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Rapid detection method for trace TCDD (Tetrachlorodibenzo-p-dioxin)

A detection method, the technology of dioxin, which is applied in the field of rapid detection of trace dioxin, can solve the problems of high cost, long time-consuming, complicated pretreatment, etc., and achieve the effect of less sample amount, simple preparation, and green and environmentally friendly materials

Active Publication Date: 2013-11-20
FUJIAN AGRI & FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the existing problems of high cost, complicated pretreatment, and long time consumption in existing dioxin detection, the purpose of the present invention is to provide a rapid detection method for trace dioxin, which is easy to operate, high in sensitivity, and can save a lot of Advantages of economy and time cost

Method used

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  • Rapid detection method for trace TCDD (Tetrachlorodibenzo-p-dioxin)
  • Rapid detection method for trace TCDD (Tetrachlorodibenzo-p-dioxin)

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Experimental program
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Effect test

Embodiment 1

[0036] (1) Configure methyl cellulose with a mass fraction of 0.15% (molecular weight is 30,000, methoxyl content is 27.5%), add sodium citrate with a mass of 35% methyl cellulose, stir well, and raise the temperature to 75°C temperature, under the condition of stirring, add the silver ammonia solution with the same volume concentration as the methyl cellulose solution, which is 10mmol / L, and react at a temperature of 75°C for 3 hours to obtain the silver colloid modified by methyl cellulose.

[0037] (2) Prepare dioxin standard solutions with 8 gradient concentrations (10ng / L, 20ng / L, 30ng / L, 40ng / L, 50ng / L, 60ng / L, 70ng / L, 80ng / L) in ethanol, Mix 1ml of dioxin standard solutions with different concentrations and 1ml of silver colloid evenly, centrifuge, collect the precipitated part, and test it with a laser Raman spectrometer to obtain the SERS spectrum of dioxin, see figure 1 .

[0038] The wave number obtained is 1303cm -1 、1407 cm -1 、926 cm -1 、1031 cm -1 、734 cm ...

Embodiment 2

[0046] (1) Configure methyl cellulose with a mass fraction of 0.5% (molecular weight is 350,000, methoxyl content is 27.5%), add sodium citrate with a mass of 45% methyl cellulose, stir well, and raise the temperature to 70°C temperature, under the condition of stirring, add the silver ammonia solution with the same volume concentration as the methyl cellulose solution, which is 15mmol / L, and react at a temperature of 70°C for 2.5 hours to obtain a methyl cellulose modified silver colloid.

[0047] (2) Use ethanol to prepare dioxin standard solutions with 8 gradient concentrations (50ng / L, 60ng / L, 70ng / L, 80ng / L, 90ng / L, 100ng / L, 110ng / L, 120ng / L,) , Mix 1ml of dioxin standard solutions with different concentrations and 1ml of silver colloid evenly, centrifuge, collect the precipitated part, and test it with a laser Raman spectrometer to obtain the SERS spectrum of dioxin.

[0048] The wave number obtained is 1303cm -1 、1407 cm -1 、926 cm -1 、1031 cm -1 、734 cm -1 The rel...

Embodiment 3

[0056] (1) Configure methyl cellulose with a mass fraction of 0.1% (molecular weight is 40,000, methoxyl content is 28%), add sodium citrate with a mass of 40% methyl cellulose, stir well, and raise the temperature to 78°C Temperature, under the condition of stirring, add silver ammonia solution with the same volume concentration as the methylcellulose solution, which is 7.5mmol / L, and react at a temperature of 78°C for 2.5 hours to obtain a methylcellulose-modified silver glue.

[0057] (2) Use ethanol to prepare dioxin standard solutions with 8 gradient concentrations (50ng / L, 60ng / L, 70ng / L, 80ng / L, 90ng / L, 100ng / L, 110ng / L, 120ng / L,) , Mix 1ml of dioxin standard solutions of different concentrations with 1ml of silver colloid evenly, centrifuge, collect the precipitated part, and test it with a laser Raman spectrometer to obtain the SERS spectrum of dioxin.

[0058] The wave number obtained is 1303cm -1 、1407 cm -1 、926 cm -1 、1031 cm -1 、734 cm -1 The relationship be...

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Abstract

The invention discloses a rapid detection method for trace TCDD (Tetrachlorodibenzo-p-dioxin). The method comprises the following steps: preparing an SERS (Surface Enhanced Raman Scattering) substrate for detection by using methylcellulose, sodium citrate and a silver-ammonia solution as raw materials; mixing TCDD solutions with different concentrations with the substrate, carrying out centrifugal separation on the obtained mixture, and testing the obtained object by using a laser Raman spectrometer so as to obtain an SERS spectrum chart of TCDD; obtaining a relation between a TCDD Raman spectrum absorption intensity with a certain wave number and a TCDD concentration, and establishing a mathematical relation between the Raman spectrum absorption intensity and the TCDD concentration; and testing a TCDD solution with an unknown concentration by using the laser Raman spectrometer, and according to the mathematical relation between the Raman spectrum absorption intensity with the certain wave number and the TCDD concentration, calculating the TCDD concentration. The method disclosed by the invention solves the problems that current TCDD detection cost is high, and samples are required to be subjected to multi-step separation, and the like, has the advantages of easiness for operation, high sensitivity, and capability of reducing a lot of economic and time costs, and has a wide application prospect.

Description

technical field [0001] The invention relates to a rapid detection method of trace dioxins. Specifically, a rapid detection method of trace dioxins is carried out by using nano-silver as a substrate through Raman spectroscopy. Background technique [0002] Dioxin analogs are a class of widespread environmental pollutants, such as polychlorinated dibenzodioxins, polychlorinated dibenzofurans, and polychlorinated biphenyls. They are difficult to degrade in the environment, can pollute the environment persistently, and have high lipolysis, which is easy to produce bioaccumulation and biomagnification. Toxicity studies have shown that dioxins have strong carcinogenicity, teratogenicity, immunotoxicity, reproductive toxicity, and liver toxicity. [0003] The detection of dioxins belongs to trace analysis. Due to the very complex environmental matrix, the detection of dioxin-like compounds is extremely difficult, which is a difficult point in modern analytical chemistry. Chromat...

Claims

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Application Information

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IPC IPC(8): G01N21/65
Inventor 陈礼辉卢玉栋黄六莲
Owner FUJIAN AGRI & FORESTRY UNIV
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