Compact Electron Paramagnetic Resonance on a Chip Spectrometer Using a Single Sided Permanent Magnet

IF 8.2 1区 化学 Q1 CHEMISTRY, ANALYTICAL ACS Sensors Pub Date : 2024-09-26 DOI:10.1021/acssensors.4c00788
Michele Segantini, Gianluca Marcozzi, Tarek Elrifai, Ekaterina Shabratova, Katja Höflich, Mihaela Deaconeasa, Volker Niemann, Rainer Pietig, Joseph E. McPeak, Jens Anders, Boris Naydenov, Klaus Lips
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Abstract

Electron paramagnetic resonance (EPR) spectroscopy provides information about the physical and chemical properties of materials by detecting paramagnetic states. Conventional EPR measurements are performed in high Q resonator using large electromagnets which limits the available space for operando experiments. Here we present a solution toward a portable EPR sensor based on the combination of the EPR-on-a-Chip (EPRoC) and a single-sided permanent magnet. This device can be placed directly into the sample environment (i.e., catalytic reaction vessels, ultrahigh vacuum deposition chambers, aqueous environments, etc.) to conduct in situ and operando measurements. The EPRoC reported herein is comprised of an array of 14 voltage-controlled oscillator (VCO) coils oscillating at 7 GHz. By using a single grain of crystalline BDPA, EPR measurements at different positions of the magnet with respect to the VCO array were performed. It was possible to create a 2D spatial map of a 1.5 mm × 5 mm region of the magnetic field with 50 μm resolution. This allowed for the determination of the magnetic field intensity and homogeneity, which are found to be 254.69 mT and 700 ppm, respectively. The magnetic field was mapped also along the vertical direction using a thin film a-Si layer. The EPRoC and permanent magnet were combined to form a miniaturized EPR spectrometer to perform experiments on tempol (4-hydroxy-2,2,6,6-teramethylpiperidin-1-oxyl) dissolved in an 80% glycerol and 20% water solution. It was possible to determine the molecular tumbling correlation time and to establish a calibration procedure to quantify the number of spins within the sample.

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使用单面永久磁铁的紧凑型电子顺磁共振芯片光谱仪
电子顺磁共振(EPR)光谱学通过检测顺磁态提供有关材料物理和化学特性的信息。传统的 EPR 测量是在高 Q 值谐振器中使用大型电磁铁进行的,这限制了操作实验的可用空间。在此,我们提出了一种基于 EPR 芯片(EPRoC)和单面永久磁铁组合的便携式 EPR 传感器解决方案。该装置可直接置于样品环境(如催化反应容器、超高真空沉积室、水环境等)中进行原位和操作测量。本文报告的 EPRoC 由 14 个压控振荡器 (VCO) 线圈阵列组成,振荡频率为 7 GHz。通过使用单晶 BDPA,在磁体相对于 VCO 阵列的不同位置进行了 EPR 测量。在分辨率为 50 μm 的 1.5 mm × 5 mm 磁场区域绘制出了二维空间图。这样就可以确定磁场强度和均匀性,发现它们分别为 254.69 mT 和 700 ppm。使用非晶硅薄膜层还可以沿垂直方向绘制磁场图。将 EPRoC 和永磁体组合成一个微型 EPR 光谱仪,对溶解在 80% 甘油和 20% 水溶液中的 tempol(4-羟基-2,2,6,6-三甲基哌啶-1-氧)进行实验。这样就可以确定分子翻滚的相关时间,并建立一个校准程序来量化样品中的自旋数量。
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来源期刊
ACS Sensors
ACS Sensors Chemical Engineering-Bioengineering
CiteScore
14.50
自引率
3.40%
发文量
372
期刊介绍: ACS Sensors is a peer-reviewed research journal that focuses on the dissemination of new and original knowledge in the field of sensor science, particularly those that selectively sense chemical or biological species or processes. The journal covers a broad range of topics, including but not limited to biosensors, chemical sensors, gas sensors, intracellular sensors, single molecule sensors, cell chips, and microfluidic devices. It aims to publish articles that address conceptual advances in sensing technology applicable to various types of analytes or application papers that report on the use of existing sensing concepts in new ways or for new analytes.
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