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Determination of residual dimethyl sulfoxide by high-resolution continuum source graphite furnace molecular absorption spectrometry
Spectrochimica Acta Part B: Atomic Spectroscopy ( IF 3.2 ) Pub Date : 2021-03-01 , DOI: 10.1016/j.sab.2020.106050
Mao Dong Huang , Norbert Esser , Karsten Hinrichs , Qin Tan , Jörg Rappich , Norbert H. Nickel , Thomas Dittrich

Abstract High-resolution continuum source molecular absorption spectrometry (HR-CSMAS) has been extended to the determination of sulfur-containing organic molecule, on the example of dimethyl sulfoxide (DMSO) as a residual solvent in CH3NH3PbI3 perovskite thin films. For this purpose, DMSO molecules were converted into CS molecules by pyrolysis in a graphite furnace at low temperature and the sulfur content was determined by measuring molecular absorption of CS at 258.055 nm. An aqueous solution of DMSO was used for calibration. A characteristic mass of 17 ng was achieved for S after pyrolysis at 160 °C by using Pd as a chemical modifier. Furthermore, the content of DMSO was normalized to that of Pb whereas the content of Pb was determined by reducing the Pb in the perovskite to metallic Pb with Zn powder and measuring absorption of the weak Pb line at 261.418 nm by high-resolution continuum source atomic absorption spectrometry (HR-CSAAS). The Pb content remained constant whereas the S/Pb molar ratio decreased with increasing annealing time. Our results open new opportunities for the characterization of residual DMSO in wide classes of materials.

中文翻译:

高分辨连续源石墨炉分子吸收光谱法测定残留二甲亚砜

摘要 高分辨率连续源分子吸收光谱法 (HR-CSMAS) 已扩展到含硫有机分子的测定,以二甲基亚砜 (DMSO) 作为 CH3NH3PbI3 钙钛矿薄膜中的残留溶剂为例。为此,通过在石墨炉中低温热解将 DMSO 分子转化为 CS 分子,并通过测量 CS 在 258.055 nm 处的分子吸收来确定硫含量。DMSO 水溶液用于校准。通过使用 Pd 作为化学改性剂,在 160 °C 下热解后,S 的特征质量为 17 ng。此外,DMSO 的含量被归一化为 Pb 的含量,而 Pb 的含量是通过用锌粉将钙钛矿中的 Pb 还原为金属 Pb 并通过高分辨率连续源原子吸收光谱法测量 261.418 nm 处的弱 Pb 线的吸收来确定的(HR-CSAAS)。Pb 含量保持不变,而 S/Pb 摩尔比随着退火时间的增加而降低。我们的结果为表征各种材料中残留的 DMSO 开辟了新的机会。
更新日期:2021-03-01
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