Method for accurately detecting dioxin generated by phenols in chlorine bleaching aqueous solution system
An aqueous solution and dioxin technology, applied in the field of accurate detection of dioxins produced by phenols, to achieve accurate qualitative, reduce false positive results, and avoid interference
Active Publication Date: 2020-01-21
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology
The current research has not yet started from the molecular structure of phenols and PCDD / Fs, and introduced 13 C 6 Labeled phenols and 13 C 6 12 C 6 -PCDD / Fs, eliminate the interference of natural PCDD / Fs in the environment, especially low-chlorinated PCDD / Fs, and directly confirm that phenols are the precursor substances for the formation of PCDD / Fs.
Method used
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Embodiment 1
[0077] Mix 0.5g phenol with 0.5mg 13 C 6 -Phenol is bleached, extracted, purified and analyzed according to the above steps, and the phenol in the detection calculation sample 12 C 12 -PCDD / Fs natural compounds and 13 C 6 12 C 6 -PCDD / Fs. At the same time, the bleaching experiment with only 0.5 g of phenol and the blank experiment with phenol unbleached were carried out as a control group, and all the reaction conditions, pretreatment and instrumental analysis steps were the same. 2 copies in parallel. The recovery rate of the internal standard was 25-73%. The detection limit of the instrument and the detection limit of the method are shown in Table 2.
[0078] Table 2
[0079]
[0080]
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The invention provides a method for accurately detecting dioxin generated by phenols in a chlorine bleaching aqueous solution system. Specifically, the method is characterized in that: phenols markedby <13>C<6> are added into a natural phenol aqueous solution chlorine bleaching system to mix, then a mixture is used for bleaching, a bleaching sample is obtained and then extracted and purified, a high-resolution gas chromatography-high resolution mass spectrometry is used to perform qualitative and quantitative analysis on a dioxin target object, and whether the phenols can be converted to generate PCDD / Fs in the process is judged through detection of the PCDD / Fs generated by bleaching, especially <13>C<6><12>C<6>-PCDD / Fs. The method of the invention has the beneficial effects that: the method starts from the essence of a structure, has strict logic and simple operation, and can accurately judge whether the phenols are precursor substances for generating the PCDD / Fs in the chlorine bleaching process, at the same time, the adopted mass spectrometry method can simultaneously measure the content of the <13>C<6><12>C<6>-PCDD / Fs in a sample, thereby expanding the range of dioxin detection and improving analysis and detection efficiency.
Description
technical field [0001] The invention relates to a method for accurately detecting dioxins produced by phenols in a chlorine bleach aqueous solution system, belonging to the field of persistent pollutant analysis. Specifically, it is added to the natural phenolic aqueous solution chlorine bleaching system 13 C 6 The labeled phenols are used for bleaching. After the bleached samples are extracted and purified, high-resolution gas chromatography-high-resolution mass spectrometry is used for qualitative and quantitative analysis of dioxin targets. By detecting PCDD / Fs generated by bleaching, especially 13 C 6 12 C 6 -PCDD / Fs, to determine whether phenols can be transformed into PCDD / Fs in this process, and provide a direct basis for the study of the formation mechanism of PCDD / Fs. Background technique [0002] Dioxin (PCDD / Fs) is one of the first persistent pollutants in the Stockholm Convention. It has high toxicity, environmental persistence, long-distance migration and b...
Claims
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IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14
Inventor 夏科学倪余文张亦弛张海军陈吉平
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI