The Design of High Temperature Capillary Gas Chromatography Columns Based on Polydimethylsiloxane
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1 The Design of High Temperature Capillary Gas Chromatography Columns Based on Polydimethylsiloxane Jarl Snider, D. J. Hotnisky, Kristi Sellers, Dinesh V. Patwardhan Ph. D. Restek Corporation
2 utline Background Definition of Terminology Unique Attributes of High Temperature Column Applications Conclusions
3 Polydimethylsiloxane H n H H 3 C n
4 Thermal Stability of PDMS Beginning of decomposition Adapted from loxane Polymers, ed. Clarson & Semlyen, 1993.
5 Bleed Chromatography of loose silicones from the column Bleed pa temperature
6 Typical Chemical Structure of Bleed Me Me Me Me Me Me D 3 Me Me Me Me Me Me Me Me D 4
7 Challenge nce the decomposition temperature for PDMS is 343 C, it is a challenge to make a column that is stable and has low bleed at 380 C.
8 rigin of Bleed Polymer Synthesis ligomers that are created in a column s lifetime
9 Polymer Synthesis rigin of Bleed... Adapted from Inorganic Polymers, Mark, Allcock, & West 1992.
10 Polymer Synthesis licone Polymers can be synthesized using well known catalysts (KH, HCl) under equilibration polymerization conditions. We use newer, more advanced catalysts, better synthetic techniques.
11 rigin of Bleed... Polymer Synthesis ligomers that are created in a column s lifetime
12 rigin of Bleed... ligomers that are created in a column s lifetime (FS tubing) [ ] (polymer coating) D 3 /D 4 bleed PDMS H H
13 Enhancement of Thermal Stability by Using Additives lphenylene CH3 CH3 CH3 x y z CH3 CH3 CH3
14 Additives... n m A column with true ne selectivity cannot be obtained by having silphenylene in the backbone.
15 Stx TM -1 HT The polymer or the phase is PDMS. n
16 rigin of Bleed... deactivation fused silica
17 rigin of Bleed... deactivation fused silica
18 Deactivation of the Fused lica Surface We are using an advanced deactivation called ltek. It is a deposition process, unlike silazane or silicone deactivation.
19 Aroclor
20 Aroclor
21 Aroclor
22 Aroclor Run Conditions Column: Stx-HT1 Serial #: Description: 30m, 0.32mmID, 0.10µm Sample: Aroclor Solutions Part #32009, 32011, Concentration: Solvent: Sample ze: Instrument: Injector: 400ppb Hexane 1.0µL HP5890 Splitless/275 C Splitless Hold Time: 1.0min. SplitVentFlow: 40cc/min. Septa Purge: 5cc/min. Carrier Gas: Helium Head Pressure: 8.5psi Column Flow Rate: 1.9cc/min. Linear Velocity: 31cm/sec. Detector: ECD/310C Make up Gas Flow: 40cc/min. Temp. Program: 75 C(1.0min.) 15 C/min. to 150 C(0) 5 C/min. 300 C(10min.)
23 PCB Congeners Column: Stx-HT1 Serial #: Description: 30m, 0.32mmID, 0.10µm Sample: PCB Congener Standard #2 Part #32294 Concentration: 100ng Solvent: Iso-ctane Sample ze: 1.0µL Elution rder: 1. BZ#28 2. BZ#52 3. BZ# BZ# BZ# BZ# BZ#180 Instrument: Injector: Splitless Hold Time: SplitVentFlow: Septa Purge: Carrier Gas: Head Pressure: Column Flow Rate: Linear Velocity: Detector: Make up Gas Flow: HP5890 Splitless/275 C 0.80min. 40cc/min. 5cc/min. Helium 8.5psi 1.9cc/min. 31cm/sec. ECD/310 C 40cc/min. 2 *PCBs numbered according to Ballschmiter Temp. Program: 100 C(0.80min.) 15 C/min. to 325 C(10min.)
24 10ppm Aliphatics C24 2. C26 3. C28 4. C30 5. C m, 3.32mmID, 0.01µm Stx -1HT (cat.# 11709) Solvent: Hexane ven temp.: 30 C (hold 0.5 min.) to 240 C at 15 C/min. to 380 C at 10 C/min. (hold10min.) Det.: FID at 340 C Inj.: splitless at 250 C Carrier: hydrogen Flow rate: 4.0cc/min. at 30 C Make-up gas flow: 40cc/min
25 Bleed Comparison 15.61pA 39.02pA 11.27pA 6.07pA Rtx -1MS 6.94pA Stx -1HT 4.34pA 340 C 360 C 380 C
26 1 50ppm Hydrocarbons Aliphatic hydrocarbons: 1. C9 2. C10 3. C12 4. C14 5. C C18 7. C19 8. C20 9. C C C C C Aromatic Hydrocarbons: 1. napthalene 2. 2-methylnaphthalene 3. acenaphthylene 4. acenaphthene 5. fluorene 6. phenanthrene 7. anthracene 8. fluoranthene 9. pyrene 10. benzo(a)anthracene 11. chrysene 12. benzo(b)fluoranthene 13. benzo(k)fluoranthene 14. benzo(a)pyrene 15. indeno(1,2,3-cd)pyrene 16. dibenzo(a.h)anthracene 17. benzo(g,h)perylene
27 Analysis Conditions 30m, 3.32mmID, 0.01µm Stx -1HT (cat.# 11709) ven temp.: 30 C (hold 0.5 min.) to 240 C at 15 C/min. to 380 C at 10 C/min. (hold10min.) Det.: FID at 340 C Inj.: splitless at 250 C Carrier: hydrogen Flow rate: 4.0cc/min. at 30 C Make-up gas flow: 40cc/min. 1.0µL injections of MA EPH Aliphatic Hydrocarbon standard (cat.# 31459, solvent: hexane) & MA EPH Aromatic Hydrocarbon standard (cat.# 31458, solvent: methylene 50ppm concentration.
28 4 5 ASTM D m, 3.32mmID, 0.01µm Stx -1HT (cat.# 11709) ven temp.: 30 C to 380 C at 10 C/min. Det.: FID at 380 C Inj.:coolon-column Carrier: helium Flow rate: 1.3cc/min. at 30 C Linear velocity: 22cm/sec. at 30 C Make-up gas flow: 45cc/min. Head pressure: 6.0psi C7 2. C8 3. C9 4. C10 5. C11 6. C12 7. C14 8. C16 9. C C C C C C C C C C C C C C C
29 XTI Mix on Rtx-1 & Stx-1HT Stx -1HT Rtx ,2-hexanediol 2. nitro-di-n-propylamine 3. benzoic acid 4. C ,4-dinitrophenol 6. nitrophenol 7. nitroaniline 8. pentachlorophenol 9. carbazole 10. C C C benzo(b)fluoranthene 14. benzo(k)fluoranthene
30 Summary Definitions The design of low bleed & stable column system was discussed Several applications were shown
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