G Batley SETAC Berlin 2012 4 SEMFFFICPMS Scanning
環境樣品流向圖 G. Batley, SETAC Berlin 2012 4
現行奈米銀檢測常用 SEM、FFF-ICP-MS • 掃描式電子顯微鏡(Scanning Electron Microscope, SEM) • 場流分離-感應耦合電漿質譜儀 (Field-Flow Fractionation and Inductively Coupled Plasma Mass Spectrometry, FFF-ICP-MS)進行分析 • 儀器成本高、操作與分析困難度也相對高。 8
FFF-ICP-MS 10
離子濃度 100, 000 particle / m. L = 100, 000 particle / L 20 nm NP-Ag = 4/3(10 nm*10 nm)*π Þ 4. 19 X 10 -18 cm 3 Ag的密度=10. 5 g/cm 3 Þ 1個20 nm銀奈米 = 4. 39 X 10 -17 g 100, 000 particle /L = 4. 39 ng/L=4. 39 ppt 12
SP-ICP-MS基礎原理-1 Steady-state Signal Particle Size Information Individual Signal Events 14
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SP-ICP-MS基礎原理-2 Sample flow rate (m. L/min) NP concentration (particles/m. L) Compute this for Ag NP standard Observed pulse frequency (particles/min) Efficiency term Solve for this 19
SP-ICP-MS基礎原理-3 20
SP-ICP-MS基礎原理-3 Pace et al. 2011, Anal. Chem, 83, 9361 -9369; Pace et al 2012, ES&T, 46, 12272 -12280 21
分析條件 Perkin. Elmer Nex. ION 300 d 22
Ion Calibration Curve 23
特製樣品結果-3天後 Sample Analyte Most Freq. Size (nm) Sample Ag 106. 905 30 Mean Size Mean Inten. Part. Conc. No. of Peaks (nm) (counts) (parts/m. L) 36 181 17. 02 3514 Diss. Inten. (counts) Diss. Conc. (ppb) 0. 04 0. 106 30
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