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
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[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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