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Method for rapidly concentrating 16 polycyclic aromatic hydrocarbons in water

A polycyclic aromatic hydrocarbon and water quality technology, applied in the field of environmental monitoring and analytical chemistry, can solve the problems of target loss, difficult practical application, complicated operation process, etc., and achieve the effect of simple operation

Inactive Publication Date: 2016-11-23
BAOWU CHARCOAL MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are two shortcomings in this concentration method. ①The rotary evaporation method does not use vacuum, and the rotary evaporation speed is very slow. It is difficult to be practically applied in daily monitoring and analysis. Generally, the rotary vacuum method with vacuum is used.
②Because the rotary evaporator cannot control the specific concentration amount, it needs to be concentrated to a certain amount and then transferred to the nitrogen blowing device to concentrate to the specified scale. There may be a bumping phenomenon in vacuum, and the sample needs to be redone. Therefore, in practical applications, the concentration and replacement methods of direct nitrogen blowing should still be considered.

Method used

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  • Method for rapidly concentrating 16 polycyclic aromatic hydrocarbons in water
  • Method for rapidly concentrating 16 polycyclic aromatic hydrocarbons in water
  • Method for rapidly concentrating 16 polycyclic aromatic hydrocarbons in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Concentration conditions: use the concentration device Turbo Vap II type automatic nitrogen blowing concentrator (Sweden Biotage Company, formerly the U.S. Caliper Life Sciences company) to prepare 150ml of 4ug / l 16 kinds of PAHs mixed standard sample / dichloromethane solution at the temperature of the water bath Concentrate to about 1.0mL at 30°C and nitrogen pressure of 9-13psi, add 5mL of chromatographically pure acetonitrile, then use a nitrogen blower to concentrate to 1.0mL at a water bath temperature of 50°C, pass through a 0.45um filter membrane, and sample 10uL Perform liquid chromatography detection.

[0026] Liquid chromatography detection conditions:

[0027] Agilent 1200 HPLC system: (USA) G1315D-DAD detector, G1321A-FLD fluorescence detector, Quaternary quaternary pump, G1316A-Colcom column oven, G1322A-Degasser vacuum degasser.

[0028] Liquid chromatography column: ZORBAX Eclipse PAH 4.6*250mm*5um

[0029] Injection volume: 10uL (automatic injection); C...

Embodiment 2

[0045] Concentration conditions: Use YH-RE rotary evaporator (Shanghai Yuhua Instrument Co., Ltd.) to concentrate the prepared 4ug / l 16 kinds of PAHs mixed standard sample / dichloromethane solution under the conditions of water bath temperature 30°C and vacuum degree 0.03MPa To 1-2ml, add 5mL of chromatographically pure acetonitrile, transfer to a common nitrogen blower, concentrate to 1.0mL at a water bath temperature of 50°C, pass through a 0.45um filter membrane, and sample 10uL for liquid chromatography detection.

[0046] The detection conditions of liquid chromatography are the same as in Example 1.

[0047] The concentrated recovery results are shown in Table 4, and the spectrograms are shown in figure 2 .

[0048] Table 4 4ppm mixed standard sample / dichloromethane solution rotary evaporation concentration data

[0049]

[0050]

Embodiment 3

[0052] Extraction conditions: add 2ug 16 polycyclic aromatic hydrocarbon mixed standard samples to 1L blank water sample, put it into a 2000mL separatory funnel, add an appropriate amount of decafluorobiphenyl liquid as a recovery indicator, in order to improve extraction efficiency and reduce emulsification phenomenon, shorten the separation time of the two phases, and add an appropriate amount of 30g NaCl to the water phase. Add about 50mL of dichloromethane, shake gently and release the gas, repeat this action several times, after fully deflated, vibrate vigorously for about 10min in an airtight condition, and collect the dichloromethane solution in the lower layer in 250mL in a triangular beaker. Repeat the extraction twice, combine the organic phases, and add anhydrous sodium sulfate until flowing anhydrous sodium sulfate exists.

[0053] The concentration and replacement conditions of the dichloromethane extract, and the liquid chromatography detection conditions are th...

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Abstract

The invention discloses a method for rapidly concentrating 16 polycyclic aromatic hydrocarbons in water. The method comprises the specific steps that after a water sample is subjected to liquid-liquid extraction, a Turbo Vap series full-automatic nitrogen blowing concentration instrument is adopted to concentrate methylene dichloride under the conditions of the temperature of 30-45 DEG C and nitrogen pressure of 4-13 psi and replace an acetonitrile solvent at the temperature of 50 DEG C, liquid chromatography detection is performed, the adding standard recovery can be 65.2-99.1%, and the quality control requirement for the recovery rate 60-120% of in-blank standard-addition components proposed by the HJ478-2009 standard of 'liquid-liquid extraction and solid-phase extraction high efficiency liquid chromatography for determining polycyclic aromatic hydrocarbons in water' is met. The nitrogen blowing concentration instrument is adopted to perform concentration and replace the acetonitrile solvent and is quicker, simpler and more convenient to operate than a rotary evaporation and nitrogen blowing mode, and a recovery effect is good. The method can be used for rapid concentration and accurate quantification of 16 polycyclic aromatic hydrocarbons in water.

Description

technical field [0001] The invention relates to the fields of analytical chemistry and environmental monitoring, and specifically discloses a method for rapidly concentrating and accurately quantifying 16 kinds of polycyclic aromatic hydrocarbons in water. Background technique [0002] Polycyclic aromatic hydrocarbons (referred to as PAHs or PNA) are a very important class of three chemical substances (carcinogenic, teratogenic, mutagenic), because of their biodegradability and accumulation, they are widely present in water, air, soil, organisms and other environments. Environmental pollution caused by polycyclic aromatic hydrocarbons has attracted more and more attention, and it has become a priority monitoring substance in many countries in the world. In 1976, EPA listed 16 PAHs as priority pollutants, namely: naphthalene, dihydroacenaphthene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene, chrysene, benzo, Fluoranthene, benzo[...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02
Inventor 施中
Owner BAOWU CHARCOAL MATERIAL TECH CO LTD
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