Method for determining trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water

A technology of dimethylnitrosamine and disinfection by-products, which is applied in the field of determination of trace nitrogen-containing disinfection by-products of dimethylnitrosamine in water, can solve the problems of complex operation steps, reduced detection cycle, long detection cycle, etc. Achieve the effects of improving extraction efficiency, reducing matrix interference, and shortening the detection cycle

Active Publication Date: 2012-06-27
TONGJI UNIV
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Problems solved by technology

[0004] Aiming at problems such as low recovery rate, long detection period and complicated operation steps of the current conventional detection method, the purpose of the present invention is to provide a method for measuring trace amounts of nitrogen-containing disinfection by-product nitrosamine dimethyl (NDMA) in water; The method is simple to operate, has high measurement accuracy, and can effectively reduce the detection cycle

Method used

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  • Method for determining trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water
  • Method for determining trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water
  • Method for determining trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water

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Embodiment 1

[0033] The water sample was Mill-Q water (ultrapure water). In 12 groups of 500mL Mill-Q water (ultrapure water), NDMA standard was added so that the NDMA concentration was 1 μg / L. Since the water sample has no suspended solids and particulate impurities, it does not need to be filtered.

[0034] Acidification pretreatment method: use sodium hydroxide or sulfuric acid to adjust the pH value of 12 groups of water samples to be tested to 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, and The water samples were placed in brown bottles and stored in a dark place.

[0035] Acidification, drying and filling of solid phase extraction materials; wood powder activated carbon used for solid phase extraction, with an average particle diameter of ≤40μm, is acidified with sulfuric acid water with a pH of 2.3, and the wood powder activated carbon is dried in an oven at 105°C after acidification dry; use a balance to take 1g of dried wood powder activated carbon and fill it into a 6mL solid-phase e...

Embodiment 2

[0043] The water sample was Mill-Q water (ultrapure water). NDMA standard was added to 5 groups of 500mL Mill-Q water (ultrapure water), so that the NDMA concentration was 1 μg / L, and the pH value of the water sample was 7, so the water sample did not need to be filtered and adjusted for pH.

[0044] Acidification pretreatment method: take 500mL water sample, put the water sample in a brown bottle and store it in a dark place.

[0045] Acidification, drying and filling of solid phase extraction materials; wood powder activated carbon used for solid phase extraction, with an average particle diameter of ≤40μm, is acidified with sulfuric acid water with a pH of 2.3, and the wood powder activated carbon is dried in an oven at 105°C after acidification Dry. Weigh 1g of dried wood powder activated carbon with a balance and fill it into a 6mL solid-phase extraction (SPE) column of high molecular weight polyethylene. The sieve plate is made of ultra-high molecular weight polyethylen...

Embodiment 3

[0055] figure 1 It is the operation flowchart of the embodiment of the present invention. The water sample is surface water. Preparation process before extraction: first filter each water sample in the water purification process through a cellulose acetate membrane with a pore size less than or equal to 0.45 μm to filter out suspended solids and particulate impurities, and the water samples in the water purification process are weakly acidic. Acidification pretreatment method: Take 500mL of the filtered water sample, place it in a brown bottle and take dark measures, use sodium hydroxide to adjust the pH value of the water sample to be tested to 7, and store it in the dark.

[0056] Acidification, drying and filling of solid phase extraction materials; wood powder activated carbon used for solid phase extraction, with an average particle diameter of ≤40μm, is acidified with sulfuric acid water with a pH of 2.3, and the wood powder activated carbon is dried in an oven at 105°C...

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Abstract

The invention belongs to the environmental protection and water treatment technical field, and discloses a method for determining trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water. The method comprises the following steps 1) acidifying and pretreating a sample; 2) acidifying, drying and filling a solid phase extraction material; 3) controlling a solid phase extraction process, eluting and purifying an eluate; 4) naturally volatilizing the sample and controlling with constant volume; 5) using a liquid chromatography-mass spectrometry for analyzing dimethyl nitrosamine to obtain the determination result. Compared with the current international test methods, the method of the invention has the characteristics of rapidity, simpleness, little application amount of the poisonous and harmful organic solvent, accurate analysis and the like.

Description

technical field [0001] The invention belongs to the technical field of environmental protection and water treatment, and relates to a method for measuring trace nitrogen-containing disinfection by-product nitrosamine dimethyl (NDMA) in water. Background technique [0002] Nitrosamine dimethyl (NDMA) is a new chlorinated disinfection byproduct widely detected in drinking water in the United States and Canada recently. NDMA in water was first discovered in 1989 in a tap water plant that used chloramine disinfection in Ohsweken District, Ontario, Canada, and then NDMA was also detected in several other water plants that used the same disinfection process. At present, there are reports of NDMA detection in water plants in the United States, Canada, and Europe. The survey found that the substance was detected in water plants using combined chlorine disinfection, even in water plants using ion exchange technology [Choi J, Valentine R L. Formation of N-nitrosodimethylamine (NDMA) ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 覃操徐斌徐倩李冕夏圣骥高乃云
Owner TONGJI UNIV
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