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Supercritical Fluids - Instrumental Analytical Chemistry - Lecture Slides, Slides of Analytical Chemistry

Supercritical Fluids, Properties, Sf Instrumentation, Flow Diagram, Pressure Programing, Mw Range for Sfc, Typical Sfc Separation, Selectivity by Fluorescence, Supercritical Fluid Extraction are some points from this lecture of Instrumental Analytical Chemistry.

Typology: Slides

2011/2012

Uploaded on 12/23/2012

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Download Supercritical Fluids - Instrumental Analytical Chemistry - Lecture Slides and more Slides Analytical Chemistry in PDF only on Docsity! Supercritical Fluids TABLE 29-1 Comparison of Properties of Supercritical Fluids with Liquids and Gases (all of the data are order-of-magnitude only} Gas (STP) Supercritical Fluid Liguid Density on) (6-2) x10" 0-05 062 Diffusion coefficient (cm?) (I) x 10°! or 02-2) x 10° Viscosity (gem! 5°!) (1-3) x 104 (+3) x 104 23) x 10° Docsity.com Properties TABLE 29-2. Properties of Some Supercritical Fluids* Critical Critical Cita Point Density at Fuid Temperature, °C Pressure, atm Density, ginal 400 atm, g/ml, (0, 313 79 47 0.46 N,0 345 1 ES) (14 NH; 1325 125 0.24 (49 tt 152.0 i5 0.23 (150) Docsity.com Flow Diagram Sp ses AL FLUO TECHNOLOGIES. ING , (ee Standard SFT-150 Flow Diagram & Docsity.com Pressure Programing Sample: 1. cholesteryl octanoate 2. cholesteryl decylate 3. cholesteryl laurate 4. cholesteryl myristate 5. cholesteryl palmitate 6. cholesteryl stearate Column: DB-1 Mobile phase: CQ, Temperature: 90°C Detector; FID Linear pressure gradient 3000 to 4000 psi in 15 min [sobaric, 3000 psi 1 234 s I L | | a oO 5 10 15 min oO 5 10 min we 29-2 Effect of pressure programming in supercrit- fluid chromatography. (Courtesy of Brownlee Labs., Santa ta, CAD Docsity.com SFC vs HPLC 0.070 F- HPLC 0.060 0.050 0.040 HETP, mm 0.030 SFr 0.020 0.010 J+ 9e +} 0.000 i! l I l o 02 O4 O86 O8 10 12 Average linear velocity, cm/s Figure 29-3 Performance characteristics of a $-ym ODS column when elution is carried out with a conventional obile phase (HPLC) and supercritical carbon dioxide SFC. vom D. R. Gere, Application Note 800-3. Hewlett-Packard Company, 1983. With permission.) Docsity.com Typical SFC Separation —_—___J L 1 l 1 ao 80 180 2820 Pressure (ATM) L 1 i L o 20 a0 so Time mind Migmece 29-G ‘Separation of oligomers of dimethyl polysilaxane by supercritical Hhuid chromatography. ran C. M. Witte and RR. K. Houck, HRO & CO, 1986, 9. 2. With per rhissiov.! Docsity.com Selectivity by Fluorescence 400 nm Excitation 32433 nm Excitation CORO Figure 29-7 Portions of the supercritical flild chro- metogramse of polyayclic aromatics in a catbon-black ex- ®) tract, illustrating the selectivity achieved by fluerescence exeitation at twnwrvelengéhs. (Fao. O. Ag, (lite nr Houck, HAC & CO, 1986, &, 3. bith paraiiesion.) Docsity.com SFC Size Example with Pressure Triton X—100 CH, CH; Sone cd —cH,—¢ oun. oF 10dumiox 30m Fs ¢ CH, (OCH2CH),08 Splitless cH, CH, a ee re re ee 2 1g i poe pe tg 20 30 9 19 Time (min} | I 185 185 210 235 233 Pressure {bar} Figare 29-8 Chromatograms for the nonionic surfactant Triton X-100 with total current mass spectrometric detec- tion. (Repristted with permission from R. DD, Sititti and H. R. Udser, & Anal Chem., 8947, 59, 17. Gapyright 1987 American Cremical Soc any} Docsity.com
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