在线超临界流体色谱联用技术测定超临界二氧化碳中芘溶解度

Static Solubility Measurement of Pyrene in Supercritical Carbon Dioxide Using On-Line Supercritical Chromatography

中文关键词:  超临界流体色谱  接口  在线分析  溶解度  超临界二氧化碳

英文关键词:SFC  interface  on-line analysis  solubility  supercritical carbon dioxide

中文摘要:

      设计了一种单阀外循环接口，采用静态溶解度测定方法，联用在线超临界流体色谱，准确测定了芘在超临界二氧化碳中的溶解度.通过釜内磁力搅拌和接口外循环的双重作用，促进芘在超临界二氧化碳中的溶解平衡过程，确保在测定芘溶解度时体系已达到溶解平衡状态，确定了溶解平衡时间，消除了联用体系中因芘的溶解度过高而产生的体系堵塞问题.

英文摘要:

      A single-valve exterior recirculating interface was set up to combine the high pressure magnetic stirred vessel with the on-line supercritical fluid chromatograph(SFC). It was used to measure the solubility of pyrene in supercritical carbon dioxide in line with the static solubility test method. In the method, a programmable increasing pressure was used to produce a series of successive saturated supercritical fluid carbon dioxide solutions for the on-line SFC solubility measurements. The coupled static solubility system provides a convenient means to ensure that the dissolving equilibrium is established prior to the performance of the on-line SFC solubility measurements and also facilitates a self-validation accuracy check procedure. For pyrene, the solubility results were obtained at 40℃ under the pressure range of 10 to 28 MPa using 2 MPa steps, which were also relatively higher than the values reported by other authors.