Pre-treatment Method for Determination of Volatile Thio-ether Compounds in Offensive Odorous Sediment

Active Publication Date: 2017-05-25
NANJING INST OF GEOGRAPHY & LIMNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The invention is a method for extracting and purifying volatile thio-ether compounds in sediment. The method ensures that the compounds are not lost or overlapped during detection. It uses a two-step continuous extraction method that can simultaneously extract and purify multiple compounds. The method selects the optimal extraction temperature, time, and ultrasonic power, as well as the solid phase extraction column and eluent. It also controls system error of sulfide loss and produces no volatilization of compounds. Compared to traditional methods, the invention takes less time and has a higher standard recovery rate, ensuring accuracy of determination.

Problems solved by technology

The largest disadvantage of this method is over-emphasis on qualitative analysis of odorous compounds, only a part of weak absorbed dimethyl trisulfide compound in the sediment is resolved and then collected for determination, and most of the compound still resides in the sediment.
It is reported in literature that Taihu lake water crisis in 2007 is mainly due to water body smelliness caused by excessively high content of dimethyl trisulfide and dimethyl disulfide.
With further research work, acquiring content and categories of volatile thio-ether compounds in the sediment simply by qualitative or semi-quantitative method cannot satisfy the requirement for accurately learning environmental geochemical information of volatile thio-ether compounds at the sediment-water interface.

Method used

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  • Pre-treatment Method for Determination of Volatile Thio-ether Compounds in Offensive Odorous Sediment
  • Pre-treatment Method for Determination of Volatile Thio-ether Compounds in Offensive Odorous Sediment
  • Pre-treatment Method for Determination of Volatile Thio-ether Compounds in Offensive Odorous Sediment

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embodiment 1

[0033]According to the invention, the extraction method of volatile thio-ether compounds in sediment sample collected in Cyanobacteria area of Meiliang Bay, Taihu Lake is as follows:

[0034](1) Sample collection and sealed storage away from light: collecting a cylindrical core sample of fresh sediment from a lake or river bed by a sediment corer and retaining a water column which is 20 cm long, and removing stones, animal and plant residues such as snails, corbicula fluminea and plant root system in the sludge sample; collecting 0-10 cm fresh sludge samples on the surface, rapidly filling 30 g into a 50 mL brown glass bottle after mixing adequately and retaining water of about 1 cm, and then sealing.

[0035](2) Sample refreshing and anaerobic pre-treatment: adding 5 mL of 0.1% HgCl2 to the surface of fresh sediment for sterilization, adding 15 g of dry ice at the same time, finally placing the brown sample bottle into a liquid nitrogen container for cold storage, and transporting back t...

embodiment 2

[0046]According to the invention, the extraction method of volatile thio-ether compounds in sediment sample collected in reed wetland of Meiliang Bay, Taihu Lake is as follows:

[0047](1) Sample collection and sealed storage away from light: collecting a cylindrical core sample of fresh sediment from a lake or river bed by a sediment corer and retaining a water column which is 22 cm long, and removing stones, animal and plant residues such as snails, corbicula fluminea and plant root system in the sludge sample; collecting 0-10 cm fresh sludge samples on the surface, rapidly filling 30 g into a 50 mL brown glass bottle after mixing adequately and retaining water of about 1 cm, and then sealing.

[0048](2) Sample refreshing and anaerobic pre-treatment: adding 10 mL of 0.1% HgCl2 to the surface of fresh sediment for sterilization, adding 15 g of dry ice at the same time, finally placing the brown sample bottle into a liquid nitrogen container for cold storage, and transporting back to lab...

embodiment 3

[0058]By the technical scheme of the invention, the collected river bed sediment is subject to pre-treatment for extracting volatile thio-ether compounds:

[0059](1) Sample collection and sealed storage away from light: collecting a cylindrical core sample of fresh sediment from a lake or river bed by a sediment corer and retaining a water column which is 25 cm long, and removing stones, animal and plant residues such as snails, corbicula fluminea and plant root system in the sludge sample; collecting 0-10 cm fresh sludge samples on the surface, rapidly filling 25 g into a 50 mL brown glass bottle after mixing adequately and retaining water of about 1 cm, and then sealing.

[0060](2) Sample refreshing and anaerobic pre-treatment: adding 15 mL of 0.1% HgCl2 to the surface of fresh sediment for sterilization, adding 15 g of dry ice at the same time, finally placing the brown sample bottle into a liquid nitrogen container for cold storage, and transporting back to laboratory in time for de...

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Abstract

Method for determining volatile thio-ether compounds in offensive odorous sediment including: pre-treating a sediment sample, extracting volatile thio-ether compounds, separating and purifying the extraction supernatant in a solid phase extraction column, eluting with ethyl acetate, and finally collecting the eluent, which is then concentrated and used for determination by gas chromatography.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]This application claims priority from CN Application No. 201510819428.3, filed Nov. 23, 2015, the contents of which are incorporated herein in the entirety by reference.FIELD OF THE INVENTION[0002]The invention belongs to the field of environmental protection technology, and specifically to a pre-treatment method for the determination of volatile thio-ether compounds in offensive odorous sediment.BACKGROUND OF THE INVENTION[0003]At present, with respect to the problem of black and odorous water body occurring in city river beds and local lake areas in China, but the focuses of pre-treatment technique related to volatile thio-ether compounds in the water body are on water body, biological samples such as fish. Patent 201120511340.2 has mentioned a determination method, comprising accelerating volatilization of dimethyl trisulfide in the sediment by microwave heating method, and then collecting volatilized odorous gas compounds by purging a...

Claims

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Application Information

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IPC IPC(8): G01N1/34G01N1/42G01N33/18G01N1/40
CPCG01N1/34G01N1/4044G01N1/405G01N1/42G01N1/4077G01N33/18G01N33/0044A61L2/18G01N33/24Y10T436/25Y10T436/255Y10T436/25125Y10T436/182G01N2001/4094G01N30/02G01N30/06G01N30/88G01N2030/062G01N2030/025G01N2001/4061
Inventor GU, XIAOZHICHEN, KAININGSUN, SHUYUNLIU, MIAOKANG, JIAWANG, YADONG
Owner NANJING INST OF GEOGRAPHY & LIMNOLOGY
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