Method of detecting content of 1,1-dichloroacetone in drinking water by GC/MS combination

A technology of dichloroacetone and drinking water, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as not having qualitative analysis functions, and achieve the effect of small relative standard deviation

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

GC-ECD can better quantify DCAce in water, but it does not have the function of qualitative analysis, and it has certain defects in the qualitative analysis of substances.

Method used

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  • Method of detecting content of 1,1-dichloroacetone in drinking water by GC/MS combination
  • Method of detecting content of 1,1-dichloroacetone in drinking water by GC/MS combination
  • Method of detecting content of 1,1-dichloroacetone in drinking water by GC/MS combination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: terminator selection

[0033] 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 influence of the terminator on the stability of DCAce as much as possible. The effect of commonly used terminators on the stability of DCAce needs to be investigated.

[0034] Prepare multiple water samples of DCAce with a concentration of 100 μg / L (preparation method: take an appropriate amount of 5 mg / L DCAce standard, place it in a brown volumetric flask, and prepare a standard solution with a mass concentration of 10 μg / mL with deionized water, Then dilute the standard solution with ultrapure water to the required concentration), select one of the water s...

Embodiment 2

[0035] Embodiment 2: the selection of extractant

[0036]First, pass 100 μg / L of DCAce water sample (preparation method is the same as in Example 1) 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, and place it on a shaker to At a speed of 720r / min, oscillate until the salt is completely dissolved, the solution is transparent, and the liquid level rises slightly; after that, add 2mL of extractant, place it on the shaker at a speed of 720r / min, shake for 5min, remove the sample bottle, and Set aside for 5min, take the upper layer extract, and carry out the determination of GC / MS. 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 standard addition recovery rate of methyl tert-butyl ether is above 90%, and the standard addition recover...

Embodiment 3

[0037] Embodiment 3: the selection of internal standard substance

[0038] 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. Configure multiple 100μg / L DCAce water samples (the preparation method is the same as in Example 1), take 25mL water samples and add them to 40mL glass bottles, then add 8g of anhydrous sodium sulfate, place on the shaker at 720r / min Shake until the salt is completely dissolved, the solution is transparent, and the liquid level rises slightly; after that, add 2 mL of extractant A (containing 150 μg / L 1,2-dibromopropane) and extractant B (containing 150 μg / L decane), placed on an oscillator at a speed of 720r / min, oscillated for 5 minutes, removed the sample bottle, and stood still for 5 minutes, then took the upper layer extractant f...

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Abstract

The invention discloses a method of detecting the content of 1,1-dichloroacetone in drinking water by GC/MS combination. The method includes the following steps of: (1) 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 drinking water sample; shaking uniformly, adjusting the pH value of the drinking water sample to be 4.0-6.0, 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 drinking water 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) detecting the extract by using gas chromatography/mass spectrometer, performing quantitative detection by selecting an ion mode, and obtaining the content of the 1,1-dichloroacetone in the drinking water by adoption of an internal standard method. The method by the invention has advantages of rapidness and low cost.

Description

technical field [0001] The invention relates to water quality detection and analysis technology, in particular to a method for GC / MS combined detection of 1,1-dichloroacetone (DCAce) content in drinking water. Background technique [0002] Chlorine disinfection, as a cost-effective drinking water disinfection method, has been used by water purification plants for more than 100 years. Disinfection and disinfection by-products (DBPs) are given great attention. The main research direction of the control technology of chlorine disinfection by-products in drinking water is to seek disinfectants to replace chlorine, to determine and remove the precursors of disinfection by-products, and to reduce disinfection by-products. Alternative disinfectants are mainly ozone, chlorine dioxide, chloramine, potassium permanganate, ferrate and their combined processes. However, with the single or combined use of multiple disinfectants, more and more drinking water disinfection By-products (DB...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 丁春生徐洋洋张涛
Owner ZHEJIANG UNIV OF TECH
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