Method for quantitatively detecting perfluorooctanoic acid and salts thereof in fluororubber
A technology for the quantitative detection of perfluorooctanoic acid, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of expensive instruments, difficulty in widespread promotion, and high quantitative sensitivity of the SIM method, and achieves less interference from impurities, simple derivatization steps, and reproducible results good sex effect
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Embodiment 1
[0022] 1. Instrument
[0023] American Agilent 6892-5973N GC / MS;
[0024] Porous vacuum extraction device with large volume sampling tube.
[0025] 2. Chromatographic conditions
[0026] Chromatographic column: DB-1ms 30m×0.32mm×0.10μm;
[0027] Column temperature: 100℃;
[0028] Vaporization chamber: 260℃;
[0029] Ion source: 150℃;
[0030] Quadrupole: 230℃;
[0031] Injection volume: 0.5μL, split ratio 1:10;
[0032] SIM ion: Start monitoring at m / z 59, 69, 131 at 11.8 minutes.
[0033] 3. Sample analysis
[0034] The quantitative method adopts the external standard curve method, and the external standard curve is measured with the preparation of perfluorooctanoic acid standard.
[0035] Prepare perfluorooctanoic acid standard solutions with mass concentrations of 0, 0.1, 0.5, 1.2, 3.5, and 6 mg / L, and perform GC / MS analysis after derivatization. The regression curve is as follows figure 1 As shown, the correlation coefficient is 0.9991, and the equation is as follows:
[0036] Y=24756X
[003...
Embodiment 2
[0043] Prepare 1.00mg / L perfluorooctanoic acid aqueous solution, choose CHROMABOND EASY and HR-P SPE cartridges and BESEP Carbon carbon black cartridges of Germany MN company respectively for solid phase extraction enrichment, dry the extraction cartridge with high-purity nitrogen, and use 5ml methanol The dried extraction column was eluted at a rate of 1ml / min. The eluent was collected in a headspace bottle with a volume of 10ml, and the eluent was purged with nitrogen and concentrated to 2ml. Add 0.2g analytically pure concentrated sulfuric acid to the concentrated eluate, seal it and place it in a 70°C water bath for derivatization for 60 minutes and cool. Extract with 2ml of n-hexane, make the volume constant, analyze by GC / MS, and measure the recovery rate. The results are shown in Table 2.
[0044] Table 2 Average recovery rate of solid phase extraction
[0045]
[0046] It can be seen from this example that the CHROMABOND EASY solid-phase extraction cartridge can obtain bet...
Embodiment 3
[0048] Acetyl chloride and absolute ethanol are formulated into a derivatization reagent in a volume ratio of 1:20.
[0049] Carry out 3 parallel experiments, add 10%wt analytically pure concentrated sulfuric acid to 2ml of 1.00mg / L PFOA methanol solution, seal it and place it in a 70°C water bath for derivatization for 60 minutes, and cool. Extract with 2ml n-hexane, make the volume constant, and analyze by GC / MS.
[0050] Carry out 3 parallel experiments, add 2ml acetyl chloride acidified methanol derivatization reagent to 2ml 1.00mg / L PFOA methanol solution, seal it and place it in a water bath at 70°C for 60min derivatization and cool. Extract with 2ml n-hexane, make the volume constant, and analyze by GC / MS.
[0051] The derivatization efficiency of the two different acidification systems is shown in Table 3, and the trend chart is shown as image 3 Shown.
[0052] Table 3 Derivatization efficiency of different derivatization systems
[0053]
[0054] It can be seen from Table 3 ...
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