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A kind of detection method of amide compounds in environmental water samples

An amide compound and detection method technology, which is applied in the field of chemical analysis, can solve the problems of large fluctuation of standard addition recovery rate, cumbersome operation, and reduce the accuracy of detection results, and achieve stable standard addition recovery rate, ensure stability, and increase The effect of stable recovery rate

Inactive Publication Date: 2017-01-25
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using these methods, before testing the environmental water samples, it is necessary to carry out different degrees of pretreatment on the environmental water samples to meet the sampling requirements of the testing instruments. The influence of conditions is large, resulting in large fluctuations in the standard recovery rate of the existing environmental water sample detection methods, thereby reducing the accuracy of the detection results

Method used

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  • A kind of detection method of amide compounds in environmental water samples
  • A kind of detection method of amide compounds in environmental water samples
  • A kind of detection method of amide compounds in environmental water samples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] GC-MS detection of standard samples

[0052] Add 5ml standard solutions of acetochlor, alachlor, promethachlor, butachlor and pretilachlor with a concentration of 1mg / mL into different 20mL headspace vials, adjust the pH value of the solution to 10.5, add a stirring bar , add a saturated amount of sodium chloride to the solution, seal it with a gland, and age the extraction optical fiber (the coating thickness is 65 μm, and the coating material is PDMS / DVB) at the injection port of the headspace bottle at 250 ° C for 20 min , and then insert the extraction optical fiber into the headspace bottle, and then place the headspace bottle in a constant temperature water bath equipped with a magnetic stirrer for extraction. Set the stirring speed to 400 rpm, adjust the temperature of the water bath to 75°C, and control the extraction time to 40min. After the extraction was completed, the extraction optical fiber was directly inserted into the inlet of the GC-MS detector (Agile...

Embodiment 2

[0062] Establishment of standard curve

[0063] First, prepare a series of standard solutions according to the concentration in Table 2;

[0064] Table 2 Concentration table of a series of standard solutions

[0065]

[0066]

[0067]Take 5 mL of the above-mentioned standard solutions and add them to different 20 mL headspace bottles respectively, adjust the pH value of the solution to 10.5, add a stirring bar, add a saturated amount of sodium chloride to the solution, seal it with a gland, and extract the optical fiber (coated The thickness is 65 μm, and the coating material is PDMS / DVB) aging at 250°C for 20 minutes at the injection port of the headspace bottle, then inserting the extraction optical fiber into the headspace bottle, and then placing the headspace bottle at a constant temperature equipped with a magnetic stirrer Extract in a water bath. Set the stirring speed to 400 rpm, adjust the temperature of the water bath to 75°C, and control the extraction time ...

Embodiment 3

[0075] Quantitative detection of environmental water samples

[0076] Take 10ml of the environmental water sample to be tested in a centrifuge tube, centrifuge at 4000 rpm for 5min, and pass the supernatant through the water phase filter membrane to remove suspended solids. Get 5ml filtrate and add in the 20mL headspace bottle, adjust the pH value of the solution to be 10.5, add a stirring bar, add saturated amount of sodium chloride to the solution, seal with a gland, extract the optical fiber (the thickness of the coating is 65 μm, the coating The material is PDMS / DVB) aged at 250°C for 20min at the injection port of the headspace bottle, then the extraction optical fiber was inserted into the headspace bottle, and then the headspace bottle was placed in a constant temperature water bath equipped with a magnetic stirrer for extraction. Set the stirring speed to 400 rpm, adjust the temperature of the water bath to 75°C, and control the extraction time to 40min. After the ext...

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Abstract

The application belongs to the field of chemical analysis, in particular to a method for detecting amides in environmental water samples. The detection method of amide compounds in the environmental water sample provided by the application comprises the following steps: a), the environmental water sample is mixed with alkali and sodium chloride to obtain the environmental water sample to be extracted; the pH of the environmental water sample to be extracted is The value is 10-11; b), using the extraction optical fiber to perform solid-phase microextraction on the environmental water sample to be extracted to obtain an environmental water sample extraction; the temperature of the solid-phase microextraction is 70-80°C; c) . Detecting the extracted sample of the environmental water sample to obtain the type and / or content of the amide compounds contained in the environmental water sample. The present invention utilizes solid-phase microextraction to directly extract amide compounds in environmental water samples, and ensures the stability of the extraction effect by adopting appropriate extraction temperature and pH value of the extract, so that the detection method provided by the present invention has the advantages of Stable spike recovery.

Description

technical field [0001] The invention belongs to the field of chemical analysis, in particular to a method for detecting amide compounds in environmental water samples. Background technique [0002] Alachlor, acetochlor, pretilachlor, butachlor, and propachlor are the five most commonly used and important amide herbicides. Their efficacy is not limited by geographical and climatic conditions, and they are mainly used in corn. , Soybean, cotton, wheat, rice, peanut and other crop fields have been widely used in our country in recent years. [0003] Although these amide herbicides have excellent herbicidal properties, they also have the disadvantages of direct toxicity, low volatility, low photolysis, and easy residue. With the extensive use of amide herbicides in my country, a large number of them remain in lakes and ponds, causing mass death of fish and frogs, and posing a huge potential threat to humans and the ecological environment. According to the difference in structu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 刘宝峰李俊玲
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI