Quantitative detection method of pentachlorophenol in soil
A quantitative detection method, the technology of pentachlorophenol, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of complex derivatization process, high polarity of pentachlorophenol, low vapor pressure, etc., and achieve low toxicity and stable recovery rate , the effect of less reagent
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Embodiment 1
[0037] Embodiment 1: Extraction and purification of PCP in soil
[0038] 1) Extraction of PCP
[0039] Accurately weigh 2.0 g of the soil sample and place it in a 30 mL centrifuge tube, add 2 mL of sulfuric acid with a concentration of 6 mol / L, add 10 mL of acetonitrile and shake and mix on a vortex mixer, then add 2 mL of n-hexane, and shake and mix evenly. Shake on a shaker for 30 minutes, ultrasonic at 40°C for 1 hour, centrifuge at 5000 r / min for 5 minutes, and wait for purification.
[0040] 2) Purification of the extract
[0041] Weigh 20mg ODSC 18 1. Put 200mg of anhydrous magnesium sulfate in a 15mL centrifuge tube, and vortex to mix. Take 2 mL of the extract to be purified, add it into the mixed purification system, mix on a vortex for 2 min, and centrifuge at 9000 r / min for 5 min. Take 1 mL of the supernatant and pass it through a 0.45 μm filter membrane for determination on the machine.
Embodiment 2
[0042] Embodiment 2: the selection of high performance liquid chromatography (HPLC) condition of the present invention and working curve
[0043] The standard solutions were prepared with chromatographic standard substances from DR. Ehrenstorfer Company in Germany, and they were respectively prepared into methanol standard series and matrix standard series. Assay by HPLC.
[0044] 1) HPLC determination conditions
[0045] Chromatographic column: Agilent5 m SB-C 18 Reversed-phase column, 4.6×250mm;
[0046] Mobile phase: 85% methanol + 15% water containing 0.1% glacial acetic acid, using isocratic elution for 10 minutes. The flow rate is 1.0mL / min;
[0047] Injection volume: injection volume 10L;
[0048] Column temperature: 35°C;
[0049] Detector: ultraviolet detector (DAD), detection wavelength 225nm.
[0050] 2) Selection of working curve
[0051] The substrate solution is prepared from soil through the above-mentioned pretreatment method. Prepare standard concentr...
Embodiment 3
[0052] Embodiment 3: the minimum detection limit and the linear range of the detection method of the present invention
[0053] Prepare the standard concentration with matrix solution as 0.0500mg / L, 0.100mg / L, 0.200mg / L, 0.500mg / L, 1.00mg / L, 2.00mg / L, 5.00mg / L, 10.0mg / L, 20.0mg / L The PCP standard series of L was measured on the machine. Get standard curve y=7.53x+1.28, R=0.9995, R 2 =0.9991, the linear range is 0.1-20mg / L.
[0054] According to the optimized pre-treatment and instrument conditions, continuously measure 7 same low-concentration spiked samples, using the formula MDL=S×t (n-1,1-a=0.99) , to calculate the detection limit of the method. Among them, MDL is the detection limit of the method, t is the value when the confidence level is 99%, and the degree of freedom is n-1, and S is the standard deviation of the concentration of n spiked determinations. Obtained through table lookup and calculation, S=0.45g / g, t=3.14, n=7, and MDL=1.413g / g obtained by substitution...
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