The design and performance of an electrochemical cell and solution flow system optimized for the collection of X‐ray absorption spectra from solutions of species sensitive to photodamage is described. A combination of 3D CAD and 3D printing techniques facilitates highly optimized design with low unit cost and short production time. Precise control of the solution flow is critical to both minimizing the volume of solution needed and minimizing the photodamage that occurs during data acquisition. The details of an integrated four‐syringe stepper‐motor‐driven pump and associated software are described. It is shown that combined electrochemical and flow control can allow repeated measurement of a defined volume of solution, 100 µl, of samples sensitive to photoreduction without significant change to the X‐ray absorption near‐edge structure and is demonstrated by measurements of copper(II) complexes. The flow in situ electrochemical cell allows the collection of high‐quality X‐ray spectral measurements both in the near‐edge region and over an extended energy region as is needed for structural analysis from solution samples. This approach provides control over photodamage at a level at least comparable with that achieved using cryogenic techniques and at the same time eliminates problems associated with interference due to Bragg peaks.

中文翻译：

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使用 X 射线光谱电化学技术控制氧化还原状态和光还原——通过增材工程在设计和制造方面取得进展

描述了为从对光损伤敏感的物种溶液收集 X 射线吸收光谱而优化的电化学电池和溶液流动系统的设计和性能。3D CAD 和 3D 打印技术的结合有助于以较低的单位成本和较短的生产时间进行高度优化的设计。溶液流量的精确控制对于最大限度地减少所需溶液的体积和最大限度地减少数据采集过程中发生的光损伤至关重要。描述了集成四注射器步进电机驱动泵和相关软件的详细信息。结果表明，结合电化学和流量控制可以重复测量定义体积的溶液，100 µl，对光还原敏感的样品的 X 射线吸收近边结构没有显着变化，并通过铜 (II) 配合物的测量得到证明。流量原位电化学电池允许在近边缘区域和扩展能量区域收集高质量的 X 射线光谱测量值，这是对溶液样品进行结构分析所需的。这种方法在至少与使用低温技术所达到的水平相当的水平上提供对光损伤的控制，同时消除了与由于布拉格峰引起的干扰相关的问题。