Method for detecting organochlorine pesticide in soil
A detection method and organochlorine technology, applied in the field of analysis and detection, can solve the problems of expensive instruments and equipment, low analyte concentration, short operation time, etc., and achieve the effects of high efficiency, accurate qualitative and quantitative, and less solvent.
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[0030] Example 1
[0031] 1.1 Blank soil sample preparation
[0032] Collect a batch of soil near the drinking water source to remove impurities such as grass roots and gravel, put it on a sample pan, spread it to a thickness of about 20mm, freeze-dry, pass through a 60-mesh sieve and grind evenly to obtain a soil sample to be tested. The traditional method of rapid solvent extraction-solid phase extraction cartridge purification was used to test the 8 organochlorine pesticides in the samples, and the soil samples with the detection concentration lower than the detection limit of the method were selected as the blank soil samples to be tested.
[0033] 1.2 Preparation of the spiked soil for testing
[0034] Accurately weigh 50.0g of the blank soil to be tested, add 10mL of the standard solution of 8 kinds of organochlorine pesticides in n-hexane with a concentration of 1.0mg / L, then add 10mL of n-hexane solvent to immerse the soil, stir under a fume hood to make the mixture uniform, ...
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[0037] Example 2
[0038] This application also tested the optimization of chromatographic conditions and the selection of internal standard substances of the above detection method, and the test results are as follows.
[0039] 2.1 Optimization of chromatographic conditions
[0040] The purpose of optimizing the chromatographic conditions is to make the separation and detection time the shortest and the best effect, while maximizing the detection sensitivity of the chromatogram. According to the principle of similar compatibility, since the organochlorine pesticides are all weakly polar substances, the HP-5 capillary column is selected. The gas chromatogram of 8 kinds of organochlorine pesticide standard mixed solutions is as follows figure 2 As shown, the experimental results show that under the chromatographic conditions, the target compound and the internal standard substance can be separated well, which can meet the experimental requirements.
[0041] 2.2 Selection of internal...
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[0043] Example 3
[0044] This application also tested the above detection methods. By examining the type of dispersant, eluent and elution volume, and the ratio of sample to dispersant, the recovery rate and standard deviation of organochlorine pesticides under different conditions were measured. The test results are as follows.
[0045] 3.1 Drawing of standard curve
[0046] Using n-hexane as the solvent, accurately pipette the stock solutions of 8 kinds of mixed organochlorine pesticides and prepare them into standard solutions with concentrations of 50, 100, 150, 200, 250 μg / L, and add 80 ppb 13 C 12 -PCB-153 is used as the internal standard, draw the standard curve with the concentration ratio as the abscissa and the peak area value as the ordinate. The calculated standard curve equation and correlation coefficient are shown in Table 1. From the data in Table 1, it can be seen that at 50 The linear correlation of 8 kinds of organochlorine pesticides in the mass concentration ran...
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