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Fe3S4-magnetic effervescent tablets and method for detecting polybrominated biphenyl ether

An effervescent tablet, fe3s4 technology, applied in chemical instruments and methods, measuring devices, other chemical processes, etc., can solve the problems of high cost, unenvironmental protection, long time consumption, etc., and achieve the effect of improving the recovery rate

Active Publication Date: 2019-04-16
WENZHOU MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The first object of the present invention is to provide a method for detecting PBDEs, which aims to solve the problems of long time consumption, high cost and environmental protection in the existing sample pretreatment methods

Method used

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  • Fe3S4-magnetic effervescent tablets and method for detecting polybrominated biphenyl ether
  • Fe3S4-magnetic effervescent tablets and method for detecting polybrominated biphenyl ether
  • Fe3S4-magnetic effervescent tablets and method for detecting polybrominated biphenyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: based on Fe 3 S 4 Magnetic Effervescent Tablet-Assisted Ionic Liquid Based Dispersion Liquid-Liquid Microextraction Technology

[0038] Step 1: Magnetic Nanoparticle Fe 3 S 4 preparation of

[0039] with FeCl 3 ·6H 2 O and thiourea as raw materials, dissolved in ethylene glycol, 20-40min intense magnetic stirring to dissolve completely and mix evenly, then transfer the mixture to a polytetrachlorethylene liner, and then put the liner into a stainless steel high temperature Put it in a high-pressure reaction kettle, put it into a constant temperature oven to heat, set the temperature at 180°C, and react for 12 hours; After washing three times, it was separated by magnet, and the obtained solid was dried in a vacuum oven at 60°C for 12 hours. After the sample is cooled to room temperature in a vacuum drying oven, it is collected, ground and weighed, and the final sample is marked as Fe 3 S 4 Magnetic nanoparticles, such as figure 1 As shown in A. ...

Embodiment 2

[0044] Example 2: Synthetic Fe 3 S 4 and commercial Fe 3 o 4 Comparison of Extraction Efficiencies

[0045] Synthetic Fe 3 S 4 and commercial Fe 3 o 4 The extraction efficiency of the six PBDEs homologues was measured by extraction recovery. Weighed 10 mg of the two kinds of magnetic nanoparticles respectively, and both formed similar uniformly dispersed solutions by the established method. Such as figure 2 As shown, commercial Fe 3 o 4 The extraction recoveries of PBDEs are low (almost all lower than 60%). with Fe 3 o 4 Compared to the synthesized Fe 3 S 4 The extraction ability of PBDEs is higher (ERs are greater than 80%). Above-mentioned phenomenon can be described with following part (the characterization that magnetic nano material is carried out, as XRD, SEM, magnetic hysteresis analysis, FT-IR, Zeta potential and N 2 Adsorption-desorption isotherms, etc.) to explain the characteristics. Based on the above results, this paper chooses Fe 3 S 4 Optima...

Embodiment 3

[0046] Example 3: Fe 3 S 4 repeatability

[0047] Prepared Fe 3 S 4 The reproducibility of magnetic nanoparticles is of great significance in practical applications. Fe used for the investigation 3 S 4 The recovery ability, wash with acetonitrile and ultrapure water 3 times respectively, after washing, no analyte to be detected can be detected, and the Fe can be reused 3 S 4 Proceed to the next extraction cycle. Such as image 3 As shown, Fe 3 S 4The loss of extraction recovery of magnetic nanoparticles was less than 15% after repeated at least 6 times, demonstrating that the as-prepared Fe 3 S 4 Magnetic nanoparticles are very reproducible.

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Abstract

The invention discloses a method for detecting polybrominated biphenyl ether by using a Fe3S4-magnetic effervescent tablet assisted ionic liquid-based dispersion liquid liquid microextraction combinedtechnology. The Fe3S4 is synthesized by using FeCl3 6H2O and thiourea as raw materials and adopting a solvothermal method for extracting the polybrominated biphenyl ether, and the extraction efficiency of the Fe3S4 is improved by about 21-32% compared with that of a prior commercial magnetic nano material (such as Fe3O4); the effervescent precursors of the effervescent tablets are environmental-friendly and non-toxic inorganic acid salts and basic salts, and replace toxic dispersed organic solvents in the prior dispersion liquid micro-extraction; according to the combined technology, novel environmental-friendly extractant ionic liquid [C4MIM] [PF6] is adopted to replace the prior toxic chlorine-containing solvent, and the whole combined technology embodies the environment-friendly concept. Under the optimum conditions, the technology is used in liquid matrix samples, the recovery of polybrominated diphenyl ether can reach 77.3-106.7%, and the minimum detection limit is as low as 0.012-0.078 Mug / L. The method also has high precision (1.32-4.83%).

Description

technical field [0001] The invention belongs to the technical field of persistent organic pollutants (POPs) detection, and relates to a Fe 3 S 4 - Magnetic effervescent tablets and methods for their use in the detection of polybrominated diphenyl ethers. Background technique [0002] Polybrominated diphenyl ethers (PBDEs) have been used as flame retardants in furniture, textiles, plastics, paints and electrical appliances for many years due to their high performance and high cost performance. As an additive flame retardant, PBDEs can easily dissipate into the environment during the production process or product use. Due to the persistence, bioaccumulation, high toxicity and long-distance migration ability of PBDEs, based on these characteristics, PBDEs have been considered as persistent organic pollutants (POPs) in the past few decades. Pollutants are everywhere. In the past decade, the detection rate of PBDEs in the global environment, human beings and other organisms h...

Claims

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Application Information

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IPC IPC(8): B01J20/28B01J20/06B01J20/30G01N30/06
CPCB01J20/06B01J20/28007B01J20/28009G01N30/06G01N2030/062Y02C20/40
Inventor 李艳艳王学东刘伟董国忠王慧利周佩佩高明
Owner WENZHOU MEDICAL UNIV
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