Method for analyzing and detecting four heterocyclic pesticides in environmental water sample
A detection method and a heterocyclic technology, applied in the directions of analyzing materials, measuring devices, material separation, etc., can solve the problems of long time, complicated extraction process, large amount of extraction agent, etc., and achieve simple operation, cheap and easy to obtain raw materials, good The effect of adsorption efficiency
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Embodiment 1
[0045] The analysis and detection method of four kinds of phenoxycarboxylic acid pesticides in the environmental water sample that embodiment relates specifically comprises the following steps:
[0046] S1. Preparation of metal-organic framework material MIL-53 and MIL-53 film:
[0047] (1) Dissolve 3g of aluminum nitrate nonahydrate in 44mL of DMF, then add 1g of terephthalic acid and 16mL of ultrapure water, and fully stir to dissolve;
[0048] (2) reacting the mixture prepared in step (1) at 110-150° C. in a solvothermal reactor for 48 hours, washing the prepared mixture in the solvothermal reactor with DMF to obtain a MIL-53 mixed solution, The metal-organic framework material MIL-53 was prepared by vacuum drying at 100° C. for 12 hours.
[0049] (3) Weigh 0.12g of MIL-53 powder. Add 5mL of acetone to dissolve. Polyvinylidene fluoride and DMF are prepared in proportion as a mixed solvent. Add 2 mL of mixed solvent to the MIL-53 solution;
[0050] (4) Apply the mixed s...
Embodiment 2
[0057] This embodiment investigates the main factors affecting the extraction recovery of four phenoxycarboxylic acid pesticides, calculates the optimum value of each factor when the extraction recovery is the highest, and then determines the four phenoxycarboxylic acid pesticides under the conditions of the optimum value of each factor. The working curve related parameters and method detection limit and precision of oxycarboxylic acid pesticides, the specific process includes the following steps:
[0058] S1, calculate the optimal value of each factor when the extraction recovery rate of four kinds of phenoxycarboxylic acid pesticides is the highest:
[0059] (1) The investigation of the amount of adsorbent to the extraction recovery
[0060] The present invention investigates the influence of the amount of MOF on the extraction recovery rate, and the invention weighs 60, 80, 100, 120, and 140 mg of metal-organic framework material MIL-53 to prepare MOF membranes, and the con...
Embodiment 3
[0077]Determination of four phenoxycarboxylic acid pesticide residues in laboratory tap water, Laoshan Reservoir in Qingdao City, and seawater. After collecting 3 kinds of water samples, filter them with fast qualitative filter paper with a pore size of 80-120 μm, and then filter with a 0.45 μm filter membrane. The filtered water sample is measured by the method described in Example 1, and the accuracy test is carried out with the method described in Example 2, and the concentrations of four kinds of heterocyclic pesticides are respectively prepared as 1 μg / L, 10 μg / L, 40 μg / L The actual water samples with low, medium and high concentrations of L were subjected to standard addition recovery test, and each concentration point was measured 3 times, and the average value, relative standard deviation and standard recovery rate of the three determinations were calculated; among them, the three kinds of water None of the four phenoxycarboxylic acid pesticides were detected in the sam...
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