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Method for synchronously detecting plurality of organophosphorus fire retardants in bottom mud

A simultaneous detection and organophosphorus technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of poor detection effect of organophosphorus flame retardants, and achieve the effect of high degree of automation, good reproducibility, and sensitive quantitative detection.

Inactive Publication Date: 2014-09-17
NANJING UNIV
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Problems solved by technology

[0006] The purpose of the present invention is to provide a method for synchronous detection of multiple organophosphorus flame retardants in sediment, establish an effective ASE-GPC-SPE combined pretreatment technology, and optimize each extraction, purification and detection pretreatment conditions, by combining with GC-MS, it overcomes the problem of inability to simultaneously detect multiple organophosphorus flame retardants in sediment and the poor detection effect of various organophosphorus flame retardants in complex environments

Method used

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  • Method for synchronously detecting plurality of organophosphorus fire retardants in bottom mud
  • Method for synchronously detecting plurality of organophosphorus fire retardants in bottom mud
  • Method for synchronously detecting plurality of organophosphorus fire retardants in bottom mud

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Embodiment 1

[0036] This embodiment focuses on analyzing the optimization of the GC-MS method for the determination of organophosphorus flame retardants in standard solutions.

[0037] Step 1, preparation of standard samples: prepare a mixed standard solution with a gradient of 5-500ng / L. Specifically, take a certain amount of organophosphorus flame retardant mixed standard stock solution and internal standard recovery mixed stock solution with a pipette gun and place them in the sample injection vial, then add 240ng of internal standard PCB156-d3, and dilute with ethyl acetate to 1 mL to obtain a standard solution of the corresponding concentration.

[0038]Step 2: Perform GC-MS detection on the above-mentioned mixed standard solution of each concentration, set the chromatographic conditions as follows: flow rate 1mL / min; inlet temperature 250°C, sample volume 1μL, pulse splitless injection; chromatographic column initial temperature 50 ℃, after keeping for 1min, the temperature was prog...

Embodiment 2

[0045] EXAMPLE 2 OPFRs spiked recovery experiment in sediment samples

[0046] Step 1: Take 6 parts of 5g freeze-dried and sieved sediment samples, add 100ng of OPFRs mixed standard stock solution to 5 parts, and add 100ng of four recovery indicator internal standard mixed stock solutions. In the other part, only the recovery indicator internal standard mixed stock solution was added, as a control blank.

[0047] Step 2: Put 6 samples into the ASE extraction cell, use ethyl acetate as the extraction solvent, heat for 5 minutes at 1500 psi pressure, 90°C extraction temperature, and statically extract for 5 minutes, cycle twice, use 60% of the volume of the extraction cell % solvent to flush the extraction cell, and finally purged with nitrogen for 110s. After the extraction, the extract (about 60 mL) was collected and evaporated to 1 mL by rotary evaporation, then a mixed solvent of ethyl acetate:cyclohexane (1:1, v / v) was added, and the volume was adjusted to a 10 mL GPC vial...

Embodiment 3

[0052] Example 3 Sampling Analysis and Detection of Organophosphorus Flame Retardant in Taihu Lake Bottom Mud

[0053] Step 1: Sample collection and processing. When sampling, use a grab-type mud extractor to collect surface sediment and immediately freeze it for storage. After being transported back to the laboratory, it was frozen in a -20°C refrigerator, freeze-dried with a freeze dryer, ground with a mortar, passed through a 100-mesh metal sieve, and stored at -20°C for analysis.

[0054] Step 2: Take 5g of sediment samples at each point, and perform pretreatment on the samples according to the sample pretreatment method in Step 2 to Step 4 in Example 2.

[0055] Step 3: The processed sample solution is subjected to qualitative and quantitative detection by GC-MS according to Step 5 in Example 2. The concentrations of OPFRs at the five sites measured are shown in Table 3.

[0056] Concentration of OPFRs in Taihu Lake sediments sampled at 35 points

[0057]

[0058] N...

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Abstract

The invention discloses a method for synchronously detecting a plurality of organophosphorus fire retardants in bottom mud, belonging to the detection field of trace amount of organophosphorus fire retardants in the environment. The method comprises the main steps of firstly, extracting a target object in a sample through an accelerated solvent extraction instrument; purifying by a gel permeation chromatography; further purifying and enriching by adopting a solid-phase small extraction column; and finally, concentrating and making up to the constant volume and detecting and quantifying by using a gas chromatograph-mass spectrometer. According to the invention, a pre-treatment method for the organophosphorus fire retardants in the bottom mud is established and optimized, the automation degree is high and the repeatability is good; the gas chromatograph-mass spectrometer is used for carrying out quantitative detection, the detection limit is low and the sensitivity is high; the detection limit to nine types of the organophosphorus fire retardants are lower than 0.340 microgram per gram. According to the method, the synchronous analysis and detection on the plurality of trace amount of organophosphorus fire retardants in a complicated environment medium, namely the bottom mud, is realized; the sensitivity and the accuracy are achieved, and the method makes up the disadvantages of the technology in the field.

Description

technical field [0001] The invention relates to a method for detecting trace organic phosphorus flame retardants in the environment, more specifically, relates to a method for synchronous detection of multiple organic phosphorus flame retardants in bottom mud. Background technique [0002] Organic Phosphate Flame Retardants (OPFRs) have long-lasting flame retardant effects, good compatibility with polymer substrates, water resistance, heat resistance and migration resistance, and are widely used in electronics, textiles, chemicals, building materials and other industries middle. The widespread use of organophosphorus flame retardants will also have certain impacts on humans and the ecological environment. Some organophosphorus flame retardants are very stable and bioaccumulative, and long-term contact with them will have adverse effects on the human body, such as immune system function degradation, reproductive system disorders, thyroid insufficiency, and even some organoph...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/08
Inventor 何欢严小菊庄园孙成杨绍贵
Owner NANJING UNIV
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