Solubility measurements of noble metal acetylacetonates in supercritical carbon dioxide by high performance liquid chromatography (HPLC)
Solubility measurements of noble metal acetylacetonates in supercritical carbon dioxide by high performance liquid chromatography (HPLC)
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DOI：
10.1016/j.supflu.2007.11.002
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发表时间：
2008-03-01
影响因子：
3.9
通讯作者：
Hiaki, Toshihiko
中科院分区：
文献类型：
--
作者：
Yoda, Satoshi;Mizuno, Yoko;Hiaki, Toshihiko
建立了一种将超临界二氧化碳(SCCO(2))溶液直接注入高压液相色谱仪测定贵金属乙酰丙酮类化合物溶解度的方法。我们发现使用(1)反相高效液相色谱(RP-HPLC)分离色谱图上的样品峰和噪声峰，以及(2)SCCO(2)亲水洗脱剂消除噪声峰是有效的。用这种改进的方法，我们在313K下测量了铂、钯、Ru、Rh和银乙酰丙酮贵金属络合物在10~30 Mpa的scCO2中的溶解度，测量的样品量小于0.1g，实验时间比标准的动态流动法短。Ru和Rh乙酰丙酮的摩尔分数y(2)为10(-5)~10(-4)，Pd和铂乙酰丙酮的摩尔分数为10-5，银乙酰丙酮的摩尔分数y(-7)为10(-7)。用该模型成功地关联了Pd、Pt、Ru和Rh乙酰丙酮酸盐的溶解度数据。(C)2007 Elsevier B.V.保留所有权利。
A method has been developed for measuring the solubility of noble metal acetylacetonates by the direct injection of the supercritical carbon dioxide (scCO(2)) solution into a high pressure liquid chromatograph. We found the use of (1) reverse phase high pressure liquid chromatography (RP-HPLC) to separate the sample peak from the noise peak on chromatogram, and (2) a scCO(2)-philic eluent to eliminate the noise peak, to be effective. Using this improved method, we measured the solubilities of noble metal complexes of Pt, Pd, Ru, Rh and Ag acetylacetonates in scCO2 from 10 to 30 MPa at 313 K. Measurements were conducted with smaller amounts of samples (less than 0.1 g) and with shorter experimental times than by the standard dynamic flow method. The molar fraction y(2) was of the order 10(-5) to 10(-4) for Ru and Rh acetylacetonate, 10-5 for Pd and Pt acetylacetonate, and 10(-7) for Ag acetylacetonate. The solubility data for Pd, Pt, Ru, and Rh acetylacetonates were successfully correlated using the Chrastil model. (c) 2007 Elsevier B.V. All rights reserved.