Key Laboratory of Salt Lake Resources Chemistry of Qinghai Province, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, Xining, 810008, Qinghai, China.
Department of Chemistry, Faculty of Science, Fukuoka University, Nanakuma, Jonan, Fukuoka, 814-0180, Japan.
Anal Sci. 2023 Jun;39(6):977-987. doi: 10.1007/s44211-023-00306-8. Epub 2023 Mar 1.
A single liquid droplet in the air generated by ultrasonic levitation provides such analytical advantages as a small sample volume (~ μL) for expensive proteins, container-free condition for deeply supercooling and supersaturation, time-dependent observation, and homogeneous rapid mixing. The investigation of the properties and structure of a droplet at a molecular level is highly needed for understanding the physicochemical behaviors of a droplet and an underlying mechanism of processes in the droplet. We develop in situ Raman and synchrotron X-ray scattering methods of a single liquid droplet of ~ 1 mm size ultrasonically levitated. The composition of a supersaturated Mg(NO) droplet and speciation in the droplet are determined by analyzing the nitrate N-O and the water O-H stretching vibrational Raman bands. The X-ray interference function of an supersaturated Mg(NO) droplet is subjected to an empirical potential structure refinement modeling to reveal the ion solvation, association, and solvent water structure. Furthermore, crystallization of Mg(NO)⋅nHO from a saturated droplet is observed and identified.
超声悬浮产生的单个液滴具有许多分析优势,例如可用于昂贵蛋白质的小样品量(约 μL)、深过冷和过饱和的无容器条件、时变观察和均匀快速混合。为了理解液滴的物理化学行为和液滴中过程的潜在机制,非常需要在分子水平上研究液滴的性质和结构。我们开发了原位拉曼和同步辐射 X 射线散射方法,用于超声悬浮的约 1mm 尺寸的单个液滴。通过分析硝酸盐 N-O 和水 O-H 伸缩振动拉曼带,确定了过饱和 Mg(NO) 液滴的组成和液滴中的形态。对过饱和 Mg(NO) 液滴的 X 射线干涉函数进行经验势结构精修建模,以揭示离子溶剂化、缔合和溶剂水结构。此外,还观察到并鉴定了从饱和液滴中结晶的 Mg(NO)⋅nHO。