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Extraction and quantitative analysis of water, sediment, soil and biosolids for trace-level trimethylsilanol

机译:痕量三甲基硅烷醇的水,沉积物,土壤和生物固体的提取和定量分析

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摘要

Methylsilanols such as trimethylsilanol (TMS) are considered as the major hydrolytic degradation products of methylsiloxanes, a class of anthropogenic organometallic substances with a wide range of applications. The distribution of these silanols in various environmental compartments, therefore, could provide direct information on silanols' chemical fate and environmental exposure. Existing methods for the quantification of the silanols are not sensitive and robust enough for analyzing environmental media where trace- and ultra-trace-level concentrations may be expected. In the present study, solid-phase extraction (SPE) and solvent extraction in combination with gas chromatography-mass spectrometry (GC/MS) were tested for analyzing water, sediment, soil and biosolids samples for TMS. ISOLUTE (R) ENV+ solid-phase sorbent was found to be most suitable for extraction of water samples for ultra-trace TMS, while direct solvent extraction worked for solids samples such as soil, sediment and biosolids. Coupling with an isotopic internal standard and SPE extraction, direct GC/MS analysis without derivatization can reach a method detection limit for TMS as low as 0.10 mu g L-1 in water. The detection limits for solid samples varied from 0.21 ng g(-1) ww (wet weights) to 10 ng g(-1) ww, mostly limited by background concentrations of TMS in extraction solvents. It was also observed that prolonged sample storage may lead to a reduction in TMS concentrations, regardless of the concentrations of coexisting methylsiloxanes.
机译:甲基硅烷醇(例如三甲基硅烷醇(TMS))被认为是甲基硅氧烷的主要水解降解产物,甲基硅氧烷是一类具有广泛应用的人为有机金属物质。因此,这些硅烷醇在各种环境室中的分布可以提供有关硅烷醇的化学命运和环境暴露的直接信息。现有的硅烷醇定量方法不够灵敏且不够稳健,无法分析可能需要痕量和超痕量浓度的环境介质。在本研究中,测试了固相萃取(SPE)和溶剂萃取结合气相色谱-质谱(GC / MS)来分析水,沉积物,土壤和生物固体样品中的TMS。已发现ISOLUTE ENV +固相吸附剂最适合用于超痕量TMS的水样品的萃取,而直接溶剂萃取适用于土壤,沉积物和生物固体等固体样品。结合同位素内标和SPE萃取,无需衍生化的直接GC / MS分析就可以达到水中TMS的方法检测极限,低至0.10μg L-1。固体样品的检出限从0.21 ng g(-1)ww(湿重)到10 ng g(-1)ww不等,主要受萃取溶剂中TMS的背景浓度限制。还观察到,不管共存甲基硅氧烷的浓度如何,延长的样品存储时间都可能导致TMS浓度降低。

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