Deactivated aluminum oxide and preparation method thereof and method for qualitative/quantitative analysis of short-chain chlorinated paraffins (SCCPs)
A technology of short-chain chlorinated paraffins and aluminum oxide, which is applied in the fields of alumina/aluminum hydroxide, chemical instruments and methods, and analytical materials, and can solve the problems of lack of characteristics, low-chlorinated monomer response discrimination, complexity, etc. question
Active Publication Date: 2019-10-25
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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Problems solved by technology
[0005] Due to the limitation of the ionization principle of the ion source, ECNI-MS has no response to low-chlorinated CPs monomers with less than 5 chlorine atoms. As the most commonly used ionization method, electron impact (EI) ion source does not have low-chlorinated CPs. The problem of monomer response discrimination, but because the EI bombardment energy is too high, SCCPs undergo a variety of fragmentation reactions during the ionization process, resulting in a large number of ion fragments, which is very complex, and the m / z is small, lacks characteristics, and is difficult to distinguish, so Usually not used for detection of SCCPs
At present, using the commonly used electron bombardment ion source low-resolution mass spectrometry (EI-HLMS), the qualitative and quantitative selection of universal ions for SCCPs has not been reported.
Method used
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Embodiment 1
[0108] 1. Preparation of deactivated aluminum oxide and determination of degradation efficiency:
[0109] Select the chromatographic column with basic alumina, (100-200 mesh, purchased from Shanghai Wusi Chemical Reagent Factory), wash with methanol and dichloromethane of 3 times the volume of pesticide residue grade successively, after the organic solvent has evaporated, Activated at 660°C for 6h. Weigh 100g of activated basic alumina and add deionized water successively to make the water content 0.1wt%, shake for half an hour, and after standing for 2h to balance, weigh 30g and fill it into a chromatographic glass column (inner diameter 1cm, long 30cm), add 1000ng of chlorine-containing 63% C10-C13SCCPs (the source is the purchased commercial standard sample) at the head of the column, add 100mL of pesticide residue grade dichloromethane into the constant pressure funnel, elute with 15 drops / min, and the eluent receives In a 150mL chicken heart bottle, concentrate to 2-3mL ...
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The invention discloses deactivated aluminum oxide capable of degrading short-chain chlorinated paraffins (SCCPs), a method for qualitative / quantitative analysis of the short-chain chlorinated paraffins by an ionization source low resolution mass spectrum. The water content of the deactivated aluminum oxide is 0.02wt %-1wt %. The deactivated aluminum oxide can be used for degradation of the SCCPs,and the ionization source low resolution mass spectrum can be used for the qualitative / quantitative analysis of trace short-chain chlorinated paraffins.
Description
technical field [0001] The application relates to an inactivated aluminum oxide and a preparation method thereof, and a method for qualitatively / quantitatively analyzing short-chain chlorinated paraffins, belonging to the field of environmental sample processing. Background technique [0002] Short-chain chlorinated paraffins (SCCPs) are industrial products of straight-chain chlorinated alkanes with a chain length of 10-13 carbon atoms, and there are tens of thousands of similar substances. Similar to persistent organic pollutants (POPs), they are chemically stable, have long-distance migration and bioaccumulation capabilities, and are detected in the atmosphere, water, sediment and biological communities, and even human food and tissues. SCCPs have obvious acute toxicity to aquatic organisms and potential carcinogenicity, which has attracted widespread attention from the international community. The POPs Review Committee of the Stockholm Convention intends to list SCCPs as ...
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IPC IPC(8): C01F7/02G01N30/02G01N30/06G01N30/72
CPCC01F7/021C01P2002/80C01P2002/89G01N30/02G01N30/06G01N30/72
Inventor 赵兴茹董靖刘承友万文胜暴志蕾乔肖翠
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI