Method for determining 2,4,6-tribromophenol content of sea water and fresh water

A determination method and technology of tribromophenol, which is applied in the field of determination of 2.4.6-tribromophenol content in seawater and fresh water, can solve problems such as not found, and achieve the effect of easy implementation, convenient method and reliable implementation

Active Publication Date: 2009-12-09
谱尼测试集团股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] 2.4.6-Tribromophenol has not found any reports on the detection of 2.4.6-Tribromophenol at home and abroad; domestic research on the pollution of these compounds has just started
At present, there are only methods for the determination of 2.4.6-trichlorophenol in drinking water by GC-ECD and GC / MS; but there is no method for the determination of 2.4.6-tribromophenol in seawater and fresh water by gas chromatography

Method used

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  • Method for determining 2,4,6-tribromophenol content of sea water and fresh water
  • Method for determining 2,4,6-tribromophenol content of sea water and fresh water
  • Method for determining 2,4,6-tribromophenol content of sea water and fresh water

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Effect test

Embodiment 1

[0031] Embodiment 1, the detection of 2.4.6-tribromophenol content in rainwater:

[0032] Take a sufficient amount of sample from the storage bottle and place it at room temperature, let the sample temperature return to room temperature, transfer 500mL water sample to a clean 500-mL glass separatory funnel with a stopper, add 13mL to the water sample Concentrated sulfuric acid was used to cleanse and acidify the sample. Cover the plug, shake and mix, and check the pH value of the water sample with precision pH test paper, and adjust the pH with concentrated sulfuric acid to make the pH<2. Add 30 mL of n-hexane into the separatory funnel and shake vigorously for 3 minutes, then let it stand for 5 minutes to facilitate the separation of the aqueous phase and the organic phase, and transfer the organic layer to a conical centrifuge tube. The above extraction process was repeated twice again, and the three extracted organic phases were combined. The acid in the extract phase was...

Embodiment 2

[0065] Embodiment 2, the mensuration of 2.4.6-tribromophenol content in seawater:

[0066]Take a sufficient amount of sample from the storage bottle and place it at room temperature, let the sample temperature return to room temperature, transfer 500mL water sample to a clean 500-mL glass separatory funnel with a stopper, add 13mL to the water sample Concentrated sulfuric acid was used to cleanse and acidify the sample. Cover the plug, shake and mix, and check the pH value of the water sample with precision pH test paper, and adjust the pH with concentrated sulfuric acid to make the pH<2. Add 30 mL of n-hexane into the separatory funnel and shake vigorously for 3 minutes, then let it stand for 5 minutes to facilitate the separation of the aqueous phase and the organic phase, and transfer the organic layer to a conical centrifuge tube. The above extraction process was repeated twice again, and the three extracted organic phases were combined. The acid in the extract phase was...

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Abstract

The invention relates to a method for determining the 2,4,6-tribromophenol content of sea water and fresh water, which comprises the following steps: extracting a sample with normal hexane under an acidic condition (pH is less than 2), drying a resulting extract and concentrating the resulting extract, derivatizing the resulting concentrate with aceticanhydride in an alkaline environment (pH is between 10.5 and 11.5), and analyzing the resulting derivative by using an ECD detector; weighting a standard 2,4,6-tribromophenol, dissolving the standard 2,4,6-tribromophenol in solution of normal hexane, adjusting the volume of the solution, using the solution as stock solution, and adding 4,4- dibromooctafluorobiphenyl (internal standard) into the stock solution; diluting the standard stock solution with 2,4-dichlorobenzoic acid (substitute) to obtain a standard solution for use with concentration gradient; derivatizing the standard solution for use with aceticanhydride, and testing the sample by using a gas chromatograph ECD detector; and finally, obtaining a result through calculation. The method for detecting the 2,4,6-tribromophenol content of sea water and fresh water has the advantages of high speed, effectiveness, detection limit of 0.01 ug/L and error rate no more than 10 percent. Therefore, the method is a reliable and easy-to-implement method for detecting the 2,4,6-tribromophenol content of sea water and fresh water and can satisfy demands of searches and production.

Description

technical field [0001] The invention relates to a method for determining the content of 2.4.6-tribromophenol in seawater and fresh water, in particular to a method for determining the content of 2.4.6-tribromophenol in seawater and fresh water by gas chromatography. Background technique [0002] 2.4.6-Tribromophenol, white needle-like prismatic crystals. The melting point is 95-96°C (sublimation), the boiling point is 244°C, and the relative density is 2.55. Soluble in alcohol, chloroform, ether and caustic alkali solution, almost insoluble in water. 2,4,6-Tribromophenol is a reactive flame retardant with high bromine content and a fungicide. [0003] 2.4.6-Tribromophenol There is no report on the detection of 2.4.6-tribromophenol at home and abroad; domestic research on the pollution of these compounds has just started. At present, there are only GC-ECD and GC / MS methods for the determination of 2.4.6-trichlorophenol in drinking water; but there is no method for the dete...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 宋薇
Owner 谱尼测试集团股份有限公司
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