 ;

[0039] 2) Use the SPME with graphene as the functional adsorption coating in Example 1 to extract the volatile matter on the female beetle under the same conditions, the extraction time is 2min, and then carry out the GC-MS analysis and separation and detection under the same conditions , get as Figure 7 The results shown.

[0040] It can be seen from the figure that the extraction efficiency of the graphene extraction head prepared in Example 1 is better than that of the 100 μm thick PDMS extraction head.

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Abstract

The invention discloses a method for rapidly preparing a solid-phase microextraction fiber coating. An intermediate carrier coating, which has adhesive force and is partially polymerized, is coated outside solid fibers to adhere materials difficult to coat, such as carbon nanosheets; and the method is used for preparing novel solid-phase microextraction (SPME) fiber tips. The carrier coating with adhesive force comprises organic silicon rubber or fluorinated silicone rubber and the like which are not completely polymerized; and an external functional adsorption coating contains carbon nanosheets and the like and is used for extraction. The method is advanced in thinking and clear in concept; each coating is simple and convenient to prepare and is controllable in thickness; the obtained coating has uniformity, stability and high-temperature resistance and can be used for preparing solid-phase microextraction fibers which can be used for efficiently extracting trace polycyclic aromatic hydrocarbon and takes graphene as a functional adsorption layer; and a corresponding detection line can achieve 1ng / L, extraction reproducibility is 1%-9%, external-standard recovery rate is 87-105% and the number of extraction times is greater than 120.

Description

technical field [0001] The invention belongs to the fields of analytical chemistry and environmental analysis, and relates to a method for rapidly preparing solid-phase microextraction fiber extraction coatings. Background technique [0002] Solid phase microextraction (SPME) is a new type of sample pretreatment technology, which was first proposed by the Pawliszyn research group in Canada in 1989. This technology integrates sampling, extraction, enrichment and sample injection, does not consume solvents, and can be used online with other instruments. It has developed rapidly in less than 20 years, and various types of extraction media have emerged continuously. . The basic principle of SPME is to immobilize the coating material with adsorption function on the surface of a certain matrix fiber by physical or chemical methods, make direct or indirect contact with the sample, enrich and concentrate the target analyte, and combine it with The sample injection device or direct...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/281B01J20/32
Inventor 陈义
Owner INST OF CHEM CHINESE ACAD OF SCI
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