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Analysis method of hexabromocyclododecane in atmosphere

A technology of hexabromocyclododecane and analysis method, applied in the field of analysis of hexabromocyclododecane in the atmosphere

Inactive Publication Date: 2017-08-18
DALIAN JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention solves the above-mentioned problems by optimizing the existing methods of extraction, purification and liquid chromatography-mass spectrometry analysis of hexabromocyclododecane in the atmosphere

Method used

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  • Analysis method of hexabromocyclododecane in atmosphere
  • Analysis method of hexabromocyclododecane in atmosphere
  • Analysis method of hexabromocyclododecane in atmosphere

Examples

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preparation example Construction

[0033] The preparation method of following composite chromatographic column and the method utilizing composite chromatographic column to purify sample are:

[0034] Add 2g of anhydrous sodium sulfate Ⅰ, 1g of neutral silica gel Ⅰ, 3g of basic Silica gel, 1g neutral silica gel II, 5g acidified silica gel, 1g neutral silica gel III, 7g anhydrous sodium sulfate II to obtain a composite chromatography column, use 20mL n-hexane to activate the composite chromatography column; add the sample to the composite chromatography column , followed by 50mL n-hexane, 100mL n-hexane / dichloromethane (V / V, 9:1) for pre-washing, discarding the eluent; then 180mL n-hexane / dichloromethane (V / V, 4 : 1) Carry out elution, collect the eluate of n-hexane / dichloromethane (V / V, 4:1), and concentrate the eluate to 1-2mL by rotary evaporation. Stream dry.

Embodiment 1

[0036] A kind of analysis method of hexabromocyclododecane in atmosphere, described analysis method comprises the steps:

[0037] Standard curve creation

[0038] Contain 20μL, 1μg / mL quantitative internal standard D respectively 18-Acetonitrile solutions of α-HBCD, β-HBCD, and γ-HBCD at 100, 50, 20, 10, 5, and 1 ng / mL of γ-HBCD were analyzed using the above-mentioned LC-MS analysis conditions, and a standard curve was drawn. see attached results Figure 1-3 ,table 3.

[0039] Table 3 standard curve results

[0040] compound Standard Curve Equation R 2

α-HBCD Y=0.03553C 0.9976 β-HBCD Y=0.05614C 0.9995 γ-HBCD Y=0.03827C 0.9989

[0041] *Y: peak area ratio; C: compound concentration, ng / mL

[0042] Analytical Method Recovery Determination

[0043] Preparation of Mixed Standards

[0044] Add 20 μL of 1 μg / mL D 18 -Add the acetonitrile solution of β-HBCD to 20 μL, 1 μg / mL of the acetonitrile solution of α-HBCD, β-HBCD, γ-HBCD, an...

Embodiment 2

[0052] A passive air sampler equipped with a glass fiber filter (GFF) and a polyurethane foam disc (PEG-PUF) immobilized with PEG20M was sampled outdoors on the 5th floor of a certain research institute for 4 consecutive months to collect HBCDs in the atmospheric particle phase. Add 40 μL of GFF and PEG-PUF to collect HBCDs in the atmospheric gas phase, respectively, and 1 μg / L extraction internal standard D 18 -β-HBCD, and then use 250mL n-hexane to perform Soxhlet extraction for 20h, and concentrate the extract to 1-2mL by rotary evaporation, add the concentrated extract to the above-mentioned composite chromatography column, and use the above-mentioned composite chromatography The method of column purification sample, to obtain the purified sample, add 20 μL, 1 μg / L quantitative internal standard D to the purified sample 18 - The acetonitrile solution of γ-HBCD was adjusted to 200 μL with acetonitrile, vortexed, oscillated and mixed, and the above solution was analyzed usin...

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Abstract

The invention relates to an analysis method of hexabromocyclododecane in atmosphere, and belongs to the technical field of the environment atmosphere and waste gas monitoring. The analysis method comprises the purification step of purifying by use of a composite chromatographic column, wherein the fillers of the composite chromatographic column are orderly as follows from bottom to top: anhydrous sodium sulfate I, neutral silica gel I, alkali silica gel, neutral silica gel II, acidified silica gel, neutral silica gel III, and anhydrous sodium sulfate II; the eluant is orderly as follows: n-hexane, n-hexane / dichloromethane (V / V=9: 1), n-hexane / dichloromethane (V / V=4: 1); partial eluant of the n-hexane / dichloromethane (V / V=4: 1) is collected to remove the solvent. The analysis method disclosed by the invention is simple and convenient for operation, fast in analysis, wide in linear range, good in reproducibility, accurate in result, and good in recovery rate.

Description

technical field [0001] The invention relates to an analysis method for hexabromocyclododecane in the atmosphere, and belongs to the technical field of ambient atmosphere and waste gas monitoring. Background technique [0002] In May 2013, hexabromocyclododecane (HBCDs) was added to Annex A of the Stockholm Convention on Persistent Organic Pollutants. As a brominated flame retardant, HBCDs are mainly used in materials such as expanded polystyrene (EPS), extruded polystyrene (XPS), textiles and high-impact polystyrene (HIPS). It is also used in transportation, interior decoration and household appliances, and has become the third largest brominated flame retardant in the world after polybrominated diphenyl ethers (PBDEs) and tetrabromobisphenol A (TBBPA). The molecular formula of HBCDs is C 12 h 18 Br 6 , with a molecular weight of 642. HBCDs have a complex three-dimensional structure. HBCDs molecules have six chiral centers, and theoretically 16 different isomers can be ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 朱秀华王龙星李岩陈吉平高媛金静王炜董学伟
Owner DALIAN JIAOTONG UNIVERSITY
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