Method for detecting polar phenol type chlorinated/brominated disinfection by-products in water
A technology for disinfection by-products and phenols, which is used in measurement devices, instruments, scientific instruments, etc., can solve the problem of high detection limit and quantification limit, inability to use trace amounts of polar phenol-based chlorinated/brominated disinfection by-products, Time-consuming and other problems, to achieve high sensitivity, improve reproducibility and recovery, and reduce errors
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Embodiment 1
[0037] figure 1 It shows that the technical scheme of the present invention can simultaneously realize the separation and detection of 13 novel polar phenolic chlorinated / brominated disinfection by-products at one time. Its concrete method comprises the following steps:
[0038] 1) Prepare different concentration gradients (10 -12 g / L-10 -6 g / L) containing 3,5-dichloro-4-hydroxybenzaldehyde, 3-bromo-5-chloro-4-hydroxybenzaldehyde, 3,5-dibromo-4-hydroxybenzaldehyde, 3,5- Dichloro-4-hydroxybenzoic acid, 3-bromo-5-chloro-4-hydroxybenzoic acid (by volume), 3,5-dibromo-4-hydroxybenzoic acid, 3,5-dichlorosalicylic acid , 3-bromo-5-chlorosalicylic acid, 3,5-dibromosalicylic acid, 2,4,6-trichlorophenol, 2,6-dichloro-4-bromophenol, 2,6-dibromo Standard working solution of -4-chlorophenol and 2,4,6-tribromophenol. Wherein, 3-bromo-5-chloro-4-hydroxybenzoic acid has no available standard substance, thus according to literature (Pan, Y., Zhang, X., 2013.Four groups of new aromatic ha...
Embodiment 2
[0054] In Example 2, one or more substances in the 13 novel polar phenolic chlorinated / brominated disinfection by-products were measured simultaneously using the technical solution of the present invention. Its concrete method comprises the following steps:
[0055] Step 1) preparation of standard working solutions with different concentration gradients, 2) preparation of the water samples to be tested, and step 3) pretreatment of the water samples to be tested, are the same as those described in Example 1.
[0056] In step 4), the 13 kinds of phenolic chlorinated / brominated disinfection by-products were randomly combined, that is, one or more of the 13 phenolic chlorinated / brominated disinfection by-products were combined, divided into Times (2-12 times) are detected by the detection method of the present invention. The parameter settings of the established ultra-high performance liquid chromatography / electrospray ionization triple quadrupole mass spectrometer (UPLC / ESI-tqMS...
Embodiment 3
[0061] In Example 3, the detection method of the present invention was used to separate and detect 13 novel polar phenolic chlorinated / brominated disinfection by-products contained in the water produced by the waterworks. Its concrete method comprises the following steps:
[0062] 1) The method for preparing standard working solutions with different concentration gradients is the same as that described in Example 1.
[0063] 2) Collect 1L of fresh factory water, and quickly transport the water samples back to the laboratory under refrigerated conditions at 4°C.
[0064] 3) Take 100 mL of the water sample in 2) and titrate the residual chlorine content in the water, and then add 5% sodium arsenite in excess molar ratio to the remaining 0.9 L water sample to terminate the reaction. Use H again 2 SO 4 Adjust the pH to 0.5. Add 90 g Na per liter of acidified sample 2 SO 4 Make it saturated, then add 90mL methyl tert-butyl ether for extraction, place it for 15min and then use...
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