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GC-MS method for measuring volatile characteristic organic matters in water based on multifunctional on-line sample introduction

A volatile organic compound, GC-MS technology, applied in the field of gas chromatography tandem mass spectrometry, can solve the problems of single application performance of pretreatment instruments, long pretreatment cycle, complex water quality matrix, etc. Influence of recovery rate, effect of small sample usage

Inactive Publication Date: 2019-08-23
SHANDONG WATER & WASTEWATER MONITORING CENT
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the deficiencies of long pretreatment cycle, serious organic reagent pollution, complex water quality matrix and single application performance of pretreatment instruments in the above water sample pretreatment and measurement process, and provides a multi-functional online sampling method for the determination of volatile organic compounds in water. Gas Chromatography Tandem Mass Spectrometry Method

Method used

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  • GC-MS method for measuring volatile characteristic organic matters in water based on multifunctional on-line sample introduction
  • GC-MS method for measuring volatile characteristic organic matters in water based on multifunctional on-line sample introduction
  • GC-MS method for measuring volatile characteristic organic matters in water based on multifunctional on-line sample introduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1: the mensuration of strong volatile organic compound benzene series

[0053] Detection of 9 benzene series of strong volatile organic compounds (benzene, toluene, ethylbenzene, p-xylene, m-xylene, o-xylene, cumene, chlorobenzene and styrene) under different water conditions by headspace method and dynamic head The recovery rate of the analyte by air method.

[0054] Headspace method: adopt the method of the present invention to measure the recovery rate of the above 9 kinds of benzene series: add 4.0 μg L to surface reservoir water and pipe network water -1 9 kinds of mixed water samples of benzene series. Accurately measure 10mL water sample, and use the headspace method for determination. After the sample vial was heated at 60°C for 30 minutes to reach gas-liquid equilibrium, 1 mL of the upper layer gas was extracted by the headspace method for gas chromatography-tandem mass spectrometry to detect the recovery rate of the analyte.

[0055] Dynamic head...

Embodiment 2

[0077] Embodiment 2: the mensuration of olfactory substance

[0078] Detect the recoveries of semi-volatile organic compounds geosmin and dimethylisoborneol under different water conditions by solid phase microextraction and magnetic stirring adsorption method:

[0079] This specific embodiment adopts the following steps:

[0080] (1) Solid-phase microextraction method: Accurately measure 10mL of water sample, select 65 / 10μm PDMS / DVB mixed-coated microfiber head, extract the water sample with the micro-extraction fiber head under the conditions of 60°C and 250rpm for 30min, the air quality of the fiber head after extraction After 180s analysis of the injection port, the sample was injected for determination.

[0081] (2) Magnetic stirring adsorption extraction method: Accurately measure 10 mL of water sample, place a magnetic stirring bar with a length of 10 mm and a PDMS coating thickness of 1 mm at the bottom of the sample bottle, and stir and adsorb at 1000 r / min for 1 h. ...

Embodiment 3

[0099] Embodiment 3: the mensuration of 666

[0100] Detection of weak volatile organic compounds four kinds of HCH (α-CHH, β-CHH, γ-CHH, δ-HCH) under different water conditions by solid-phase microextraction and magnetic stirring adsorption method The recovery rate of the measured substance:

[0101] This specific embodiment adopts the following steps:

[0102] (1) Solid-phase microextraction method: Accurately measure 10 mL of water sample, select a micro-extraction fiber head with 50 / 30 μm DVB / CAR / PDMS mixed coating, extract the water sample with the micro-extraction fiber head at 60°C and 250 rpm for 40 min, extract After analyzing for 180s at the gas injection port of the rear fiber head, the samples were injected for measurement.

[0103] (2) Magnetic stirring adsorption extraction method: Accurately measure 10 mL of water sample, place a magnetic stirring bar with a length of 10 mm and a PDMS coating thickness of 1 mm at the bottom of the sample bottle, and stir and a...

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Abstract

The invention discloses a GC-MS method for measuring volatile characteristic organic matters in water based on multifunctional on-line sample introduction. According to the method, two kinds of onlinepretreatment methods of headspace and dynamic headspace of benzene series (benzene, methylbenzene, ethylbenzene, p-xylene, m-xylene, o-xylene, isopropyl benzene, chlorobenzene and styrene) are established; two kinds of online pretreatment methods of a solid-phase micro-extraction method and a magnetic stirring adsorption extraction method of two kinds of odor substances (geosmin and dimethyl isocamphitol), and four kinds of a formula which is as shown in the specification are established; and then online sample introduction GC-MS detection is carried out. The detection result shows that the detection limit, the recovery rate, the precision and the like of the on-line method for detecting the volatile organic matters in the three categories can meet the measurement requirements; the onlinedetermination efficiency is improved by one half to two thirds, and the method is simple, convenient, environment-friendly and efficient. According to the method, the sample detection sensitivity iseffectively improved by adding the aid and a secondary adsorption mode, and meanwhile, the traditional thermal desorption sample introduction mode is changed, and the accuracy and operability of sample detection are both optimized.

Description

technical field [0001] The invention relates to a pretreatment and determination method for organic substances in water, in particular to a gas chromatography tandem mass spectrometry method for measuring organic substances with different volatile characteristics in water by using multifunctional online sampling. Background technique [0002] There are many kinds of organic pollutants in water bodies, which are highly harmful and toxic, and most of them are trace substances. Therefore, higher requirements are put forward for the enrichment and detection technology of water samples. Organic matter in water can be roughly divided into two categories: one is natural organic matter (NOM), including humus, microbial secretions, dissolved plant tissue and animal waste; the other is synthetic organic matter (SOC), Includes pesticides, synthetics for commercial use, and some industrial waste. Among them, the three major categories of organic compounds with different volatile charac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 贾瑞宝孙韶华顿咪娜宋艳王明泉赵清华
Owner SHANDONG WATER & WASTEWATER MONITORING CENT
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