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Micro solid-phase extraction method of membrane-protected coordination polymer of polybrominated diphenyl ethers in multiple mediums

A technology of polybrominated diphenyl ethers and coordination polymers, which is applied in the fields of applied chemistry and analytical chemistry, can solve the problems of narrow independent application range, etc., and achieve the effects of shortening pretreatment time, high sensitivity and good reproducibility

Inactive Publication Date: 2012-09-19
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The key step in the analysis and detection of polybrominated diphenyl ethers is the pretreatment technology of its samples. Extremely narrow, but its linkage with other pre-processing technologies is excellent

Method used

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  • Micro solid-phase extraction method of membrane-protected coordination polymer of polybrominated diphenyl ethers in multiple mediums
  • Micro solid-phase extraction method of membrane-protected coordination polymer of polybrominated diphenyl ethers in multiple mediums
  • Micro solid-phase extraction method of membrane-protected coordination polymer of polybrominated diphenyl ethers in multiple mediums

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Preparation of membrane-protected complex micro-SPE bags

[0020] Add 1mol of terephthalic acid and 2mol of sodium hydroxide into the secondary water, and after fully stirring and dissolving, add 1mol of copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 O), stirring continuously for 3 hours until a blue powdery precipitate is formed in the solution. The filtered and air-dried blue powder was placed in a brown light bottle for later use.

[0021] Cut the 0.2μm pore diameter polypropylene film to 3.0cm×1.0cm size, fold the long side in half, heat seal the openings on both sides with a small plastic sealing machine, take 10mg of the above synthesized copper terephthalate complex and pour it into the polypropylene film bag, then completely seal the polypropylene film bag and trim the raw edges. Finally, the micro solid phase extraction bags with good sealing performance were cleaned ultrasonically for 5 minutes in pure water and methanol, and then soaked in methanol for ...

Embodiment 2

[0036] Embodiment 2 standard-added soil sample analysis

[0037] (1) Preparation of membrane-protected complex micro-SPE bags

[0038] Add 1mol of terephthalic acid and 2mol of sodium hydroxide into the secondary water, and after fully stirring and dissolving, add 1mol of copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 O), stirring continuously for 3 hours until a blue powdery precipitate is formed in the solution. The filtered and air-dried blue powder was placed in a brown light bottle for later use.

[0039] Take a 0.22μm pore size polypropylene film and cut it to a size of 2.0cm×0.8cm, fold the long side in half, heat seal the openings on both sides with a small plastic sealing machine, take 10mg of the above synthesized copper terephthalate complex and pour it into the polypropylene film bag, then completely seal the polypropylene film bag and trim the raw edges. Finally, the micro solid phase extraction bags with good sealing performance were cleaned ultrasonically for...

Embodiment 3

[0051] Embodiment 3 standard-added soil sample analysis

[0052] (1) Preparation of membrane-protected complex micro-SPE bags

[0053] Add 1mol of terephthalic acid and 2mol of sodium hydroxide into the secondary water, and after fully stirring and dissolving, add 1mol of copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 O), stirring continuously for 3 hours until a blue powdery precipitate is formed in the solution. The filtered and air-dried blue powder was placed in a brown light bottle for later use.

[0054] Take a 0.22μm pore diameter polypropylene film and cut it to a size of 3.0cm×1.5cm, fold the long side in half, heat seal the openings on both sides with a small plastic sealing machine, take 10mg of the above synthesized copper terephthalate complex and pour it into the polypropylene film bag, then completely seal the polypropylene film bag and trim the raw edges. Finally, the micro solid phase extraction bags with good sealing performance were cleaned ultrasonically...

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Abstract

The invention provides a micro solid-phase extraction method of a membrane-protected coordination polymer of polybrominated diphenyl ethers in multiple mediums. The micro solid-phase extraction method is used for constructing a metal organic coordination polymer material with nano ducts and a multi-dimensional structure through metal ion nodes and organic ligand chains and is protected by a membrane to manufacture a micro solid-phase extraction device, wherein the micro solid-phase extraction device is used for extraction and preenrichment of trace amount of polybrominated diphenyl ethers (PBDEs) in a multi-medium environment sample and carrying out quantitative analysis by combining analysis measures, such as a GC (Gas Chromatograph). According to the micro solid-phase extraction method,the target products can be selectively enriched by constructing coordination polymers with different apertures by controlling synthesis conditions; meanwhile, the environment-friendly purpose is achieved because an organic solvent is used or less organic solvent is used; a manufactured micro solid-phase extraction bag can be repeated by more than 20 times, so that cost is low, extraction speed ishigh and no purification is needed; and the micro solid-phase extraction method is used for extracting the PBDEs in soil and can achieve higher sensitivity, better repeatability and lower detection limit by combining analysis measures, such as the GC.

Description

technical field [0001] The invention relates to a micro-solid-phase extraction method for a membrane-protected coordination polymer. Specifically, a complex material is used as an adsorbent, combined with micro-solid-phase extraction technology to extract and enrich PBDEs in a multi-media environmental sample Methods, combined with appropriate analytical instruments (such as GC) for detection, belong to the field of applied chemistry and analytical chemistry. Background technique [0002] Micro solid phase extraction technology is developed on the basis of traditional solid phase extraction technology combined with new solid phase micro extraction technology. Traditional solid-phase extraction and solid-phase microextraction techniques are mainly used for the direct extraction of organic matter in aqueous matrices, and it is difficult to pre-concentrate difficult-to-volatilize target pollutants from soil / sediment. The solid-phase microextraction technology is limited by the...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 周友亚张超艳李可及周惠艳颜增光白利平李发生
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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