Detection method for -2,3,4,7,8-PeCDF in incinerator fly ash and flue gas

A technology of 8-PCDF and detection method, applied in the field of dioxin toxicity indicator-2, can solve the problem of low applicability and high

Active Publication Date: 2015-03-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

The emergence and development of resonance-enhanced multiphoton ionization-time-of-flight mass spectrometry (REMPI-TOFMS) provides convenient conditions for on-site real-time detection of such markers; however, this method is not generally applicable
At present, there is no simple, cheap and universally applicable method to realize the quantitative detection of 23478-PeCDF

Method used

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  • Detection method for -2,3,4,7,8-PeCDF in incinerator fly ash and flue gas
  • Detection method for -2,3,4,7,8-PeCDF in incinerator fly ash and flue gas
  • Detection method for -2,3,4,7,8-PeCDF in incinerator fly ash and flue gas

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Experimental program
Comparison scheme
Effect test

preparation example Construction

[0053] 1), the preparation of extraction internal standard substance solution: 13 C 12 -2,3,4,7,8-PeCDF is used as the extraction internal standard substance, and nonane is used to prepare a 100ng / mL extraction internal standard solution, and it is stored at a low temperature of -20°C.

[0054] 2), preparation of internal standard substance solution for sample injection: 13 C 12 -1, 2, 3, 7, 8-PeCDF is used as the internal standard substance for injection, and nonane is used to prepare a 100 ng / mL internal standard solution for injection, and it is stored at a low temperature of -20°C.

[0055] 3), containing 2,3,4,7,8-PCDF, 13 C 12 -2,3,4,7,8-PeCDF, 13 C 12 -1,2,3,7,8-PeCDF series standard solution configuration: use 1.0mgL of 2,3,4,7,8-PCDF -1 13 C 12 -2,3,4,7,8-PeCDF and 13 C 12 -2,3,4,7,8-PeCDF nonane solution is prepared as a standard solution with a series of concentrations.

[0056] 4) Extraction of dioxin samples: Weigh 0.5g of fly ash samples (or collected f...

Embodiment 1

[0087] Example 1 Precision and Accuracy

[0088] First, through the determination of a series of mixed standard solutions, according to the formula in the quantitative method (1), calculate the corresponding factor (RR) and relative response factor (RF).

[0089] Table 1

[0090]

[0091] Weigh each 0.5g of fly ash samples 1#, 2#, extract once according to the steps 4), 5), and 6) in the method description, and after purification, operate according to 7), 8), and 9) in the method description to complete the sample The instrumental analysis of above-mentioned obtains with RR and RF, according to the content of 2,3,4,7,8-PeCDF in the sample calculated according to 2) and 3) in the quantitative analysis method, and recovery rate, measurement result is as table 2. The same sample was analyzed by high-resolution gas chromatography-tandem high-resolution mass spectrometry (HRGC-HRMS), and the results of the two methods were compared with each other, and the results are shown in...

Embodiment 2

[0096] Embodiment 2 detection limit

[0097] Taking the mixed standard solution as the research object, 2,3,4,7,8-PeCDF and 13 C 12 The concentrations of -1, 2, 3, 7, 8-PeCDF were 10ng / mL, 13 C 12 - 2,3,4,7,8-PeCDF concentration of 100ng / mL mixed standard solution, diluted to 2,3,4,7,8-PeCDF concentration of 2ng / mL respectively. Repeat the measurement 6 times, calculate the concentration of 2,3,4,7,8-PeCDF in the mixed standard solution according to the above-mentioned quantitative method (2), and calculate the relative standard deviation of the measured value to obtain 2,3,4, The instrument detection limit of 7,8-PeCDF was 0.003ng. The 3-fold signal-to-noise ratio (3S / N) at the peak of 2,3,4,7,8-PeCDF in the fly ash 1# sample extract was used as the detection limit of the sample, and the detection limit of the 1# sample was 0.018ng. Although the detection limit obtained has a certain gap compared with high-resolution mass spectrometry, it can basically meet the needs of ...

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Abstract

The present invention provides a detection method for -2,3,4,7,8-PeCDF in incinerator fly ash and flue gas, wherein quantitative analysis is performed by adopting a multi-dimensional gas chromatography and mass spectrometry combined method. According to the detection method, a purified sample is subjected to primary separation through one-dimensional gas chromatography to achieve the one-step purification purpose, wherein the separation column is quartz capillary chromatographic column DB-5, and the detector is an electron capture detector; and the peak at which the target object exist is cut through a cutting device arranged inside a one-dimensional chromatographic column incubator and then enters second dimensional chromatography to carry out further separation detection, and mass spectrometry detection is performed, wherein the ion source is negative chemical ionization (NCI), and the mass analyzer is a quadrupole mass analyzer. According to the present invention, the isotope internal standard method is adopted to perform quantification; the quantification on the dioxin toxicity indicator -2,3,4,7,8-PeCDF is achieved based on the multi-dimensional gas chromatography and mass spectrometry series connection method; and the rapid analysis on the dioxin content in incinerator fly ash and flue gas is achieved, the analytical instrument is simple, the spectrum and the quantitative method are simple, and the detection result is accurate.

Description

technical field [0001] The invention relates to a method for detecting dioxin toxicity indicator-2,3,4,7,8-PeCDF in incinerator fly ash and flue gas. Specifically, the heart-cutting concept and technology in multidimensional gas chromatography (MDGC) are used to achieve effective separation of some components in dioxin samples, and quantitative analysis is performed in conjunction with mass spectrometers. Background technique [0002] Dioxins (PCDD / Fs) usually refer to polychlorinated dibenzo-pdioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs), according to the number of chlorine atoms and substitution Depending on the position, there are 210 isomers in this type of compound, and there are 17 kinds of toxic dioxins, most of which are 2, 3, 7, 8-position chlorinated compounds, of which 2, 3, 7, 8-TCDD The most toxic. Because the chemical structure and toxicological properties of coplanar polychlorinated diphenyls (co-PCBs) are similar to dioxins, they are also called...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 陈吉平王雪丽倪余文
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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