二氧化矽奈米顆粒的優異物化特性，使其被廣泛應用在民生用品及工業製程。其中一項應用是將二氧化矽奈米顆粒作為半導體工業中化學機械研磨製程的研磨漿液主成分，該製程會排放大量含有二氧化矽奈米顆粒的研磨廢水。已有研究表明二氧化矽奈米顆粒可能導致潛在的(生態)毒理效應，但關於二氧化矽奈米顆粒的環境暴露資訊仍相當缺乏，因此迫切需要建立可以鑑定水環境中的二氧化矽奈米顆粒的檢測方法。
本研究的目的在於開發尺寸排除層析法串聯感應耦合電漿質譜儀方法與單顆粒式感應耦合電漿質譜儀方法，並評估其用於鑑定水環境中二氧化矽奈米顆粒的可行性。將兩根TSKgel G5000PWXL管柱與感應耦合電漿質譜儀相串聯，並以1% FL-70 (v/v) (pH = 11)作為流洗液，這是一種離子型與非離子型界面活性劑的混合物，流速控制在0.25 mL/min，直徑20、50及80 nm的二氧化矽顆粒混合物可以被流洗出來，質量偵測極限約為2.5 mg/L，其粒徑分布與動態光散射的鑑定結果相符；藉由使用微米級取樣時間(100、50及25微米)，單顆粒式感應耦合電漿質譜儀方法可在不外加反應氣體的條件下偵測到直徑200 nm及300 nm的二氧化矽顆粒，質量偵測極限約為1.11-3.75 μg/L。為了評估兩方法的實際應用可行性，我們以兩方法分析光電業的化學機械研磨製程廢水，並與動態光散射分析結果進行交互比對，單顆粒式感應耦合電漿質譜儀方法分析結果顯示廢水中二氧化矽顆粒的平均粒徑為368.6 ± 13 nm，而尺寸排除層析法串聯感應耦合電漿質譜儀方法則未偵測到二氧化矽顆粒，結果顯示廢水中的二氧化矽顆粒多非奈米級。整體而言，單顆粒式感應耦合電漿質譜儀方法無法偵測奈米級二氧化矽顆粒，但有較低的質量偵測極限(μg/L)；尺寸排除層析法串聯感應耦合電漿質譜儀方法可以偵測奈米級二氧化矽顆粒，但有較高的質量偵測極限(mg/L)。

Due to their extrordinary physic-chemical properties, silica nanoparticles (SiO2NPs) offers economic and technical benefit for wide applications. One primary use of SiO2NPs is chemical mechanical planarization (CMP) process in semiconductor manufacturing where SiO2NPs are used as abrasives to polish silicon wafers. There have been existing research showing that SiO2NPs could lead to potential (eco)toxicity, but the information regarding the exposure of SiO2NPs is largely absent. There is an urgent need to establish detection methods that can characterize SiO2NPs in aqueous matrices and waste streams.
The objective of the study was to develop and compare two methods, namely size exclusion chromatography (SEC) hyphenated to inductively coupled plasma mass spectrometry (ICP-MS) and single particle-ICP-MS (spICP-MS), in the characterization of SiO2NPs in aqueous environments. For the optimal SEC-ICP-MS method developed, by using two TSKgel G5000PWXL columns in series, and 1% FL-70 (v/v) (pH = 11) at flow rate of 0.25 mL/min, SiO2NPs mixture of 20 nm, 50 nm, and 80 nm diameter were eluted with satisfactory size separation resolution and the mass detection limit is about 2.5 mg/L. The size distribution analyzed by SEC-ICP-MS agreed with that obtained from dynamic light scattering (DLS) analysis. As for spICP-MS, microsecond dwell times (100 μs, 50 μs, and 25 μs) allowed for the characterization of 200 nm and 300 nm diameter SiO2 particles without reaction gas, and the mass detection limit is about 1.11-3.75 μg/L. To further evaluate the utility of both methods, a CMP wastewater from the semiconductor manufacturer in southern Taiwan was analyzed and compared with the result obtained by DLS. The spICP-MS analysis shows that the mean size of SiO2 particles is 368.6 ± 1.3 nm, and SEC-ICP-MS can not detecte the SiO2 particles. The result demonstrates that most of SiO2 particles in the CMP wastewater is not nano-sized. Overall, spICP-MS can not detect nano-sized SiO2, and the mass detection limit is low level (μg/L). SEC-ICP-MS can detect SiO2NPs, and the mass detection limit is high level (mg/L).

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