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首页> 外文OA文献 >Gas chromatographic electron capture negative ionization mass spectrometric (GC/ECNI/MS) determination of unique fluorinated compounds in the sediments of Lake Ontario and the effect of high-boiling alcohols (as injection solvents) on chromatographic behaviour of polycyclic aromatic hydrocarbons in gas chromatography
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Gas chromatographic electron capture negative ionization mass spectrometric (GC/ECNI/MS) determination of unique fluorinated compounds in the sediments of Lake Ontario and the effect of high-boiling alcohols (as injection solvents) on chromatographic behaviour of polycyclic aromatic hydrocarbons in gas chromatography

机译：气相色谱电子捕获负离子化质谱（GC / ECNI / ms）测定安大略湖沉积物中独特的氟化物及高沸点醇（作为注入溶剂）对气相色谱中多环芳烃色谱行为的影响

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Part I - Fluorinated CompoundsA method has been developed for the extraction, concentration, anddetermination of two unique fluorinated compounds from the sediments of LakeOntario. These compounds originated from a common industrial landfill, andhave been carried to Lake Ontario by the Niagara River. Sediment samples fromthe Mississauga basin of Lake Ontario have been evaluated for these compoundsand a depositional trend was established. The sediments were extracted byaccelerated solvent extraction (ASE) and then underwent clean-up, fractionation,solvent exchange, and were concentrated by reduction under nitrogen gas. Theconcentrated extracts were analyzed by gas chromatography - electron capturenegative ionization - mass spectrometry.The depositional profile determined here is reflective of the operation of thelandfill and shows that these compounds are still found at concentrations wellabove background levels. These increased levels have been attributed to physicaldisturbances of previously deposited contaminated sediments, and probablecontinued leaching from the dumpsite.Part II - Polycyclic Aromatic HydrocarbonsGas chromatography/mass spectrometry is the most common method forthe determination of polycyclic aromatic hydrocarbons (PAHs) from variousmatrices. Mass discrimination of high-boiling compounds in gas chromatographicmethods is well known. The use of high-boiling injection solvents showssubstantial increase in the response of late-eluting peaks. These solvents have anincreased efficiently in the transfer of solutes from the injector to the analyticalcolumn. The effect of I-butanol, I-pentanol, cyclopentanol, I-hexanol, tolueneand n-octane, as injection solvents, was studied.Higher-boiling solvents yield increased response for all PAHs. I -Hexanolis the best solvent, in terms of P AH response, but in this solvent P AHs were moresusceptible to chromatographic problems such as peak splitting and tailing.Toluene was found to be the most forgiving solvent in terms of peak symmetryand response. It offered the smallest discrepancies in response, and symmetryover a wide range of initial column temperatures.
机译：第一部分-氟化物已开发出一种方法，用于从安大略湖的沉积物中提取，浓缩和测定两种独特的氟化物。这些化合物起源于一个普通的工业垃圾填埋场，并已被尼亚加拉河带到安大略湖。已经评估了安大略湖密西沙加盆地的沉积物样品中的这些化合物，并确定了沉积趋势。沉淀物通过加速溶剂萃取（ASE）进行萃取，然后进行净化，分馏和溶剂交换，然后在氮气下还原浓缩。通过气相色谱-电子捕获负离子化-质谱法对浓缩的提取物进行分析。此处确定的沉积曲线反映了垃圾填埋场的运行情况，表明这些化合物的浓度仍高于背景水平。这些增加的水平归因于先前沉积的受污染沉积物的物理扰动，以及从垃圾场可能继续浸出。第二部分-多环芳烃气相色谱/质谱法是测定各种基质中多环芳烃（PAHs）的最常用方法。气相色谱法中高沸点化合物的质量区分是众所周知的。高沸点进样溶剂的使用显示后期洗脱峰的响应显着增加。这些溶剂有效地增加了溶质从进样器到分析柱的转移。研究了异丁醇，异戊醇，环戊醇，异己醇，甲苯和正辛烷作为注射溶剂的作用，高沸点溶剂对所有PAH的响应均增加。就P AH反应而言，I-己醇是最佳溶剂，但在这种溶剂中，P AH对色谱问题（如峰分裂和拖尾）更敏感。就峰的对称性和响应而言，甲苯是最宽容的溶剂。它在宽范围的初始色谱柱温度范围内提供了最小的响应差异和对称性。

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