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Ultrasensitive method for analyzing trace polybrominated diphenyl ethers in water

A technology of trihydroxybenzene and p-phenylenediamine, which is applied in analytical materials, chemical instruments and methods, material separation, etc., can solve problems such as poor chemical stability, hinder practical application, etc., and achieve low detection limit and good thermal stability. and chemical stability, the effect of excellent reproducibility

Active Publication Date: 2019-01-08
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, some nanoporous materials such as Metal Organic Frameworks (MOFs), which play a role in adsorption, usually show poor chemical stability due to the weak coordination bonds between the building units, which hinders its development to a certain extent. further practical application

Method used

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  • Ultrasensitive method for analyzing trace polybrominated diphenyl ethers in water
  • Ultrasensitive method for analyzing trace polybrominated diphenyl ethers in water
  • Ultrasensitive method for analyzing trace polybrominated diphenyl ethers in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Example 1 Preparation of TpPa-1, TpPa-1 coated fiber and solid phase microextraction device

[0078] (1) Synthesis of TpPa-1

[0079] In a 25mL hydrothermal reactor, add 2,4,6-trihydroxybenzene-1,3,5-tricarbaldehyde (Tp) (126mg, 0.60mmol), p-phenylenediamine (Pa-1) (96mg, 0.90mmol), 1.5mL of mesitylene, 1.5mL of 1,4-dioxane and 0.5mL of 3M aqueous acetic acid. Then, sonicate for 10 min to form a homogeneous mixture. Next, nitrogen gas was introduced thereinto for 30 minutes in order to remove oxygen in the reaction. Finally, the reaction kettle was heated in an oven at 120° C. for 3 days. The red reaction precipitate was centrifuged to obtain a red solid, which was washed with anhydrous acetone (5-6 times), and then the solid was dried in an oven at 80°C for 24 hours to obtain 80% (178 mg) of a dark red powder, which was TpPa-1, and was used Coated fibers were prepared below.

[0080] (2) Preparation of TpPa-1 coated fiber

[0081] Soak one end of the stainless ...

Embodiment 2

[0087] Example 2 Detection of five kinds of PBDEs in water by solid-phase microextraction-gas chromatography-mass spectrometry

[0088] 5 PBDEs: BDE-28, BDE-47, BDE-100, BDE-99 and BDE-154.

[0089] Detection method: The SPME device (comprising TpPa-1 coated fibers) prepared in Example 1 was inserted into a headspace vial containing 10 mL of sample solution. The TpPa-1 coating is completely immersed in the sample solution, and the temperature and speed are controlled by heating the magnetic stirrer, and the ionic strength is adjusted by adding NaCl. After the extraction is completed, the solid-phase microextraction device is placed in the gas sampling port for high-temperature desorption and sample injection. Among them, the solid-phase microextraction device needs to be aged under nitrogen protection at 280°C for 30 minutes before each extraction.

[0090] Condition parameters are: 0% (w / v) NaCl; extraction time: 40 min; extraction temperature: 70°C; desorption temperatur...

Embodiment 3

[0093] Example 3 Condition Optimization of Solid Phase Microextraction-Gas Chromatography Detection Method

[0094] According to the above detection method, the parameters in the extraction process and the desorption process are optimized to screen out better experimental conditions. The optimization process is as follows:

[0095] 1. Single factor method to optimize the conditions of solid phase microextraction

[0096] Based on the TaPa-1 coated fiber prepared in Example 1 and the solid-phase microextraction device assembled therefrom, the PBDEs (i.e. BDE-28, BDE-47, BDE-100, BDE-99) in the enrichment and detection water and BDE-154) SPME method for optimization. In order to obtain higher extraction efficiency, the present embodiment utilizes TaPa-1 coating fiber to extract the concentration in the water sample to be 50ng L -1 The PBDEs (the concentration of the five PBDEs are the same), the experimental parameters in the SPME extraction process and desorption process we...

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Abstract

The invention provides an ultrasensitive method for analyzing trace polybrominated diphenyl ethers in water. The method relates to a coated fiber and a solid-phase micro-extraction device containing the coated fiber as well as application of the coated fiber and the device, wherein the coated fiber comprises a fiber carrier and a coating material attached to the surface thereof, and the coating material is TpPa-1. By adopting the coated fiber, the high enrichment ratios, low detection limits, wide linear range, good repeatability and superior reproducibility are achieved.

Description

technical field [0001] The invention relates to water quality detection, in particular to a method for ultrasensitive analysis of trace polybrominated diphenyl ethers in water. Background technique [0002] Polybrominated diphenyl ethers (PBDEs), a brominated flame retardant, save more lives and reduce damage by slowing down the process of ignition and combustion, providing a longer escape time. Therefore, PBDEs have been widely used in a series of products, such as furniture decoration, textile products, electrical appliances, plastics and some building materials. Due to widespread use, the concentration of PBDEs in the environment has increased dramatically. At the same time, PBDEs are a kind of refractory, highly toxic, and highly fat-soluble in the environment, and can be enriched and amplified in the food chain, causing potential health hazards, such as neurotoxicity, endocrine disorders, reproductive toxicity, and cancer. Therefore, based on the above reasons, the de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/286B01J20/30C02F1/28G01N30/02G01N30/06C02F101/36
CPCB01J20/02B01J20/22B01J20/28023B01J20/286B01J2220/4806B01J2220/4812C02F1/281C02F1/285C02F2101/36G01N30/02G01N30/06G01N2030/009
Inventor 刘璐赵汝松孟维坤徐桂菊王丽娟
Owner SHANDONG ANALYSIS & TEST CENT
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