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Method of detecting bromonitromethane content in drinking water by GC/MS combination

A technology for bromonitromethane and drinking water is applied in the field of bromonitromethane content, which can solve problems such as health hazards, and achieve the effects of saving water samples and high sample cost.

Inactive Publication Date: 2014-06-04
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After 2000, studies have found that some newly discovered DBPs that have not been included in the regulations, such as halogenated disinfection by-products, are far more harmful to the human body than THMs
HNMs have strong cytogenotoxicity and mutagenicity, and HNMs will be produced in common chlorine, chloramine and ozone disinfection processes, especially in the combined disinfection process of ozone and chloramine or chlorine, a higher concentration of HNMs will be produced , causing great harm to people's health

Method used

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  • Method of detecting bromonitromethane content in drinking water by GC/MS combination
  • Method of detecting bromonitromethane content in drinking water by GC/MS combination
  • Method of detecting bromonitromethane content in drinking water by GC/MS combination

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: terminator selection

[0030] Usually the residual chlorine in drinking water after disinfection is between 0.05 ~ 4.0mg / L, and there will be a relatively high content of residual chlorine in the test water samples generated by DBPs, and it is necessary to add a reducing terminator to eliminate the strong Oxidative residual chlorine terminates the chlorination reaction process. In order to avoid the impact of the terminator on the stability of BNM as much as possible. The effect of commonly used terminators on the stability of BNM needs to be investigated.

[0031] Use pure water to prepare multiple water samples of BNM with a concentration of 100 μg / L, select one of the water samples to measure the peak area M immediately by the gas phase / mass spectrometer in the full scan (SCAN) mode, in addition, separately to other BNM Add the terminator (ascorbic acid, sodium thiosulfate, sodium sulfite, ammonium chloride) to the water sample to make the concentrati...

Embodiment 2

[0032] Embodiment 2: the selection of extractant

[0033]First pass the water sample through a 0.22 μm microporous membrane, then add 8 g of anhydrous sodium sulfate to a glass bottle containing 25 mL of water sample, place it on an oscillator at a speed of 720 r / min, and oscillate until the salt is completely dissolved, and the solution It is transparent, and the liquid level rises slightly; after that, add 2mL of extractant, place it on a shaker at a speed of 720r / min, oscillate for 5min, remove the sample bottle, let it stand for 5min, take the upper layer of extractant, and perform GC / MS analysis. Determination. In this experiment, two kinds of extractants (methyl tert-butyl ether and ethyl acetate) were used, and the extraction effects of the two were compared, that is, the one with higher recovery rate was superior. The extraction recovery rate of methyl tert-butyl ether (MTBE) to BNM is 92.5%-106.2%, while the recovery rate of ethyl acetate (ETAC) is 82.5%-104.2%. The...

Embodiment 3

[0034] Embodiment 3: the selection of internal standard substance

[0035] In the present invention, 1,2-dibromopropane and n-decane were used as internal standard substances for comparative study, which were dissolved in methyl tert-butyl ether and prepared step by step to a concentration of 150 μg / L. Used as extractant in follow-up experiments. Prepare multiple 100μg / L BNM water samples with pure water, take 25mL water samples and add them to 40mL glass bottles, then add 8g of anhydrous sodium sulfate, place on the shaker at a speed of 720r / min, and oscillate until The salt is completely dissolved, the solution is transparent, and the liquid level rises slightly; after that, add 2 mL of extractant (containing 1,2-dibromopropane 150 μg / L) and extractant (containing 150 μg / L n-decane) respectively, and set On the shaker at a speed of 720r / min, oscillate for 5min, remove the sample bottle, let stand for 5min, take the upper extractant respectively, and carry out GC / MS determin...

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Abstract

The invention discloses a method of detecting the bromonitromethane content in drinking water by GC / MS combination. The method includes: (1) a step of sample pretreatment, namely a step of adding a terminating agent ascorbic acid according to a ratio that 0.4-0.5 mmol of the terminating agent ascorbic acid is added for each liter of a sample, shaking uniformly, adjusting the pH value of the drinking water sample to be 6.0-7.5, adding anhydrous sodium sulfate according to a ratio that 6-8 g of the anhydrous sodium sulfate is added for each 25 mL of the mixture of the terminating agent ascorbic acid and the sample, oscillating until the salt is completely dissolved, and adding methyl tertiary butyl ether containing an internal standard substance 1,2-dibromopropane for extraction, with the volume ratio of the drinking water sample to the methyl tertiary butyl ether being 25:1-2; and (2) a step of GC / MS detection, namely a step of detecting the extract by using gas chromatography / mass spectrometer, performing quantitative detection by selecting an ion mode, and obtaining the bromonitromethane content in the drinking water by adoption of an internal standard method. The method of detecting the bromonitromethane content in drinking water by GC / MS combination has advantages of rapidness and low cost.

Description

technical field [0001] The invention relates to a method for detecting the content of bromopicrin (BNM) in drinking water by GC / MS combination. Background technique [0002] In 1974, research found that when chlorine was used as a disinfectant, trihalomethanes (THMs) were also produced while causing olfactory and taste reactions. In 1976, the U.S. Environmental Protection Agency (US.EPA) found that chloroform and other trihalomethanes were common in drinking water after chlorination. At the same time, the National Cancer Institute of the United States found that chloroform is carcinogenic to animals. Since then, people began to pay attention to the research of disinfection by-products (DBPs) in drinking water. In the 1990s, apart from THMs, the research objects of disinfection byproducts in drinking water were mainly haloacetic acids (HAAs), whose carcinogenic risk is much higher than that of trihalomethanes. After 2000, studies have found that some newly discovered DBPs ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 丁春生孟壮张涛
Owner ZHEJIANG UNIV OF TECH
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