Solid-phase extraction-gas chromatography and mass spectrometry combined separation and detection method for discharge of organic acid by biomass combustion in snow ice sample

Abstract

A solid-phase extraction-gas chromatography and mass spectrometry combined separation and detection method for discharge of organic acid by biomass combustion in a snow ice sample comprises the following steps: preparing a sample: filtering the sample with a quartz filter membrane; performing SPE preparation: fixing an HLB small column on a special SPE device; activating the HLB small column; adjusting the PH value: taking 50 mL of filtered sample, adding hydrochloric acid (PH is about 2) and shaking uniformly; loading the sample: adding the sample which is shaken uniformly into the HLB column; leaching and blow-drying; eluting and collecting eluent; concentrating; determining the volume and putting on a machine: after deriving and cooling to room temperature, adding normal hexane, determining the volume to be 200 mL and preparing to put on a gas chromatograph-mass spectrometer (GC / MS) to perform test. The detection method provided by the invention has the characteristics of small use amount of the samples, high field operability, simplicity in operation and the like; furthermore, the detection method has low detection limit, high recovery rate and high precision.

Description

technical field [0001] The invention relates to a method for detecting chemical components of snow and ice, in particular to a solid phase extraction-gas chromatography mass spectrometry separation and detection method for organic acids emitted from biomass combustion in snow and ice samples. Background technique [0002] p-Hydroxybenzoic acid, vanillic acid, and dehydroabietic acid in snow and ice are unique indicators of biomass combustion emissions, which can be used to distinguish whether carbonaceous components come from biomass combustion or fossil fuel combustion. However, snow and ice samples There are still very few studies on medium organic acids as indicators of combustion emissions, the main reason being the limitations of sample pretreatment methods and instruments. [0003] At present, there are mainly two methods for the separation and analysis of organic acids in snow and ice that can be used as combustion emission indicators: one is to collect a large number...

AI Technical Summary

Problems solved by technology

This method has a low detection limit, but the operation is relatively complicated, it cannot be operated in the field, a large amount of sample is required, and a large amount of organic reagents are consumed in the extraction process

The other is to use HPLC-ESI-MS / MS to measure organic acids directly. This method has the characteristics of less sample consumption and rapid detection, but the detection limit is relatively high, which cannot meet the requirements of trace organic acids in some snow and ice samples. acid concentration test requirements, and this method has high requirements for instruments, which cannot be realized in most laboratories

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