A kind of detection method of perfluorinated compound in soil and sediment
A technology of perfluorinated compounds and detection methods, applied in the field of detection of perfluorinated compounds in soil and sediments, can solve the problems of low content, complex soil matrix, difficult determination and quantification of extractable organic fluorine, etc., and achieve a large detection range, The effect of high selectivity and sensitivity and shortened extraction time
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Embodiment 1
[0044] The detection method of perfluorinated compounds in soil and sediment described in the present invention, comprises the following steps,
[0045] (1) Pretreatment: pick out the organic residues in the soil and sediment, freeze-dry, grind and pass through a 50-mesh sieve to obtain sample powder, store it in a freezer at -20°C, and store it for later use;
[0046] (2) Extraction:
[0047] In the first stage of extraction, weigh 1g of the pretreated sample powder and place it in a polypropylene or polyethylene centrifuge tube, add 2.0ng of isotope-labeled compound, then add methanol, vortex for 1min and let it stand for 30min, then put it in a water bath at 50°C Ultrasonic extraction for 10 minutes, the ultrasonic power is 350w, and then centrifuged at a speed of 5000r / min for 15 minutes, the supernatant is collected and placed in a collection container, and the lower layer of slag is left in a centrifuge tube. The isotope-labeled compound is 13 C 4 -PFOA, 13 C 4 -PFOS...
Embodiment 2
[0054] The detection method of perfluorinated compounds in soil and sediment described in the present invention, comprises the following steps,
[0055] (1) Pretreatment: remove the organic residues in the soil and sediment, freeze-dry, grind and pass through a 60-mesh sieve to obtain sample powder, store at -20°C for later use;
[0056] (2) Extraction:
[0057] In the first stage of extraction, weigh 1g of the pretreated sample powder and place it in a polypropylene or polyethylene centrifuge tube, add 2.0ng of the isotope-labeled compound, then add the extractant methanol, vortex for 1min, let stand for 30min, and then 55℃ Ultrasonic extraction in a water bath for 15 minutes, the ultrasonic power is 340w, and then centrifuged at a speed of 5000r / min for 15 minutes, the supernatant is collected and placed in a collection container, and the lower layer of slag is left in a centrifuge tube. The isotope-labeled compound is 13 C 4 -PFOA, 13 C 4 -PFOS, 13 C 2 -PFDA,d 5 -NEt...
Embodiment 3
[0066] The detection method of perfluorinated compounds in soil and sediment described in the present invention, comprises the following steps,
[0067] (1) Pretreatment: pick out the organic residues in the soil and sediment, freeze-dry, grind and pass through a 50-mesh sieve to obtain sample powder, store it in a freezer at -20°C, and store it for later use;
[0068] (2) Segmented extraction:
[0069] In the first stage of extraction, weigh 1g of the pretreated sample powder and place it in a polypropylene or polyethylene centrifuge tube, add 2.0ng of the isotope-labeled compound, then add the extractant acetone, vortex for 1min, let stand for 30min, and then 60℃ Ultrasonic extraction in water bath for 20min, ultrasonic power 330w, centrifuge at 5000r / min for 15min, collect the supernatant and put it in the collection container, leave the lower layer of slag in the centrifuge tube, the isotope labeled compound is 13 C 4 -PFOA, 13 C 4 -PFOS, 13 C 2 -PFDA,d 5 -NEtFOSAA,...
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