Method for adsorbing and desorbing six phenoxy carboxylic acid herbicides in water with nitrate-type layered double hydroxides (LDHS) adsorbent

A technology of phenoxycarboxylic acid and hydrotalcite, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of easy operation, good dispersion and high adsorption capacity

Inactive Publication Date: 2016-10-12
丁立平 +1
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  • Application Information

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Problems solved by technology

[0008] In view of the current lack of high-efficiency adsorbents for phenoxycarboxylic acid herbicides in water and their application methods, the purpose of the present invention is to use nitrate-type hydrotalcite as an adsorbent to provide its ability to treat six phenoxycarboxylic acid herbicides in water. Adsorption and desorption methods

Method used

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  • Method for adsorbing and desorbing six phenoxy carboxylic acid herbicides in water with nitrate-type layered double hydroxides (LDHS) adsorbent
  • Method for adsorbing and desorbing six phenoxy carboxylic acid herbicides in water with nitrate-type layered double hydroxides (LDHS) adsorbent
  • Method for adsorbing and desorbing six phenoxy carboxylic acid herbicides in water with nitrate-type layered double hydroxides (LDHS) adsorbent

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preparation example Construction

[0031] a) The preparation method of nitrate-type hydrotalcite adsorbent: get 190g magnesium nitrate (0.04mol) and 93g aluminum nitrate (0.02mol) and dissolve in 500mL deionized water that removes carbon dioxide, get 79g sodium hydroxide (0.12mol) and dissolve in Add 500mL of deionized water with carbon dioxide removed dropwise into the three-necked bottle, stir vigorously under the protection of nitrogen, adjust the drop rate to keep the pH value at about 10, and crystallize the obtained colloidal solution at 75°C for 20h after the dropwise addition , suction filtration, the filter cake was washed with hot water until pH<8, and dried in vacuum to obtain nitrate-type hydrotalcite.

[0032] b) Acetonitrile, formic acid, ammonium formate: chromatographically pure; water is grade 1 water in accordance with GB / T 6682.

[0033] c) Solid standard substances of six phenoxycarboxylic acid herbicides: purity greater than or equal to 98.0%, Dr. Ehrenstorfer Company, Germany.

[0034] d)...

Embodiment 1

[0044] (1) Adjust the pH value of the aqueous solution

[0045] Accurately pipette 1.0mL of the above stock solution (accurate to 0.01mL), dilute to 100.0mL with tap water to obtain six phenoxycarboxylic acid herbicide aqueous solutions with a concentration of 10mg / L, and adjust its pH to 4.0, airtight and marked, take the liquid and filter it to be analyzed by high performance liquid chromatography.

[0046] (2) Adsorption

[0047] Weigh 0.2g of nitrate-type hydrotalcite in a 50mL centrifuge tube, take 10.0mL of the above diluted solution, vortex for 3min, shake for 10min, centrifuge at 4500r / min for 3min, take 1.0mL of the supernatant and filter it for HPLC spectrum analysis.

[0048] (3) washing

[0049] Add 10 mL of deionized water to the above centrifuge tube, vortex for 3 min, shake for 10 min, centrifuge at 4500 r / min for 5 min, and discard the supernatant;

[0050] (4) Desorption

[0051] Add 2.00mL of disodium hydrogen phosphate solution with a concentration of 0...

Embodiment 2

[0058] (1) Adjust the pH value of the aqueous solution

[0059] Accurately pipette 2.0mL of the above-mentioned stock solution (accurate to 0.01mL), and use well water as the diluent to set the volume to 100.0mL to obtain six kinds of phenoxycarboxylic acid herbicide aqueous solutions with a concentration of 20mg / L, and adjust its pH to To 10.0, airtight, marked with a mark, take the liquid and filter it for HPLC analysis.

[0060] (2) Adsorption

[0061] Weigh 0.4g of nitrate-type hydrotalcite in a 50mL centrifuge tube, take 10.0mL of the above diluted solution, vortex for 3min, oscillate for 15min, centrifuge at 2500r / min for 3min, take 1.0mL of supernatant and filter it for HPLC spectrum analysis.

[0062] (3) washing

[0063] Add 10 mL of deionized water to the above centrifuge tube, vortex for 3 min, shake for 15 min, centrifuge at 3500 r / min for 3 min, and discard the supernatant;

[0064] (4) Desorption

[0065] Add 2.00 mL of disodium hydrogen phosphate solution w...

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Abstract

The invention relates to a method for adsorbing and desorbing six phenoxy carboxylic acid herbicides in water with a nitrate-type layered double hydroxides (LDHS) adsorbent. Aiming at the problem that an efficient adsorbent for phenoxy carboxylic acid herbicides in water and an application method of the efficient adsorbent are unavailable at present, the method adopting nitrate-type LDHS as an adsorbent and used for adsorbing and desorbing the six phenoxy carboxylic acid herbicides in water through the steps of regulation of the pH value of a water sample, adsorption through a dispersive solid-phase extraction method, washing with deionized water, desorption with a disodium hydrogen phosphate desorbent, and the like is created. The selected nitrate-type LDHS adsorbent is good in dispersity in an aqueous solution and has an efficient adsorption capability for the six phenoxy carboxylic acid herbicides; adsorption and desorption are carried out through a dispersive solid-phase extraction method, the operation is simple, convenient, easy, fast and efficient; meanwhile, no organic solvent is needed for adsorption and desorption, so that the method accords with the idea of environmental friendliness.

Description

technical field [0001] The invention belongs to the field of adsorbent application in analytical chemistry, and more specifically relates to a method for adsorbing and desorbing six kinds of phenoxycarboxylic acid herbicides in water by a nitrate-type hydrotalcite adsorbent. Background technique [0002] my country's mandatory standard "GB 5749-2006 Drinking Water Standard" has made strict regulations on the limit value of herbicide residues, including a variety of phenoxycarboxylic acid herbicides. Phenoxycarboxylic acid herbicides represented by 2,4-D are the second most selective herbicides in agricultural production, and are widely used in paddy fields, non-cultivated lands, pastures, etc. These herbicides are soluble in water in the form of anions, and can diffuse rapidly after application, and pollute people's water sources with the transfer of water bodies. With the increasing amount and scope of use, such substances have become an important factor in the safety of d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 丁立平蔡春平许仁杰吴文凡
Owner 丁立平
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