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A technology for pollutants and screening, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of cumbersome operation, insufficient scanning speed, and lack of
Active Publication Date: 2019-03-22
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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However, the scanning speed of GC-MS / MS is not enough, and the instrument is expensive; LC-MS / MS detection is mainly for non-volatile organic pollutants, and the instrument is expensive and the operation is cumbersome
Therefore, there is still a lack of rapid screening of chlorine-substituted (-Cl) organic pollutants, bromine-substituted (-Br) organic pollutants, nitro-substituted (-NO 2 ) method for organic pollutants
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example 1
[0137] After the sample to be tested is analyzed by two-dimensional gas chromatography-EI mass spectrometry, the mass spectra arranged in the order of mass-to-charge ratio are obtained, and some of the mass spectra are as follows: Figure 4 shown. Take the existing chloroform as an example, in this figure, m / z=14, m / z+105 / 107 / 109 / 111=119 / 121 / 123 / 125, at m / z=119 / 121 / The mass spectrum peak can be observed at 123 / 125, and S / N>3, R>3%, and this signal exists in the corresponding split ECD detector result, and S / N>3, R>3%, therefore, The substance to be tested contains trichloro( 35 Cl and 37 Cl) Pollutants. It can be combined with NIST spectral library for further identification.
example 2
[0139] After the sample to be tested is analyzed by two-dimensional gas chromatography-EI mass spectrometry, the mass spectra arranged in the order of mass-to-charge ratio are obtained, and some of the mass spectra are as follows: Figure 5 shown. Taking the existing monobromoacetonitrile as an example, in this figure, m / z=40, m / z+79 / 81=119 / 121, mass spectrum peaks can be observed at m / z=119 / 121, and S / N>3, R>3%, there is this signal in the corresponding split ECD detector result, and S / N>3, R>3%, therefore, contain monobromo( 79 Br and 81 Br) pollutants. It can be combined with NIST spectral library for further identification.
example 3
[0141] After the sample to be tested is analyzed by two-dimensional gas chromatography-EI mass spectrometry, the mass spectra arranged in the order of mass-to-charge ratio are obtained, and some of the mass spectra are as follows: Figure 6 shown. Taking the existing nitrobenzene as an example, in this figure, m / z=77, m / z+46=123, a mass spectrum peak can be observed at m / z=123, and S / N>3, R >3%, the signal exists in the corresponding split ECD detector result, and S / N>3, R>3%, therefore, the analyte contains nitro-substituted pollutants. It can be combined with NIST spectral library for further identification.
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Abstract
The invention provides a screening method for pollutants in water. The screening method comprises the following steps of: obtaining a sample to be detected from a water sample to be detected; carryingout two-dimensional gas chromatographic analysis on the sample to be detected to obtain an intermediate analyte; bombarding one part of the intermediate analyte through an EI ion source to generate ions with different mass-to-charge ratios; carrying out mass spectrum analysis to obtain first spectrograms which are arrayed according to the size sequence of the mass-to-charge ratios; carrying out ECD (Electron Capture Detector) detection on the other part of the intermediate analyte to obtain second spectrograms; screening the first spectrograms by adopting a mass spectrum difference value method and comparing with the second spectrograms; if a screening result of the mass spectrum difference value method has an effective signal which represents organic chloride, organic bromide or a nitrylsubstitute possibly and the second spectrograms also have the effective signal, determining that the sample contains the organic chloride, the organic bromide or the nitryl substitute. By adopting the method provided by the invention, reliable screening of chlorine substituted (-Cl) organic pollutants, bromine substituted (-Bl) organic pollutants and nitryl substituted (-NO2) organic pollutants can be conveniently and rapidly realized.
Description
technical field [0001] The invention relates to screening of pollutants in water, in particular to a screening method of pollutants in water. Background technique [0002] At present, chlorine-substituted (-Cl) organic pollutants, bromine-substituted (-Br) organic pollutants, nitro-substituted (-NO 2 ) organic pollutants, etc. The life and health risks brought by these water pollutants have aroused widespread concern. Most chlorine-substituted (-Cl) organic pollutants, bromine-substituted (-Br) organic pollutants, nitro-substituted (-NO 2 ) Organic pollutants have the characteristics of strong toxicity and refractory degradation. The screening of organic pollutants in water is particularly important to ensure water quality safety. [0003] Existing chlorine-substituted (-Cl) organic pollutants, bromine-substituted (-Br) organic pollutants, nitro-substituted (-NO 2 ) The detection methods of organic pollutants are mainly gas chromatography-dual mass spectrometry detectio...
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