Method for analyzing chloroacetic acid in drinking water by GC/MS
A gas spectrometer and chloroacetic acid technology, applied in the direction of analysis materials, instruments, scientific instruments, etc., can solve the problems of few detection items, weak qualitative ability, and affect the accurate judgment of detection results, so as to improve accuracy and avoid interference effect
Active Publication Date: 2016-12-07
SHANGHAI BAOSTEEL IND TECHNOLOGICAL SERVICE
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Problems solved by technology
[0003] GC-ECD determination of chloroacetic acid is very sensitive and easy to operate, so it is widely used, but its disadvantage is that there are few items that can be detected, and because GC-ECD is only qualitative by retention time, the qualitative ability is weak, when detecting actual samples It often affects the accurate judgment of the test results due to the interference peaks
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[0016] The method for analyzing chloroacetic acid in drinking water by gas chromatography-mass spectrometer of the present invention comprises the following steps:
[0017] Step 1. Add 50ml of drinking water sample to a 60ml extraction bottle, add 2ml of concentrated sulfuric acid to the extraction bottle, adjust the pH to ≤0.5, add 4g of anhydrous copper sulfate and 15g of anhydrous sodium sulfate, shake to dissolve completely, and then add 4ml of methyl tert-butyl ether containing 500ug / l internal standard 1,2 dibromopropane, and shake;
[0018] Step 2. After shaking, take the supernatant of the extraction bottle into a 40ml glass bottle, add 3ml of freshly prepared 10% sulfuric acid / methanol solution, bathe in a water bath at a temperature of 50±2°C for 2 hours, cool to room temperature and add saturated NaHCO 3 solution, until no bubbles appear when adding, then take the supernatant, and dilute to 10ml with n-hexane;
[0019] Step 3, adding 10 g of florisil to a chromato...
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The invention discloses a method for analyzing chloroacetic acid in drinking water by a gas chromatograph-mass spectrometer. The method comprises the following steps: extracting 50ml of drinking water samples, putting supernatant liquid into a 40ml glass bottle for derivatization, and setting the volume to be 10ml by adopting n-hexane; adding florisil into a chromatographic column, adding 1cm of anhydrous sodium sulfate at the top of the chromatographic column, pre-eluting the chromatographic column by using 10ml of n-hexane, removing eluent, when upper liquid level drops to the top end of the sodium sulfate layer, transferring a sample extracting solution to the chromatographic column, when the upper liquid level of the chromatographic column drops to the top end of the sodium sulfate layer again, adding 10ml of 20% ether-n-hexane, continuing to elute the chromatographic column, collecting the solution by using a 500ml K-D bottle with a 10ml concentration tube, concentrating collected fraction to be 1ml, putting the fraction into the gas chromatograph-mass spectrometer for analysis and determination, and selecting unique fragment ions of chloroacetic acid for scanning to obtain analysis results of chloroacetic acid in drinking water. The method disclosed by the invention avoids the interference caused by the introduction of interference substances in a detection process, and improves the accuracy of analysis and verification of chloroacetic acid in drinking water.
Description
technical field [0001] The invention relates to a method for analyzing chloroacetic acid in drinking water with a gas chromatography spectrometer. Background technique [0002] Haloacetic acids in drinking water are important disinfection by-products, and their toxicity and suspected carcinogenicity are of special concern, including monochloroacetic acid (MCAA), dichloroacetic acid (DCAA), trichloroacetic acid (TCAA), monobromoacetic acid (MBAA), dibromoacetic acid (DBAA), tribromoacetic acid (TBAA), monobromochloroacetic acid (BCAA), monobromodichloroacetic acid (BDCAA), dibromochloroacetic acid (DBCAA), and in practice Generally, only two chloroacetic acids, dichloroacetic acid (DCAA) and trichloroacetic acid (TCAA), are detected in the sample and are the most valued. At present, the determination of chloroacetic acid in water at home and abroad is generally based on GB / T 5750.10-2006 drinking water standard inspection method disinfection by-product index or EPA 552.3 sta...
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IPC IPC(8): G01N30/02
Inventor 凌冰黄晓栾启夏周宏明
Owner SHANGHAI BAOSTEEL IND TECHNOLOGICAL SERVICE