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
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[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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