UV-visible spectroscopic measurement of solubilities in supercritical CO2 using high-pressure fiber-optic cells

UV-visible spectroscopic measurement of solubilities in supercritical CO2 using high-pressure fiber-optic cells
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DOI:
10.1021/ac971077h
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发表时间:
1998-06-01
影响因子:
7.4
通讯作者:
Wai, CM
Wai, CM
中科院分区:
化学1区
文献类型:
--
作者:
Carrott, MJ;Wai, CM

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介绍了一种基于光纤的微尺度紫外可见光谱法测量超临界CO2溶解度的系统的设计和构造。该系统由三个高压光纤单元组成,路径长度从38 μ m到1厘米不等,由标准的1/16英寸构成。不锈钢配件和硅纤维。它能够承受超过300 atm的压力,并且可以获得整个w可见光范围(200-900 nm)的光谱。使用具有不同路径长度的三个细胞,可以在几个数量级的浓度范围内测量高或低溶解度的化合物。铀络合物UO2(tta)(2)的溶解度在40摄氏度和100-325大气压范围内测定了高超临界CO2的TBP,发现在未改性的超临界CO2中,金属物种的溶解度可能超过10(-2)M。此外,该系统的小体积允许用相对少量的化合物测量溶解度。
The design and construction of a microscale, fiber-optics-based system for the measurement of solubilities in supercritical CO2 by UV-visible spectroscopy is described. This system consists of three high-pressure fiberoptic cells, with path lengths ranging from 38 mu m to 1 cm, constructed from standard 1/16-in. stainless steel fittings and silica fibers. It is capable of withstanding pressures in excess of 300 atm, and spectra over the entire W-visible range (200-900 nm) can be obtained. Use of three cells with different path lengths enables compounds of high or low solubility to be measured over a concentration range of several orders of magnitude. The solubility of a uranium complex, UO2(tta)(2).TBP, hi supercritical CO2 at 40 degrees C and over the pressure range 100-325 atm was determined, and it was found to be possible to attain solubilities in excess of 10(-2) M for metal species in unmodified supercritical CO2. Also, the small volume of this system allows solubilities to be measured with relatively small amounts of compounds.