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Analysis method of monomer stable carbon isotopes of polybrominated diphenyl ethers (PBDEs) in sediments

A technology for stabilizing carbon isotopes and polybrominated diphenyl ethers, applied in the field of isotope analysis, can solve problems such as complex sample matrix and multiple co-overflow impurities

Inactive Publication Date: 2016-11-16
SOUTH CHINA INST OF ENVIRONMENTAL SCI MEP
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Problems solved by technology

Therefore, in order to obtain a sufficiently high PBDE content, the experiment requires a larger sample volume, which will undoubtedly make the sample matrix very complicated, and more co-overflow impurities need to be dealt with

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  • Analysis method of monomer stable carbon isotopes of polybrominated diphenyl ethers (PBDEs) in sediments

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Embodiment Construction

[0020] The following will be combined with figure 1 The technical solution of the present invention is described in detail.

[0021] This example provides the monomeric stable carbon isotope analysis method of polybrominated diphenyl ethers in the sediment of the present invention. This method requires the following experimental reagents and materials.

[0022] Experimental reagents mainly include: PBDEs industrial product TBDE-71X, PBDEs standard products: BDEs 28, BDEs47, BDEs85, BDEs 99, BDEs 100, BDEs 153, BDEs 154; , distilled water, acetone, dichloromethane, n-hexane, concentrated sulfuric acid , Neutral silica gel, anhydrous sodium sulfate, Florisil. All solvents were of analytical grade (AR) and double-distilled in an all-glass system before use.

[0023] Alumina: 100-200 mesh, manufactured by China Wuhan Chemical Reagent Company. It was extracted with DCM for 72 hours, and the extract solution was changed once during the period. After drying in a fume hood, activ...

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Abstract

The invention relates to an analysis method of monomer stable carbon isotopes of polybrominated diphenyl ethers (PBDEs) in sediments. The analysis method is characterized by comprising the following steps: step one, firstly freezing and drying a sediment sample, grinding the sediment sample and screening the sediment sample via a 200-mesh sieve; step two, placing the sediment sample in a Sohxlet extraction paper tube, and extracting for 48 hours at 60 DEG C via normal hexane / acetone to obtain an extraction solution; step three, purifying the extraction solution via acidic and neutral composite silica gel columns for a first time; step four, purifying the sample via an aluminum oxide composite silica gel column for a second time; step five, purifying the sample via a florisil column for a third time by pre-leaching via 10mL of normal hexane after feeding the sample to remove part of organic matter impurities, and eluting via 20mL of normal hexane to obtain an elution solution containing a target compound; step six, completing quantitative analysis of PBDEs; and step seven, completing analysis of monomer stable carbon isotopes of PBDEs. The analysis method is capable of effectively removing sulfur element impurities and some organic matter impurities in the sediment samples with high sample weight, and obtaining samples with clean matrixes; the method is suitable for analysis and detection of environmental pollutants.

Description

technical field [0001] The invention relates to an isotope analysis method, in particular to a monomer stable carbon isotope analysis method of polybrominated diphenyl ethers in sediments. Background technique [0002] Monomer Isotope Analysis (CSIA) is also known as Gas Chromatography-Isotope Ratio Mass Spectrometry (GC-IRMS). Organic compounds usually have their own stable characteristic isotopic composition when they enter the environment. Under a specific environment, if the isotopic composition of the compound remains unchanged, its isotopic composition can be directly used for source tracing. Due to the influence of certain biological processes in the environment, such as microbial degradation and biological enzyme metabolism, the isotopic composition of some compounds will change regularly. In 1976, Sano proposed for the first time to add a combustion furnace between gas chromatography and mass spectrometry to realize the on-line analysis of the isotopic composition ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N2030/025G01N2030/062
Inventor 郑晶曾艳红郑晓波罗孝俊胡国成王美欢任明忠麦碧娴
Owner SOUTH CHINA INST OF ENVIRONMENTAL SCI MEP
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