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Direct ToF-SIMS analysis of organic halides and amines on TLC plates

机译:TLC板上的有机卤化物和胺类的直接ToF-SIMS分析

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It has been reported that: "direct analysis of thin layer chromatography (TLC) plates with secondary ion mass spectrometry (SIMS) yields no satisfactory results" (J. Chromatogr. A 1084 (2005) 113-118). While this statement appears to be true in general, we have identified two important classes of compounds, organic halides and amines, that appear to yield to such direct analyses. For example, five organic halides with diverse structures were eluted on normal phase TLC plates. In all cases the halide signals in the negative ion time-of-flight secondary ion mass spectrometry (ToF-SIMS) spectra were notably stronger than the background signals. Similarly, a series of five organic antines with diverse structures were directly analyzed by positive ion ToF-SIMS. In all but one of the spectra characteristic, and sometimes even quasi-molecular ions, were observed. Most likely, the good halide ion yields are largely a function of the electronegativity of the halogens. We also propose that direct analysis of amines on normal phase silica gel is facilitated by the acidity, i.e., proton donation, of surface silanol groups. (c) 2006 Elsevier B.V. All rights reserved.
机译:据报道:“用二次离子质谱法(SIMS)直接分析薄层色谱(TLC)板没有令人满意的结果”(J.Chromatogr.A 1084(2005)113-118)。虽然这种说法总的来说似乎是正确的,但我们已经确定了两种重要的化合物,即有机卤化物和胺,它们似乎可以直接进行此类分析。例如,在正相TLC板上洗脱了五种结构不同的有机卤化物。在所有情况下,负离子飞行时间二次离子质谱(ToF-SIMS)光谱中的卤化物信号明显强于背景信号。同样,通过正离子ToF-SIMS直接分析了一系列五个具有不同结构的有机安替尼。除了其中一个光谱特征外,其他所有光谱特征均被观察到,有时甚至是准分子离子。良好的卤化物离子产率很可能很大程度上取决于卤素的电负性。我们还建议通过表面硅烷醇基团的酸度(即质子给体)促进在正相硅胶上直接分析胺。 (c)2006 Elsevier B.V.保留所有权利。

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