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纳米机械取样材料进行纳米尺度质谱化学分析。

Nanomechanical sampling of material for nanoscale mass spectrometry chemical analysis.

机构信息

Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, TN, 37831-6493, USA.

University of Tennessee, Knoxville, Knoxville, TN, 37996, USA.

出版信息

Anal Bioanal Chem. 2021 Apr;413(10):2747-2754. doi: 10.1007/s00216-020-02967-0. Epub 2020 Oct 6.

Abstract

The ability to spatially resolve the chemical distribution of compounds on a surface is important in many applications ranging from biological to material science. To this extent, we have recently introduced a hybrid atomic force microscopy (AFM)-mass spectrometry (MS) system for direct thermal desorption and pyrolysis of material with nanoscale chemical resolution. However, spatially resolved direct surface heating using local thermal desorption becomes challenging on material surfaces with low melting points, because the material will undergo a melting phase transition due to heat dissipation prior to onset of thermal desorption. Therefore, we developed an approach using mechanical sampling and collection of surface materials on an AFM cantilever probe tip for real-time analysis directly from the AFM tip. This approach allows for material to be concentrated directly onto the probe for subsequent MS analysis. We evaluate the performance metrics of the technique and demonstrate localized MS sampling from a candelilla wax matrix containing UV stabilizers avobenzone and oxinoxate from areas down to 250 nm × 250 nm. Overall, this approach removes heat dissipation into the bulk material allowing for a faster desorption and concentration of the gas phase analyte from a single heating pulse enabling higher signal levels from a given amount of material in a single sampling spot.Graphical abstract.

摘要

在许多应用领域,包括生物和材料科学,对表面化合物的化学分布进行空间分辨的能力都非常重要。为此,我们最近开发了一种混合原子力显微镜(AFM)-质谱(MS)系统,用于对材料进行纳米级化学分辨率的直接热解吸和热裂解。然而,在熔点较低的材料表面上,通过局部热解吸进行空间分辨的直接表面加热变得具有挑战性,因为在热解吸开始之前,由于热耗散,材料将经历熔化相变。因此,我们开发了一种使用机械采样和在 AFM 悬臂探针尖端收集表面材料的方法,可直接从 AFM 尖端进行实时分析。这种方法允许将材料直接浓缩到探针上,以便进行后续的 MS 分析。我们评估了该技术的性能指标,并展示了从 250nm×250nm 面积的坎迪利拉蜡基质中局部 MS 采样,其中包含 UV 稳定剂阿伏苯宗和氧苯酮。总体而言,这种方法消除了向体材料的热耗散,从而可以更快地解吸和浓缩气相分析物,仅通过单个加热脉冲即可从单个采样点的给定量材料中获得更高的信号水平。

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