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Method for rapidly determining content of phenol in wastewater through purge and trap-gas chromatography-mass spectrometry

A purge-and-trap and gas-mass spectrometry technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of complex pretreatment process, cumbersome steps, and large consumption of organic solvents, so as to avoid sample purity and anhydrous state , improve detection efficiency, and simplify the experimental process

Pending Publication Date: 2022-03-22
SHANGHAI INST OF TECH +1
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0005] Ruan Guohong and others disclose a method for detecting phenol with high performance liquid chromatography (HPLC) in "Research on the High Performance Liquid Chromatography Analysis Method of Phenol, Hydroquinone and Glycinol in Water". Low, but due to the use of ultraviolet detectors (UV), its sensitivity is limited (mg / L level), and the separation performance is poor
There are also studies on the determination of phenol content in environmental water by gas chromatography. However, when detecting phenol in wastewater, pretreatments such as derivatization, liquid-liquid extraction, or solid-phase extraction are required for the water sample. The pretreatment process is complicated and the steps are cumbersome. The extraction process will consume a large amount of organic solvent, causing further organic pollution

Method used

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  • Method for rapidly determining content of phenol in wastewater through purge and trap-gas chromatography-mass spectrometry
  • Method for rapidly determining content of phenol in wastewater through purge and trap-gas chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The specific determination steps of the phenol content in the wastewater discharged from the production of a chemical plant are as follows:

[0041] 1. Collect water samples in a brown glass bottle, add 0.08mol / L phosphoric acid after collection, adjust the pH to 5, take 10mL water sample into the sample bottle, add a magnetic stirrer and seal the cap. Place the vial in the purge and trap injector.

[0042] 2. Set the analysis conditions of purge and trap as follows: transfer line temperature 140°C, purge flow rate 40mL / min, purge time 11min, purge temperature 20°C, sample volume 10ml, sample bottle temperature 40°C, dry purge time 2min , Dry purge flow rate 100mL / min, dry purge temperature 20°C.

[0043]3. The collected and extracted phenol was analyzed by gas chromatography-mass spectrometry. The gas chromatography conditions were: chromatographic column 60m×250μm×1.4μm, constant flow mode with a flow rate of 1mL / min, and an inlet temperature of 270°C. In the split ...

Embodiment 2

[0049] The specific determination steps of phenol content in the effluent water of an aerobic pool in a pharmaceutical factory are as follows:

[0050] 1. Collect water samples in a brown glass bottle, add 0.12mol / L phosphoric acid after collection, adjust the pH to 6, take 15mL water samples into the sample bottle, add a magnet and seal the cap. Place the vial in the purge and trap injector.

[0051] 2. Set the analysis conditions of purge and trap as follows: transfer line temperature 140°C, purge flow rate 40mL / min, purge time 11min, purge temperature 20°C, sample volume 10mL, sample bottle temperature 40°C, dry purge time 2min , the dry purge flow rate is 100ml / min, and the dry purge temperature is 20°C.

[0052] 3. The collected and extracted phenol was analyzed by gas chromatography-mass spectrometry. The gas chromatography conditions were: chromatographic column 60m×250μm×1.4μm, constant flow mode with a flow rate of 1mL / min, and an inlet temperature of 270°C. In the ...

Embodiment 3

[0062] The specific determination steps of phenol content in the water quality of the sewage treatment plant inlet are as follows:

[0063] 1. Collect water samples in a brown glass bottle, add 0.1mol / L phosphoric acid after collection, adjust the pH to 5, take 15mL water sample into the sample bottle, add a magnet and seal the cap. Place the vial in the purge and trap injector.

[0064] 2. The analysis conditions for setting the purge and trap device are: transfer line temperature 130°C, purge flow rate 40mL / min, purge time 11min, purge temperature 20°C, sample volume 10mL, sample bottle temperature 50°C, drying purge time 2min, dry purge flow rate 100mL / min, dry purge temperature 20°C.

[0065] 3. The collected and extracted phenol was analyzed by gas chromatography-mass spectrometry. The gas chromatography conditions were: chromatographic column 60m×250μm×1.4μm, constant flow mode with a flow rate of 1mL / min, and an inlet temperature of 270°C. In the split injection mode ...

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Abstract

The invention relates to a method for rapidly determining the content of phenol in wastewater by purge and trap-gas chromatography-mass spectrometry, which comprises the following steps: 1) collecting a wastewater sample, adding phosphoric acid, and adjusting the pH value of the wastewater sample to weak acidity; (2) purging phenol in the wastewater sample by using a purging and trapping sample injector, trapping the phenol by using a trapping trap, and then analyzing the phenol to enter a gas chromatograph-mass spectrometer; and (3) carrying out qualitative and quantitative analysis on the phenol trapped by the trapping trap by using a gas chromatograph-mass spectrometer. Compared with the prior art, the method for measuring the phenol content in the industrial wastewater is simple, rapid, efficient and accurate, the wastewater with complex components and high organic matter concentration can be directly purged, the pretreatment processes such as separation and purification are omitted, an organic solvent is not needed for extraction, the detection cost is reduced, and the method is suitable for large-scale popularization and application. The time for detecting a group of water samples is shortened from two hours to about 30 minutes, and the detection limit is 0.01-1 mg / L.

Description

technical field [0001] The invention belongs to the technical field of phenol detection in waste water, and relates to a method for rapidly measuring phenol content in waste water by purge and trap-gas chromatography. Background technique [0002] Phenol is a common raw material in the production of industrial and agricultural products, and it is one of the main pollutants in the downstream water system of industrial production. Because phenol has chemical characteristics such as refractory and high toxicity, phenol is not easy to be degraded in water and will continue to accumulate. When the sewage treatment plant at the end of the waterway adopts primary treatment, it is generally required that the volatile phenol content in the sewage discharged into the urban sewer shall not exceed 0.5mg / L. [0003] At present, 4-aminoantipyrine spectrophotometry (GB / T7490-1987) is widely used in the detection method of phenol in water. However, this method often has a high absorbance ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/08G01N30/16
CPCG01N30/02G01N30/72G01N30/08G01N30/16G01N2030/025
Inventor 朱勇强李媛媛梁星孙晓森徐梦雅
Owner SHANGHAI INST OF TECH
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