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SGE GC Application Guide

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The document is an applications guide for SGE's analytical sciences products, particularly focusing on capillary gas chromatography and its various applications across multiple fields such as environmental, food, pharmaceutical, and forensic analysis. It emphasizes the unique capabilities of SGE's Forté™ GC capillary columns, detailing their design advantages, performance characteristics, and guidelines for selecting the appropriate columns for specific applications. Additionally, it highlights the importance of factors such as internal diameter, film thickness, and column length in achieving effective chromatographic separation.

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Applications Guide Environmental Food, Flavors and Fragrances ForensicChemical Fuels and Petrochemical Pharmaceutical 5 years 1 9 6 0 - 2 0 1 0 AUSTRALIA & PACIFIC REGION CHINA EUROPE INDIA JAPAN MIDDLE EAST USA
For further information on our full range of products, please visit www.sge.com SGE Capillary Columns SGE Analytical Science Few companies can claim to be able to provide a total solution for analytical science; SGE is one of those few. From sample preparation, to injection, the separation and throughout the chromatographic process in either LC or GC there is a SGE product that has been designed to provide you with the results you need time and again. This brochure highlights some of SGE’s capabilities in capillary gas chromatography, specifically in the technically demanding area of capillary columns. SGE columns are engineered for consistent separation performance and can be found in many laboratories being tasked to perform everything from routine analyses to the latest R&D challenges. forte™ GC Capillary Columns With over 30 year’s experience, GC capillary columns truly are SGE’s strength, its forte. SGE is the only independent manufacturer of GC capillary columns that has the skill and technology to control all critical processes from producing the fused silica capillary tubing, through the phase synthesis, to the validation of the performance of each column. SGE offers a comprehensive range of forte™ GC capillary columns for almost any chromatographic application providing the best possible combination of, Performance, Robustness, Reproducibility, Low Bleed and Inertness. With this brochure we bring to you a small taste of the applications you might consider running on an SGE GC capillary column. If the application is not in this guide, please visit our website www.sge.com.
For further information on our full range of products, please visit www.sge.com Contents Guidelines for Choosing Columns 1-2 SGE Capillary Column 37-39 Part Number Listing Environmental 4-12 Food, Flavors and Fragrances 13-18 Fuels and Petrochemical 19-22 Chemical 23-27 Recommended Column by Application 3 GC Column Replacement Guide 39 GC Troubleshooting and Maintenance 40 Pharmaceutical 28-32 Forensic 33-36
Guidelines for Choosing Columns 1 2 3 4 6 7 8 9 10 11 12 13 14 16 5 0 min 120 min 26 15 1 2 3 4 6 8 9 10 11 12 13 14 15 16 7 5 ComponentsComponents 1. Naphthalene 2. Acenaphthylene 3. Ethylbenzene 4. Fluorene 5. Phenanthrene 6. Anthracene 7. Fluoranthene 8. Pyrene 9. Benzo(a)anthracene 10. Chrysene 11. Benzo(b)fluoranthene 12. Benzo(k)fluoranthene 13. Benzo(a)pyrene 14. Indeno(1,2,3,-c,d)pyrene 15. Dibenzo(a,h)anthracene 16. Benzo(g,h,i)perylene Effect of Internal Diameter. Polynuclear Aromatic Hydrocarbon (PAH) analysis. 2 Internal Diameter NORMAL - 0.25 mm ID Chromatogram using a conventional (30 m x 0.25 mm ID) BPX5 column with a 0.25 µm film. FAST - 0.10 mm ID Chromatogram using a FAST (10 m x 0.1 mm ID) BPX5 column with a 0.1 µm film. • The smaller the diameter the greater the efficiency, hence better resolution. Fast columns (0.1 mm ID) are used for faster analysis because the same resolution can be achieved in a shorter time. 0.5 4.0 min 1 2 3 4, 5 6 1 2 3 4 5 6 Components 1. Benzene 2. Toluene 3. Ethylbenzene 4. p-Xylene 5. m-Xylene 6. o-Xylene SolGel-WAX™ Polar SolGel-1ms™ Non-Polar 1 Effect of Stationary Phase. BTEX analysis on a polar (SolGel-WAX™) column and a 100% dimethyl polysiloxane (SolGel-1ms™), both 30 m x 0.25 mm ID X 0.25 µm film. Stationary Phase • Select the least polar phase that will perform the separation you require • Non-polar stationary phases separate analytes predominantly by order of boiling point. • Increase the amount of phenyl and/or cyanopropyl content in the phase, and the separation is then influenced more by differences in dipole moments or charge distributions (BP10 (1701), BPX35, BPX50, BP225 and BPX70) • To separate compounds that differ more in their hydrogen bonding capacities (for example aldehydes and alcohols), polythylene glycol type phases are best suited - SolGel-WAX™, BP20 (WAX) and BP21 (FFAP) 1 For further information on our full range of products, please visit www.sge.com BPX5 BPX70BPX50 BPX35 BPX90 BP225 BP21 BP20 SolGelWax Cydex-B BPX-Volatiles HT8 HT5 BP1, BPX1, SolGel-1ms Polyethylene glycolCyanopropyl Polysilphenylene siloxaneCyanopropylphenyl siloxanePolycarborane siloxanePhenyl Polysilphenylene siloxaneDimethyl polysiloxane i P Wax BPX B BPX-Volatiles HT �-bonding H-bonding Van der Waals Stationary Phase Polarity
PHASE RATIO 0 20 min R = 3.60 R (Resolution) = 3.14 R = 4.96 4 Effect of Film Thickness. • For samples with a variation in solute concentration, a thicker film column is recommended. This will reduce the possibility of broad overloaded peaks co-eluting with other compounds of interest. If the separation of two solutes is sufficient and co-elution is still unlikely, even with large differences in concentration, then a thinner film can be used. The greater the film thickness the greater the retention of solutes, therefore the higher the elution temperature. As a rule, doubling the film thickness results in an increase in elution temperature of approximately 15-20° under isothermal conditions. Usingatemperatureprogram,theincreaseinelutiontemperatureisslightlyless. Film thickness • From the phase ratio value ß, a column can be categorized for the type of application it would best suit. The smaller the ß value, the greater the ratio of phase to the column inner diameter, making it better suited for analyzing volatile compounds. Columns which have thin films are generally better suited for high molecular weight compounds and are characterized by large ß values. Above shows the phase ratio (ß) available for the SGE range of capillary columns. Keeping a similar phase ratio when changing column internal diameters will ensure that your chromatographic parameters will not need substantial changes. ß= ——— where ß = ratio id = column internal diameter (µm) d = film thickness (µm)f f4d id Formula to calculate Phase Ratio Film thickness (µm) Column ID (mm) 0.1 0.15 0.22 0.25 0.32 0.53 0.10 250 - 550 625 800 1325 0.15 - 250 - - - 883 0.25 - 150 220 250 320 530 0.50 - 75 110 125 160 265 1.00 - - 55 63 80 132 3.00 - - - - 27 44 5.00 - - - - 16 26 • Always try to select the shortest column that will provide the required resolution for the application. If the maximum column length available is being used, and resolution of the sample mixture is still inadequate then try changing the stationary phase or internal diameter. • Resolution is proportional to the square root of the column efficiency. Therefore, doubling the column length will only increase the resolving power of the column by approximately 40%. 0.25 µm 0.50 µm 1.0 µm 4.7 min 7.4 min 13.2 min 0 Effect of Length 3 Column Length 3.7 min 7.5 min 20 min R = 2.91 R = 2.05 R = 4.15 15.3 min 15 metres 30 metres 60 metres 2For further information on our full range of products, please visit www.sge.com
Recommended Column by Application PHASE Application SolGel-1ms BP1 BPX1 BP1-PONA BPX5 BP5 HT5 HT8 BPX35 BPX-Volatiles BP624 BP10 BPX50 SolGel-WAX™ BP20 BP21 BPX70 CYDEX-B BPX90 Acidic/Neutral Drugs Acids Alcohols Amines Aliphatic Amines Aromatic Antidepressants Aromatic -PAH Aroclors Beverages -Alcohols Butter-Fat Chiral - Componds Chlorinated Aromatics Cigarette Lighter Fuel Dioxins Essential Oils Food - FAME Glucose - Methylated Herbicides Industrial Solvents Ketones Monomers Nitroaromatics Organochlorine Pesticides Organophosphorous Pesticides Paraffins PCB’s Petroleum Phenols Phthalates Plant Sterols Polymers Polywax Pyrethroids Racehorse Doping Mixture Sedatives Semivolatiles Silicon Oil Solvents Sugars-Alditol Acetates Triglycerides TRPH Volatiles Xylenes Indicates recommended phases to be used for the application Indicates alternative phases that can be used for the application 3 For further information on our full range of products, please visit www.sge.com
Applications • Analysis of PCB'S, PCDT'S, and other complex mixtures using BPX5 and SolGel-1ms • HT8: The Perfect PCB Column • Fast Pesticide Screening Using a BPX5 GC Capillary Column • Analysis of Polychlorinated Dibenzodioxins and Furans on BPX5 • Analysis of Polynuclear Aromatic Hydrocarbons on BPX35 • Analysis of Polynuclear Aromatic Hydrocarbons on BPX5 • Analysis of Volatile Organic Pollutants on BPX-Volatiles • Applications using BPX90 • Analysis of Volatiles in Drinking Water on 25 m BP624 Column • Polychlorinated Biphenyls PCB Analysis The widespread use of GC-MS for Environmental analyses requires both low bleed and inertness. The broad range of compounds of interest means that medium polarity phases become more useful. BPX5, BPX35, and BPX50 provide a range of polarities, all with low bleed, high temperature limits, and robustness. For specialized applications such as PCBs, SGE’s HT8 delivers unique separation capabilities. Environmental 4For further information on our full range of products, please visit www.sge.com
ANALYSIS OF PCB'S, PCDT'S, AND OTHER COMPLEX MIXTURES USING BPX5 AND SOLGEL-1ms Time 16.00 18.00 20.00 22.00 24.00 26.00 28.00 30.00 32.00 34.00 36.00 38.00 40.00 42.00 44.00 46.00 48.00 50.00 0 Time 16.00 18.00 20.00 22.00 24.00 26.00 28.00 30.00 32.00 34.00 36.00 38.00 40.00 42.00 44.00 46.00 48.00 50.00 % 0 100 2378-D 2378-F OCDFOCDD Hepta-Hexa- F D D FF F D D F F D DF F Penta-Tetra- Octa- % 100 Tri- Tetra- Penta- Hexa- Hepta- Octa- OCDT SIM 7-Group Analysis of 44 mono- to deca-PBDE's via cool-on-column (3-µL). Deca-PBDE 209 at 310 °C, PBDEs 33/28 and 138/166 partially resolved, PBDE 85 coeluted with 155. - 44 Mono-Deca-PBDEs - 6890 GC/Autospec HRMS - Cool-on-column inlet - (No liner but 0.53 mm retention gap) 12.5 m BPX5 0.15 mm ID 0.1 µm - 0.25 m 0.53 mm ID plus - 2 m 0.25 mm retention gaps - He programmed 245-415 kPa - 150 ºC-315 ºC @ 3 ºC/minTime 5.00 7.50 10.00 12.50 15.00 17.50 20.00 22.50 25.00 27.50 30.00 32.50 35.00 37.50 40.00 42.50 45.00 47.50 50.00 52.50 55.00 % 0 100 Deca- 209206 208 207 Nona-Octa- 203 190 181 Hepta- 183 166 138 153 154 126 85/155 118 116 99 119 Hexa- 10077 66 47 71 49 75 37 35 28 33 25 17 32 30 15 13 12 11/8 7 10 32 1 Mono- Di- Tri- Tetra- Penta- SIM 2-Group Analysis for non-o-PCBs. Tetra-PCB's 77 and 81 (A) are resolved from residual o-PCB's (97, 87, 110, and 136). Penta-126 (B), and hexa-169 (C) also detected in eluate 2-basic alumina of DX-3 QC sediment extract (5 of 500 µL) Ion chromatograms (not smoothed). PBDE's are in same eluate (Peterman et al., 2006). Tetra-PBDE 47 from (M-2 Br)+ incidentally detected (B); 0.3 ng/g near lab background. - Dioxin-like non-ortho PCBs - HP 5890A GC/VG 70S HRMS - Heated (275 ºC) Direct inlet - 4 mm Siltek Cyclo-Uniliner - 30 m SolGel-1ms 0.15 mm ID 0.1 µm - 2.5 m x 0.25 mm ID retention gap - He constant at 415 kPa - 155 ºC (1 min) - 205 ºC @ 1.8 ºC/min then to 310 ºC @ 3.6 ºC/min ACKNOWLEDGEMENT Paul H. Peterman, US Geological Survey, Columbia Environmental Research Center. For additional information see SGE application note AN-0030-C. SGE liners undergo a high temperature deactivation process making them ideal for using with active compounds EXPERTTIP Environmental 5 For further information on our full range of products, please visit www.sge.com
e Chromatogram on the left demonstrates clearly the significant difference in selectivity of the HT8 column. By GC/MS, quantitation of CB28 using a standard 5% phenylpolysiloxane column is impossible as coelution with CB31 (with the same number of chlorines) occurs. HT8 separates the two congeners by a full minute allowing quantitation to be performed with ease. AROCLOR 1260 Column and Oven conditions are as listed for Aroclor 1242 .dtS.tnI902071 177 199 156 191 208 189 205 206 195 194 207 174/162/128 179/132 151 77/149 92 84 136/86 110 135 115/87 200/172 190/203 176 173 144 146 402131 101/150 118 153/122 180 138 97/117 107/108/134 197/171 550554setunim0453 AROCLOR 1260 Congener # Cl Position Cl # Identification by GC/MS 130 234-235 6 178 2356-235 7 141 2345-25 6 164 236-345 6 163 2356-34 6 138 234-245 6 160 23456-3 6 175 2346-235 7 158 2346-34 6 187 2356-245 7 182 2345-246 7 129 2345-23 6 138 141 187/182 183/166 185/159 164/163 178 130 105 137 129 AROCLOR 1242 Congener # Cl Position Cl # Identification by GC/MS 42 23-24 4 96 236-26 5 35 34-3 3 64 235-4 4 72 25-35 4 103 246-25 5 71 26-34 4 41 234-2 4 68 24-35 4 37 34-4 3 100 246-24 5 72/64 103/71 96/35 68/37 42 41 40 28/53 52/69 20/33/45 31 44 95 74 70 66 110 84 22 49/43 47/48/65 97/117/86 115/87 77/149 107/108/134 10 4 9 7 6 8 19 18 17 16 29 51 38 25 26/50 32 15 27 12/24 101/150 60/113 118 36 75 59 67 63 91/121/155 76/80 56 99 85 81148 20 045303setunim52 AROCLOR 1242 Phase: HT8, 0.25 µm film Column: 50 m x 0.22 mm ID Initial Temp: 80 °C, 2 min Rate 1: 30 °C/min Temp 2: 170 °C Rate 2: 3 °C/min Final Temp: Split, 300 °C Carrier Gas: He, 40 psi Detector: ECD, 330 °C Standard 5% Phenylsiloxan 31/28 HT8: THE PERFECT PCB COLUMN HT8 31 28 Separation of CB31 and CB28 Environmental 6For further information on our full range of products, please visit www.sge.com
Time (s) 300 400 500 600 700 800 900 1000 Spectrum # 348 1048 1748 2449 3149 3849 4550 5250 7e+006 6e+006 5e+006 4e+006 3e+006 2e+006 1e+006 0 ____ TIC Phenol3-phenoxy- Dimpylate Phosphamidon Cyclohexane1,2,3,4,5,6hexachloro Primicarb Phosphionthioticamide,P,P-diphenyl- Cycohexene1,3,4,5,6pentachloro-,s Mefenoxam Carbaril Malathion Chlorpyrifos Fenthion Aldrine Clofenvifos Quinalphos Captan Imazali 2-Methylphenothiazine Mitotane Dieldrin Ethion Mitotane Trizaophos Octyladipate p,p’-DDT Endosulfansulfate Btethrin Fenoxycarb Time (s) 520 540 560 580 600 620 640 660 680 700 7e+006 6e+006 5e+006 4e+006 3e+006 2e+006 1e+006 0 FAST PESTICIDE SCREENING USING A BPX5 GC CAPILLARY COLUMN Phase: SGE forte BPX5DX Column: 40 m x 0.18 mm ID x 0.18 μm Initial Temp: 80 ºC, 1 min Rate 1: 25 ºC/min to 300 ºC Final Temp: 300 ºC, 7 min Detector Type: LECO™ TOF Mass spectrometer Carrier Gas: He Carrier Gas Flow: constant flow mode at 1 mL/min Average Linear Velocity: ~75 cm/sec Injection Mode: splitless Injection Temperature: 270 ºC Total run time: 16.8 min Detector voltage: 1700 V Data acquisition speed: 10 Hz Column Part Number: 054229 ACKNOWLEDGEMENT SGE would like to thank Prof Jana Hajšlová and Jakub Schurek from VSCHT (Prague, CZ) for providing these chromatograms. Environmental 7 For further information on our full range of products, please visit www.sge.com
The list of some pesticides used in the sample, and their retention times Environmental 8For further information on our full range of products, please visit www.sge.com Peak number Name R.T. (s) 50 Penconazole 585.765 51 Tolylfluanide 587.622 52 Quinalphos 590.478 53 Procymidone 592.191 54 Captan 599.902 55 Methidathion 601.33 56 o,p'-DDE 602.044 57 Folpet 602.901 58 Imazalil 611.755 59 Bupirimate 614.325 60 2-Methylphenothiazine 616.896 61 p,p'-DDE 617.895 62 Mitotane 623.179 63 Dieldrin 628.605 64 Ethion 635.46 65 Mitotane 642.314 66 m,p'-DDD 643.171 67 o,p'-DDT 644.17 68 Triazophos 647.455 69 Endosulfan I 648.883 70 Octyl adipate 651.168 71 p,p'-DDT 665.019 72 Endosulfan sulfate 670.731 73 Tebuconazole 673.444 74 Bifenthrin 680.013 75 Fenoxycarb 693.436 76 Bromopropylate 695.436 77 Phosmet 701.576 78 Endrin ketone 709.43 79 λ-Cyhalothrin 718.141 80 Tetradifon 721.854 81 Phosalone 723.282 82 Fenarimol 754.126 83 Azinphos-ethyl 759.124 84 Permethrin 768.264 85 Permethrin 774.975 86 Pyridaben 786.114 87 Cyfluthrin 805.534 88 Cyfluthrin 807.248 89 Cypermethrin 819.957 90 Cypermethrin 826.383 91 Cypermethrin 831.238 92 Cypermethrin 833.095 93 Esfenvalerate 895.927 94 Fenvalerate α 914.062 95 Difenoconazole 950.476 96 Difenoconazole 956.617 97 Deltamethrin 972.182 Peak number Name R.T. (s) 1 Methamidophos 341.292 2 Dichlorovos 342.291 3 Phosphorodithioic acid, O,O-diethyl ester 381.561 4 Mevinphos 404.552 5 Carbamic acid, phenyl-, 1-methylethyl ester 418.261 6 Methacrifos 427.4 7 Benzene, (3-chloro-1-propenyl) 433.969 8 Butyl dimethyl phosphate 436.539 9 1-Naphthalenol 442.965 10 Bibenzyl 445.107 11 Cyclohexene, pentachloro- 449.534 12 Heptenophos 453.39 13 Endosulfan 462.672 14 Omethoate 465.099 15 Diphenylamine 476.095 16 Carbamic acid, (4-chlorophenyl), 1-methylethyl ester 479.094 17 Monocrotophos 485.091 18 Cyclohexane, 1,2,3,4,5,6-hexachloro- 500.228 19 Benzene, hexachloro- 501.799 20 Phenol, 3-phenoxy- 504.512 21 Dimethoate 505.083 22 Dimpylate 509.796 23 Phosphamidon 514.651 24 α-Lindane 515.222 25 Benzonitrile, pentachloro- 517.792 26 Cyclohexane, 1,2,3,4,5,6-hexachloro- 518.792 27 Etrimfos 520.22 28 Pirimicarb 526.36 29 Tetrachloroisophthalonitrile 527.217 30 Phosmet 527.788 31 Phosphinothioic amide, P,P-diphenyl- 532.072 32 Phosphamidon 534.786 33 γ-Lindane 535.642 34 Cyclohexene, 1,3,4,5,6-pentachloro-, ç- 540.498 35 Methyl chlorpyrifos 542.497 36 Mefenoxam 547.78 37 Pirimiphos methyl 551.065 38 Carbaril 553.492 39 Heptachlor 554.92 40 Malathion 557.348 41 Fenitrothion 558.205 42 Chlorpyrifos 563.346 43 Dichlofluanid 563.774 44 Fenthion 567.915 45 Parathion 569.2 46 Triadimefon 569.772 47 Aldrine 574.341 48 cis-Chlorfenvinphos 577.483 49 Clofenvinfos 584.194
setunim0302010 9 10 12 11 13 14 15 16 ANALYSIS OF POLYNUCLEAR AROMATIC HYDROCARBONS ON BPX35 1 2 3 4 65 7 8 Phase: BPX35, 0.25 µm Column: 30 m x 0.22 mm ID Initial Temp: 100 °C,1 min Rate: 10 °C/min Final Temp: 360 °C, 10 min Carrier Gas: He, 25 psi Detector: FID 380 °C Column Part Number: 054714 Components 1. Naphthalene 2. Acenaphthylene 3. Acenaphthene 4. Fluorene 5. Phenanthrene 6. Anthracene 7. Pyrene 8. Fluoranthene 9. Benzo (a) anthracene 10. Chrysene 11. Benzo (b) fluoranthene 12. Benzo (k) fluoranthene 13. Benzo (a) pyrene 14. Indeno (1,2,3, -c,d)pyrene 15. Dibenzo (a,h) anthracene 16. Benzo (g,h,i) perylene ANALYSIS OF POLYNUCLEAR AROMATIC HYDROCARBONS ON BPX5 5 10 20 minutes 30 40 1 2 3 4 5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 1 6 1 5 Polynuclear Aromatic Hydrocarbons (EPA 625 PAHs) Phase: BPX5, 0.25 µm film Column: 25 m x 0.22 mm ID Initial Temp: 50 °C, 2 min Rate: 8 °C/min Final Temp: 290 °C, 10 min Carrier Gas: HP5971 MSD Detector: Split 40:1 Carrier Gas: He, 15 psi Column Part Number: 054113 Components (0.5ng each component) 1. Naphtalene 2. Acenaphtylene 3. Acentaphthene 4. Fluorene 5. Phenanthrene 6. Anthracene 7. Pyrene 8. Fluoranthene 9. Chrysene 10. Benzo (a) anthracene 11. Benzo (b) fluoranthene 12. Benzo (k) fluoranthene 13. Benzo (a) pyrene 14. Indeno (1,2,3, -c,d)pyrene 15. Dibenzo (a,h) anthracene 16. Benzo (g,h,i) perylene SGE wishes to acknowledge Dr P.Ambridge, Dr A.Fernandes and C.Brook at AEA Technology, Harwell, U.K. ANALYSIS OF POLYCHLORINATED DIBENZODIOXINS AND FURANS ON BPX5 Single Ion Chromatograms of TCDF Isomers Single Ion Chromatograms of TCDD Isomers 2,3,7,8 - TCDF m/z 321.8936 m/z 333.9339 13C12 - 2,3,7,8 - TCDF 2,3,7,8 -TCDD 13C12 - 2,3,7,8 -TCDD 17 18 19 20 21 minutes 18 19 20 21 minutes m/z 317.9389 0 100% 0 100% m/z 305.8987 0 100% 0 100% Phase: BPX5, 0.25 µm Column: 50 m x 0.22 mm ID Initial Temp: 80 °C Rate 1: 10 °C/min Temp1: 240 °C Rate 2: 2 °C/min Temp 2 : 280 °C Rate 3: 10 °C/min Final Temp: 320 °C Detector: Mass Spectrometer Column Part Number: 054114 Remember : the lower the temperature, the longer your column will last. EXPERTTIP Environmental 9 For further information on our full range of products, please visit www.sge.com
57 58 59 60 54 55 12.00 14.00 16.00 18.00 20.00 22.00 24.00 22 23 24 25 26 27 28 29 30 31 32 33 34 35, 36 37 38 39 40 41, 42 43, 44 45 46 47 48 49 50 51 52 53 54 55 56 Phase: BPX-Volatiles 1 µm film 502.2 mix: 200 ppm in Methanol Column: 40 m x 0.18 mm ID Initial Temp: 40 °C , 0 min Rate 1: 6 °C to 210 °C Rate 2: 15 °C to 240 °C Final Temp: 240 °C, 5 min Detector Type: Mass Spectrometer Carrier Gas: He, 40.3 psi Carrier Gas Flow : 1.2 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 50:1 Injection Volume: 1 µL Injection Temperature: 250 °C Autosampler: No Liner Type : 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054860 ms-NoVent™Part No: 113400 HP5973 restrictor: 113409 Full scan: 45-450 m/z ANALYSIS OF VOLATILE ORGANIC POLLUTANTS ON BPX-VOLATILES 2.00 4.00 6.00 8.00 10.00 1600000 1200000 800000 400000 0 1 2 3 4 5 6 7 9 10 8 11 13 1412 15 16,17 18 19 20 21 1 2 3 4 5 6 1.60 2.00 2.40 2.80 3.20 3.60 4.00 4.40 Components 1. Dichlorodifluoromethane 2. Chloromethane 3. Vinyl chloride 4. Bromomethane 5. Chloromethane 6. Trichlorofluoromethane 7. 1,1-Dichloroethene 8. Dichloromethane 9. trans-1,2-Dichloroethene 10. 1,1-Dichloroethane 11. 2,2-Dichloropropane 12. cis-1,2-Dichloroethene 13. Bromochloromethane 14. Chloroform 15. 1,1,1-Trichloroethane 16. 1,1-Dichloropropene 17. Carbon tetrachloride 18. Benzene 19. 1,2-Dichloroethane 20. Trichloroethene 21. 1,2-Dichloropropane 22. Dibromomethane 23. Bromodichloromethane 24. cis-1,3-Dichloropropene 25. Toluene 26. trans-1,3-Dichloropropene 27. 1,1,2-Trichloroethane 28. Tetrachloroethene 29. 1,3-Dichloropropane 30. Dibromochloromethane 31. 1,2-Dibromethane 32. Chlorobenzene 33. Ethylbenzene 34. 1,1,2-Dibromochloromethane 35. p-Xylene 36. m-Xylene 37. o-Xylene 38. Styrene 39. Bromoform 40. Isopropylbenze 41. Bromobenzene 42. 1,1,2,2-Tetrachlorethane 43. 1,2,3-Trichloropropane 44. n-Propyl benzene 45. 2-Chlorotoulene 46.1,3,5-Trimethylbenzene 47. 4-Chlorotoulene 48. tert-Butylbenzene 49. 1,2,4-Trimethylbenzene 50. sec-Bythlbenzene 51. 1,3-Dichlorobenzene 52. p-lsopropyltoulene 53. 1,2-Dichlorobenzene 54. n-Butylbenzene 55. 1,4-Dichlorobenzene 56. 1,2-Dibromo-3-chloropropane 57. 1,2,4-Trichlorobenzene 58. Hexachlorobutadiene 59. Naphthalene 60.1,2,3-Trichlorobenzene Chromatogram showing analysis of commonly screened volatile organic pollutants 32 33 35, 36 37 38 39 40 41, 42 43, 44 45 46 47 48 49 50 51 52 53 14.00 15.00 16.00 17.00 18.00 19.00 20.00 Environmental 10For further information on our full range of products, please visit www.sge.com
setunim975 1 5 ANALYSIS OF VOLATILES IN DRINKING WATER ON 25 M BP624 COLUMN VOLATILES IN DRINKING WATER Phase: BP624, 1.2 µm Column: 25 m x 0.22 mm ID Initial Temp: 50 °C, 2 min Rate: 15 °C/min Final Temp: 170 °C Detector: HP5970 MSD Injection Mode: Hexadecane extract Carrier Gas: He, 15 psi Column Part Number: 054826 Components 1. Difluorobenzene 2. Benzene 3. Toluene - (d8) 4. Toluene 5. Chlorobenzene - (d5) 6. Ethyl benzene 7. p and m-Xylene 8. o-Xylene 9. Bromofluorobenzene 2 3 4 6 7 8 9 10 20 10 20 5 15 9 14 12 17 9 14 Ronnel and heptachlor ceolute Aldrin and fenthion coelute Baseline separation Adrin and fenthion coelute fenthion (m/z 278) Aldrin and methylparathion (m/z 263) Ronnel (m/z 285) Heptachlor (m/z 272) Chlorpyrifos (m/z 314) Chlorphyifos methyl (m/z 286) Diazinon (m/z 137) Ronnel (m/z 285) Parathion (m/z 291) Fenthion (m/z 278) APPLICATIONS USING BPX90 10.0 15. 20.0 4.0 10.0 15.0 HCCH isomers and HCB Separation of aromatics Separation of hexabromocylododecanes Selectivity for pesticides and thiophosphate esters Condition column at either 20 ° above the maximum method temperature or the recommended maximum column temperature (whichever is lower). EXPERTTIP Environmental 11 For further information on our full range of products, please visit www.sge.com
04SETUNIM52 68 69 70 77 80 82 83 85 86 88 89 94 99 104 105 110 113 115 119 87 81 91 92 130 131 129 128 108 109 98 100 114 116 117 118 121 122 123 127 134 133 135 71 73 74 76 72 75 79 90 126124 112 107 97 102 132 POLYCHLORINATED BIPHENYLS PCB ANALYSIS Phase: HT8, 0.25 µm Column: 25 m x 0.22 mm ID Initial Temp: 60 °C, 2 min Rate: 12 °C/min Final Temp: 360 °C, 10 min Detector: lon Trap MS Injection Mode: PTV Carrier Gas: He, 15 psi Components 1. PCB 18 2. PCB 31 3. PCB 28 4. PCB 52 5. PCB 44 6. PCB 70 7. PCB 101 8. PCB 110 9. PCB 149 10. PCB 153 11. PCB 138 12. PCB 180 13. PCB 170 1 2 3 4 5 6 7 8 9 10 11 12 13 16:40 18:20 20:00 21:40 23:00 MINUTES 30 35 40 45 50 min Phase: HT8, 0.25 µm Column: 50 m x 0.22 mm ID Initial Temp: 60 °C Rate 1: 40 °C/min Temp 1: 200 °C Rate 2: 3 °C/min Temp 2: 320 °C Detector: ECD Carrier Gas: He, 40 psi Performance Specifications HT8 8% Phenyl (Equiv) Polycarborane - Siloxane Minimum Operating Temp.: -20 °C Maximum Cycling Temp.: 370 °C (Polyimide) GC/MS Analysis of PCB mixture Components 1. PCB1 2. PCB2 3. PCB3 4. PCB10 5. PCB4 6. PCB9 7. PCB7 8. PCB6 9. PCB 8/5 10. PCB19 11. PCB18 12. PCB11 13. PCB17 14. PCB13 15. PCB24 16. PCB27 17. PCB15 18. PCB32 19. PCB16 20. PCB54 21. PCB23 22. PCB34 23. PCB29 24. PCB26 25. PCB25 26. PCB31 27. PCB8/53 28. PCB51 29. PCB21 30. PCB33/45/20 31. PCB22 32. PCB46 33. PCB36 34. PCB52/69 35. PCB43 36. PCB49 37. PCB47/48/75 38. PCB44 39. PCB59 40. PCB42 41. PCB35 42. PCB64 43. PCB71/103 44. PCB41 45. PCB37 46. PCB68 47. PCB100 48. PCB40 49. PCB57 50. PCB67 51. PCB63 52. PCB102 53. PCB95 54. PCB74 55. PCB121/ 155/91 56. PCB70 57. PCB80 58. PCB66 59. PCB96/55 60. PCB84/92 61. PCB125 62. PCB90 63. PCB101 64. PCB60 65. PCB56 66. PCB152 67. PCB99 68. PCB119 69. PCB83 70. PCB136 71. PCB86 72. PCB97 73. PCB89 74. PCB115 75. PCB87 76. PCB154 77. PCB85 78. PCB10/81 79. PCB151 80. PCB144 81. PCB147 82. PCB135 83. PCB77/82 84. PCB149 85. PCB124 86. PCB143 87. PCB134/ 107/131 88. PCB123 89. PCB133 90. PCB118 91. PCB165 92. PCB143/114 93. PCB132/179 94. PCB122 95. PCB153 96. PCB176 97. PCB141 98. PCB105 99. PCB137 100. PCB130 101. PCB178 102. PCB163 103. PCB138 104. PCB160 105. PCB158/175 106. PCB187/182 107. PCB183/129 108. PCB126 109. PCB185 110. PCB159/202 111. PCB174/128 112. PCB177/201 113. PCB167 114. PCB171 115. PCB197 116. PCB173 117. PCB200 118. PCB156/172 119. PCB157 120. PCB180 121. PCB193 122. PCB191 123. PCB198 124. PCB199 125. PCB170 126. PCB190/ 196/203 127. PCB169 128. PCB208 129. PCB207 130. PCB195 131. PCB189 132. PCB194 133. PCB205 134. PCB206 135. PCB209 Part Number: 054676 PCB ANALYSIS Phase: HT8, 0.25 µm film Column: 50 m x 0.22 mm ID Initial Temp: 90 °C, 1 min Rate 1: 20 °C/min Temp 1: 170 °C,7.5 min Rate 2: 3.5 °C/min Temp 2: 285 °C Rate 3: 20 °C/min Temp 3: 320 °C Carrier Gas: H₂, 43 cm/sec Detector: ECD 78 84 93 95 103 106 111 120 125 02SETUNIM5 1 2 4 5 6 7 8 9 10 11 12 13 3 19 18 17 20 21 22 23 24 25 26 27 30 31 32 33 34 35 36 37 38 40 43 44 45 48 54 56 58 59 60 61 62 66 67 63 64 65 53 49 50 51 52 55 57 46 47 42 39 41 28 29 16 15 14 Aroclor 1254 Environmental 12For further information on our full range of products, please visit www.sge.com
GC analysis in the Food, Flavors and Fragrances area covers a diverse range of compounds that vary in both polarity and boiling point. As a consequence a range of different columns are often required. Chromatograms are often complex, and any single column may not give enough separation of all of the compounds that may be present. Pairs of columns such as BPX5 and SolGel-WAX™ may be used to overcome this problem. For specific classes of compounds such as fatty acids, specialized columns are often necessary. Short chain fatty acids may be analyzed as free acids on the Nitroterephthalic acid (TPA) modified Polyethylene Glycol BP21 phase. Longer chain fatty acids are usually analyzed as fatty acid methyl esters on wax phases such as BP20 and SolGel-WAX™, or for more demanding applications, BPX70 or BPX90. Applications • Comparison of Geranium Oils on SolGel-WAX™ • Analysis of Eucalyptus Oil on SolGel-WAX™ • Analysis of Lavender Oil on Cydex-B • Analysis of Lavender Oil on BPX-5 • Analysis of Tasmanian Lavender Oil on SolGel-WAX™ • Analysis of Wine on BP20 • Analysis of Scotch Whisky on BP20 • Analysis of Teatree Oil on BPX5 • Analysis of Omega-3 Fatty Acids using BPX70 • BPX90 – a Highly Polar Phase for FAME Analysis • Analysis of PUFA-1 Marine FAME on BPX70 • Analysis of PUFA-2 Animal FAME on BPX70 • Analysis of PUFA-1 Marine FAME on BPX70 Food, Flavors and Fragrances 13 For further information on our full range of products, please visit www.sge.com
ANALYSIS OF EUCALYPTUS OIL ON SOLGEL-WAX™ Subtraction of the two TIC chromatograms shows the difference between the two essential oils. COMPARISON OF GERANIUM OILS ON SOLGEL-WAX™ 5.00 10.00 15.00 20.00 25.00 30.00 5.00 10.00 15.00 20.00 25.00 30.00 Comparison of total ion chromatograms (TIC) for Geranium oils from Reunion Island (green trace) and South Africa (red trace). EXPERIMENTAL CONDITIONS Column: SGE forte SolGel-WAX™, 30 m x 0.25 mm x 0.25 µm (SGE P/N 054796) Temperature Program: 60 °C for 3 min, then 4 °C/min to 220 °C Carrier Gas: He Flow: 0.6 mL/min Injection 0.3 µL split ratio 30:1 Volume Injection temp: 250 °C Liner: SGE P/N 092019 single tapered with quartz wool Phase: SolGel-WAX™, 0.25 µm film Sample: Neat Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 8 °C/min to 220 °C Final Temp: 220 °C, 5 min Detector Type: Mass Spectrometer Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.2 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054796 ms-NoVent™ Part Number: 113400 HP5973 restrictor: 113409 Full Scan/SIM: 45-450 m/z Components 1. α-Pinene 2. ß -Pinene 3. Sabinene 4. Limonene 5. 1,8 -Cineole 6. p-Cymene 7. Linalool L 8. Terpinen-4-ol 9. α-Terpineol 10. α-Terpinenyl acetate 11. d-Carvoαne ACKNOWLEDGEMENT We thank M. Bernet and M. Didtsch of the ISIPCA Group, Research and Studies Centre for Fragrance, Cosmetics and Food Flavors, France, for providing these chromatograms. For more information see SGE application note AN-0020-C. 4.00 6.00 8.00 10.00 12.00 14.00 0 1000000 2000000 3000000 4000000 5000000 6000000 7000000 8000000 1 2 3 4 5 6 7 8 9 10 11 Food, Flavors and FragrancesFood, Flavors and Fragrances 14For further information on our full range of products, please visit www.sge.com
Components 1. 3-Octanone 2. Octenyl acetate 3. Octanol 4. cis Linalool oxide 5. trans Linalool oxide 6. Linalool L 7. Linalyl acetate 8. Terpinen-4-ol 9. Lavandulyl acetate 10. Borneol L 11. Caryophyllene oxide ANALYSIS OF TASMANIAN LAVENDER OIL SOLGEL-WAX™ Phase: SolGel-WAX™, 0.25 µm film Sample: Neat Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 8 °C/min to 220 °C Final Temp: 220 °C, 5 min Detector Type: Mass Spectrometer Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.2 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054796 ms-NoVent™ Part Number: 113400 HP5973 restrictor: 113409 Full Scan/SIM: 45-450 m/z4.00 6.00 8.00 10.00 12.00 14.00 16.00 0 2000000 4000000 6000000 8000000 1e+07 1.2e+07 1.4e+07 1 2 3 4 5 6 7 8 9 10 11 ANALYSIS OF LAVENDER OIL ON BPX5 10.0 12.0 14.0 16.0 18.0 20.0 22.0 24.0 26.0 28.0 0 40000 80000 120000 160000 200000 240000 280000 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 Phase: BPX5, 0.25 µm film Lavender Oil: Lavender Oil in ethanol Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 5 °C/min to 260 °C Final Temp: 260 °C Detector Type: Mass Spectrometer Carrier Gas: He, 7.0 psi Carrier Gas Flow: 1.0 mL/min Constant Flow: On Average Linear Velocity: 36 cm/sec at 40 °C Injection Mode: Split Split Ratio: 200:1 Purge on (Split) Vent Flow: 200 mL/min Injection Volume: 0.2 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Double Taper Liner Liner Part Number: 092018 Column Part Number: 054101 Components 1. ß- Pinene 2. 1-Octen-3-ol 3. 3-Octanol 4. 3-Octanol 5. p-Cymene 6. Limonene 7. cis-Ocimene 8. cis-Linaloxide 9. trans-Linalool oxide 10. Linalool L 11. Octenyl acetate 12. Camphor 13. Lavandulol 14. Borneol L 15. Terpinen-4-ol 16. α-Terpineol 17. Linalyl acetate 18. Lavundyl Acetate 19. Geranyl Acetate 20. α-Santalene 21. ß-Caryophyllene 22. α-Cadinine 23. α-Cryophyllene oxide Components 1. (+) Linalool 2. ( - ) Linalool ANALYSIS OF LAVENDER OIL ON CYDEX-B Better resolution is often obtained from chiral columns by using lower temperatures and higher carrier gas velocities than for conventional columns. EXPERTTIP LAVENDER OIL Phase: CYDEX-B, 0.25 µm film Column: 50 m x 0.22 mm ID Initial Temp: Isothermal at 90 °C Final Temp: FID Detector: 32 x 10-¹²AFS Injection Mode: Split Column Part Number: 054901 Food, Flavors and Fragrances 15 For further information on our full range of products, please visit www.sge.com
8.0 10.0 12.0 14.0 16.0 18.0 20.0 22.0 24.0 26.0 28.0 0 2000000 4000000 6000000 8000000 1e+07 1.2e+07 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 Phase: BP20, 0.25 µm film Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 5 °C/min to 200 °C Final Temp: 200 °C Detector Type: Mass Spectrometer Carrier Gas: He, 7.0 psi Constant Flow: 1.0 mL/min. Average Linear Velocity: 36 cm/sec at 40 °C Injection Mode: Split Split Ratio: 200:1 Purge on (Split) Vent Flow: 200 mL/min. Injection Volume: 0.2 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Double Taper Liner Liner Part Number: 092018 Column Part Number: 054101 ANALYSIS OF WINE ON BP20 0 105 minutes 1 2 3 4 5 6 7 8 9 10 Phase: BP20, 1.0 µm Column: 25 m x 0.32 mm ID Initial Temp: 40 °C, 2 min Rate 1: 5 °C/min Temp 2: 50 °C Rate 2: 15 °C/min Final Temp: 190 °C Carrier Gas: H₂,6psi Injection Mode: 2 µL Column Part Number: 054442 Components 1. Acetaldehyde 2. Ethyl Acetate 3. Methanol 4. Isopropanol 5. Ethanol 6. Propanol 7. Isobutanol 8. Isoamyl Alcohol 9. Acetic Acid 10. Unknown ANALYSIS OF TEATREE OIL ON BPX5 Components 1. Thujene 2. α-Pinene 3. Sabinene 4. 3-Octanol 5. ß-Pinene 6. α-Phellandrene 7. α-Terpinene 8. p-Cymene 9. Limonene 10. 1,8-Cineole 11. y-Terpinene 12. Terpinolene 13. Terpinen-4-ol 14. α-Terpineol 15. α -Gurjunene 16. (trans)-ß-Caryophyllene 17. Aromadendrene 18. Alloaromadendrene 19. Ledene 20. Germacrene B 21. α-Cadinene 22. 1s, cis-Calamenene 23. Globulol ANALYSIS OF SCOTCH WHISKY ON BP20 Phase: BP20, 1.0 µm Column: 12 m x 0.53 mm ID Initial Temp: 55 °C, 3 min Rate: 10 °C/min Final Temp: 120 °C, 0 min Detector: FID Sensitivity: 128 x 10-¹²AFS Injection Mode: Split Column Part Number: 054447 Components 1. Acetaldehyde 2. Ethyl Acetate 3. Methanol 4. Ethanol 5. Propan-1-ol 6. 2-Methylpropan-1-ol 7. 2-Methylbutan-1-ol+3- Methylbutan-1-ol 1 2 3 4 5 6 7 0 3 6 minutes For extended life of polar columns, always use an oxygen trap in the carrier gas line. EXPERTTIP Food, Flavors and FragrancesFood, Flavors and Fragrances 16For further information on our full range of products, please visit www.sge.com
Phase: BPX70, 0.25 µm film Sample: 10 ppm in methanol Column: 25 m x 0.32 mm ID Initial Temp: 80 °C, 2 min Rate 1: 50 °C/min to 130 °C, 10 min Rate 2: 2 °C/min to 172°C Final Temp: 172 °C , 6 min Detector Type: FID Detector Temp: 300 °C Carrier Gas: He, 10 psi Carrier Gas Flow: 2.2 mL/min. Constant Flow: On Average Linear Velocity: 39 cm/sec at 80 °C Injection Mode: Split Split Ratio: 58:1 Injection Volume: 1 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Focus Liner™ Liner Part Number: 092002 Column Part Number: 054606 ACKNOWLEDGEMENT SGE would like to thank Masterfoods UK for supplying the sample and chromatographic conditions for this chromatogram. For more information see SGE technical poster TP-0100-C The chromatogram shows the excellent separation of a complex mixture of FAME compounds. Note the excellent peak shape and separation of the Omega-1,2 and 3 fatty acid isomers both structural and cis and trans. 55 10 15 20 25 30 35min 15 10 5 12 17 21 22 30 32 34 pA 45 40 35 30 25 20 1 2 3 5 6 7 8 9 10 11 13 14 15 16 18 19 20 23 24 25 26 27 28 3129 33 Components 1. C6 2. C8 3. C10 4. C11 5. C12 6. C13 7. C14 8. C14:1 cis 9 9. C15 10. C16 11. C16:1 cis 9 12. C17 13. C17:1 cis 10 14. C18 15. C18:1 trans 9 16. C18:1 cis 9 17. C18:1 cis 12 18. C18:2 trans 9,12 19. C18:2 cis 9,12 20. C18:3 cis 6,9,12 21. C18:3 cis 9,12,15 22. C18:4 cis 6,9,12,15 23. C20 24. C21:1 cis 11 25. C20:2 cis 11,14 26. C20:3 cis 8,11,14 27. C20:4 cis 5,8,11,14 28. C20:3 cis 11,14,17 29. C22 30. C20:5,8,11,14,17 31. C22:1 cis 13 32. C22:4 cis 7,10,13,16 33. C24 34. C22:6 cis 4,7,10,13,16,19 ANALYSIS OF OMEGA-3 FATTY ACIDS USING A BPX70 WHAT IS DIFFERENT ? • BPX90 is a highly polar phase of the poly (biscyanopropylsiloxane) type. • The phase has excellent thermal stability and a wide operating range (70 - 280 °C). • The separation mechanisms gives short elution times relative to other polar phases. BPX90 shows low selectivity for non-polar analytes and saturated FAME. • BPX90 shows enhanced selectivity for polyunsaturated FAME and the selectivity can be tuned with film thickness. • BPX90 is effective for the separation of cis and trans isomers and positional isomers of FAME analytes. Supelco 37 FAME test mixture. Columns 15 m x 0.25 mm ID x 0.25 micron film. Temperature programmed 70°C (hold 1 min) to 150 °C (20 °C/min) to 250 °C (10 °C/min) then hold at 250 °C (5 min). Injector: 240 °C. Detection MS. C18-C22 FAME test mixture. Columns 30 m x 0.25 mm ID x 0.25 micron film. Isothermal: 180°C. Injector: 240 °C. Detection FID at 280 °C. FAME POLARITY TEST BPX90 – A HIGHLY POLAR PHASE FOR FAME ANALYSIS C14:0 C15:0 C16:0 C17:0 C18:0 C20:0 C21:0 C22:0 C23:0 C24:0 C14:1 C15:1 C16:1 C17:1 C18:1n9trans C18:n9cis C20:1 C22:1n9 C24:1 C14:0 C15:0 C16:0 C17:0 C18:0 C20:0 C21:0 C22:0 C23:0 C24:0 C14:1 C15:1 C16:1 C17:1 C18:1n9trans C18:n9cis C20:1 C22:1n9 C24:1 C18:2n6trans C18:2n6cis C18:3n6 C18:3n3 C20:2 C20:3n6 C20:3n3 C20:4n6 C22:2 C20:5n3(EPA) C22n6(DHA) C18:2n6trans C18:2n6cis C18:3n6 C18:3n3 C20:2 C20:3n6 C20:4n6 C20:3n3 C20:5n3(EPA) C22:2 C22n6(DHA) BPX70 BPX90 Food, Flavors and Fragrances 17 For further information on our full range of products, please visit www.sge.com
ANALYSIS OF PUFA-2 ANIMAL FAME ON BPX70 PUFA-2 ANIMAL FAME Phase: BPX70, 0.25 µm film Column: 25 m x 0.22 mm ID Initial Temp: 150 °C, 0 min Program Rate: 2 °C/min Final Temp: 210 °C, 5 min Carrier Gas: He, 15 psi Detector: FID, 280 °C Sensitivity: 32 x 10-¹²AFS Injection Mode: Split, 50:1 Column Part Number: 054602 Components 1. C14:0 2. C16:0 3. C16:1n7 4. C18:0 5. C18:1n9 6. C 18:2n7 7. C18:2n6 8. C18:3n3 9. C20:0 10. C20:1n11 11. C20:3n6 12. C20:4n6 13. C20:5n3 14. C22:4n6 15. C22:5n3 16. C22:6n3 14 16 13 12 4 7 11 2 1 3 5 6 15 8 0351 minutes 9 10 0 ANALYSIS OF PUFA-1 MARINE FAME ON BPX70 PUFA-2 ANIMAL FAME Phase: BPX70, 0.25 µm Column: 50 m x 0.22 mm ID Initial Temp: 150 °C, 0 min Program Rate: 2 °C/min Final Temp: 210 °C, 5 min Carrier Gas: He, 15 psi Detector: FID, 280 °C Sensitivity: 32 x 10-¹²AFS Injection Mode: Split, 50:1 Column Part Number: 054603 1 2 3 4 5 6 7 8 10 9 03setunim51 Components 1. C18:1n9 2. C18:1n7 3. C18:2n6 4. C18:3n3 5. C18:4n3 6. C 20:0 7. C20:1n9 8. C20:4n6 9. C20:5n3 10. C22:1n11 ANALYSIS OF PUFA-1 MARINE FAME ON BPX70 Phase: BPX70, 0.25 µm film Column: 25 m x 0.22 mm ID Initial Temp: 150 °C, 0 min Program Rate: 2 °C/min Final Temp: 210 °C, 5 min Carrier Gas: He, 15 psi Detector: FID, 280 °C Sensitivity: 32 x 10-¹²AFS Injection Mode: Split, 50:1 Column Part Number: 054602 Components 1. C14:0 2. C16:0 3. C16:1n7 4. C18:1n9 5. C18:1n7 6. C 18:2n6 7. C18:3n3 8. C18:4n3 9. C20:0 10. C20:1n9 11. C20:4n6 12. C20:5n3 13 16 14 12 11 8 9 7 6 10 5 2 15 30 minutes 4 15 0 1 3 To fully utilize the high thermal stability of BPX70 columns SGE recommend the use of helium when operating above 220/230°C for extended periods. EXPERTTIP Food, Flavors and FragrancesFood, Flavors and Fragrances 18For further information on our full range of products, please visit www.sge.com
For Fuels and Petrochemical analysis by GC, one of the main considerations is the thermal stability of the column, both physical and chemical. Phases must have high temperature limits to allow the analysis of high boiling point compounds and columns must be able to physically withstand repeated cycling to extreme temperatures. Columns such as SGE’s BPX1 and HT5 have been created with these demands in mind. Where higher polarity is required, such as the separation of aromatic compounds, SolGel-WAX™ and BPX90 provide enhanced selectivity without the unnecessary sacrifice of maximum temperature limits. Applications • Total Recoverable Petroleum Hydrocarbons (TRPH) Analysis on Standard and Fast BPX5 • Analysis of Polywax 655 and Refinery Lubrication Oil on HT5 • The Separation of Aromatics from Olefins in Petroleum Samples using BPX90 • Unleaded Gasoline on BPX5 • Fast GC For TPH Analysis • Simulated Distillation using BPX1-SimD Fuels and Petrochemical 19 For further information on our full range of products, please visit www.sge.com
TOTAL RECOVERABLE PETROLEUM HYDROCARBONS (TRPH) ANALYSIS ON STANDARD AND FAST BPX5 Chromatogram showing separation of Total Recoverable Petroleum Hydrocarbons using a conventional 30 m x 0.25 mm ID BPX5 column with a 0.25 micron film. Chromatogram showing separation of Total Recoverable Petroleum Hydrocarbon using a FAST BPX5 column. Phase: BPX5, 0.25 µm film TRPH (C8-C40): 5 ng/µL in dichloromethane Column: 30 m x 0.25 mm ID Initial Temp: 40 °C , 2 min Rate 1: 30 °C/min to 330 °C Rate 2: NA Final Temp: 330 °C, 9 min Detector Type: FID, 350 °C Carrier Gas: He, 14.4 psi Carrier Gas Flow : 1.29 mL/min Constant Flow: On Average Linear Velocity: 40 cm/sec at 40 °C Injection Mode: Split, 120:1 Purge On Time: NA Purge On (Split) Vent Flow: 160 mL/min Injection Volume: 1µL Injection Temperature: 250 °C Autosampler: Yes Liner Type : 4 mm ID FocusLiner™ with single taper Liner Part Number: 092003 Column Part Number: 054101 Phase: BPX5, 0.10 µm film TRPH (C8-C40) Standard: 5 ng/µL in dichlormethane Column: 10 m x 0.10 mm ID Initial Temp: 40 °C , 1 min Rate 1: 30 °C/min to 330 °C Rate 2: NA Final Temp: 330 °C, 0 min Detector Type: FID, 350 °C Carrier Gas: He, 28 psi Carrier Gas Flow : 0.52 mL/min Constant Flow: On Average Linear Velocity: 55 cm/sec at 40 °C Injection Mode: Split, 120:1 Purge On Time: NA Purge On (Split) Vent Flow: 62 mL/min Injection Volume: 1 µL Injection Temperature: 250 °C Autosampler: Yes Liner Type : 2.3 mm ID FocusLiner™ Liner Part Number: 092005 Column Part Number: 054099 NORMAL FAST C8 C10 C12 C14 C16 C18 C20 C22 C24 C26 C28 C30 C32 C34 C36 C38 C40 0 minutes 20 C8 C10 C12 C14 C16 C18 C20 C22 C24 C26 C28 C30 C32 C34 C36 C38 C40 0 minutes 10 ANALYSIS OF POLYWAX 655 AND REFINERY LUBRICATION OIL ON HT5 POLYWAX 655 AND REFINERY LUBRICATION OIL Phase: HT5, 0.1 µm Column: 6 m x 0.53 mm ID Initial Temp: 50 °C Rate: 10 °C/min Final Temp: 480 °C, 15 min Detector: FID Sensitivity: 40 x 10-¹² AFS Injection Mode: On-Column Carrier Gas: H2, 20 mL/min Solvent: CS₂ Column Part Number: 054661 POLYWAX 655 50 TEMPERATURE(°C) 480 REFINERY LUBRICATION OIL 320 450 570 650 700 750 boiling point (0°C) Fuels and Petrochemical 20For further information on our full range of products, please visit www.sge.com
The separation of a petroleum sample using a BPX90 column (30 m x 0.25 mm ID, 250 micron film) showing the resolution of aromatic families and the separation from more abundant alkanes. THE SEPARATION OF AROMATICS FROM OLEFINS IN PETROLEUM SAMPLES USING BPX90 UNLEADED GASOLINE ON BPX5 Sample Introduction: Injector Temp: 240 °C Injection Volume: 0.1 µL Autosampler Syringe: 0.5 µL Removable Needle Part No. 000410 Septa: Auto-Sep T™ Part No. 041882 Injection Type: Split Purge On Time: NA Purge On (Split) Vent: 200 mL/min Split Ratio: 149 :1 Liner Type: FocusLiner™ single taper Part No.092003 Pressure/Flow Values: Carrier Gas: He Constant Flow: On Pressure: 13.6 psi Column Flow: 1.34 mL/min Linear Velocity: 30 cm/sec @ 25 °C Oven Parameters: Initial Temp: 25 °C Initial Time: 1 min Rate 1: 30 °C/min Final Temp 1: 240 °C Hold Time: 1 min Run Time: 9.17 min Detector Parameters: Detector Type: FID @ 280 °C 2 4 1 5 3 0 2 4 6 min Components 1. Benzene 2. Toluene 3. Ethylbenzene 4. m,p-Xylene 5. o-Xylene Phase: BPX5, 0.25 µm film Column: 30 m x 0.25 mm ID Column Part Number: 054101 Fuels and Petrochemical 21 For further information on our full range of products, please visit www.sge.com
Reference Gas Oil MT-60CS2 Blank FAST GC FOR TPH ANALYSIS Phase: BPX5, 0.1 µm Column: 5 m x 0.1 mm ID Initial Temp: 50 °C Rate 1: 45 °C/min Final Temp: 300 °C, 0 min Detector Temp: 270 °C Detector: FID Carrier: He, Inlet pressure 40 psi (constant flow mode, linear velocity of 75 cm/sec) C8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 28 30 C32 0 1 2 3 4 5 6 minutes 20 60 100 140 pA Chromatogram of TPH standards from C8 to C32 Chromatogram showing elution of BTEX in under one minute Benzene Toluene Ethyl Benzene p-m, xylene o- xyleneC8 C12 0 0.5 1 1.5 2 minutes 20 60 100 140 pA 0302setunim010 10pA base line 25pA 420˚C SIMULATED DISTILLATION USING BPX1-SIMD Phase: BPX1, 0.1 µm Column: 5 m x 0.53 mm ID Initial Temp: 40 °C Rate: 15 °C Final Temp: 420 °C, 5 min Detector Temp: 440 °C Carrier Gas: He, 10 mL/min Instrument: HP 6890 Column Part Number: 054800 Separation Systems Injector Initial Temp: 40 °C Rate: 15 °C Final Temp: 420 °C, 5 min Standard mix for HTSD using BPX1-SimD setunim02010 C20 C40 C60 C80 C100 setunim02010 C60 C80 C40 C90 C110 C100 Enlarged section of the chromatogram above A portion of the previous chromatogram from C40 to the end of the analysis (expanded vertically) shows excellent resolution and the ability to see beyond C110. 0 10 minutes 20 30 3.2 min 200 400 pA 21.277 min IBP 0.6 5% -6.2 10% -3.4 20% -2.9 30% -1.1 40% 0.7 50% 1.1 60% 2.1 70% 2.3 80% 1.8 90% 1.2 95% 0.2 FRP 0.3 Gas Oil Reference All of the data presented was produced by Dr. Lubkowitz and the staff at Separation Systems Inc. on a system using the Separation System programmed temperature vaporization injector (PTV) and the SIMDIS EXPERT® software Fuels and Petrochemical 22For further information on our full range of products, please visit www.sge.com
For general chemical analysis, a good rule of thumb is to use the lowest polarity column that provides sufficient separation. Particular classes of compounds, such as alcohols, amines, or organic acids, may require thicker film phases, or specific phases such as the BPX35 or BP21 to avoid undue peak tailing. Applications • Analysis of 18 Alcohols on BP20 • Analysis of Aliphatic Alcohols on BP1 • Analysis of 15 Organic Acids on BP20 • US EPA 625 Phenols Mix on BPX50 • Analysis of Organic Acids in Water on BP21 • Analysis of Amines on BP1 • Analysis of Aromatic Amines on BP5 • Analysis of Aromatic Amines from Diazo Dyes on BPX35 • Analysis of Ketones on Thick Film BPX5 • Analysis of Triethylamine and Triethanolamine on SolGel-1ms™ ChemicalChemical 23 For further information on our full range of products, please visit www.sge.com
0201inutes0 m ANALYSIS OF 15 ORGANIC ACIDS ON BP20 Components 1. Valeric Acid 2. Caproic Acid 3. Heptanoic Acid 4. Octanoic Acid 5. Nonanoic Acid 6. Decanoic Acid 7. Undecanoic Acid 8. Dodecanoic Acid 9. Tridecanoic Acid 10. Tetradecanoic Acid 11. Pentadecanoic Acid 12. Hexadecanoic Acid 13. Heptadecanoic Acid 14. Octadecanoic Acid 15. Arachidic Acid ORGANIC ACIDS Phase: BP20, 0.25 µm Column: 30 m x 0.32 mm ID Initial Temp: 70 °C Rate: 10 °C/min Final Temp: 260 °C, 5 min Detector: FID Injection Mode: Split Carrier Gas: H2, 6 psi Column Part Number: 054433 1 2 3 4 5 6 7 8 9 1 0 1 2 1 1 1 3 1 4 1 5 ANALYSIS OF 18 ALCOHOLS ON BP20 0 2 4 6 8 10 12 minutes 1 2 3 4 5 6 7 8 9 1 0 1 1 1 2 1 4 1 5 1 6 1 7 1 8 1 3 Components 1. Methanol 2. Propan-2-ol 3. Ethanol 4. sec-Butan-1-ol 5. n-Propanol + 2-Methyl-3-Buten-2-ol 6. d,l-3-Methyl-2-Butan-1-ol 7. Pentan-3-ol 8. d,l-2-Pentan-1-ol 9. n-Butanol 10. 2,4-Dimethyl Pentan-3-ol 11. Hexan-3-ol 12. 2-Methyl Prop- 2-en-1-ol 13. Crotyl Alcohol (2-Buten-1-ol) 14. Hexan-2-ol 15. Pentan-1-ol 16. 2-Methyl Pentan-1-ol 17. 2-Ethyl Butan-1-ol 18.Hexan-1-ol ALCOHOLS Phase: BP20, 0.25 µm film Column: 30 m x 0.25 mm ID Initial Temp: 45 °C, 2 min Rate: 3 °C/min Final Temp: 80 °C, 0 min Detector: FID Sensitivity: 128 x 10-¹² AFS Injection Mode: Split Column Part Number: 054427 After installing a new column purge with oxygen free carrier gas for at least 30 minutes before heating GC oven. EXPERTTIP ANALYSIS OF ALIPHATIC ALCOHOLS ON BP1 0 minutes 10 76 5 4 321 Components 1. Octanol 2. Decanol 3. Undecanol 4. Dodecanol 5. Tetradecanol 6. Hexadecanol 7. Eicosanol ALCOHOLS Phase: BP1, 3.0 µm film Column: 12 m x 0.53 mm ID Initial Temp: 100 °C Rate: 10 °C/min Final Temp: 260 °C Carrier Gas: N2 Injection Volume: 0.1 µL Column Part Number: 054097 Chemical 24For further information on our full range of products, please visit www.sge.com
ANALYSIS OF AMINES ON BP1 Components 1. Aniline 2. Decylamine 3. Dicyclohexylamine 4. Dodecylamine 5. Tetradecylamine ANALYSIS OF AMINES Phase: BP1, 3.0 µm film Column: 12 m x 0.53 mm ID Initial Temp: 70 °C Rate: 10 °C/min Final Temp: 250 °C Carrier Gas: N2 Injection Volume: 0.1 µL Column Part Number: 054097 0 minutes 10 1 2 3 4 5 US EPA 625 PHENOLS MIX ON BPX50 US EPA 625 PHENOLS MIX Phase: BPX50, 0.25 µm Column: 30 m x 0.25 mm ID Injector Mode: Split, 40:1 Initial Oven Temp: 50°C, 1 min Rate 1: 8 °C/min Final Temp: 300 °C, 10 min Detector: HP 5973 MSD Column Part Number: 054751 8.00 10.00 12.00 14.00 18.0016.00 22.0020.00 1 3 7 98 2 4 5 6 10 30000 Abundance 20000 10000 Components 1. 2-Chlorophenol 2. 2-Nitrophenol 3. 2, 4-Dimethylphenol 4. 2, 4-Dichlorophenol 5. 4-Chloro-3-methylphenol 6. 2, 4, 6-Trichlorophenol 7. 2, 4- Dinitrophenol 8. 4-Nitrophenol 9. 2-Methyl-4, 6-dinitrophenol 10. Pentachlorophenol ANALYSIS OF ORGANIC ACIDS IN WATER ON BP21 SETUNIM510150 1 2 3 4 5 6 7 8 9 Components 1. Acetic Acid 2. Propanoic Acid 3. iso-Butyric Acid 4. n-Butyric Acid 5. iso-Valeric Acid 6. n-Valeric Acid 7. n-Caproic Acid 8. n-Heptanoic Acid 9. Lactic Acid ORGANIC ACIDS IN WATER (0.03M OXALIC ACID) Phase: BP21, 0.5 µm film Column: 30 m x 0.53 mm ID Initial Temp: 85 °C, 0 min Rate: 6 °C/min Final Temp: 180 °C, 5 min Detector: FID Sensitivity: 64 x 10-¹² AFS Injection Mode: On-Column Column Part Number: 054477 On-column injection and the addition of a 0.03M Oxalic acid (2%) to the injection solution increases the acidity of the column to allow lactic acid to be detected. EXPERTTIP Chemical 25 For further information on our full range of products, please visit www.sge.com
ANALYSIS OF AROMATIC AMINES FROM DIAZO DYES ON BPX35 Phase: BPX35 0.25 µm film Azo Dyes Standard: 10 ppm solution in DCM Column: 30 m x 0.25 mm ID Initial Temp: 50 °C, 2 min Rate 1: 15 °C/min to 240 °C Rate 2: 10 °C/min to 280 °C Final Temp: 280 °C, 25 min Detector Type: MSD Carrier Gas: He, 7.1 psi Carrier Gas Flow : 1.0 mL/min Constant Flow: On Average Linear Velocity: 36 cm/sec at 50 °C Injection Mode: Splitless Purge On Time: 1.0 min Purge On (Split) Vent Flow: 60 mL/min Injection Volume: 1 µL Injection Temperature: 250 °C Autosampler: No Liner Type : 4 mm ID Double Taper Liner Part Number: 092018 Column Part Number: 054701 Components 1. Indolin 2. o-Toluidine 3. 2,4-Diaminoanisole 4. p-Chloroailine 5. p-a residine 6. 2,4,6-Trimethylaniline 7. 4-Chlorotoludine 8. Unknown 9. 2-Naphtylamine 10. Unknown 11. 4-Aminodiphenyl 12. 4,4’-Oxydianiline 13. 4,4’-Diaminodiphenylmethane 14. Benzidine 15. 3,3’-Dimethyl- 4,4’diaminodiphenyl- methane 16. 3,3’-dimethylbenzidine 17. 4,4’-Thiodianiline 18. 3,3’-Dichlorobenzidine 19. 4,4’-Methylene- bis(2chloraniline) 20. 3,3’-Dimethoxybenzidine 10.0 15.0 20.0 25.0 30.0 0 100000 200000 300000 400000 500000 600000 700000 800000 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18, 19, 20 ANALYSIS OF AROMATIC AMINES ON BP5 Components 1. Pyridine 2. 2-Methyl Pyridine 3. gamma - BHC 4. Aniline 5. o-Toluidine 6. m-Toluidine 7. 2,6-Dimethylaniline 8. 1,4-Phenyldiamine 9. Nicotine 10. Biphenylamine 11. Bibenzylamine 21SETUNIM60 3 4 6 5 7 8 9 1 0 1 1 Phase: BP5, 1.0 µm film Column: 12 m x 0.53 mm ID Initial Temp: 60 °C, 0 min Rate: 10 °C/min Final Temp: 190 °C, 0 min Detector: FID Sensitivity: 128 x 10-¹²AFS Injection Mode: Split Column Part Number: 054197 Using a thicker film helps prevent amines from tailing. EXPERTTIP SilTite™ ferrules eliminate the need for re-tightening following temperature cycling and reduce oxygen levels within the system improving performance EXPERTTIP ChemicalChemical 26For further information on our full range of products, please visit www.sge.com
ANALYSIS OF KETONES ON THICK FILM BPX5 Phase: BPX5, 1.0 µm film Sample: 300 ppm in dichloromethane Column: 60 m x 0.25 mm ID Initial Temp: 40 °C , 5 min Rate 1: 10 °C/min to 80 °C Rate 2: 30 °C/min to 260 °C Final Temp: 260 °C, 4 min Detector Type: FID Detector Temp: 360 °C Carrier Gas: He, 27.6 psi Carrier Gas Flow : 1.9 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.4 µL Injection Temperature: 250 °C Autosampler: No Liner Type : 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054123 Components 1. Ethanol 2. Acetone 3. 2-Butanone 4. 3-Methyl-2-butanone 5. 2-Pentanone 6. 3-pentanone 7. 4-Methyl-2-pentanone 8. 3-Methyl-2-pentanone 9. 3-Hexanone 10. 2-Hexanone 11. Mesityl oxide 12. Cyclopentanone 13. 2-Methyl-3-hexanone 14. 4-Methyl-2-hexanone 15. 5-Methyl-2-hexanone 16. 3-Heptanone 17. 2-Heptanone 18. Cyclohexanone 19. 2-Octanone 20. 2-Nonanone 21. 2-Decanone 22. 2-Undecanone 23. 2-Dodecanone min4 6 8 10 12 14 16 pA 10 20 30 40 50 60 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 ANALYSIS OF TRIETHYLAMINE AND TRIETHANOLAMINE ON SOLGEL-1ms™ min0 2 4 6 8 10 12 14 16 18 counts 5000 10000 15000 20000 25000 30000 Triethanolamine Triethylamine Solvent Phase: SolGel-1ms, 0.25 µm film Amine mix: 10 ng/µL in dichloromethane Column: 30 m x 0.32 mm ID Initial Temp: 40 °C , 5.0 min Rate 1: 20 °C/min to 200 °C Final Temp: 200 °C, 7 min Detector Type: FID Detector Temp: 300 °C Carrier Gas: He, 9.9 psi Carrier Gas Flow : 2.2 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 100 °C Mode of Injection: Split Split Ratio: 50:1 Injection Volume: 0.3 µL Injection Temperature: 250 °C Autosampler: No Column Part Number: 054798 To prevent decreasing retention times in your chromatography, replace the septum daily. EXPERTTIP Chemical AnalysisChemical 27 For further information on our full range of products, please visit www.sge.com
GC analysis of Pharmaceuticals covers a wide range of compounds that can vary greatly in their molecular weight, reactivity,andpH.FromtheanalysisoflowmolecularweightresidualsolventsonaG43(BPX-Volatiles)tohighermolecular weight compounds on a G42 (BPX35), a wide range of GC columns are often specified in the test methods. Proper deactivation of GC consumables such as liners and columns becomes increasingly important where system inertness has to be demonstrated. SGE’s unique, high temperature gas phase deactivation ensures maximum inertness and minimal activity from our columns and consumables. Applications • USP Methods • Analysis of Tricyclic Antidepressants on BPX35 • Analysis of Dioxane Impurities on BP20 • Analysis of a Common Solvent Mixture on a Thick Film BPX5 • Analysis of a Common Pharmaceutical Solvent on BPX-Volatiles • Analysis of a Common Pharmaceutical Solvent on BPX-Volatiles • Analysis of Class I Solvents on BPX-Volatiles • Analysis of the Separation of the Class III Solvents on BPX-Volatiles Pharmaceutical 28For further information on our full range of products, please visit www.sge.com
Method Phase Composition SGE Phase Recommendation G1 Dimethylpolysiloxane oil BP1, SOLGEL-1ms™ G2 Dimethylpolysiloxane gum BP1, SOLGEL-1ms G3 50% Phenyl - 50% Methylpolysiloxane BPX50 G5 3-Cyanopropylpolysiloxane BPX70 G7 50% 3-Cyanopropyl - 50% Phenylmethylsilicone BP225 G14 Polyethylene glycol (average molecular weight of 950-1,050) BP20(WAX), SOLGEL-WAX™ G15 Polyethylene glycol (average molecular weight of 3,000-3,700) BP20(WAX), SOLGEL-WAX G16 Polyethylene glycol (average molecular weight of 15,000) BP20(WAX), SOLGEL-WAX G17 75% Phenyl - 25% Methylpolysiloxane BPX50 G19 25% Phenyl - 25% Cyanopropylmethylsilicone BP225 G20 Polyethylene glycol (average molecular weight of 380-420) BP20(WAX), SOLGEL-WAX G25 Polyethylene glycol TPA (Carbowax 20M terephthalic acid) BP21(FFAP) G27 5% Phenyl - 95% Methylpolysiloxane BP5, BPX5 G28 25% Phenyl - 75% Methylpolysiloxane BPX35 G32 20% Phenylmethyl - 80% Dimethylpolysiloxane BPX35 G35 Polyethylene glycol diepoxide esterified with nitroterephthalic acid BP21(FFAP) G36 1% Vinyl - 5% Phenylmethylpolysiloxane BP5, BPX5 G38 Phase G1 plus a tailing inhibitor BP1, SOLGEL-1ms G39 Polyethylene glycol (average molecular weight of 1,500) BP20(WAX), SOLGEL-WAX G41 Phenylmethyldimethylsilicone (10% phenyl substituted) BP5, BPX5 G42 35% Phenyl - 65% Dimethylvinylsiloxane BPX35 G43 6% Cyanopropylphenyl - 94% Dimethylpolysiloxane BP624 G46 14% Cyanopropylphenyl - 86% methylpolysiloxane BP10 (1701) USP Methods Fused Silica Tubing ETP multiplier Quality guaranteed• Chemically inert and thermally stable• Suitable for organic and aqueous solvents• Ideal for biotechnology applications• Custom-made tubing available upon request• Available deactivated for guard column material• Tubing protected with a high temperature• Polyimide resin (+400 ˚C) Air stable• 2 year shelf life guarantee• Discrete dynode design results in extend operating life• Total compatibility with all major quadrupole,• magnetic sector and TOF instruments 29 For further information on our full range of products, please visit www.sge.com
ANALYSIS OF Tricyclic Antidepressants on BPX35 TRICYCLIC ANTIDEPRESSANTS Phase: BPX35, 0.25 μm Column: 25 m x 0.22 mm ID Initial Temp: 210 °C, 1 min Rate: 5 °C/min Final Temp: 280 °C Carrier Gas: Helium, 150 kpa Injection Mode: Split (20:1) Detector: FID, 380 °C Column Part Number: 054711 Components 1. Amitriptyline 2. Trimipramine 3. Nortriptyline 4. Doxepin 5. Desipramine analysis of Dioxane Impurities on BP20 Phase: BP20, 1.0 μm Column: 25m x 0.53 mm ID Initial Temp.: 40°C, 2 min Rate: 10 °C/min Final Temp.: 120 °C Detector: FID, 280 °C Injector Mode: Split, 30:1, Carrier Gas: Hydrogen, 2 psi Injection Volume: 0.2 μL Column Part Number.: 054448 Components 1. Methanol 2. Dichloromethane 3. Ethanol 4. Dioxane impurity 5. Dioxane Analysis of a Common Solvent Mixture on a Thick Film BPX5 Phase: BPX5, 1.0 μm film Sample: neat Column: 60m x 0.25 mm ID Initial Temp: 32 °C, 5 min. Rate 1: 20 °C/min to 190 °C, Final Temp: 190°C, 2 min. Detector Type: FID Detector Temp.: 360 °C Carrier Gas: He, 26.9 psi Carrier Gas Flow: 1.9 mL/min. Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.3 μL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054123 Components 1. Methanol 2. Ethanol 3. Acetone 4. Isopropyl alcohol 5. Acetonitrile 6. Dichloromethane 7. 2-Butanone 8. Ethyl acetate 9. Benzene Pharmaceutical Pharmaceutical 30For further information on our full range of products, please visit www.sge.com
ANALYSIS OF Common pharmaceutical solvent on BPX-Volatiles Phase: BPX-Volatiles, 1.4 μm film Sample: 200 ppm in methanol Column: 30 m x 0.25 mm ID Initial Temp: 35 °C, 15 min Rate 1: 5 °C/min to 100 °C Final Temp: 100 °C, 2 min Detector Type: Mass Spectrometer Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 35 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.5 μL Injection Temp: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part No: 054980 Full Scan / SIM: Full scan 25-450 Components 1. Methanol 2. Ethanol 3. Ethyl ether 4. Acetone 5. iso-propyl alcohol 6. Acetonitrile 7. Methylene chloride 8. t-Butanol 9. Hexane 10. Propanol 11. 2-Butanone 12. Ethyl acetate 13. 2-Butanol 14. Tetrahydrofuran 15. Chloroform 16. Cyclohexane 17. Benzene 18. n-Heptane 19. n-Butanol 20. 1,4-Dioxane 21. Pyridine 22. Toluene 23. Dimethylformamide ANALYSIS OF Common pharmaceutical solvent on BPX-VOLATILES Phase: BPX-Volatiles 1.4 μm film USEPA 502.2 mix: 200 ppm in Methanol Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 0 min Rate 1: 6 °C to 210 °C Rate 2: 15 °C to 240 °C Final Temp: 240 °C, 5 min Detector Type: Mass Spectrometer Carrier Gas: He, 22.8 Carrier Gas Flow: 1.3 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 50:1 Injection Volume: 1 mL Injection Temp: 250 °C Autosampler: No Liner Type: 4mm ID Single Taper Liner Liner Part No: 092017 Column Part No: 054980 Full Scan / SIM: Full scan 45-450 Components 1. Dichlorodifluoromethane 2. Chloromethane 3. Vinyl chloride 4. Bromomethane 5. Chloroethane 6. Trichlorofluoromethane 7. 1,1-Dichloroethene 8. Dichloromethane 9. trans-1,2-Dichloroethene 10. 1,1-Dichloroethane 11. 2,2-Dichloropropane 12. cis-1,2-Dichloroethene 13. Bromochloromethane 14. Chloroform 15. 1,1,1-Trichloroethane 16. 1,1-Dichloropropene 17. Carbon tetrachloride 18. Benzene 19. 1,2-Dichloroethane 20. Trichloroethene 21. 1,2-Dichloropropane 22. Dibromomethane 23. Bromodichloromethane 24. cis-1,3-Dichloropropene 25. Toluene 26. trans-1,3- Dichloropropene 27. 1,1,2-Trichloroethane 28. Tetrachloroethene 29. 1,3-Dichloropropane 30. Dibromochloromethane 31. 1,2-Dibromoethane 32. Chlorobenzene 33. Ethylbenzene 34. 1,1,1,2-Tetrachloroethane 35. m-Xylene 36. p-Xylene 37. o-Xylene 38. Styrene 39. Bromoform 40. Isopropylbenzene 41. Bromobenzene 42. 1,1,2,2-Tetrachloroethane 43. 1,2,3-Trichloropropane 44. n-Propyl benzene 45. 2-Chlorotoluene 46. 1,3,5-Trimethylbenzene 47. 4-Chlorotoluene 48. tert-Butylbenzene 49. 1,2,4-Trimethylbenzene 50. sec-Butylbenzene 51. 1,3-Dichlorobenzene 52. p-Isopropyltoluene 53. 1,2-Dichlorobenzene 54. n-Butylbenzene 55. 1,4-Dichlorobenzene 56. 1,2-Dibromo-3- chloropropane 57. 1,2,4-Trichlorobenzene 58. Hexachlorobutadiene 59. Naphthalene 60. 1,2,3-Trichlorobenzene Pharmaceutical 31 For further information on our full range of products, please visit www.sge.com
ANALYSIS OF Class i solvents on bpx-volatiles Phase: BPX-Volatiles 1.4 μm film Sample: 200 ppm in methanol Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 6 °C/min to 80 °C Final Temp: 80 °C Detector Type: Mass Spectrometer Carrier Gas: He, 6.7 psi Carrier Gas Flow: 0.9 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 50 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.4 μL Injection Temp: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part No: 054980 Full Scan / SIM: Full scan 30-450 Components 1. 1,1-Dichloroethene 2. 1,1,1-Trichloroethane 3. Carbon tetrachloride 4. Benzene 5. 1,2-Dichloroethane ANALYSIS OF THE separation of THE CLASS III SOLVENTS ON BPX-VOLATILES Components 1. Pentene 2. Ethanol 3. Ethyl ether 4. Acetone 5. iso-Propyl alcohol 6. Ethyl formate 7. Methyl acetate 8. Dichloromethane 9. Methylt-butyl ether 10. n-Propanol 11. Ethyl acetate 12.2-Butanone (MEK) 13. Tetrahydrofuran 14. iso-Butanol 15. sec-Butanol 16. iso-Propyl acetate 17. Heptane 18. Acetic acid 19. n-Butanol 20. Propyl acetate 21. 4-Methyl-2-pentanone 22. Iso-Amyl alcohol 23. Iso-Butyl acetate 24. n-Amyl alcohol 25. Butyl acetate 26. Dimethyl sulfoxide Phase: BPX-Volatiles 1.4 μm film Sample: 200 ppm in methanol Column: 30 m x 0.25 mm ID Initial Temp: 50 °C, 5 min Rate 1: 10 °C/min to 85 °C, 1 min Rate 2: 15 °C/min to 170 °C, Final Temp: 170 °C Detector Type: Mass Spectrometer Carrier Gas: He, 6.7 psi Carrier Gas Flow: 0.9 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 50 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.4 μL Injection Temp: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part No: 054980 Pharmaceutical Pharmaceutical 32For further information on our full range of products, please visit www.sge.com
Forensic Forensic and Toxicology analyses face similar challenges as those found in pharmaceutical assays. These methods are often very challenging due to the analysis of very active compounds as well as coming from samples that are detrimental to GC systems. These compounds are generally basic in nature that makes inertness of the system components critical to successful determinations. The robustness is another critical aspect of clinical analyses. The natures of sample compounds and matrices are extremely arduous on the analytical system. SGE’s columns are designed to withstand these ordeals and provide excellent lifetimes in difficult analyses. Applications • Analysis of Acid/Neutral Drugs on BPX35 • Analysis of Basic Drugs on BPX35 • Analysis of Underivatized Barbiturates on BP5 • Analysis of Various Drugs on BPX50 • Analysis of a Variety of Antidepressant and Anticonvulsant Drugs on BPX50 Forensic 33 For further information on our full range of products, please visit www.sge.com
Analysis of Acid/Neutral Drugs on BPX35 Components 1. Ethosuximide 2. Barbital 3. Aprobarbital 4. Butabarbital 5. Amobarbital 6. Pentabarbital 7. Secobarbital 8. Meprobamate 9. Carisoprodal 10. Glutethimide 11. Phenobarbital 12. Methaqualone 13. Primidone ACID/NEUTRAL DRUGS Phase: BPX35, 0.25 μm Column: 25 m x 0.22 mm ID Initial Temp: 100 °C, 1min Rate: 10 °C/min Final Temp: 300 °C, 5 min Carrier Gas: He, 150 kpa Injection Mode: Split, ( 20:1 ) Detector: FID, 380 °C Column Part Number: 054711 Analysis of Basic Drugs on BPX35 Components (Concentration: 100-200 ug/ml) 1. Benzocaine 2 Unknown 3. Meperidine 4. Diphenhydramine 5. Lidocaine 6. Tripelennamine 7. Amitriptyline 8. Tetracaine 9. Pyrilamine 10. Unknown 11. Diazepam 12. Flurazepam 13. Papaverine 14. Triazolam BASIC DRUGS Phase: BPX35, 0.25 μm Column: 25m x 0.22 mm ID Initial Temp: 100 °C Rate: 5 °C/min Final Temp.: 325 °C, 5 min. Carrier Gas: Helium 150 kpa Injection Mode: Split, 0.5 μL (20:1) Detector: FID, 380 °C Column Part Number: 054711 Forensic 34For further information on our full range of products, please visit www.sge.com
Analysis of Underivatized Barbiturates on BP5 Components 1. Barbital 2. Butabarbital 3. Amobarbital 4. Pentabarbital 5. Secobarbital 6. Hexabarbital UNDERIVATIZED BARBITURATES Phase: BP5, 1.0 μm Column: 12m x 0.53 mm I.D. Temp: 195 °C Carrier Gas: Hydrogen Carrier Flow: 10 mL/min Injection Volume: 0.1 μL Column Part Number: 054197 Analysis of Various Drugs on BPX50 Components 1. N,N-Dimethylaniline 2. Benzothiazole 3. Selegeline 4. Pethidine 5. Unknown 6. a-octadecene 7. Octadecanoic acid butyl ester 8. Methadone 9. N,N-Dimethylstearamide 10. Chloroquine 11. Dextromoramide 12. Sitosterol 13. Buspirone Phase: BPX50, 0.25 μm film Sample: 5-10 ppm in methanol Column: 30 m x 0.25 mm ID Initial Temp: 150 °C, 0.5 min. Rate 1: 10 °C/min to 180 °C, Rate 2: 1.5 °C/min to 220 °C Rate 2: 30 °C/min to 260 °C Final Temp: 260 °C, 5 min. Detector Type: FID Detector Temp.: 320 °C Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min. Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Splitless Purge on Time: 0.5 min Purge on (Split) Vent Flow: 60 mL/min Injection Volume: 1 μL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054751 Full Scan / SIM: Full scan 45-450 Forensic 35 For further information on our full range of products, please visit www.sge.com
Analysis of a Variety of Antidepressant and Anticonvulsant Drugs on BPX50 Components 1. Benzothiazole 2. Selegeline 3. Methsuximide 4. Ketamine 5. Unknown 6. Brompheniramine 7. Imipramine 8. Mianserin 9. Diothiepin 10. Carbamazepine 11. Prazepam 12. Diltiazem 13. Pholcodine Phase: BPX50, 0.25 μm film Sample: 5-10 ppm in methanol Column: 30 m-x 0.25 mm ID Initial Temp: 150 °C, 0.5 min. Rate 1: 10 °C/min to 180 °C, Rate 2: 1.5 °C/min to 220 °C Rate 2: 30 °C/min to 260 °C Final Temp: 260 °C, 5 min. Detector Type: FID Detector Temp.: 320 °C Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min. Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Splitless Purge on Time: 0.5 min Purge on (Split) Vent Flow: 60 mL/min Injection Volume: 1 μL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054751 Full Scan / SIM: Full scan 45-450 Acenaphytlene 2-Chlorophenol Decylamine Undecanol 4 mm ID liner with quartz wool in center of liner (incorrectly positioned) SGE FocusLiner ™ (quartz wool correctly positioned) Promoting uniform sample vaporization Maximizing sample vaporization on an inert surface Acting as a particulate filter for dirty samples Improving injection reproducibility 10-fold Wiping needle tip during injection through fixed quartz wool Liner deactivated at high temperatures with wool in situ using SGE’s high quality deactivation processes FocusLiner™ improves reproducibility by: Forensic 36For further information on our full range of products, please visit www.sge.com
SGE Capillary Column Part Number Listing Phase Length (m) ID (mm) Film Thickness (µm) Part No. BP1 10 0.1 0.1 054022 BP1 12 0.15 0.25 054028 BP1 25 0.15 0.25 054029 BP1 12 0.22 0.1 054040 BP1 12 0.22 0.25 054046 BP1 12 0.22 1 054052 BP1 15 0.22 0.25 054049 BP1 25 0.22 0.1 054041 BP1 25 0.22 0.25 054047 BP1 25 0.22 1 054053 BP1 30 0.22 0.25 054050 BP1 50 0.22 0.1 054042 BP1 50 0.22 0.25 054048 BP1 50 0.22 1 054054 BP1 60 0.22 0.25 054051 BP1 15 0.25 0.1 054039 BP1 15 0.25 0.25 054043 BP1 30 0.25 0.25 054044 BP1 30 0.25 0.5 054820 BP1 30 0.25 1 054056 BP1 60 0.25 0.25 054045 BP1 60 0.25 0.5 054812 BP1 60 0.25 1 054815 BP1 12 0.32 0.25 054058 BP1 12 0.32 0.5 054064 BP1 12 0.32 1 054070 BP1 15 0.32 0.25 054061 BP1 25 0.32 0.25 054059 BP1 25 0.32 0.5 054065 BP1 25 0.32 1 054071 BP1 25 0.32 4 054076 BP1 25 0.32 5 054081 BP1 30 0.32 0.25 054062 BP1 30 0.32 0.5 054068 BP1 30 0.32 1 054813 BP1 30 0.32 1.5 054811 BP1 30 0.32 3 054073 BP1 30 0.32 4 054077 BP1 50 0.32 0.25 054060 BP1 50 0.32 0.5 054066 BP1 50 0.32 1 054072 BP1 50 0.32 5 054082 BP1 60 0.32 0.25 054067 BP1 60 0.32 0.5 054069 BP1 60 0.32 1 054810 BP1 60 0.32 5 054085 BP1 12 0.53 1 054086 BP1 12 0.53 3 054097 BP1 15 0.53 0.5 054870 BP1 15 0.53 1 054089 BP1 25 0.53 1 054087 BP1 25 0.53 3 054098 BP1 25 0.53 5 054095 BP1 30 0.53 0.5 054092 BP1 30 0.53 1 054090 BP1 30 0.53 2.6 054819 BP1 30 0.53 3 054808 BP1 30 0.53 5 054806 BP1 50 0.53 1 054088 BP1 50 0.53 5 054096 BP1 60 0.53 0.5 054871 BP1 60 0.53 3 054809 BP1 60 0.53 5 054807 BP1-PONA 50 0.15 0.5 054950 BP1-PONA 100 0.25 0.5 054818 BPX1 10 0.1 0.1 054777 BPX1 6 0.53 2.65 0548025 BPX1 10 0.53 0.1 054803 BPX1 10 0.53 0.9 054801 BPX1 10 0.53 2.65 054802 BPX1 Aluminum Clad 5 0.53 0.1 054800 BPX1 Aluminum Clad 5 0.53 0.17 054782 BPX1 Aluminum Clad 10 0.53 0.1 054779 BPX1 10 0.53 2.65 054802 BPX1 Aluminum Clad 5 0.53 0.1 054800 BPX1 Aluminum Clad 5 0.53 0.17 054782 BPX1 Aluminum Clad 10 0.53 0.1 054779 SolGel-1ms 30 0.25 0.25 054795 Phase Length (m) ID (mm) Film Thickness (µm) Part No. SolGel-1ms 60 0.25 0.25 054793 SolGel-1ms 30 0.32 0.25 054798 SolGel-1ms 60 0.32 0.25 054794 BP5 12 0.22 0.25 054167 BP5 25 0.22 0.25 054168 BP5 30 0.22 0.25 054171 BP5 50 0.22 0.25 054169 BP5 50 0.22 1 054175 BP5 15 0.25 0.25 054182 BP5 30 0.25 0.25 054183 BP5 30 0.25 1 054203 BP5 60 0.25 0.25 054184 BP5 60 0.25 1 054215 BP5 12 0.32 0.25 054179 BP5 15 0.32 0.25 054176 BP5 25 0.32 0.25 054180 BP5 25 0.32 0.5 054186 BP5 25 0.32 1 054192 BP5 30 0.32 0.25 054177 BP5 30 0.32 0.5 054216 BP5 30 0.32 1 054189 BP5 50 0.32 0.5 054187 BP5 50 0.32 1 054193 BP5 60 0.32 0.25 054178 BP5 60 0.32 1 054188 BP5 12 0.53 1 054197 BP5 15 0.53 1 054194 BP5 15 0.53 1.5 054199 BP5 25 0.53 1 054198 BP5 30 0.53 0.5 0541935 BP5 30 0.53 1 054195 BP5 30 0.53 5 054196 BP5 60 0.53 1.5 054204 BPX5 10 0.1 0.1 054099 BPX5 10 0.15 1.2 054106 BPX5 12 0.15 0.25 054103 BPX5 12 0.15 0.4 054107 BPX5 25 0.15 0.25 054104 BPX5 25 0.15 0.4 054108 BPX5 30 0.15 0.15 054110 BPX5 50 0.15 0.25 054105 BPX5 40 0.18 0.18 054229 BPX5 12 0.22 0.25 054112 BPX5 25 0.22 0.25 054113 BPX5 25 0.22 1 054116 BPX5 30 0.22 0.25 054142 BPX5 50 0.22 0.25 054114 BPX5 50 0.22 1 054117 BPX5 7 0.25 0.25 054149 BPX5 15 0.25 0.1 0542170 BPX5 15 0.25 0.25 054100 BPX5 15 0.25 1 054121 BPX5 30 0.25 0.1 0541011 BPX5 30 0.25 0.25 054101 BPX5 30 0.25 0.5 0541025 BPX5 30 0.25 1 054122 BPX5 60 0.25 0.25 054102 BPX5 60 0.25 1 054123 BPX5 6 0.32 1 0541261 BPX5 12 0.32 0.25 054118 BPX5 12 0.32 0.5 054124 BPX5 12 0.32 1 054127 BPX5 15 0.32 0.25 054144 BPX5 15 0.32 1 054152 BPX5 25 0.32 0.25 054119 BPX5 25 0.32 0.5 054125 BPX5 25 0.32 1 054128 BPX5 25 0.32 3 054136 BPX5 30 0.32 0.25 054145 BPX5 30 0.32 0.5 0541205 BPX5 30 0.32 1 054153 BPX5 50 0.32 0.25 054120 BPX5 50 0.32 0.5 054126 BPX5 50 0.32 1 054129 BPX5 60 0.32 0.25 054146 BPX5 60 0.32 1 054154 BPX5 12 0.53 0.25 054133 BPX5 12 0.53 1 054130 37 For further information on our full range of products, please visit www.sge.com
SGE Capillary Column Part Number Listing Phase Length (m) ID (mm) Film Thickness (µm) Part No. BPX5 12 0.53 3 054138 BPX5 15 0.53 0.5 0541344 BPX5 15 0.53 1 054147 BPX5 15 0.53 1.5 0541347 BPX5 15 0.53 3 054159 BPX5 25 0.53 0.25 054134 BPX5 25 0.53 1 054131 BPX5 25 0.53 3 054139 BPX5 30 0.53 0.5 0541345 BPX5 30 0.53 1 054148 BPX5 30 0.53 1.5 0541348 BPX5 30 0.53 3 054160 BPX5 50 0.53 1 054132 BPX5 60 0.53 1 054158 HT5 12 0.22 0.1 054631 HT5 25 0.22 0.1 054632 HT5 15 0.25 0.1 054633 HT5 30 0.25 0.1 054634 HT5 12 0.32 0.1 054641 HT5 15 0.32 0.5 054667 HT5 25 0.32 0.1 054642 HT5 30 0.32 0.5 054668 HT5 6 0.53 0.1 054655 HT5 10 0.53 0.5 054670 HT5 12 0.53 0.15 054657 HT5 15 0.53 0.5 054671 HT5 25 0.53 0.15 054658 HT5 30 0.53 0.5 054672 HT5 Aluminum Clad 12 0.22 0.1 054635 HT5 Aluminum Clad 25 0.22 0.1 054636 HT5 Aluminum Clad 12 0.32 0.1 054651 HT5 Aluminum Clad 25 0.32 0.1 054652 HT5 Aluminum Clad 50 0.32 0.1 054653 HT5 Aluminum Clad 5 0.53 0.075 054673 HT5 Aluminum Clad 6 0.53 0.1 054661 HT5 Aluminum Clad 12 0.53 0.15 054662 HT5 Aluminum Clad 25 0.53 0.15 054665 HT8 10 0.1 0.1 054690 HT8 40 0.18 Proprietary 054686 HT8 12 0.22 0.25 054674 HT8 25 0.22 0.25 054675 HT8 50 0.22 0.25 054676 HT8 30 0.25 0.25 054677 HT8 60 0.25 0.25 054683 HT8 12 0.32 0.25 054679 HT8 25 0.32 0.25 054680 HT8 50 0.32 0.25 054681 HT8 60 0.32 0.25 054682 HT8 12 0.53 0.5 054684 HT8 25 0.53 0.5 054685 BPX35 10 0.1 0.1 054699 BPX35 15 0.22 0.25 054713 BPX35 25 0.22 0.25 054711 BPX35 30 0.22 0.25 054714 BPX35 50 0.22 0.25 054712 BPX35 15 0.25 0.25 054700 BPX35 15 0.25 1 054703 BPX35 30 0.25 0.25 054701 BPX35 30 0.25 0.5 0547025 BPX35 30 0.25 1 054704 BPX35 60 0.25 0.25 054702 BPX35 60 0.25 1 054705 BPX35 15 0.32 0.25 054723 BPX35 15 0.32 0.5 054718 BPX35 15 0.32 1 054716 BPX35 25 0.32 0.25 054721 BPX35 30 0.32 0.25 054724 BPX35 30 0.32 0.5 0547158 BPX35 30 0.32 1 054717 BPX35 50 0.32 0.25 054722 BPX35 60 0.32 0.25 054725 BPX35 15 0.53 0.5 054734 BPX35 15 0.53 1 054736 BPX35 30 0.53 0.5 054735 BPX35 30 0.53 1 054737 BPX608 25 0.32 0.4 054823 BP624 25 0.22 1.2 054826 BP624 30 0.22 1.2 054827 Phase Length (m) ID (mm) Film Thickness (µm) Part No. BP624 15 0.25 1.4 054839 BP624 30 0.25 1.4 054840 BP624 60 0.25 1.4 054842 BP624 25 0.32 1.8 054830 BP624 30 0.32 1.8 054832 BP624 50 0.32 1.8 054831 BP624 60 0.32 1.8 054841 BP624 25 0.53 3 054834 BP624 30 0.53 3 054836 BP624 50 0.53 3 054835 BP624 60 0.53 3 054838 BPX-Volatiles 20 0.18 1 054978 BPX-Volatiles 40 0.18 1 054979 BPX-Volatiles 30 0.25 1.4 054980 BPX-Volatiles 60 0.25 1.4 054981 BPX-Volatiles 30 0.32 1.8 054982 BPX-Volatiles 60 0.32 1.8 054983 BPX-Volatiles 30 0.53 3 054984 BPX-Volatiles 60 0.53 3 054985 BP10 12 0.22 0.25 054252 BP10 25 0.22 0.25 054253 BP10 50 0.22 0.25 054254 BP10 15 0.25 0.25 054255 BP10 30 0.25 0.25 054256 BP10 30 0.25 1 054271 BP10 60 0.25 0.25 054257 BP10 15 0.32 0.25 054258 BP10 15 0.32 0.5 054264 BP10 25 0.32 0.25 054262 BP10 25 0.32 0.5 054268 BP10 30 0.32 0.25 054259 BP10 30 0.32 0.5 054265 BP10 30 0.32 1 054270 BP10 50 0.32 0.5 054269 BP10 60 0.32 0.25 054260 BP10 60 0.32 0.5 054266 BP10 15 0.53 1 054282 BP10 25 0.53 1 054280 BP10 30 0.53 1 054283 BPX50 10 0.1 0.05 054739 BPX50 10 0.1 0.07 054738 BPX50 10 0.1 0.1 054740 BPX50 30 0.15 0.15 054741 BPX50 15 0.25 0.25 054750 BPX50 30 0.25 0.25 054751 BPX50 60 0.25 0.25 054752 BPX50 15 0.32 0.25 054760 BPX50 30 0.32 0.25 054761 BPX50 60 0.32 0.25 054762 BPX50 15 0.53 0.5 054770 BPX50 30 0.53 0.5 054771 BPX50 30 0.53 1 054772 BP225 25 0.22 0.25 054352 BP225 50 0.22 0.25 054353 BP225 25 0.32 0.25 054358 BP225 25 0.53 0.5 054364 BP20 10 0.1 0.1 054405 BP20 12 0.22 0.25 054420 BP20 25 0.22 0.25 054421 BP20 30 0.22 0.25 054424 BP20 50 0.22 0.25 054422 BP20 60 0.22 0.25 054425 BP20 15 0.25 0.25 054426 BP20 30 0.25 0.25 054427 BP20 30 0.25 0.5 054415 BP20 30 0.25 1 054439 BP20 60 0.25 0.25 054428 BP20 60 0.25 0.5 054458 BP20 15 0.32 0.25 054432 BP20 25 0.32 0.25 054430 BP20 25 0.32 0.5 054436 BP20 25 0.32 1 054442 BP20 30 0.32 0.25 054433 BP20 30 0.32 0.5 054438 BP20 30 0.32 1 054444 BP20 50 0.32 0.25 054431 BP20 50 0.32 0.5 054437 BP20 50 0.32 1 054443 38For further information on our full range of products, please visit www.sge.com
SGE Capillary Column Part Number Listing Phase Length (m) ID (mm) Film Thickness (µm) Part No. BP21 30 0.53 0.5 054477 BP21 30 0.53 1 054478 BPX70 10 0.1 0.2 054600 BPX70 12 0.22 0.25 054601 BPX70 25 0.22 0.25 054602 BPX70 30 0.22 0.25 054612 BPX70 50 0.22 0.25 054603 BPX70 60 0.22 0.25 054613 BPX70 15 0.25 0.25 054621 BPX70 30 0.25 0.25 054622 BPX70 60 0.25 0.25 054623 BPX70 120 0.25 0.25 054624 BPX70 12 0.32 0.25 054605 BPX70 25 0.32 0.25 054606 BP21 50 0.32 0.25 054469 BP21 60 0.32 0.25 054472 BP21 12 0.53 0.5 054473 BP21 15 0.53 0.5 054476 BP21 25 0.53 0.5 054474 BP21 30 0.53 0.5 054477 BP21 30 0.53 1 054478 BPX70 10 0.1 0.2 054600 BPX70 12 0.22 0.25 054601 BPX70 25 0.22 0.25 054602 BPX70 30 0.22 0.25 054612 BPX70 50 0.22 0.25 054603 BPX70 60 0.22 0.25 054613 BPX70 15 0.25 0.25 054621 BPX70 30 0.25 0.25 054622 BPX70 60 0.25 0.25 054623 BPX70 120 0.25 0.25 054624 BPX70 12 0.32 0.25 054605 BPX70 25 0.32 0.25 054606 BPX90 15 0.25 0.25 054570 BPX90 15 0.32 0.50 054573 BPX90 30 0.25 0.25 054580 BPX90 60 0.25 0.25 054590 BPX90 60 0.32 0.50 05493 BPX90 30 0.25 0.25 054980 Phase Length (m) ID (mm) Film Thickness (µm) Part No. BP20 60 0.32 0.25 054434 BP20 60 0.32 0.5 054457 BP20 60 0.32 1 054445 BP20 12 0.53 1 054447 BP20 12 0.53 2 054455 BP20 15 0.53 0.5 054961 BP20 15 0.53 1 054450 BP20 25 0.53 1 054448 BP20 25 0.53 2 054456 BP20 30 0.53 0.5 054440 BP20 30 0.53 1 054451 BP20 60 0.53 0.5 054963 BP20 60 0.53 1 0544515 SolGel-WAX™ 30 0.25 0.25 054796 SolGel-WAX™ 30 0.25 1 054787 SolGel-WAX™ 60 0.25 0.25 054791 SolGel-WAX™ 30 0.32 0.25 054788 SolGel-WAX™ 30 0.32 0.5 054797 SolGel-WAX™ 60 0.32 0.25 054789 SolGel-WAX™ 60 0.32 0.5 054792 SolGel-WAX™ 30 0.53 0.5 054786 SolGel-WAX™ 30 0.53 1 054785 BP21 25 0.22 0.25 054462 BP21 50 0.22 0.25 054463 BP21 15 0.25 0.25 054464 BP21 30 0.25 0.25 054465 BP21 60 0.25 0.25 054466 BP21 12 0.32 0.25 054467 BP21 15 0.32 0.25 054470 BP21 25 0.32 0.25 054468 BP21 30 0.32 0.25 054471 BP21 50 0.32 0.25 054469 BP21 60 0.32 0.25 054472 BP21 12 0.53 0.5 054473 BP21 15 0.53 0.5 054476 BP21 25 0.53 0.5 054474 BP21 30 0.53 0.5 054477 BP21 30 0.53 1 054478 BP21 25 0.53 0.5 054474 Column to Replace Description SGE Phase DB-1, HP-1, Ultra-1, SPB-1, CP-Sil 5CB, RSL-150, RSL-160, Rtx®-1, ZB-1, CB-1, OV®-1, PE-1, 007-1(MS), SP-2100, SE-30, RH-1, CC-1, CP-Sil 5CB MS, VF-1ms, Petrocol DH 100% Dimethyl Polysiloxane BP1 Unique highly inert phase SolGel + 100% Dimethyl Polysiloxane SolGel-1ms™ DB-HT Sim Dis, DB-2887, Rtx-2887, HP-1, Petrocol 2887, Petrocol EX2887 100% Dimethyl Polysiloxane BPX1 Petrocol DH, DB-Petro 100% Dimethyl Polysiloxane BP1-PONA DB-5, DB-5.625, Rtx-5, HP-5, Ultra-2, PTE-5, PB-5, MDN-5, CP-Sil 8CB, VB-5 ZB-5 5% Phenyl Polysiloxane BP5 DB-5, DB-5ms, HP-5, Ultra-2, Rtx®-5, Rtx-5Sil MS, Rtx 5MS, AT-5, AT-5MS, 007-5MS, SPB-5,CP-Sil 8CB, VF-5ms, RSL-200, CB-5, OV®-5, PE-5, 007-2(MPS-5), SE-52, SE-54, XTI-5, PTE-5, CC-5, RH-5ms, ZB-5 5% Phenyl Polysilphenylene-siloxane BPX5 MXT-1 SimDist, HT-SimDist, DistCB, MXT-500 5% Phenyl Polycarborane-siloxane HT5 No equivalent, unique high temperature column with special selectivity 8% Phenyl Polycarborane-siloxane HT8 DB-35, DB-35ms, Rtx-35, HP-35, HP-35MS, SPB-35, MDN-35, VB-50, ZB-35 35% Phenyl Polysilphenylene-siloxane BPX35 DB-608, Rtx-35, SPB-608 35% Phenyl Polysilphenylene-siloxane BPX608 OV-17, SP-2250, DB-17ms, DB-17ht, Rtx-50, SPB-50, HP-50+, HP-17, VB-50/608, ZB-50 50% Phenyl Polysilphenylene-siloxane BPX50 DB-23, CP-Sil 88, VF-23ms, SP-2330, SP-2380, Rtx®-2330, 007-23, AT-Silar, PE-23 70% Cyanopropyl Polysilphenylene-siloxane BPX70 Unique highly inert phase SolGel + Polyethylene Glycol SolGel-WAX™ DB-Wax, Rtx-Wax, Stabilwax, HP20M, HP-Wax, HP-INNOWax, Supelcowax-10, AT-Wax, Nukol, CP Wax 2CB, VB-WAX, ZB-WAX Polyethylene Glycol BP20 (Wax) DB-FFAP, HP-FFAP, Stabilwax-DA, CP Wax 58CB, VB-FFAP, ZB-FFAP Polyethylene Glycol (TPA treated) BP21 (FFAP) DB-1701, Rtx-1701, HP-1701, SPB-7, CP-Sil 19CB, VB-1701, ZB-1701 14% Cyanopropylphenyl Polysiloxane BP10 (1701) HP-225, DB-225, Rtx-225 50% Cyanopropylphenyl Polysiloxane BP225 DB-624, HP-VOC, Rtx Volatiles, VOCOL, VB-624, ZB-624 Cyanopropylphenyl Polysiloxane BP624, BPX-Volatiles Cyclodex-B, Rt-BDEXm Permethylated Beta Cyclodextrin CYDEX-B Unique highly polar phase 90% Cynopropyl Polysilphenylene-siloxane BPX90 GC Column Replacement Guide 39 For further information on our full range of products, please visit www.sge.com
GC Troubleshooting and Maintenance Symptom Possible cause Solution High baseline level Septum bleed and/or contaminated liner Replace septa and insert a new inlet liner. Poor carrier gas quality causing phase decomposition Ensure gas traps are installed correctly to remove moisture, organics and oxygen. Ensure high purity carrier gas is used. Maximum temperature of the phase has been exceeded Lower maximum program temperature. Highly acid or alkaline samples Neutralize sample before injecting Dirty samples Filter sample. Use a FocusLiner™. Dilute sample. Contaminated solvent Use a high purity solvent. Split peaks Poor manual injection technique Increase the plunger depression speed. Mixed solvent Change to a single solvent Compound degradation Can happen with some pesticides. Lower injector temperature. Recondition capillary column and re-inject sample. Column inserted too far into injector Reposition column according to manufacturer’s instructions. Fronting peaks Too much sample injected on to column Dilute sample. Use a thicker film. Increase the split ratio. Tailing peaks Column contamination Cut 50cm off the front of the column and re-install in the injector. Recondition column. Sample not suitable for phase polarity Choose a more polar column. Poorly deactivated inlet liner Replace with a new fully deactivated inlet liner. Graphite ferrule contamination in the start of the column Cut 5cm off the front of the column and re-install in the injector Broad peaks Make-up gas flow rate for atmospheric detectors is low Increase make up gas flow according to manufacturer’s instructions. Carrier gas flow is low Check carrier gas flow. Split gas flow is too low Increase split flow or use the ‘solvent effect’ to focus peaks. Column contamination Cut 50cm off the front of the column and re-install in the injector. Co-elution of peaks Change column polarity or lower temp. program ramp rate to separate peaks. Change in sample concentration Check injector conditions are reproducible e.g. temperature and split ratio. Mass spectrometer sampling rate is too low causing Increase sampling rate or reduce number of ions detected in SIM mode. triangular-looking peaks Shifting Leaking septum Tighten septum cap or replace with new septum. retention times Carrier gas velocity has changed Verify carrier gas flow rate. Check inlet pressure on GC. Ensure pressure in gas line and gas cylinder is OK Method temperature has changed Re-check temperature method conditions Column dimensions and film thickness have changed after Re-check dimensions on column tag against column description. installing a new column Sample concentration has changed – more has been Dilute sample or increase split ratio. injected on column Dirty column. Extra non-volatile material deposited on Cut 50cm off the front of the column and re-install in the injector the column has caused a change in column polarity Recondition column. Loss of Aging column has resulted in a substantial loss of phase Replace column. peak resolution causing a loss in column resolving power Method temperature has changed Re-check temperature method conditions Carrier gas velocity has changed Re-check carrier gas velocity and optimize to Van Deemter optima. Dirty column. Extra non-volatile material deposited on Cut 50cm off the front of the column and re-install in the injector. the column has caused a change in column polarity Manual injection technique or operator has changed Ensure technique is consistent. No peaks GC incorrectly wired Check all connections from GC to computer / integrator. Wrong detector is being monitored Check injector number is consistent with detector number being monitored. FID flame is out If using water, reduce injection volume. Water can extinguish the flame. Check flame gas pressures Syringe is blocked or leaking around plunger Use a known good syringe to confirm this is the problem. Massive leak in system Check all column and injector connections. Check column for breakage. This can sometimes be difficult to locate as the fused silica can break leaving the polyimide outer coating intact. Column is blocked Cut 5cm off the front and back ends of the column and re-install. Loss of sensitivity Concentration of sample has changed Re-confirm with a known standard concentration injection. Flame gas flow rates and/or make-up gas flow have changed Check flame gas pressures System has become active Replace inlet liner with a new deactivated liner. Cut 50cm off the front of the column, re-install in the injector and re-condition the column Splitless conditions have changed Re-check solvent and method temperatures. Ghost peaks Syringe has become contaminated from previous sample Ensure syringe has been thoroughly washed with solvent between injections. Sometimes this can involve 20 solvent rinses. New standards have impurities Confirm by using a different source of primary standards. Impurities in solvent Use a different type of solvent or confirm by using a different source of the same solvent. Septum bleed Can appear as discrete peaks in temperature program runs. Will disappear with isothermal analysis. Replace septum. Could also be from sample vial septa Peaks are still eluting from previous run Peaks will appear broader for that part of the chromatogram. Confirm by extending run time and ensuring all peaks have eluted from sample. Flashback has happened Inject twice the amount of pure solvent (this may need to be repeated). Carrier gas lines may also need to be cleaned 40For further information on our full range of products, please visit www.sge.com
Authorized Distributor BR-0307-C_RevE©CopyrightSGEAnalyticalSciencePtyLtd07/2010 AUSTRALIA PACIFIC REGION SGE Analytical Science Pty Ltd Toll Free: 1800 800 167 Tel: +61 (0) 3 9837 4200 Fax: +61 (0) 3 9874 5672 Email: support@sge.com EUROPE SGE Europe Ltd European Head Office Toll Free: 00800 2790 8999 Toll Free Fax: 00800 2626 2609 Tel: +44 1908 568 844 Fax: +44 1908 566 790 Tel France: +33 1 69 29 80 90 Fax France: +33 1 69 29 09 25 Tel Germany: +49 (0) 6155 / 60746 0 Fax Germany: +49 (0) 6155 / 60746 50 Email: europe@sge.com CHINA SGE Shanghai Representative Office Tel: +86 21 6407 9382 Fax: +86 21 6407 9386 Email: china@sge.com INDIA SGE Laboratory Accessories Pvt Ltd Tel: +91 22 24715896 Fax: +91 22 24716592 Email: sgeindia@vsnl.com JAPAN SGE Japan Inc Tel: +81 45 222 2885 Fax: +81 45 222 2887 Email: japan@sge.com MIDDLE EAST SGE Gulf Tel: +971 6 557 3341 Fax: +971 6 557 3541 Email: gulfsupport@sge.com UNITED STATES OF AMERICA SGE Incorporated Toll Free: (800) 945 6154 Tel: +1 512 837 7190 Fax: +1 512 836 9159 Email: usa@sge.com www.sge.com

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SGE GC Application Guide

  • 1. Applications Guide Environmental Food, Flavors and Fragrances ForensicChemical Fuels and Petrochemical Pharmaceutical 5 years 1 9 6 0 - 2 0 1 0 AUSTRALIA & PACIFIC REGION CHINA EUROPE INDIA JAPAN MIDDLE EAST USA
  • 2. For further information on our full range of products, please visit www.sge.com SGE Capillary Columns SGE Analytical Science Few companies can claim to be able to provide a total solution for analytical science; SGE is one of those few. From sample preparation, to injection, the separation and throughout the chromatographic process in either LC or GC there is a SGE product that has been designed to provide you with the results you need time and again. This brochure highlights some of SGE’s capabilities in capillary gas chromatography, specifically in the technically demanding area of capillary columns. SGE columns are engineered for consistent separation performance and can be found in many laboratories being tasked to perform everything from routine analyses to the latest R&D challenges. forte™ GC Capillary Columns With over 30 year’s experience, GC capillary columns truly are SGE’s strength, its forte. SGE is the only independent manufacturer of GC capillary columns that has the skill and technology to control all critical processes from producing the fused silica capillary tubing, through the phase synthesis, to the validation of the performance of each column. SGE offers a comprehensive range of forte™ GC capillary columns for almost any chromatographic application providing the best possible combination of, Performance, Robustness, Reproducibility, Low Bleed and Inertness. With this brochure we bring to you a small taste of the applications you might consider running on an SGE GC capillary column. If the application is not in this guide, please visit our website www.sge.com.
  • 3. For further information on our full range of products, please visit www.sge.com Contents Guidelines for Choosing Columns 1-2 SGE Capillary Column 37-39 Part Number Listing Environmental 4-12 Food, Flavors and Fragrances 13-18 Fuels and Petrochemical 19-22 Chemical 23-27 Recommended Column by Application 3 GC Column Replacement Guide 39 GC Troubleshooting and Maintenance 40 Pharmaceutical 28-32 Forensic 33-36
  • 4. Guidelines for Choosing Columns 1 2 3 4 6 7 8 9 10 11 12 13 14 16 5 0 min 120 min 26 15 1 2 3 4 6 8 9 10 11 12 13 14 15 16 7 5 ComponentsComponents 1. Naphthalene 2. Acenaphthylene 3. Ethylbenzene 4. Fluorene 5. Phenanthrene 6. Anthracene 7. Fluoranthene 8. Pyrene 9. Benzo(a)anthracene 10. Chrysene 11. Benzo(b)fluoranthene 12. Benzo(k)fluoranthene 13. Benzo(a)pyrene 14. Indeno(1,2,3,-c,d)pyrene 15. Dibenzo(a,h)anthracene 16. Benzo(g,h,i)perylene Effect of Internal Diameter. Polynuclear Aromatic Hydrocarbon (PAH) analysis. 2 Internal Diameter NORMAL - 0.25 mm ID Chromatogram using a conventional (30 m x 0.25 mm ID) BPX5 column with a 0.25 µm film. FAST - 0.10 mm ID Chromatogram using a FAST (10 m x 0.1 mm ID) BPX5 column with a 0.1 µm film. • The smaller the diameter the greater the efficiency, hence better resolution. Fast columns (0.1 mm ID) are used for faster analysis because the same resolution can be achieved in a shorter time. 0.5 4.0 min 1 2 3 4, 5 6 1 2 3 4 5 6 Components 1. Benzene 2. Toluene 3. Ethylbenzene 4. p-Xylene 5. m-Xylene 6. o-Xylene SolGel-WAX™ Polar SolGel-1ms™ Non-Polar 1 Effect of Stationary Phase. BTEX analysis on a polar (SolGel-WAX™) column and a 100% dimethyl polysiloxane (SolGel-1ms™), both 30 m x 0.25 mm ID X 0.25 µm film. Stationary Phase • Select the least polar phase that will perform the separation you require • Non-polar stationary phases separate analytes predominantly by order of boiling point. • Increase the amount of phenyl and/or cyanopropyl content in the phase, and the separation is then influenced more by differences in dipole moments or charge distributions (BP10 (1701), BPX35, BPX50, BP225 and BPX70) • To separate compounds that differ more in their hydrogen bonding capacities (for example aldehydes and alcohols), polythylene glycol type phases are best suited - SolGel-WAX™, BP20 (WAX) and BP21 (FFAP) 1 For further information on our full range of products, please visit www.sge.com BPX5 BPX70BPX50 BPX35 BPX90 BP225 BP21 BP20 SolGelWax Cydex-B BPX-Volatiles HT8 HT5 BP1, BPX1, SolGel-1ms Polyethylene glycolCyanopropyl Polysilphenylene siloxaneCyanopropylphenyl siloxanePolycarborane siloxanePhenyl Polysilphenylene siloxaneDimethyl polysiloxane i P Wax BPX B BPX-Volatiles HT �-bonding H-bonding Van der Waals Stationary Phase Polarity
  • 5. PHASE RATIO 0 20 min R = 3.60 R (Resolution) = 3.14 R = 4.96 4 Effect of Film Thickness. • For samples with a variation in solute concentration, a thicker film column is recommended. This will reduce the possibility of broad overloaded peaks co-eluting with other compounds of interest. If the separation of two solutes is sufficient and co-elution is still unlikely, even with large differences in concentration, then a thinner film can be used. The greater the film thickness the greater the retention of solutes, therefore the higher the elution temperature. As a rule, doubling the film thickness results in an increase in elution temperature of approximately 15-20° under isothermal conditions. Usingatemperatureprogram,theincreaseinelutiontemperatureisslightlyless. Film thickness • From the phase ratio value ß, a column can be categorized for the type of application it would best suit. The smaller the ß value, the greater the ratio of phase to the column inner diameter, making it better suited for analyzing volatile compounds. Columns which have thin films are generally better suited for high molecular weight compounds and are characterized by large ß values. Above shows the phase ratio (ß) available for the SGE range of capillary columns. Keeping a similar phase ratio when changing column internal diameters will ensure that your chromatographic parameters will not need substantial changes. ß= ——— where ß = ratio id = column internal diameter (µm) d = film thickness (µm)f f4d id Formula to calculate Phase Ratio Film thickness (µm) Column ID (mm) 0.1 0.15 0.22 0.25 0.32 0.53 0.10 250 - 550 625 800 1325 0.15 - 250 - - - 883 0.25 - 150 220 250 320 530 0.50 - 75 110 125 160 265 1.00 - - 55 63 80 132 3.00 - - - - 27 44 5.00 - - - - 16 26 • Always try to select the shortest column that will provide the required resolution for the application. If the maximum column length available is being used, and resolution of the sample mixture is still inadequate then try changing the stationary phase or internal diameter. • Resolution is proportional to the square root of the column efficiency. Therefore, doubling the column length will only increase the resolving power of the column by approximately 40%. 0.25 µm 0.50 µm 1.0 µm 4.7 min 7.4 min 13.2 min 0 Effect of Length 3 Column Length 3.7 min 7.5 min 20 min R = 2.91 R = 2.05 R = 4.15 15.3 min 15 metres 30 metres 60 metres 2For further information on our full range of products, please visit www.sge.com
  • 6. Recommended Column by Application PHASE Application SolGel-1ms BP1 BPX1 BP1-PONA BPX5 BP5 HT5 HT8 BPX35 BPX-Volatiles BP624 BP10 BPX50 SolGel-WAX™ BP20 BP21 BPX70 CYDEX-B BPX90 Acidic/Neutral Drugs Acids Alcohols Amines Aliphatic Amines Aromatic Antidepressants Aromatic -PAH Aroclors Beverages -Alcohols Butter-Fat Chiral - Componds Chlorinated Aromatics Cigarette Lighter Fuel Dioxins Essential Oils Food - FAME Glucose - Methylated Herbicides Industrial Solvents Ketones Monomers Nitroaromatics Organochlorine Pesticides Organophosphorous Pesticides Paraffins PCB’s Petroleum Phenols Phthalates Plant Sterols Polymers Polywax Pyrethroids Racehorse Doping Mixture Sedatives Semivolatiles Silicon Oil Solvents Sugars-Alditol Acetates Triglycerides TRPH Volatiles Xylenes Indicates recommended phases to be used for the application Indicates alternative phases that can be used for the application 3 For further information on our full range of products, please visit www.sge.com
  • 7. Applications • Analysis of PCB'S, PCDT'S, and other complex mixtures using BPX5 and SolGel-1ms • HT8: The Perfect PCB Column • Fast Pesticide Screening Using a BPX5 GC Capillary Column • Analysis of Polychlorinated Dibenzodioxins and Furans on BPX5 • Analysis of Polynuclear Aromatic Hydrocarbons on BPX35 • Analysis of Polynuclear Aromatic Hydrocarbons on BPX5 • Analysis of Volatile Organic Pollutants on BPX-Volatiles • Applications using BPX90 • Analysis of Volatiles in Drinking Water on 25 m BP624 Column • Polychlorinated Biphenyls PCB Analysis The widespread use of GC-MS for Environmental analyses requires both low bleed and inertness. The broad range of compounds of interest means that medium polarity phases become more useful. BPX5, BPX35, and BPX50 provide a range of polarities, all with low bleed, high temperature limits, and robustness. For specialized applications such as PCBs, SGE’s HT8 delivers unique separation capabilities. Environmental 4For further information on our full range of products, please visit www.sge.com
  • 8. ANALYSIS OF PCB'S, PCDT'S, AND OTHER COMPLEX MIXTURES USING BPX5 AND SOLGEL-1ms Time 16.00 18.00 20.00 22.00 24.00 26.00 28.00 30.00 32.00 34.00 36.00 38.00 40.00 42.00 44.00 46.00 48.00 50.00 0 Time 16.00 18.00 20.00 22.00 24.00 26.00 28.00 30.00 32.00 34.00 36.00 38.00 40.00 42.00 44.00 46.00 48.00 50.00 % 0 100 2378-D 2378-F OCDFOCDD Hepta-Hexa- F D D FF F D D F F D DF F Penta-Tetra- Octa- % 100 Tri- Tetra- Penta- Hexa- Hepta- Octa- OCDT SIM 7-Group Analysis of 44 mono- to deca-PBDE's via cool-on-column (3-µL). Deca-PBDE 209 at 310 °C, PBDEs 33/28 and 138/166 partially resolved, PBDE 85 coeluted with 155. - 44 Mono-Deca-PBDEs - 6890 GC/Autospec HRMS - Cool-on-column inlet - (No liner but 0.53 mm retention gap) 12.5 m BPX5 0.15 mm ID 0.1 µm - 0.25 m 0.53 mm ID plus - 2 m 0.25 mm retention gaps - He programmed 245-415 kPa - 150 ºC-315 ºC @ 3 ºC/minTime 5.00 7.50 10.00 12.50 15.00 17.50 20.00 22.50 25.00 27.50 30.00 32.50 35.00 37.50 40.00 42.50 45.00 47.50 50.00 52.50 55.00 % 0 100 Deca- 209206 208 207 Nona-Octa- 203 190 181 Hepta- 183 166 138 153 154 126 85/155 118 116 99 119 Hexa- 10077 66 47 71 49 75 37 35 28 33 25 17 32 30 15 13 12 11/8 7 10 32 1 Mono- Di- Tri- Tetra- Penta- SIM 2-Group Analysis for non-o-PCBs. Tetra-PCB's 77 and 81 (A) are resolved from residual o-PCB's (97, 87, 110, and 136). Penta-126 (B), and hexa-169 (C) also detected in eluate 2-basic alumina of DX-3 QC sediment extract (5 of 500 µL) Ion chromatograms (not smoothed). PBDE's are in same eluate (Peterman et al., 2006). Tetra-PBDE 47 from (M-2 Br)+ incidentally detected (B); 0.3 ng/g near lab background. - Dioxin-like non-ortho PCBs - HP 5890A GC/VG 70S HRMS - Heated (275 ºC) Direct inlet - 4 mm Siltek Cyclo-Uniliner - 30 m SolGel-1ms 0.15 mm ID 0.1 µm - 2.5 m x 0.25 mm ID retention gap - He constant at 415 kPa - 155 ºC (1 min) - 205 ºC @ 1.8 ºC/min then to 310 ºC @ 3.6 ºC/min ACKNOWLEDGEMENT Paul H. Peterman, US Geological Survey, Columbia Environmental Research Center. For additional information see SGE application note AN-0030-C. SGE liners undergo a high temperature deactivation process making them ideal for using with active compounds EXPERTTIP Environmental 5 For further information on our full range of products, please visit www.sge.com
  • 9. e Chromatogram on the left demonstrates clearly the significant difference in selectivity of the HT8 column. By GC/MS, quantitation of CB28 using a standard 5% phenylpolysiloxane column is impossible as coelution with CB31 (with the same number of chlorines) occurs. HT8 separates the two congeners by a full minute allowing quantitation to be performed with ease. AROCLOR 1260 Column and Oven conditions are as listed for Aroclor 1242 .dtS.tnI902071 177 199 156 191 208 189 205 206 195 194 207 174/162/128 179/132 151 77/149 92 84 136/86 110 135 115/87 200/172 190/203 176 173 144 146 402131 101/150 118 153/122 180 138 97/117 107/108/134 197/171 550554setunim0453 AROCLOR 1260 Congener # Cl Position Cl # Identification by GC/MS 130 234-235 6 178 2356-235 7 141 2345-25 6 164 236-345 6 163 2356-34 6 138 234-245 6 160 23456-3 6 175 2346-235 7 158 2346-34 6 187 2356-245 7 182 2345-246 7 129 2345-23 6 138 141 187/182 183/166 185/159 164/163 178 130 105 137 129 AROCLOR 1242 Congener # Cl Position Cl # Identification by GC/MS 42 23-24 4 96 236-26 5 35 34-3 3 64 235-4 4 72 25-35 4 103 246-25 5 71 26-34 4 41 234-2 4 68 24-35 4 37 34-4 3 100 246-24 5 72/64 103/71 96/35 68/37 42 41 40 28/53 52/69 20/33/45 31 44 95 74 70 66 110 84 22 49/43 47/48/65 97/117/86 115/87 77/149 107/108/134 10 4 9 7 6 8 19 18 17 16 29 51 38 25 26/50 32 15 27 12/24 101/150 60/113 118 36 75 59 67 63 91/121/155 76/80 56 99 85 81148 20 045303setunim52 AROCLOR 1242 Phase: HT8, 0.25 µm film Column: 50 m x 0.22 mm ID Initial Temp: 80 °C, 2 min Rate 1: 30 °C/min Temp 2: 170 °C Rate 2: 3 °C/min Final Temp: Split, 300 °C Carrier Gas: He, 40 psi Detector: ECD, 330 °C Standard 5% Phenylsiloxan 31/28 HT8: THE PERFECT PCB COLUMN HT8 31 28 Separation of CB31 and CB28 Environmental 6For further information on our full range of products, please visit www.sge.com
  • 10. Time (s) 300 400 500 600 700 800 900 1000 Spectrum # 348 1048 1748 2449 3149 3849 4550 5250 7e+006 6e+006 5e+006 4e+006 3e+006 2e+006 1e+006 0 ____ TIC Phenol3-phenoxy- Dimpylate Phosphamidon Cyclohexane1,2,3,4,5,6hexachloro Primicarb Phosphionthioticamide,P,P-diphenyl- Cycohexene1,3,4,5,6pentachloro-,s Mefenoxam Carbaril Malathion Chlorpyrifos Fenthion Aldrine Clofenvifos Quinalphos Captan Imazali 2-Methylphenothiazine Mitotane Dieldrin Ethion Mitotane Trizaophos Octyladipate p,p’-DDT Endosulfansulfate Btethrin Fenoxycarb Time (s) 520 540 560 580 600 620 640 660 680 700 7e+006 6e+006 5e+006 4e+006 3e+006 2e+006 1e+006 0 FAST PESTICIDE SCREENING USING A BPX5 GC CAPILLARY COLUMN Phase: SGE forte BPX5DX Column: 40 m x 0.18 mm ID x 0.18 μm Initial Temp: 80 ºC, 1 min Rate 1: 25 ºC/min to 300 ºC Final Temp: 300 ºC, 7 min Detector Type: LECO™ TOF Mass spectrometer Carrier Gas: He Carrier Gas Flow: constant flow mode at 1 mL/min Average Linear Velocity: ~75 cm/sec Injection Mode: splitless Injection Temperature: 270 ºC Total run time: 16.8 min Detector voltage: 1700 V Data acquisition speed: 10 Hz Column Part Number: 054229 ACKNOWLEDGEMENT SGE would like to thank Prof Jana Hajšlová and Jakub Schurek from VSCHT (Prague, CZ) for providing these chromatograms. Environmental 7 For further information on our full range of products, please visit www.sge.com
  • 11. The list of some pesticides used in the sample, and their retention times Environmental 8For further information on our full range of products, please visit www.sge.com Peak number Name R.T. (s) 50 Penconazole 585.765 51 Tolylfluanide 587.622 52 Quinalphos 590.478 53 Procymidone 592.191 54 Captan 599.902 55 Methidathion 601.33 56 o,p'-DDE 602.044 57 Folpet 602.901 58 Imazalil 611.755 59 Bupirimate 614.325 60 2-Methylphenothiazine 616.896 61 p,p'-DDE 617.895 62 Mitotane 623.179 63 Dieldrin 628.605 64 Ethion 635.46 65 Mitotane 642.314 66 m,p'-DDD 643.171 67 o,p'-DDT 644.17 68 Triazophos 647.455 69 Endosulfan I 648.883 70 Octyl adipate 651.168 71 p,p'-DDT 665.019 72 Endosulfan sulfate 670.731 73 Tebuconazole 673.444 74 Bifenthrin 680.013 75 Fenoxycarb 693.436 76 Bromopropylate 695.436 77 Phosmet 701.576 78 Endrin ketone 709.43 79 λ-Cyhalothrin 718.141 80 Tetradifon 721.854 81 Phosalone 723.282 82 Fenarimol 754.126 83 Azinphos-ethyl 759.124 84 Permethrin 768.264 85 Permethrin 774.975 86 Pyridaben 786.114 87 Cyfluthrin 805.534 88 Cyfluthrin 807.248 89 Cypermethrin 819.957 90 Cypermethrin 826.383 91 Cypermethrin 831.238 92 Cypermethrin 833.095 93 Esfenvalerate 895.927 94 Fenvalerate α 914.062 95 Difenoconazole 950.476 96 Difenoconazole 956.617 97 Deltamethrin 972.182 Peak number Name R.T. (s) 1 Methamidophos 341.292 2 Dichlorovos 342.291 3 Phosphorodithioic acid, O,O-diethyl ester 381.561 4 Mevinphos 404.552 5 Carbamic acid, phenyl-, 1-methylethyl ester 418.261 6 Methacrifos 427.4 7 Benzene, (3-chloro-1-propenyl) 433.969 8 Butyl dimethyl phosphate 436.539 9 1-Naphthalenol 442.965 10 Bibenzyl 445.107 11 Cyclohexene, pentachloro- 449.534 12 Heptenophos 453.39 13 Endosulfan 462.672 14 Omethoate 465.099 15 Diphenylamine 476.095 16 Carbamic acid, (4-chlorophenyl), 1-methylethyl ester 479.094 17 Monocrotophos 485.091 18 Cyclohexane, 1,2,3,4,5,6-hexachloro- 500.228 19 Benzene, hexachloro- 501.799 20 Phenol, 3-phenoxy- 504.512 21 Dimethoate 505.083 22 Dimpylate 509.796 23 Phosphamidon 514.651 24 α-Lindane 515.222 25 Benzonitrile, pentachloro- 517.792 26 Cyclohexane, 1,2,3,4,5,6-hexachloro- 518.792 27 Etrimfos 520.22 28 Pirimicarb 526.36 29 Tetrachloroisophthalonitrile 527.217 30 Phosmet 527.788 31 Phosphinothioic amide, P,P-diphenyl- 532.072 32 Phosphamidon 534.786 33 γ-Lindane 535.642 34 Cyclohexene, 1,3,4,5,6-pentachloro-, ç- 540.498 35 Methyl chlorpyrifos 542.497 36 Mefenoxam 547.78 37 Pirimiphos methyl 551.065 38 Carbaril 553.492 39 Heptachlor 554.92 40 Malathion 557.348 41 Fenitrothion 558.205 42 Chlorpyrifos 563.346 43 Dichlofluanid 563.774 44 Fenthion 567.915 45 Parathion 569.2 46 Triadimefon 569.772 47 Aldrine 574.341 48 cis-Chlorfenvinphos 577.483 49 Clofenvinfos 584.194
  • 12. setunim0302010 9 10 12 11 13 14 15 16 ANALYSIS OF POLYNUCLEAR AROMATIC HYDROCARBONS ON BPX35 1 2 3 4 65 7 8 Phase: BPX35, 0.25 µm Column: 30 m x 0.22 mm ID Initial Temp: 100 °C,1 min Rate: 10 °C/min Final Temp: 360 °C, 10 min Carrier Gas: He, 25 psi Detector: FID 380 °C Column Part Number: 054714 Components 1. Naphthalene 2. Acenaphthylene 3. Acenaphthene 4. Fluorene 5. Phenanthrene 6. Anthracene 7. Pyrene 8. Fluoranthene 9. Benzo (a) anthracene 10. Chrysene 11. Benzo (b) fluoranthene 12. Benzo (k) fluoranthene 13. Benzo (a) pyrene 14. Indeno (1,2,3, -c,d)pyrene 15. Dibenzo (a,h) anthracene 16. Benzo (g,h,i) perylene ANALYSIS OF POLYNUCLEAR AROMATIC HYDROCARBONS ON BPX5 5 10 20 minutes 30 40 1 2 3 4 5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 1 6 1 5 Polynuclear Aromatic Hydrocarbons (EPA 625 PAHs) Phase: BPX5, 0.25 µm film Column: 25 m x 0.22 mm ID Initial Temp: 50 °C, 2 min Rate: 8 °C/min Final Temp: 290 °C, 10 min Carrier Gas: HP5971 MSD Detector: Split 40:1 Carrier Gas: He, 15 psi Column Part Number: 054113 Components (0.5ng each component) 1. Naphtalene 2. Acenaphtylene 3. Acentaphthene 4. Fluorene 5. Phenanthrene 6. Anthracene 7. Pyrene 8. Fluoranthene 9. Chrysene 10. Benzo (a) anthracene 11. Benzo (b) fluoranthene 12. Benzo (k) fluoranthene 13. Benzo (a) pyrene 14. Indeno (1,2,3, -c,d)pyrene 15. Dibenzo (a,h) anthracene 16. Benzo (g,h,i) perylene SGE wishes to acknowledge Dr P.Ambridge, Dr A.Fernandes and C.Brook at AEA Technology, Harwell, U.K. ANALYSIS OF POLYCHLORINATED DIBENZODIOXINS AND FURANS ON BPX5 Single Ion Chromatograms of TCDF Isomers Single Ion Chromatograms of TCDD Isomers 2,3,7,8 - TCDF m/z 321.8936 m/z 333.9339 13C12 - 2,3,7,8 - TCDF 2,3,7,8 -TCDD 13C12 - 2,3,7,8 -TCDD 17 18 19 20 21 minutes 18 19 20 21 minutes m/z 317.9389 0 100% 0 100% m/z 305.8987 0 100% 0 100% Phase: BPX5, 0.25 µm Column: 50 m x 0.22 mm ID Initial Temp: 80 °C Rate 1: 10 °C/min Temp1: 240 °C Rate 2: 2 °C/min Temp 2 : 280 °C Rate 3: 10 °C/min Final Temp: 320 °C Detector: Mass Spectrometer Column Part Number: 054114 Remember : the lower the temperature, the longer your column will last. EXPERTTIP Environmental 9 For further information on our full range of products, please visit www.sge.com
  • 13. 57 58 59 60 54 55 12.00 14.00 16.00 18.00 20.00 22.00 24.00 22 23 24 25 26 27 28 29 30 31 32 33 34 35, 36 37 38 39 40 41, 42 43, 44 45 46 47 48 49 50 51 52 53 54 55 56 Phase: BPX-Volatiles 1 µm film 502.2 mix: 200 ppm in Methanol Column: 40 m x 0.18 mm ID Initial Temp: 40 °C , 0 min Rate 1: 6 °C to 210 °C Rate 2: 15 °C to 240 °C Final Temp: 240 °C, 5 min Detector Type: Mass Spectrometer Carrier Gas: He, 40.3 psi Carrier Gas Flow : 1.2 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 50:1 Injection Volume: 1 µL Injection Temperature: 250 °C Autosampler: No Liner Type : 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054860 ms-NoVent™Part No: 113400 HP5973 restrictor: 113409 Full scan: 45-450 m/z ANALYSIS OF VOLATILE ORGANIC POLLUTANTS ON BPX-VOLATILES 2.00 4.00 6.00 8.00 10.00 1600000 1200000 800000 400000 0 1 2 3 4 5 6 7 9 10 8 11 13 1412 15 16,17 18 19 20 21 1 2 3 4 5 6 1.60 2.00 2.40 2.80 3.20 3.60 4.00 4.40 Components 1. Dichlorodifluoromethane 2. Chloromethane 3. Vinyl chloride 4. Bromomethane 5. Chloromethane 6. Trichlorofluoromethane 7. 1,1-Dichloroethene 8. Dichloromethane 9. trans-1,2-Dichloroethene 10. 1,1-Dichloroethane 11. 2,2-Dichloropropane 12. cis-1,2-Dichloroethene 13. Bromochloromethane 14. Chloroform 15. 1,1,1-Trichloroethane 16. 1,1-Dichloropropene 17. Carbon tetrachloride 18. Benzene 19. 1,2-Dichloroethane 20. Trichloroethene 21. 1,2-Dichloropropane 22. Dibromomethane 23. Bromodichloromethane 24. cis-1,3-Dichloropropene 25. Toluene 26. trans-1,3-Dichloropropene 27. 1,1,2-Trichloroethane 28. Tetrachloroethene 29. 1,3-Dichloropropane 30. Dibromochloromethane 31. 1,2-Dibromethane 32. Chlorobenzene 33. Ethylbenzene 34. 1,1,2-Dibromochloromethane 35. p-Xylene 36. m-Xylene 37. o-Xylene 38. Styrene 39. Bromoform 40. Isopropylbenze 41. Bromobenzene 42. 1,1,2,2-Tetrachlorethane 43. 1,2,3-Trichloropropane 44. n-Propyl benzene 45. 2-Chlorotoulene 46.1,3,5-Trimethylbenzene 47. 4-Chlorotoulene 48. tert-Butylbenzene 49. 1,2,4-Trimethylbenzene 50. sec-Bythlbenzene 51. 1,3-Dichlorobenzene 52. p-lsopropyltoulene 53. 1,2-Dichlorobenzene 54. n-Butylbenzene 55. 1,4-Dichlorobenzene 56. 1,2-Dibromo-3-chloropropane 57. 1,2,4-Trichlorobenzene 58. Hexachlorobutadiene 59. Naphthalene 60.1,2,3-Trichlorobenzene Chromatogram showing analysis of commonly screened volatile organic pollutants 32 33 35, 36 37 38 39 40 41, 42 43, 44 45 46 47 48 49 50 51 52 53 14.00 15.00 16.00 17.00 18.00 19.00 20.00 Environmental 10For further information on our full range of products, please visit www.sge.com
  • 14. setunim975 1 5 ANALYSIS OF VOLATILES IN DRINKING WATER ON 25 M BP624 COLUMN VOLATILES IN DRINKING WATER Phase: BP624, 1.2 µm Column: 25 m x 0.22 mm ID Initial Temp: 50 °C, 2 min Rate: 15 °C/min Final Temp: 170 °C Detector: HP5970 MSD Injection Mode: Hexadecane extract Carrier Gas: He, 15 psi Column Part Number: 054826 Components 1. Difluorobenzene 2. Benzene 3. Toluene - (d8) 4. Toluene 5. Chlorobenzene - (d5) 6. Ethyl benzene 7. p and m-Xylene 8. o-Xylene 9. Bromofluorobenzene 2 3 4 6 7 8 9 10 20 10 20 5 15 9 14 12 17 9 14 Ronnel and heptachlor ceolute Aldrin and fenthion coelute Baseline separation Adrin and fenthion coelute fenthion (m/z 278) Aldrin and methylparathion (m/z 263) Ronnel (m/z 285) Heptachlor (m/z 272) Chlorpyrifos (m/z 314) Chlorphyifos methyl (m/z 286) Diazinon (m/z 137) Ronnel (m/z 285) Parathion (m/z 291) Fenthion (m/z 278) APPLICATIONS USING BPX90 10.0 15. 20.0 4.0 10.0 15.0 HCCH isomers and HCB Separation of aromatics Separation of hexabromocylododecanes Selectivity for pesticides and thiophosphate esters Condition column at either 20 ° above the maximum method temperature or the recommended maximum column temperature (whichever is lower). EXPERTTIP Environmental 11 For further information on our full range of products, please visit www.sge.com
  • 15. 04SETUNIM52 68 69 70 77 80 82 83 85 86 88 89 94 99 104 105 110 113 115 119 87 81 91 92 130 131 129 128 108 109 98 100 114 116 117 118 121 122 123 127 134 133 135 71 73 74 76 72 75 79 90 126124 112 107 97 102 132 POLYCHLORINATED BIPHENYLS PCB ANALYSIS Phase: HT8, 0.25 µm Column: 25 m x 0.22 mm ID Initial Temp: 60 °C, 2 min Rate: 12 °C/min Final Temp: 360 °C, 10 min Detector: lon Trap MS Injection Mode: PTV Carrier Gas: He, 15 psi Components 1. PCB 18 2. PCB 31 3. PCB 28 4. PCB 52 5. PCB 44 6. PCB 70 7. PCB 101 8. PCB 110 9. PCB 149 10. PCB 153 11. PCB 138 12. PCB 180 13. PCB 170 1 2 3 4 5 6 7 8 9 10 11 12 13 16:40 18:20 20:00 21:40 23:00 MINUTES 30 35 40 45 50 min Phase: HT8, 0.25 µm Column: 50 m x 0.22 mm ID Initial Temp: 60 °C Rate 1: 40 °C/min Temp 1: 200 °C Rate 2: 3 °C/min Temp 2: 320 °C Detector: ECD Carrier Gas: He, 40 psi Performance Specifications HT8 8% Phenyl (Equiv) Polycarborane - Siloxane Minimum Operating Temp.: -20 °C Maximum Cycling Temp.: 370 °C (Polyimide) GC/MS Analysis of PCB mixture Components 1. PCB1 2. PCB2 3. PCB3 4. PCB10 5. PCB4 6. PCB9 7. PCB7 8. PCB6 9. PCB 8/5 10. PCB19 11. PCB18 12. PCB11 13. PCB17 14. PCB13 15. PCB24 16. PCB27 17. PCB15 18. PCB32 19. PCB16 20. PCB54 21. PCB23 22. PCB34 23. PCB29 24. PCB26 25. PCB25 26. PCB31 27. PCB8/53 28. PCB51 29. PCB21 30. PCB33/45/20 31. PCB22 32. PCB46 33. PCB36 34. PCB52/69 35. PCB43 36. PCB49 37. PCB47/48/75 38. PCB44 39. PCB59 40. PCB42 41. PCB35 42. PCB64 43. PCB71/103 44. PCB41 45. PCB37 46. PCB68 47. PCB100 48. PCB40 49. PCB57 50. PCB67 51. PCB63 52. PCB102 53. PCB95 54. PCB74 55. PCB121/ 155/91 56. PCB70 57. PCB80 58. PCB66 59. PCB96/55 60. PCB84/92 61. PCB125 62. PCB90 63. PCB101 64. PCB60 65. PCB56 66. PCB152 67. PCB99 68. PCB119 69. PCB83 70. PCB136 71. PCB86 72. PCB97 73. PCB89 74. PCB115 75. PCB87 76. PCB154 77. PCB85 78. PCB10/81 79. PCB151 80. PCB144 81. PCB147 82. PCB135 83. PCB77/82 84. PCB149 85. PCB124 86. PCB143 87. PCB134/ 107/131 88. PCB123 89. PCB133 90. PCB118 91. PCB165 92. PCB143/114 93. PCB132/179 94. PCB122 95. PCB153 96. PCB176 97. PCB141 98. PCB105 99. PCB137 100. PCB130 101. PCB178 102. PCB163 103. PCB138 104. PCB160 105. PCB158/175 106. PCB187/182 107. PCB183/129 108. PCB126 109. PCB185 110. PCB159/202 111. PCB174/128 112. PCB177/201 113. PCB167 114. PCB171 115. PCB197 116. PCB173 117. PCB200 118. PCB156/172 119. PCB157 120. PCB180 121. PCB193 122. PCB191 123. PCB198 124. PCB199 125. PCB170 126. PCB190/ 196/203 127. PCB169 128. PCB208 129. PCB207 130. PCB195 131. PCB189 132. PCB194 133. PCB205 134. PCB206 135. PCB209 Part Number: 054676 PCB ANALYSIS Phase: HT8, 0.25 µm film Column: 50 m x 0.22 mm ID Initial Temp: 90 °C, 1 min Rate 1: 20 °C/min Temp 1: 170 °C,7.5 min Rate 2: 3.5 °C/min Temp 2: 285 °C Rate 3: 20 °C/min Temp 3: 320 °C Carrier Gas: H₂, 43 cm/sec Detector: ECD 78 84 93 95 103 106 111 120 125 02SETUNIM5 1 2 4 5 6 7 8 9 10 11 12 13 3 19 18 17 20 21 22 23 24 25 26 27 30 31 32 33 34 35 36 37 38 40 43 44 45 48 54 56 58 59 60 61 62 66 67 63 64 65 53 49 50 51 52 55 57 46 47 42 39 41 28 29 16 15 14 Aroclor 1254 Environmental 12For further information on our full range of products, please visit www.sge.com
  • 16. GC analysis in the Food, Flavors and Fragrances area covers a diverse range of compounds that vary in both polarity and boiling point. As a consequence a range of different columns are often required. Chromatograms are often complex, and any single column may not give enough separation of all of the compounds that may be present. Pairs of columns such as BPX5 and SolGel-WAX™ may be used to overcome this problem. For specific classes of compounds such as fatty acids, specialized columns are often necessary. Short chain fatty acids may be analyzed as free acids on the Nitroterephthalic acid (TPA) modified Polyethylene Glycol BP21 phase. Longer chain fatty acids are usually analyzed as fatty acid methyl esters on wax phases such as BP20 and SolGel-WAX™, or for more demanding applications, BPX70 or BPX90. Applications • Comparison of Geranium Oils on SolGel-WAX™ • Analysis of Eucalyptus Oil on SolGel-WAX™ • Analysis of Lavender Oil on Cydex-B • Analysis of Lavender Oil on BPX-5 • Analysis of Tasmanian Lavender Oil on SolGel-WAX™ • Analysis of Wine on BP20 • Analysis of Scotch Whisky on BP20 • Analysis of Teatree Oil on BPX5 • Analysis of Omega-3 Fatty Acids using BPX70 • BPX90 – a Highly Polar Phase for FAME Analysis • Analysis of PUFA-1 Marine FAME on BPX70 • Analysis of PUFA-2 Animal FAME on BPX70 • Analysis of PUFA-1 Marine FAME on BPX70 Food, Flavors and Fragrances 13 For further information on our full range of products, please visit www.sge.com
  • 17. ANALYSIS OF EUCALYPTUS OIL ON SOLGEL-WAX™ Subtraction of the two TIC chromatograms shows the difference between the two essential oils. COMPARISON OF GERANIUM OILS ON SOLGEL-WAX™ 5.00 10.00 15.00 20.00 25.00 30.00 5.00 10.00 15.00 20.00 25.00 30.00 Comparison of total ion chromatograms (TIC) for Geranium oils from Reunion Island (green trace) and South Africa (red trace). EXPERIMENTAL CONDITIONS Column: SGE forte SolGel-WAX™, 30 m x 0.25 mm x 0.25 µm (SGE P/N 054796) Temperature Program: 60 °C for 3 min, then 4 °C/min to 220 °C Carrier Gas: He Flow: 0.6 mL/min Injection 0.3 µL split ratio 30:1 Volume Injection temp: 250 °C Liner: SGE P/N 092019 single tapered with quartz wool Phase: SolGel-WAX™, 0.25 µm film Sample: Neat Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 8 °C/min to 220 °C Final Temp: 220 °C, 5 min Detector Type: Mass Spectrometer Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.2 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054796 ms-NoVent™ Part Number: 113400 HP5973 restrictor: 113409 Full Scan/SIM: 45-450 m/z Components 1. α-Pinene 2. ß -Pinene 3. Sabinene 4. Limonene 5. 1,8 -Cineole 6. p-Cymene 7. Linalool L 8. Terpinen-4-ol 9. α-Terpineol 10. α-Terpinenyl acetate 11. d-Carvoαne ACKNOWLEDGEMENT We thank M. Bernet and M. Didtsch of the ISIPCA Group, Research and Studies Centre for Fragrance, Cosmetics and Food Flavors, France, for providing these chromatograms. For more information see SGE application note AN-0020-C. 4.00 6.00 8.00 10.00 12.00 14.00 0 1000000 2000000 3000000 4000000 5000000 6000000 7000000 8000000 1 2 3 4 5 6 7 8 9 10 11 Food, Flavors and FragrancesFood, Flavors and Fragrances 14For further information on our full range of products, please visit www.sge.com
  • 18. Components 1. 3-Octanone 2. Octenyl acetate 3. Octanol 4. cis Linalool oxide 5. trans Linalool oxide 6. Linalool L 7. Linalyl acetate 8. Terpinen-4-ol 9. Lavandulyl acetate 10. Borneol L 11. Caryophyllene oxide ANALYSIS OF TASMANIAN LAVENDER OIL SOLGEL-WAX™ Phase: SolGel-WAX™, 0.25 µm film Sample: Neat Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 8 °C/min to 220 °C Final Temp: 220 °C, 5 min Detector Type: Mass Spectrometer Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.2 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054796 ms-NoVent™ Part Number: 113400 HP5973 restrictor: 113409 Full Scan/SIM: 45-450 m/z4.00 6.00 8.00 10.00 12.00 14.00 16.00 0 2000000 4000000 6000000 8000000 1e+07 1.2e+07 1.4e+07 1 2 3 4 5 6 7 8 9 10 11 ANALYSIS OF LAVENDER OIL ON BPX5 10.0 12.0 14.0 16.0 18.0 20.0 22.0 24.0 26.0 28.0 0 40000 80000 120000 160000 200000 240000 280000 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 Phase: BPX5, 0.25 µm film Lavender Oil: Lavender Oil in ethanol Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 5 °C/min to 260 °C Final Temp: 260 °C Detector Type: Mass Spectrometer Carrier Gas: He, 7.0 psi Carrier Gas Flow: 1.0 mL/min Constant Flow: On Average Linear Velocity: 36 cm/sec at 40 °C Injection Mode: Split Split Ratio: 200:1 Purge on (Split) Vent Flow: 200 mL/min Injection Volume: 0.2 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Double Taper Liner Liner Part Number: 092018 Column Part Number: 054101 Components 1. ß- Pinene 2. 1-Octen-3-ol 3. 3-Octanol 4. 3-Octanol 5. p-Cymene 6. Limonene 7. cis-Ocimene 8. cis-Linaloxide 9. trans-Linalool oxide 10. Linalool L 11. Octenyl acetate 12. Camphor 13. Lavandulol 14. Borneol L 15. Terpinen-4-ol 16. α-Terpineol 17. Linalyl acetate 18. Lavundyl Acetate 19. Geranyl Acetate 20. α-Santalene 21. ß-Caryophyllene 22. α-Cadinine 23. α-Cryophyllene oxide Components 1. (+) Linalool 2. ( - ) Linalool ANALYSIS OF LAVENDER OIL ON CYDEX-B Better resolution is often obtained from chiral columns by using lower temperatures and higher carrier gas velocities than for conventional columns. EXPERTTIP LAVENDER OIL Phase: CYDEX-B, 0.25 µm film Column: 50 m x 0.22 mm ID Initial Temp: Isothermal at 90 °C Final Temp: FID Detector: 32 x 10-¹²AFS Injection Mode: Split Column Part Number: 054901 Food, Flavors and Fragrances 15 For further information on our full range of products, please visit www.sge.com
  • 19. 8.0 10.0 12.0 14.0 16.0 18.0 20.0 22.0 24.0 26.0 28.0 0 2000000 4000000 6000000 8000000 1e+07 1.2e+07 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 Phase: BP20, 0.25 µm film Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 5 °C/min to 200 °C Final Temp: 200 °C Detector Type: Mass Spectrometer Carrier Gas: He, 7.0 psi Constant Flow: 1.0 mL/min. Average Linear Velocity: 36 cm/sec at 40 °C Injection Mode: Split Split Ratio: 200:1 Purge on (Split) Vent Flow: 200 mL/min. Injection Volume: 0.2 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Double Taper Liner Liner Part Number: 092018 Column Part Number: 054101 ANALYSIS OF WINE ON BP20 0 105 minutes 1 2 3 4 5 6 7 8 9 10 Phase: BP20, 1.0 µm Column: 25 m x 0.32 mm ID Initial Temp: 40 °C, 2 min Rate 1: 5 °C/min Temp 2: 50 °C Rate 2: 15 °C/min Final Temp: 190 °C Carrier Gas: H₂,6psi Injection Mode: 2 µL Column Part Number: 054442 Components 1. Acetaldehyde 2. Ethyl Acetate 3. Methanol 4. Isopropanol 5. Ethanol 6. Propanol 7. Isobutanol 8. Isoamyl Alcohol 9. Acetic Acid 10. Unknown ANALYSIS OF TEATREE OIL ON BPX5 Components 1. Thujene 2. α-Pinene 3. Sabinene 4. 3-Octanol 5. ß-Pinene 6. α-Phellandrene 7. α-Terpinene 8. p-Cymene 9. Limonene 10. 1,8-Cineole 11. y-Terpinene 12. Terpinolene 13. Terpinen-4-ol 14. α-Terpineol 15. α -Gurjunene 16. (trans)-ß-Caryophyllene 17. Aromadendrene 18. Alloaromadendrene 19. Ledene 20. Germacrene B 21. α-Cadinene 22. 1s, cis-Calamenene 23. Globulol ANALYSIS OF SCOTCH WHISKY ON BP20 Phase: BP20, 1.0 µm Column: 12 m x 0.53 mm ID Initial Temp: 55 °C, 3 min Rate: 10 °C/min Final Temp: 120 °C, 0 min Detector: FID Sensitivity: 128 x 10-¹²AFS Injection Mode: Split Column Part Number: 054447 Components 1. Acetaldehyde 2. Ethyl Acetate 3. Methanol 4. Ethanol 5. Propan-1-ol 6. 2-Methylpropan-1-ol 7. 2-Methylbutan-1-ol+3- Methylbutan-1-ol 1 2 3 4 5 6 7 0 3 6 minutes For extended life of polar columns, always use an oxygen trap in the carrier gas line. EXPERTTIP Food, Flavors and FragrancesFood, Flavors and Fragrances 16For further information on our full range of products, please visit www.sge.com
  • 20. Phase: BPX70, 0.25 µm film Sample: 10 ppm in methanol Column: 25 m x 0.32 mm ID Initial Temp: 80 °C, 2 min Rate 1: 50 °C/min to 130 °C, 10 min Rate 2: 2 °C/min to 172°C Final Temp: 172 °C , 6 min Detector Type: FID Detector Temp: 300 °C Carrier Gas: He, 10 psi Carrier Gas Flow: 2.2 mL/min. Constant Flow: On Average Linear Velocity: 39 cm/sec at 80 °C Injection Mode: Split Split Ratio: 58:1 Injection Volume: 1 µL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Focus Liner™ Liner Part Number: 092002 Column Part Number: 054606 ACKNOWLEDGEMENT SGE would like to thank Masterfoods UK for supplying the sample and chromatographic conditions for this chromatogram. For more information see SGE technical poster TP-0100-C The chromatogram shows the excellent separation of a complex mixture of FAME compounds. Note the excellent peak shape and separation of the Omega-1,2 and 3 fatty acid isomers both structural and cis and trans. 55 10 15 20 25 30 35min 15 10 5 12 17 21 22 30 32 34 pA 45 40 35 30 25 20 1 2 3 5 6 7 8 9 10 11 13 14 15 16 18 19 20 23 24 25 26 27 28 3129 33 Components 1. C6 2. C8 3. C10 4. C11 5. C12 6. C13 7. C14 8. C14:1 cis 9 9. C15 10. C16 11. C16:1 cis 9 12. C17 13. C17:1 cis 10 14. C18 15. C18:1 trans 9 16. C18:1 cis 9 17. C18:1 cis 12 18. C18:2 trans 9,12 19. C18:2 cis 9,12 20. C18:3 cis 6,9,12 21. C18:3 cis 9,12,15 22. C18:4 cis 6,9,12,15 23. C20 24. C21:1 cis 11 25. C20:2 cis 11,14 26. C20:3 cis 8,11,14 27. C20:4 cis 5,8,11,14 28. C20:3 cis 11,14,17 29. C22 30. C20:5,8,11,14,17 31. C22:1 cis 13 32. C22:4 cis 7,10,13,16 33. C24 34. C22:6 cis 4,7,10,13,16,19 ANALYSIS OF OMEGA-3 FATTY ACIDS USING A BPX70 WHAT IS DIFFERENT ? • BPX90 is a highly polar phase of the poly (biscyanopropylsiloxane) type. • The phase has excellent thermal stability and a wide operating range (70 - 280 °C). • The separation mechanisms gives short elution times relative to other polar phases. BPX90 shows low selectivity for non-polar analytes and saturated FAME. • BPX90 shows enhanced selectivity for polyunsaturated FAME and the selectivity can be tuned with film thickness. • BPX90 is effective for the separation of cis and trans isomers and positional isomers of FAME analytes. Supelco 37 FAME test mixture. Columns 15 m x 0.25 mm ID x 0.25 micron film. Temperature programmed 70°C (hold 1 min) to 150 °C (20 °C/min) to 250 °C (10 °C/min) then hold at 250 °C (5 min). Injector: 240 °C. Detection MS. C18-C22 FAME test mixture. Columns 30 m x 0.25 mm ID x 0.25 micron film. Isothermal: 180°C. Injector: 240 °C. Detection FID at 280 °C. FAME POLARITY TEST BPX90 – A HIGHLY POLAR PHASE FOR FAME ANALYSIS C14:0 C15:0 C16:0 C17:0 C18:0 C20:0 C21:0 C22:0 C23:0 C24:0 C14:1 C15:1 C16:1 C17:1 C18:1n9trans C18:n9cis C20:1 C22:1n9 C24:1 C14:0 C15:0 C16:0 C17:0 C18:0 C20:0 C21:0 C22:0 C23:0 C24:0 C14:1 C15:1 C16:1 C17:1 C18:1n9trans C18:n9cis C20:1 C22:1n9 C24:1 C18:2n6trans C18:2n6cis C18:3n6 C18:3n3 C20:2 C20:3n6 C20:3n3 C20:4n6 C22:2 C20:5n3(EPA) C22n6(DHA) C18:2n6trans C18:2n6cis C18:3n6 C18:3n3 C20:2 C20:3n6 C20:4n6 C20:3n3 C20:5n3(EPA) C22:2 C22n6(DHA) BPX70 BPX90 Food, Flavors and Fragrances 17 For further information on our full range of products, please visit www.sge.com
  • 21. ANALYSIS OF PUFA-2 ANIMAL FAME ON BPX70 PUFA-2 ANIMAL FAME Phase: BPX70, 0.25 µm film Column: 25 m x 0.22 mm ID Initial Temp: 150 °C, 0 min Program Rate: 2 °C/min Final Temp: 210 °C, 5 min Carrier Gas: He, 15 psi Detector: FID, 280 °C Sensitivity: 32 x 10-¹²AFS Injection Mode: Split, 50:1 Column Part Number: 054602 Components 1. C14:0 2. C16:0 3. C16:1n7 4. C18:0 5. C18:1n9 6. C 18:2n7 7. C18:2n6 8. C18:3n3 9. C20:0 10. C20:1n11 11. C20:3n6 12. C20:4n6 13. C20:5n3 14. C22:4n6 15. C22:5n3 16. C22:6n3 14 16 13 12 4 7 11 2 1 3 5 6 15 8 0351 minutes 9 10 0 ANALYSIS OF PUFA-1 MARINE FAME ON BPX70 PUFA-2 ANIMAL FAME Phase: BPX70, 0.25 µm Column: 50 m x 0.22 mm ID Initial Temp: 150 °C, 0 min Program Rate: 2 °C/min Final Temp: 210 °C, 5 min Carrier Gas: He, 15 psi Detector: FID, 280 °C Sensitivity: 32 x 10-¹²AFS Injection Mode: Split, 50:1 Column Part Number: 054603 1 2 3 4 5 6 7 8 10 9 03setunim51 Components 1. C18:1n9 2. C18:1n7 3. C18:2n6 4. C18:3n3 5. C18:4n3 6. C 20:0 7. C20:1n9 8. C20:4n6 9. C20:5n3 10. C22:1n11 ANALYSIS OF PUFA-1 MARINE FAME ON BPX70 Phase: BPX70, 0.25 µm film Column: 25 m x 0.22 mm ID Initial Temp: 150 °C, 0 min Program Rate: 2 °C/min Final Temp: 210 °C, 5 min Carrier Gas: He, 15 psi Detector: FID, 280 °C Sensitivity: 32 x 10-¹²AFS Injection Mode: Split, 50:1 Column Part Number: 054602 Components 1. C14:0 2. C16:0 3. C16:1n7 4. C18:1n9 5. C18:1n7 6. C 18:2n6 7. C18:3n3 8. C18:4n3 9. C20:0 10. C20:1n9 11. C20:4n6 12. C20:5n3 13 16 14 12 11 8 9 7 6 10 5 2 15 30 minutes 4 15 0 1 3 To fully utilize the high thermal stability of BPX70 columns SGE recommend the use of helium when operating above 220/230°C for extended periods. EXPERTTIP Food, Flavors and FragrancesFood, Flavors and Fragrances 18For further information on our full range of products, please visit www.sge.com
  • 22. For Fuels and Petrochemical analysis by GC, one of the main considerations is the thermal stability of the column, both physical and chemical. Phases must have high temperature limits to allow the analysis of high boiling point compounds and columns must be able to physically withstand repeated cycling to extreme temperatures. Columns such as SGE’s BPX1 and HT5 have been created with these demands in mind. Where higher polarity is required, such as the separation of aromatic compounds, SolGel-WAX™ and BPX90 provide enhanced selectivity without the unnecessary sacrifice of maximum temperature limits. Applications • Total Recoverable Petroleum Hydrocarbons (TRPH) Analysis on Standard and Fast BPX5 • Analysis of Polywax 655 and Refinery Lubrication Oil on HT5 • The Separation of Aromatics from Olefins in Petroleum Samples using BPX90 • Unleaded Gasoline on BPX5 • Fast GC For TPH Analysis • Simulated Distillation using BPX1-SimD Fuels and Petrochemical 19 For further information on our full range of products, please visit www.sge.com
  • 23. TOTAL RECOVERABLE PETROLEUM HYDROCARBONS (TRPH) ANALYSIS ON STANDARD AND FAST BPX5 Chromatogram showing separation of Total Recoverable Petroleum Hydrocarbons using a conventional 30 m x 0.25 mm ID BPX5 column with a 0.25 micron film. Chromatogram showing separation of Total Recoverable Petroleum Hydrocarbon using a FAST BPX5 column. Phase: BPX5, 0.25 µm film TRPH (C8-C40): 5 ng/µL in dichloromethane Column: 30 m x 0.25 mm ID Initial Temp: 40 °C , 2 min Rate 1: 30 °C/min to 330 °C Rate 2: NA Final Temp: 330 °C, 9 min Detector Type: FID, 350 °C Carrier Gas: He, 14.4 psi Carrier Gas Flow : 1.29 mL/min Constant Flow: On Average Linear Velocity: 40 cm/sec at 40 °C Injection Mode: Split, 120:1 Purge On Time: NA Purge On (Split) Vent Flow: 160 mL/min Injection Volume: 1µL Injection Temperature: 250 °C Autosampler: Yes Liner Type : 4 mm ID FocusLiner™ with single taper Liner Part Number: 092003 Column Part Number: 054101 Phase: BPX5, 0.10 µm film TRPH (C8-C40) Standard: 5 ng/µL in dichlormethane Column: 10 m x 0.10 mm ID Initial Temp: 40 °C , 1 min Rate 1: 30 °C/min to 330 °C Rate 2: NA Final Temp: 330 °C, 0 min Detector Type: FID, 350 °C Carrier Gas: He, 28 psi Carrier Gas Flow : 0.52 mL/min Constant Flow: On Average Linear Velocity: 55 cm/sec at 40 °C Injection Mode: Split, 120:1 Purge On Time: NA Purge On (Split) Vent Flow: 62 mL/min Injection Volume: 1 µL Injection Temperature: 250 °C Autosampler: Yes Liner Type : 2.3 mm ID FocusLiner™ Liner Part Number: 092005 Column Part Number: 054099 NORMAL FAST C8 C10 C12 C14 C16 C18 C20 C22 C24 C26 C28 C30 C32 C34 C36 C38 C40 0 minutes 20 C8 C10 C12 C14 C16 C18 C20 C22 C24 C26 C28 C30 C32 C34 C36 C38 C40 0 minutes 10 ANALYSIS OF POLYWAX 655 AND REFINERY LUBRICATION OIL ON HT5 POLYWAX 655 AND REFINERY LUBRICATION OIL Phase: HT5, 0.1 µm Column: 6 m x 0.53 mm ID Initial Temp: 50 °C Rate: 10 °C/min Final Temp: 480 °C, 15 min Detector: FID Sensitivity: 40 x 10-¹² AFS Injection Mode: On-Column Carrier Gas: H2, 20 mL/min Solvent: CS₂ Column Part Number: 054661 POLYWAX 655 50 TEMPERATURE(°C) 480 REFINERY LUBRICATION OIL 320 450 570 650 700 750 boiling point (0°C) Fuels and Petrochemical 20For further information on our full range of products, please visit www.sge.com
  • 24. The separation of a petroleum sample using a BPX90 column (30 m x 0.25 mm ID, 250 micron film) showing the resolution of aromatic families and the separation from more abundant alkanes. THE SEPARATION OF AROMATICS FROM OLEFINS IN PETROLEUM SAMPLES USING BPX90 UNLEADED GASOLINE ON BPX5 Sample Introduction: Injector Temp: 240 °C Injection Volume: 0.1 µL Autosampler Syringe: 0.5 µL Removable Needle Part No. 000410 Septa: Auto-Sep T™ Part No. 041882 Injection Type: Split Purge On Time: NA Purge On (Split) Vent: 200 mL/min Split Ratio: 149 :1 Liner Type: FocusLiner™ single taper Part No.092003 Pressure/Flow Values: Carrier Gas: He Constant Flow: On Pressure: 13.6 psi Column Flow: 1.34 mL/min Linear Velocity: 30 cm/sec @ 25 °C Oven Parameters: Initial Temp: 25 °C Initial Time: 1 min Rate 1: 30 °C/min Final Temp 1: 240 °C Hold Time: 1 min Run Time: 9.17 min Detector Parameters: Detector Type: FID @ 280 °C 2 4 1 5 3 0 2 4 6 min Components 1. Benzene 2. Toluene 3. Ethylbenzene 4. m,p-Xylene 5. o-Xylene Phase: BPX5, 0.25 µm film Column: 30 m x 0.25 mm ID Column Part Number: 054101 Fuels and Petrochemical 21 For further information on our full range of products, please visit www.sge.com
  • 25. Reference Gas Oil MT-60CS2 Blank FAST GC FOR TPH ANALYSIS Phase: BPX5, 0.1 µm Column: 5 m x 0.1 mm ID Initial Temp: 50 °C Rate 1: 45 °C/min Final Temp: 300 °C, 0 min Detector Temp: 270 °C Detector: FID Carrier: He, Inlet pressure 40 psi (constant flow mode, linear velocity of 75 cm/sec) C8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 28 30 C32 0 1 2 3 4 5 6 minutes 20 60 100 140 pA Chromatogram of TPH standards from C8 to C32 Chromatogram showing elution of BTEX in under one minute Benzene Toluene Ethyl Benzene p-m, xylene o- xyleneC8 C12 0 0.5 1 1.5 2 minutes 20 60 100 140 pA 0302setunim010 10pA base line 25pA 420˚C SIMULATED DISTILLATION USING BPX1-SIMD Phase: BPX1, 0.1 µm Column: 5 m x 0.53 mm ID Initial Temp: 40 °C Rate: 15 °C Final Temp: 420 °C, 5 min Detector Temp: 440 °C Carrier Gas: He, 10 mL/min Instrument: HP 6890 Column Part Number: 054800 Separation Systems Injector Initial Temp: 40 °C Rate: 15 °C Final Temp: 420 °C, 5 min Standard mix for HTSD using BPX1-SimD setunim02010 C20 C40 C60 C80 C100 setunim02010 C60 C80 C40 C90 C110 C100 Enlarged section of the chromatogram above A portion of the previous chromatogram from C40 to the end of the analysis (expanded vertically) shows excellent resolution and the ability to see beyond C110. 0 10 minutes 20 30 3.2 min 200 400 pA 21.277 min IBP 0.6 5% -6.2 10% -3.4 20% -2.9 30% -1.1 40% 0.7 50% 1.1 60% 2.1 70% 2.3 80% 1.8 90% 1.2 95% 0.2 FRP 0.3 Gas Oil Reference All of the data presented was produced by Dr. Lubkowitz and the staff at Separation Systems Inc. on a system using the Separation System programmed temperature vaporization injector (PTV) and the SIMDIS EXPERT® software Fuels and Petrochemical 22For further information on our full range of products, please visit www.sge.com
  • 26. For general chemical analysis, a good rule of thumb is to use the lowest polarity column that provides sufficient separation. Particular classes of compounds, such as alcohols, amines, or organic acids, may require thicker film phases, or specific phases such as the BPX35 or BP21 to avoid undue peak tailing. Applications • Analysis of 18 Alcohols on BP20 • Analysis of Aliphatic Alcohols on BP1 • Analysis of 15 Organic Acids on BP20 • US EPA 625 Phenols Mix on BPX50 • Analysis of Organic Acids in Water on BP21 • Analysis of Amines on BP1 • Analysis of Aromatic Amines on BP5 • Analysis of Aromatic Amines from Diazo Dyes on BPX35 • Analysis of Ketones on Thick Film BPX5 • Analysis of Triethylamine and Triethanolamine on SolGel-1ms™ ChemicalChemical 23 For further information on our full range of products, please visit www.sge.com
  • 27. 0201inutes0 m ANALYSIS OF 15 ORGANIC ACIDS ON BP20 Components 1. Valeric Acid 2. Caproic Acid 3. Heptanoic Acid 4. Octanoic Acid 5. Nonanoic Acid 6. Decanoic Acid 7. Undecanoic Acid 8. Dodecanoic Acid 9. Tridecanoic Acid 10. Tetradecanoic Acid 11. Pentadecanoic Acid 12. Hexadecanoic Acid 13. Heptadecanoic Acid 14. Octadecanoic Acid 15. Arachidic Acid ORGANIC ACIDS Phase: BP20, 0.25 µm Column: 30 m x 0.32 mm ID Initial Temp: 70 °C Rate: 10 °C/min Final Temp: 260 °C, 5 min Detector: FID Injection Mode: Split Carrier Gas: H2, 6 psi Column Part Number: 054433 1 2 3 4 5 6 7 8 9 1 0 1 2 1 1 1 3 1 4 1 5 ANALYSIS OF 18 ALCOHOLS ON BP20 0 2 4 6 8 10 12 minutes 1 2 3 4 5 6 7 8 9 1 0 1 1 1 2 1 4 1 5 1 6 1 7 1 8 1 3 Components 1. Methanol 2. Propan-2-ol 3. Ethanol 4. sec-Butan-1-ol 5. n-Propanol + 2-Methyl-3-Buten-2-ol 6. d,l-3-Methyl-2-Butan-1-ol 7. Pentan-3-ol 8. d,l-2-Pentan-1-ol 9. n-Butanol 10. 2,4-Dimethyl Pentan-3-ol 11. Hexan-3-ol 12. 2-Methyl Prop- 2-en-1-ol 13. Crotyl Alcohol (2-Buten-1-ol) 14. Hexan-2-ol 15. Pentan-1-ol 16. 2-Methyl Pentan-1-ol 17. 2-Ethyl Butan-1-ol 18.Hexan-1-ol ALCOHOLS Phase: BP20, 0.25 µm film Column: 30 m x 0.25 mm ID Initial Temp: 45 °C, 2 min Rate: 3 °C/min Final Temp: 80 °C, 0 min Detector: FID Sensitivity: 128 x 10-¹² AFS Injection Mode: Split Column Part Number: 054427 After installing a new column purge with oxygen free carrier gas for at least 30 minutes before heating GC oven. EXPERTTIP ANALYSIS OF ALIPHATIC ALCOHOLS ON BP1 0 minutes 10 76 5 4 321 Components 1. Octanol 2. Decanol 3. Undecanol 4. Dodecanol 5. Tetradecanol 6. Hexadecanol 7. Eicosanol ALCOHOLS Phase: BP1, 3.0 µm film Column: 12 m x 0.53 mm ID Initial Temp: 100 °C Rate: 10 °C/min Final Temp: 260 °C Carrier Gas: N2 Injection Volume: 0.1 µL Column Part Number: 054097 Chemical 24For further information on our full range of products, please visit www.sge.com
  • 28. ANALYSIS OF AMINES ON BP1 Components 1. Aniline 2. Decylamine 3. Dicyclohexylamine 4. Dodecylamine 5. Tetradecylamine ANALYSIS OF AMINES Phase: BP1, 3.0 µm film Column: 12 m x 0.53 mm ID Initial Temp: 70 °C Rate: 10 °C/min Final Temp: 250 °C Carrier Gas: N2 Injection Volume: 0.1 µL Column Part Number: 054097 0 minutes 10 1 2 3 4 5 US EPA 625 PHENOLS MIX ON BPX50 US EPA 625 PHENOLS MIX Phase: BPX50, 0.25 µm Column: 30 m x 0.25 mm ID Injector Mode: Split, 40:1 Initial Oven Temp: 50°C, 1 min Rate 1: 8 °C/min Final Temp: 300 °C, 10 min Detector: HP 5973 MSD Column Part Number: 054751 8.00 10.00 12.00 14.00 18.0016.00 22.0020.00 1 3 7 98 2 4 5 6 10 30000 Abundance 20000 10000 Components 1. 2-Chlorophenol 2. 2-Nitrophenol 3. 2, 4-Dimethylphenol 4. 2, 4-Dichlorophenol 5. 4-Chloro-3-methylphenol 6. 2, 4, 6-Trichlorophenol 7. 2, 4- Dinitrophenol 8. 4-Nitrophenol 9. 2-Methyl-4, 6-dinitrophenol 10. Pentachlorophenol ANALYSIS OF ORGANIC ACIDS IN WATER ON BP21 SETUNIM510150 1 2 3 4 5 6 7 8 9 Components 1. Acetic Acid 2. Propanoic Acid 3. iso-Butyric Acid 4. n-Butyric Acid 5. iso-Valeric Acid 6. n-Valeric Acid 7. n-Caproic Acid 8. n-Heptanoic Acid 9. Lactic Acid ORGANIC ACIDS IN WATER (0.03M OXALIC ACID) Phase: BP21, 0.5 µm film Column: 30 m x 0.53 mm ID Initial Temp: 85 °C, 0 min Rate: 6 °C/min Final Temp: 180 °C, 5 min Detector: FID Sensitivity: 64 x 10-¹² AFS Injection Mode: On-Column Column Part Number: 054477 On-column injection and the addition of a 0.03M Oxalic acid (2%) to the injection solution increases the acidity of the column to allow lactic acid to be detected. EXPERTTIP Chemical 25 For further information on our full range of products, please visit www.sge.com
  • 29. ANALYSIS OF AROMATIC AMINES FROM DIAZO DYES ON BPX35 Phase: BPX35 0.25 µm film Azo Dyes Standard: 10 ppm solution in DCM Column: 30 m x 0.25 mm ID Initial Temp: 50 °C, 2 min Rate 1: 15 °C/min to 240 °C Rate 2: 10 °C/min to 280 °C Final Temp: 280 °C, 25 min Detector Type: MSD Carrier Gas: He, 7.1 psi Carrier Gas Flow : 1.0 mL/min Constant Flow: On Average Linear Velocity: 36 cm/sec at 50 °C Injection Mode: Splitless Purge On Time: 1.0 min Purge On (Split) Vent Flow: 60 mL/min Injection Volume: 1 µL Injection Temperature: 250 °C Autosampler: No Liner Type : 4 mm ID Double Taper Liner Part Number: 092018 Column Part Number: 054701 Components 1. Indolin 2. o-Toluidine 3. 2,4-Diaminoanisole 4. p-Chloroailine 5. p-a residine 6. 2,4,6-Trimethylaniline 7. 4-Chlorotoludine 8. Unknown 9. 2-Naphtylamine 10. Unknown 11. 4-Aminodiphenyl 12. 4,4’-Oxydianiline 13. 4,4’-Diaminodiphenylmethane 14. Benzidine 15. 3,3’-Dimethyl- 4,4’diaminodiphenyl- methane 16. 3,3’-dimethylbenzidine 17. 4,4’-Thiodianiline 18. 3,3’-Dichlorobenzidine 19. 4,4’-Methylene- bis(2chloraniline) 20. 3,3’-Dimethoxybenzidine 10.0 15.0 20.0 25.0 30.0 0 100000 200000 300000 400000 500000 600000 700000 800000 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18, 19, 20 ANALYSIS OF AROMATIC AMINES ON BP5 Components 1. Pyridine 2. 2-Methyl Pyridine 3. gamma - BHC 4. Aniline 5. o-Toluidine 6. m-Toluidine 7. 2,6-Dimethylaniline 8. 1,4-Phenyldiamine 9. Nicotine 10. Biphenylamine 11. Bibenzylamine 21SETUNIM60 3 4 6 5 7 8 9 1 0 1 1 Phase: BP5, 1.0 µm film Column: 12 m x 0.53 mm ID Initial Temp: 60 °C, 0 min Rate: 10 °C/min Final Temp: 190 °C, 0 min Detector: FID Sensitivity: 128 x 10-¹²AFS Injection Mode: Split Column Part Number: 054197 Using a thicker film helps prevent amines from tailing. EXPERTTIP SilTite™ ferrules eliminate the need for re-tightening following temperature cycling and reduce oxygen levels within the system improving performance EXPERTTIP ChemicalChemical 26For further information on our full range of products, please visit www.sge.com
  • 30. ANALYSIS OF KETONES ON THICK FILM BPX5 Phase: BPX5, 1.0 µm film Sample: 300 ppm in dichloromethane Column: 60 m x 0.25 mm ID Initial Temp: 40 °C , 5 min Rate 1: 10 °C/min to 80 °C Rate 2: 30 °C/min to 260 °C Final Temp: 260 °C, 4 min Detector Type: FID Detector Temp: 360 °C Carrier Gas: He, 27.6 psi Carrier Gas Flow : 1.9 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.4 µL Injection Temperature: 250 °C Autosampler: No Liner Type : 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054123 Components 1. Ethanol 2. Acetone 3. 2-Butanone 4. 3-Methyl-2-butanone 5. 2-Pentanone 6. 3-pentanone 7. 4-Methyl-2-pentanone 8. 3-Methyl-2-pentanone 9. 3-Hexanone 10. 2-Hexanone 11. Mesityl oxide 12. Cyclopentanone 13. 2-Methyl-3-hexanone 14. 4-Methyl-2-hexanone 15. 5-Methyl-2-hexanone 16. 3-Heptanone 17. 2-Heptanone 18. Cyclohexanone 19. 2-Octanone 20. 2-Nonanone 21. 2-Decanone 22. 2-Undecanone 23. 2-Dodecanone min4 6 8 10 12 14 16 pA 10 20 30 40 50 60 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 ANALYSIS OF TRIETHYLAMINE AND TRIETHANOLAMINE ON SOLGEL-1ms™ min0 2 4 6 8 10 12 14 16 18 counts 5000 10000 15000 20000 25000 30000 Triethanolamine Triethylamine Solvent Phase: SolGel-1ms, 0.25 µm film Amine mix: 10 ng/µL in dichloromethane Column: 30 m x 0.32 mm ID Initial Temp: 40 °C , 5.0 min Rate 1: 20 °C/min to 200 °C Final Temp: 200 °C, 7 min Detector Type: FID Detector Temp: 300 °C Carrier Gas: He, 9.9 psi Carrier Gas Flow : 2.2 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 100 °C Mode of Injection: Split Split Ratio: 50:1 Injection Volume: 0.3 µL Injection Temperature: 250 °C Autosampler: No Column Part Number: 054798 To prevent decreasing retention times in your chromatography, replace the septum daily. EXPERTTIP Chemical AnalysisChemical 27 For further information on our full range of products, please visit www.sge.com
  • 31. GC analysis of Pharmaceuticals covers a wide range of compounds that can vary greatly in their molecular weight, reactivity,andpH.FromtheanalysisoflowmolecularweightresidualsolventsonaG43(BPX-Volatiles)tohighermolecular weight compounds on a G42 (BPX35), a wide range of GC columns are often specified in the test methods. Proper deactivation of GC consumables such as liners and columns becomes increasingly important where system inertness has to be demonstrated. SGE’s unique, high temperature gas phase deactivation ensures maximum inertness and minimal activity from our columns and consumables. Applications • USP Methods • Analysis of Tricyclic Antidepressants on BPX35 • Analysis of Dioxane Impurities on BP20 • Analysis of a Common Solvent Mixture on a Thick Film BPX5 • Analysis of a Common Pharmaceutical Solvent on BPX-Volatiles • Analysis of a Common Pharmaceutical Solvent on BPX-Volatiles • Analysis of Class I Solvents on BPX-Volatiles • Analysis of the Separation of the Class III Solvents on BPX-Volatiles Pharmaceutical 28For further information on our full range of products, please visit www.sge.com
  • 32. Method Phase Composition SGE Phase Recommendation G1 Dimethylpolysiloxane oil BP1, SOLGEL-1ms™ G2 Dimethylpolysiloxane gum BP1, SOLGEL-1ms G3 50% Phenyl - 50% Methylpolysiloxane BPX50 G5 3-Cyanopropylpolysiloxane BPX70 G7 50% 3-Cyanopropyl - 50% Phenylmethylsilicone BP225 G14 Polyethylene glycol (average molecular weight of 950-1,050) BP20(WAX), SOLGEL-WAX™ G15 Polyethylene glycol (average molecular weight of 3,000-3,700) BP20(WAX), SOLGEL-WAX G16 Polyethylene glycol (average molecular weight of 15,000) BP20(WAX), SOLGEL-WAX G17 75% Phenyl - 25% Methylpolysiloxane BPX50 G19 25% Phenyl - 25% Cyanopropylmethylsilicone BP225 G20 Polyethylene glycol (average molecular weight of 380-420) BP20(WAX), SOLGEL-WAX G25 Polyethylene glycol TPA (Carbowax 20M terephthalic acid) BP21(FFAP) G27 5% Phenyl - 95% Methylpolysiloxane BP5, BPX5 G28 25% Phenyl - 75% Methylpolysiloxane BPX35 G32 20% Phenylmethyl - 80% Dimethylpolysiloxane BPX35 G35 Polyethylene glycol diepoxide esterified with nitroterephthalic acid BP21(FFAP) G36 1% Vinyl - 5% Phenylmethylpolysiloxane BP5, BPX5 G38 Phase G1 plus a tailing inhibitor BP1, SOLGEL-1ms G39 Polyethylene glycol (average molecular weight of 1,500) BP20(WAX), SOLGEL-WAX G41 Phenylmethyldimethylsilicone (10% phenyl substituted) BP5, BPX5 G42 35% Phenyl - 65% Dimethylvinylsiloxane BPX35 G43 6% Cyanopropylphenyl - 94% Dimethylpolysiloxane BP624 G46 14% Cyanopropylphenyl - 86% methylpolysiloxane BP10 (1701) USP Methods Fused Silica Tubing ETP multiplier Quality guaranteed• Chemically inert and thermally stable• Suitable for organic and aqueous solvents• Ideal for biotechnology applications• Custom-made tubing available upon request• Available deactivated for guard column material• Tubing protected with a high temperature• Polyimide resin (+400 ˚C) Air stable• 2 year shelf life guarantee• Discrete dynode design results in extend operating life• Total compatibility with all major quadrupole,• magnetic sector and TOF instruments 29 For further information on our full range of products, please visit www.sge.com
  • 33. ANALYSIS OF Tricyclic Antidepressants on BPX35 TRICYCLIC ANTIDEPRESSANTS Phase: BPX35, 0.25 μm Column: 25 m x 0.22 mm ID Initial Temp: 210 °C, 1 min Rate: 5 °C/min Final Temp: 280 °C Carrier Gas: Helium, 150 kpa Injection Mode: Split (20:1) Detector: FID, 380 °C Column Part Number: 054711 Components 1. Amitriptyline 2. Trimipramine 3. Nortriptyline 4. Doxepin 5. Desipramine analysis of Dioxane Impurities on BP20 Phase: BP20, 1.0 μm Column: 25m x 0.53 mm ID Initial Temp.: 40°C, 2 min Rate: 10 °C/min Final Temp.: 120 °C Detector: FID, 280 °C Injector Mode: Split, 30:1, Carrier Gas: Hydrogen, 2 psi Injection Volume: 0.2 μL Column Part Number.: 054448 Components 1. Methanol 2. Dichloromethane 3. Ethanol 4. Dioxane impurity 5. Dioxane Analysis of a Common Solvent Mixture on a Thick Film BPX5 Phase: BPX5, 1.0 μm film Sample: neat Column: 60m x 0.25 mm ID Initial Temp: 32 °C, 5 min. Rate 1: 20 °C/min to 190 °C, Final Temp: 190°C, 2 min. Detector Type: FID Detector Temp.: 360 °C Carrier Gas: He, 26.9 psi Carrier Gas Flow: 1.9 mL/min. Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.3 μL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054123 Components 1. Methanol 2. Ethanol 3. Acetone 4. Isopropyl alcohol 5. Acetonitrile 6. Dichloromethane 7. 2-Butanone 8. Ethyl acetate 9. Benzene Pharmaceutical Pharmaceutical 30For further information on our full range of products, please visit www.sge.com
  • 34. ANALYSIS OF Common pharmaceutical solvent on BPX-Volatiles Phase: BPX-Volatiles, 1.4 μm film Sample: 200 ppm in methanol Column: 30 m x 0.25 mm ID Initial Temp: 35 °C, 15 min Rate 1: 5 °C/min to 100 °C Final Temp: 100 °C, 2 min Detector Type: Mass Spectrometer Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 35 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.5 μL Injection Temp: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part No: 054980 Full Scan / SIM: Full scan 25-450 Components 1. Methanol 2. Ethanol 3. Ethyl ether 4. Acetone 5. iso-propyl alcohol 6. Acetonitrile 7. Methylene chloride 8. t-Butanol 9. Hexane 10. Propanol 11. 2-Butanone 12. Ethyl acetate 13. 2-Butanol 14. Tetrahydrofuran 15. Chloroform 16. Cyclohexane 17. Benzene 18. n-Heptane 19. n-Butanol 20. 1,4-Dioxane 21. Pyridine 22. Toluene 23. Dimethylformamide ANALYSIS OF Common pharmaceutical solvent on BPX-VOLATILES Phase: BPX-Volatiles 1.4 μm film USEPA 502.2 mix: 200 ppm in Methanol Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 0 min Rate 1: 6 °C to 210 °C Rate 2: 15 °C to 240 °C Final Temp: 240 °C, 5 min Detector Type: Mass Spectrometer Carrier Gas: He, 22.8 Carrier Gas Flow: 1.3 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Split Split Ratio: 50:1 Injection Volume: 1 mL Injection Temp: 250 °C Autosampler: No Liner Type: 4mm ID Single Taper Liner Liner Part No: 092017 Column Part No: 054980 Full Scan / SIM: Full scan 45-450 Components 1. Dichlorodifluoromethane 2. Chloromethane 3. Vinyl chloride 4. Bromomethane 5. Chloroethane 6. Trichlorofluoromethane 7. 1,1-Dichloroethene 8. Dichloromethane 9. trans-1,2-Dichloroethene 10. 1,1-Dichloroethane 11. 2,2-Dichloropropane 12. cis-1,2-Dichloroethene 13. Bromochloromethane 14. Chloroform 15. 1,1,1-Trichloroethane 16. 1,1-Dichloropropene 17. Carbon tetrachloride 18. Benzene 19. 1,2-Dichloroethane 20. Trichloroethene 21. 1,2-Dichloropropane 22. Dibromomethane 23. Bromodichloromethane 24. cis-1,3-Dichloropropene 25. Toluene 26. trans-1,3- Dichloropropene 27. 1,1,2-Trichloroethane 28. Tetrachloroethene 29. 1,3-Dichloropropane 30. Dibromochloromethane 31. 1,2-Dibromoethane 32. Chlorobenzene 33. Ethylbenzene 34. 1,1,1,2-Tetrachloroethane 35. m-Xylene 36. p-Xylene 37. o-Xylene 38. Styrene 39. Bromoform 40. Isopropylbenzene 41. Bromobenzene 42. 1,1,2,2-Tetrachloroethane 43. 1,2,3-Trichloropropane 44. n-Propyl benzene 45. 2-Chlorotoluene 46. 1,3,5-Trimethylbenzene 47. 4-Chlorotoluene 48. tert-Butylbenzene 49. 1,2,4-Trimethylbenzene 50. sec-Butylbenzene 51. 1,3-Dichlorobenzene 52. p-Isopropyltoluene 53. 1,2-Dichlorobenzene 54. n-Butylbenzene 55. 1,4-Dichlorobenzene 56. 1,2-Dibromo-3- chloropropane 57. 1,2,4-Trichlorobenzene 58. Hexachlorobutadiene 59. Naphthalene 60. 1,2,3-Trichlorobenzene Pharmaceutical 31 For further information on our full range of products, please visit www.sge.com
  • 35. ANALYSIS OF Class i solvents on bpx-volatiles Phase: BPX-Volatiles 1.4 μm film Sample: 200 ppm in methanol Column: 30 m x 0.25 mm ID Initial Temp: 40 °C, 1 min Rate 1: 6 °C/min to 80 °C Final Temp: 80 °C Detector Type: Mass Spectrometer Carrier Gas: He, 6.7 psi Carrier Gas Flow: 0.9 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 50 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.4 μL Injection Temp: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part No: 054980 Full Scan / SIM: Full scan 30-450 Components 1. 1,1-Dichloroethene 2. 1,1,1-Trichloroethane 3. Carbon tetrachloride 4. Benzene 5. 1,2-Dichloroethane ANALYSIS OF THE separation of THE CLASS III SOLVENTS ON BPX-VOLATILES Components 1. Pentene 2. Ethanol 3. Ethyl ether 4. Acetone 5. iso-Propyl alcohol 6. Ethyl formate 7. Methyl acetate 8. Dichloromethane 9. Methylt-butyl ether 10. n-Propanol 11. Ethyl acetate 12.2-Butanone (MEK) 13. Tetrahydrofuran 14. iso-Butanol 15. sec-Butanol 16. iso-Propyl acetate 17. Heptane 18. Acetic acid 19. n-Butanol 20. Propyl acetate 21. 4-Methyl-2-pentanone 22. Iso-Amyl alcohol 23. Iso-Butyl acetate 24. n-Amyl alcohol 25. Butyl acetate 26. Dimethyl sulfoxide Phase: BPX-Volatiles 1.4 μm film Sample: 200 ppm in methanol Column: 30 m x 0.25 mm ID Initial Temp: 50 °C, 5 min Rate 1: 10 °C/min to 85 °C, 1 min Rate 2: 15 °C/min to 170 °C, Final Temp: 170 °C Detector Type: Mass Spectrometer Carrier Gas: He, 6.7 psi Carrier Gas Flow: 0.9 mL/min Constant Flow: On Average Linear Velocity: 35 cm/sec at 50 °C Injection Mode: Split Split Ratio: 100:1 Injection Volume: 0.4 μL Injection Temp: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part No: 054980 Pharmaceutical Pharmaceutical 32For further information on our full range of products, please visit www.sge.com
  • 36. Forensic Forensic and Toxicology analyses face similar challenges as those found in pharmaceutical assays. These methods are often very challenging due to the analysis of very active compounds as well as coming from samples that are detrimental to GC systems. These compounds are generally basic in nature that makes inertness of the system components critical to successful determinations. The robustness is another critical aspect of clinical analyses. The natures of sample compounds and matrices are extremely arduous on the analytical system. SGE’s columns are designed to withstand these ordeals and provide excellent lifetimes in difficult analyses. Applications • Analysis of Acid/Neutral Drugs on BPX35 • Analysis of Basic Drugs on BPX35 • Analysis of Underivatized Barbiturates on BP5 • Analysis of Various Drugs on BPX50 • Analysis of a Variety of Antidepressant and Anticonvulsant Drugs on BPX50 Forensic 33 For further information on our full range of products, please visit www.sge.com
  • 37. Analysis of Acid/Neutral Drugs on BPX35 Components 1. Ethosuximide 2. Barbital 3. Aprobarbital 4. Butabarbital 5. Amobarbital 6. Pentabarbital 7. Secobarbital 8. Meprobamate 9. Carisoprodal 10. Glutethimide 11. Phenobarbital 12. Methaqualone 13. Primidone ACID/NEUTRAL DRUGS Phase: BPX35, 0.25 μm Column: 25 m x 0.22 mm ID Initial Temp: 100 °C, 1min Rate: 10 °C/min Final Temp: 300 °C, 5 min Carrier Gas: He, 150 kpa Injection Mode: Split, ( 20:1 ) Detector: FID, 380 °C Column Part Number: 054711 Analysis of Basic Drugs on BPX35 Components (Concentration: 100-200 ug/ml) 1. Benzocaine 2 Unknown 3. Meperidine 4. Diphenhydramine 5. Lidocaine 6. Tripelennamine 7. Amitriptyline 8. Tetracaine 9. Pyrilamine 10. Unknown 11. Diazepam 12. Flurazepam 13. Papaverine 14. Triazolam BASIC DRUGS Phase: BPX35, 0.25 μm Column: 25m x 0.22 mm ID Initial Temp: 100 °C Rate: 5 °C/min Final Temp.: 325 °C, 5 min. Carrier Gas: Helium 150 kpa Injection Mode: Split, 0.5 μL (20:1) Detector: FID, 380 °C Column Part Number: 054711 Forensic 34For further information on our full range of products, please visit www.sge.com
  • 38. Analysis of Underivatized Barbiturates on BP5 Components 1. Barbital 2. Butabarbital 3. Amobarbital 4. Pentabarbital 5. Secobarbital 6. Hexabarbital UNDERIVATIZED BARBITURATES Phase: BP5, 1.0 μm Column: 12m x 0.53 mm I.D. Temp: 195 °C Carrier Gas: Hydrogen Carrier Flow: 10 mL/min Injection Volume: 0.1 μL Column Part Number: 054197 Analysis of Various Drugs on BPX50 Components 1. N,N-Dimethylaniline 2. Benzothiazole 3. Selegeline 4. Pethidine 5. Unknown 6. a-octadecene 7. Octadecanoic acid butyl ester 8. Methadone 9. N,N-Dimethylstearamide 10. Chloroquine 11. Dextromoramide 12. Sitosterol 13. Buspirone Phase: BPX50, 0.25 μm film Sample: 5-10 ppm in methanol Column: 30 m x 0.25 mm ID Initial Temp: 150 °C, 0.5 min. Rate 1: 10 °C/min to 180 °C, Rate 2: 1.5 °C/min to 220 °C Rate 2: 30 °C/min to 260 °C Final Temp: 260 °C, 5 min. Detector Type: FID Detector Temp.: 320 °C Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min. Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Splitless Purge on Time: 0.5 min Purge on (Split) Vent Flow: 60 mL/min Injection Volume: 1 μL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054751 Full Scan / SIM: Full scan 45-450 Forensic 35 For further information on our full range of products, please visit www.sge.com
  • 39. Analysis of a Variety of Antidepressant and Anticonvulsant Drugs on BPX50 Components 1. Benzothiazole 2. Selegeline 3. Methsuximide 4. Ketamine 5. Unknown 6. Brompheniramine 7. Imipramine 8. Mianserin 9. Diothiepin 10. Carbamazepine 11. Prazepam 12. Diltiazem 13. Pholcodine Phase: BPX50, 0.25 μm film Sample: 5-10 ppm in methanol Column: 30 m-x 0.25 mm ID Initial Temp: 150 °C, 0.5 min. Rate 1: 10 °C/min to 180 °C, Rate 2: 1.5 °C/min to 220 °C Rate 2: 30 °C/min to 260 °C Final Temp: 260 °C, 5 min. Detector Type: FID Detector Temp.: 320 °C Carrier Gas: He, 25.7 psi Carrier Gas Flow: 1.8 mL/min. Constant Flow: On Average Linear Velocity: 35 cm/sec at 40 °C Injection Mode: Splitless Purge on Time: 0.5 min Purge on (Split) Vent Flow: 60 mL/min Injection Volume: 1 μL Injection Temperature: 250 °C Autosampler: No Liner Type: 4 mm ID Single Taper Liner Liner Part Number: 092017 Column Part Number: 054751 Full Scan / SIM: Full scan 45-450 Acenaphytlene 2-Chlorophenol Decylamine Undecanol 4 mm ID liner with quartz wool in center of liner (incorrectly positioned) SGE FocusLiner ™ (quartz wool correctly positioned) Promoting uniform sample vaporization Maximizing sample vaporization on an inert surface Acting as a particulate filter for dirty samples Improving injection reproducibility 10-fold Wiping needle tip during injection through fixed quartz wool Liner deactivated at high temperatures with wool in situ using SGE’s high quality deactivation processes FocusLiner™ improves reproducibility by: Forensic 36For further information on our full range of products, please visit www.sge.com
  • 40. SGE Capillary Column Part Number Listing Phase Length (m) ID (mm) Film Thickness (µm) Part No. BP1 10 0.1 0.1 054022 BP1 12 0.15 0.25 054028 BP1 25 0.15 0.25 054029 BP1 12 0.22 0.1 054040 BP1 12 0.22 0.25 054046 BP1 12 0.22 1 054052 BP1 15 0.22 0.25 054049 BP1 25 0.22 0.1 054041 BP1 25 0.22 0.25 054047 BP1 25 0.22 1 054053 BP1 30 0.22 0.25 054050 BP1 50 0.22 0.1 054042 BP1 50 0.22 0.25 054048 BP1 50 0.22 1 054054 BP1 60 0.22 0.25 054051 BP1 15 0.25 0.1 054039 BP1 15 0.25 0.25 054043 BP1 30 0.25 0.25 054044 BP1 30 0.25 0.5 054820 BP1 30 0.25 1 054056 BP1 60 0.25 0.25 054045 BP1 60 0.25 0.5 054812 BP1 60 0.25 1 054815 BP1 12 0.32 0.25 054058 BP1 12 0.32 0.5 054064 BP1 12 0.32 1 054070 BP1 15 0.32 0.25 054061 BP1 25 0.32 0.25 054059 BP1 25 0.32 0.5 054065 BP1 25 0.32 1 054071 BP1 25 0.32 4 054076 BP1 25 0.32 5 054081 BP1 30 0.32 0.25 054062 BP1 30 0.32 0.5 054068 BP1 30 0.32 1 054813 BP1 30 0.32 1.5 054811 BP1 30 0.32 3 054073 BP1 30 0.32 4 054077 BP1 50 0.32 0.25 054060 BP1 50 0.32 0.5 054066 BP1 50 0.32 1 054072 BP1 50 0.32 5 054082 BP1 60 0.32 0.25 054067 BP1 60 0.32 0.5 054069 BP1 60 0.32 1 054810 BP1 60 0.32 5 054085 BP1 12 0.53 1 054086 BP1 12 0.53 3 054097 BP1 15 0.53 0.5 054870 BP1 15 0.53 1 054089 BP1 25 0.53 1 054087 BP1 25 0.53 3 054098 BP1 25 0.53 5 054095 BP1 30 0.53 0.5 054092 BP1 30 0.53 1 054090 BP1 30 0.53 2.6 054819 BP1 30 0.53 3 054808 BP1 30 0.53 5 054806 BP1 50 0.53 1 054088 BP1 50 0.53 5 054096 BP1 60 0.53 0.5 054871 BP1 60 0.53 3 054809 BP1 60 0.53 5 054807 BP1-PONA 50 0.15 0.5 054950 BP1-PONA 100 0.25 0.5 054818 BPX1 10 0.1 0.1 054777 BPX1 6 0.53 2.65 0548025 BPX1 10 0.53 0.1 054803 BPX1 10 0.53 0.9 054801 BPX1 10 0.53 2.65 054802 BPX1 Aluminum Clad 5 0.53 0.1 054800 BPX1 Aluminum Clad 5 0.53 0.17 054782 BPX1 Aluminum Clad 10 0.53 0.1 054779 BPX1 10 0.53 2.65 054802 BPX1 Aluminum Clad 5 0.53 0.1 054800 BPX1 Aluminum Clad 5 0.53 0.17 054782 BPX1 Aluminum Clad 10 0.53 0.1 054779 SolGel-1ms 30 0.25 0.25 054795 Phase Length (m) ID (mm) Film Thickness (µm) Part No. SolGel-1ms 60 0.25 0.25 054793 SolGel-1ms 30 0.32 0.25 054798 SolGel-1ms 60 0.32 0.25 054794 BP5 12 0.22 0.25 054167 BP5 25 0.22 0.25 054168 BP5 30 0.22 0.25 054171 BP5 50 0.22 0.25 054169 BP5 50 0.22 1 054175 BP5 15 0.25 0.25 054182 BP5 30 0.25 0.25 054183 BP5 30 0.25 1 054203 BP5 60 0.25 0.25 054184 BP5 60 0.25 1 054215 BP5 12 0.32 0.25 054179 BP5 15 0.32 0.25 054176 BP5 25 0.32 0.25 054180 BP5 25 0.32 0.5 054186 BP5 25 0.32 1 054192 BP5 30 0.32 0.25 054177 BP5 30 0.32 0.5 054216 BP5 30 0.32 1 054189 BP5 50 0.32 0.5 054187 BP5 50 0.32 1 054193 BP5 60 0.32 0.25 054178 BP5 60 0.32 1 054188 BP5 12 0.53 1 054197 BP5 15 0.53 1 054194 BP5 15 0.53 1.5 054199 BP5 25 0.53 1 054198 BP5 30 0.53 0.5 0541935 BP5 30 0.53 1 054195 BP5 30 0.53 5 054196 BP5 60 0.53 1.5 054204 BPX5 10 0.1 0.1 054099 BPX5 10 0.15 1.2 054106 BPX5 12 0.15 0.25 054103 BPX5 12 0.15 0.4 054107 BPX5 25 0.15 0.25 054104 BPX5 25 0.15 0.4 054108 BPX5 30 0.15 0.15 054110 BPX5 50 0.15 0.25 054105 BPX5 40 0.18 0.18 054229 BPX5 12 0.22 0.25 054112 BPX5 25 0.22 0.25 054113 BPX5 25 0.22 1 054116 BPX5 30 0.22 0.25 054142 BPX5 50 0.22 0.25 054114 BPX5 50 0.22 1 054117 BPX5 7 0.25 0.25 054149 BPX5 15 0.25 0.1 0542170 BPX5 15 0.25 0.25 054100 BPX5 15 0.25 1 054121 BPX5 30 0.25 0.1 0541011 BPX5 30 0.25 0.25 054101 BPX5 30 0.25 0.5 0541025 BPX5 30 0.25 1 054122 BPX5 60 0.25 0.25 054102 BPX5 60 0.25 1 054123 BPX5 6 0.32 1 0541261 BPX5 12 0.32 0.25 054118 BPX5 12 0.32 0.5 054124 BPX5 12 0.32 1 054127 BPX5 15 0.32 0.25 054144 BPX5 15 0.32 1 054152 BPX5 25 0.32 0.25 054119 BPX5 25 0.32 0.5 054125 BPX5 25 0.32 1 054128 BPX5 25 0.32 3 054136 BPX5 30 0.32 0.25 054145 BPX5 30 0.32 0.5 0541205 BPX5 30 0.32 1 054153 BPX5 50 0.32 0.25 054120 BPX5 50 0.32 0.5 054126 BPX5 50 0.32 1 054129 BPX5 60 0.32 0.25 054146 BPX5 60 0.32 1 054154 BPX5 12 0.53 0.25 054133 BPX5 12 0.53 1 054130 37 For further information on our full range of products, please visit www.sge.com
  • 41. SGE Capillary Column Part Number Listing Phase Length (m) ID (mm) Film Thickness (µm) Part No. BPX5 12 0.53 3 054138 BPX5 15 0.53 0.5 0541344 BPX5 15 0.53 1 054147 BPX5 15 0.53 1.5 0541347 BPX5 15 0.53 3 054159 BPX5 25 0.53 0.25 054134 BPX5 25 0.53 1 054131 BPX5 25 0.53 3 054139 BPX5 30 0.53 0.5 0541345 BPX5 30 0.53 1 054148 BPX5 30 0.53 1.5 0541348 BPX5 30 0.53 3 054160 BPX5 50 0.53 1 054132 BPX5 60 0.53 1 054158 HT5 12 0.22 0.1 054631 HT5 25 0.22 0.1 054632 HT5 15 0.25 0.1 054633 HT5 30 0.25 0.1 054634 HT5 12 0.32 0.1 054641 HT5 15 0.32 0.5 054667 HT5 25 0.32 0.1 054642 HT5 30 0.32 0.5 054668 HT5 6 0.53 0.1 054655 HT5 10 0.53 0.5 054670 HT5 12 0.53 0.15 054657 HT5 15 0.53 0.5 054671 HT5 25 0.53 0.15 054658 HT5 30 0.53 0.5 054672 HT5 Aluminum Clad 12 0.22 0.1 054635 HT5 Aluminum Clad 25 0.22 0.1 054636 HT5 Aluminum Clad 12 0.32 0.1 054651 HT5 Aluminum Clad 25 0.32 0.1 054652 HT5 Aluminum Clad 50 0.32 0.1 054653 HT5 Aluminum Clad 5 0.53 0.075 054673 HT5 Aluminum Clad 6 0.53 0.1 054661 HT5 Aluminum Clad 12 0.53 0.15 054662 HT5 Aluminum Clad 25 0.53 0.15 054665 HT8 10 0.1 0.1 054690 HT8 40 0.18 Proprietary 054686 HT8 12 0.22 0.25 054674 HT8 25 0.22 0.25 054675 HT8 50 0.22 0.25 054676 HT8 30 0.25 0.25 054677 HT8 60 0.25 0.25 054683 HT8 12 0.32 0.25 054679 HT8 25 0.32 0.25 054680 HT8 50 0.32 0.25 054681 HT8 60 0.32 0.25 054682 HT8 12 0.53 0.5 054684 HT8 25 0.53 0.5 054685 BPX35 10 0.1 0.1 054699 BPX35 15 0.22 0.25 054713 BPX35 25 0.22 0.25 054711 BPX35 30 0.22 0.25 054714 BPX35 50 0.22 0.25 054712 BPX35 15 0.25 0.25 054700 BPX35 15 0.25 1 054703 BPX35 30 0.25 0.25 054701 BPX35 30 0.25 0.5 0547025 BPX35 30 0.25 1 054704 BPX35 60 0.25 0.25 054702 BPX35 60 0.25 1 054705 BPX35 15 0.32 0.25 054723 BPX35 15 0.32 0.5 054718 BPX35 15 0.32 1 054716 BPX35 25 0.32 0.25 054721 BPX35 30 0.32 0.25 054724 BPX35 30 0.32 0.5 0547158 BPX35 30 0.32 1 054717 BPX35 50 0.32 0.25 054722 BPX35 60 0.32 0.25 054725 BPX35 15 0.53 0.5 054734 BPX35 15 0.53 1 054736 BPX35 30 0.53 0.5 054735 BPX35 30 0.53 1 054737 BPX608 25 0.32 0.4 054823 BP624 25 0.22 1.2 054826 BP624 30 0.22 1.2 054827 Phase Length (m) ID (mm) Film Thickness (µm) Part No. BP624 15 0.25 1.4 054839 BP624 30 0.25 1.4 054840 BP624 60 0.25 1.4 054842 BP624 25 0.32 1.8 054830 BP624 30 0.32 1.8 054832 BP624 50 0.32 1.8 054831 BP624 60 0.32 1.8 054841 BP624 25 0.53 3 054834 BP624 30 0.53 3 054836 BP624 50 0.53 3 054835 BP624 60 0.53 3 054838 BPX-Volatiles 20 0.18 1 054978 BPX-Volatiles 40 0.18 1 054979 BPX-Volatiles 30 0.25 1.4 054980 BPX-Volatiles 60 0.25 1.4 054981 BPX-Volatiles 30 0.32 1.8 054982 BPX-Volatiles 60 0.32 1.8 054983 BPX-Volatiles 30 0.53 3 054984 BPX-Volatiles 60 0.53 3 054985 BP10 12 0.22 0.25 054252 BP10 25 0.22 0.25 054253 BP10 50 0.22 0.25 054254 BP10 15 0.25 0.25 054255 BP10 30 0.25 0.25 054256 BP10 30 0.25 1 054271 BP10 60 0.25 0.25 054257 BP10 15 0.32 0.25 054258 BP10 15 0.32 0.5 054264 BP10 25 0.32 0.25 054262 BP10 25 0.32 0.5 054268 BP10 30 0.32 0.25 054259 BP10 30 0.32 0.5 054265 BP10 30 0.32 1 054270 BP10 50 0.32 0.5 054269 BP10 60 0.32 0.25 054260 BP10 60 0.32 0.5 054266 BP10 15 0.53 1 054282 BP10 25 0.53 1 054280 BP10 30 0.53 1 054283 BPX50 10 0.1 0.05 054739 BPX50 10 0.1 0.07 054738 BPX50 10 0.1 0.1 054740 BPX50 30 0.15 0.15 054741 BPX50 15 0.25 0.25 054750 BPX50 30 0.25 0.25 054751 BPX50 60 0.25 0.25 054752 BPX50 15 0.32 0.25 054760 BPX50 30 0.32 0.25 054761 BPX50 60 0.32 0.25 054762 BPX50 15 0.53 0.5 054770 BPX50 30 0.53 0.5 054771 BPX50 30 0.53 1 054772 BP225 25 0.22 0.25 054352 BP225 50 0.22 0.25 054353 BP225 25 0.32 0.25 054358 BP225 25 0.53 0.5 054364 BP20 10 0.1 0.1 054405 BP20 12 0.22 0.25 054420 BP20 25 0.22 0.25 054421 BP20 30 0.22 0.25 054424 BP20 50 0.22 0.25 054422 BP20 60 0.22 0.25 054425 BP20 15 0.25 0.25 054426 BP20 30 0.25 0.25 054427 BP20 30 0.25 0.5 054415 BP20 30 0.25 1 054439 BP20 60 0.25 0.25 054428 BP20 60 0.25 0.5 054458 BP20 15 0.32 0.25 054432 BP20 25 0.32 0.25 054430 BP20 25 0.32 0.5 054436 BP20 25 0.32 1 054442 BP20 30 0.32 0.25 054433 BP20 30 0.32 0.5 054438 BP20 30 0.32 1 054444 BP20 50 0.32 0.25 054431 BP20 50 0.32 0.5 054437 BP20 50 0.32 1 054443 38For further information on our full range of products, please visit www.sge.com
  • 42. SGE Capillary Column Part Number Listing Phase Length (m) ID (mm) Film Thickness (µm) Part No. BP21 30 0.53 0.5 054477 BP21 30 0.53 1 054478 BPX70 10 0.1 0.2 054600 BPX70 12 0.22 0.25 054601 BPX70 25 0.22 0.25 054602 BPX70 30 0.22 0.25 054612 BPX70 50 0.22 0.25 054603 BPX70 60 0.22 0.25 054613 BPX70 15 0.25 0.25 054621 BPX70 30 0.25 0.25 054622 BPX70 60 0.25 0.25 054623 BPX70 120 0.25 0.25 054624 BPX70 12 0.32 0.25 054605 BPX70 25 0.32 0.25 054606 BP21 50 0.32 0.25 054469 BP21 60 0.32 0.25 054472 BP21 12 0.53 0.5 054473 BP21 15 0.53 0.5 054476 BP21 25 0.53 0.5 054474 BP21 30 0.53 0.5 054477 BP21 30 0.53 1 054478 BPX70 10 0.1 0.2 054600 BPX70 12 0.22 0.25 054601 BPX70 25 0.22 0.25 054602 BPX70 30 0.22 0.25 054612 BPX70 50 0.22 0.25 054603 BPX70 60 0.22 0.25 054613 BPX70 15 0.25 0.25 054621 BPX70 30 0.25 0.25 054622 BPX70 60 0.25 0.25 054623 BPX70 120 0.25 0.25 054624 BPX70 12 0.32 0.25 054605 BPX70 25 0.32 0.25 054606 BPX90 15 0.25 0.25 054570 BPX90 15 0.32 0.50 054573 BPX90 30 0.25 0.25 054580 BPX90 60 0.25 0.25 054590 BPX90 60 0.32 0.50 05493 BPX90 30 0.25 0.25 054980 Phase Length (m) ID (mm) Film Thickness (µm) Part No. BP20 60 0.32 0.25 054434 BP20 60 0.32 0.5 054457 BP20 60 0.32 1 054445 BP20 12 0.53 1 054447 BP20 12 0.53 2 054455 BP20 15 0.53 0.5 054961 BP20 15 0.53 1 054450 BP20 25 0.53 1 054448 BP20 25 0.53 2 054456 BP20 30 0.53 0.5 054440 BP20 30 0.53 1 054451 BP20 60 0.53 0.5 054963 BP20 60 0.53 1 0544515 SolGel-WAX™ 30 0.25 0.25 054796 SolGel-WAX™ 30 0.25 1 054787 SolGel-WAX™ 60 0.25 0.25 054791 SolGel-WAX™ 30 0.32 0.25 054788 SolGel-WAX™ 30 0.32 0.5 054797 SolGel-WAX™ 60 0.32 0.25 054789 SolGel-WAX™ 60 0.32 0.5 054792 SolGel-WAX™ 30 0.53 0.5 054786 SolGel-WAX™ 30 0.53 1 054785 BP21 25 0.22 0.25 054462 BP21 50 0.22 0.25 054463 BP21 15 0.25 0.25 054464 BP21 30 0.25 0.25 054465 BP21 60 0.25 0.25 054466 BP21 12 0.32 0.25 054467 BP21 15 0.32 0.25 054470 BP21 25 0.32 0.25 054468 BP21 30 0.32 0.25 054471 BP21 50 0.32 0.25 054469 BP21 60 0.32 0.25 054472 BP21 12 0.53 0.5 054473 BP21 15 0.53 0.5 054476 BP21 25 0.53 0.5 054474 BP21 30 0.53 0.5 054477 BP21 30 0.53 1 054478 BP21 25 0.53 0.5 054474 Column to Replace Description SGE Phase DB-1, HP-1, Ultra-1, SPB-1, CP-Sil 5CB, RSL-150, RSL-160, Rtx®-1, ZB-1, CB-1, OV®-1, PE-1, 007-1(MS), SP-2100, SE-30, RH-1, CC-1, CP-Sil 5CB MS, VF-1ms, Petrocol DH 100% Dimethyl Polysiloxane BP1 Unique highly inert phase SolGel + 100% Dimethyl Polysiloxane SolGel-1ms™ DB-HT Sim Dis, DB-2887, Rtx-2887, HP-1, Petrocol 2887, Petrocol EX2887 100% Dimethyl Polysiloxane BPX1 Petrocol DH, DB-Petro 100% Dimethyl Polysiloxane BP1-PONA DB-5, DB-5.625, Rtx-5, HP-5, Ultra-2, PTE-5, PB-5, MDN-5, CP-Sil 8CB, VB-5 ZB-5 5% Phenyl Polysiloxane BP5 DB-5, DB-5ms, HP-5, Ultra-2, Rtx®-5, Rtx-5Sil MS, Rtx 5MS, AT-5, AT-5MS, 007-5MS, SPB-5,CP-Sil 8CB, VF-5ms, RSL-200, CB-5, OV®-5, PE-5, 007-2(MPS-5), SE-52, SE-54, XTI-5, PTE-5, CC-5, RH-5ms, ZB-5 5% Phenyl Polysilphenylene-siloxane BPX5 MXT-1 SimDist, HT-SimDist, DistCB, MXT-500 5% Phenyl Polycarborane-siloxane HT5 No equivalent, unique high temperature column with special selectivity 8% Phenyl Polycarborane-siloxane HT8 DB-35, DB-35ms, Rtx-35, HP-35, HP-35MS, SPB-35, MDN-35, VB-50, ZB-35 35% Phenyl Polysilphenylene-siloxane BPX35 DB-608, Rtx-35, SPB-608 35% Phenyl Polysilphenylene-siloxane BPX608 OV-17, SP-2250, DB-17ms, DB-17ht, Rtx-50, SPB-50, HP-50+, HP-17, VB-50/608, ZB-50 50% Phenyl Polysilphenylene-siloxane BPX50 DB-23, CP-Sil 88, VF-23ms, SP-2330, SP-2380, Rtx®-2330, 007-23, AT-Silar, PE-23 70% Cyanopropyl Polysilphenylene-siloxane BPX70 Unique highly inert phase SolGel + Polyethylene Glycol SolGel-WAX™ DB-Wax, Rtx-Wax, Stabilwax, HP20M, HP-Wax, HP-INNOWax, Supelcowax-10, AT-Wax, Nukol, CP Wax 2CB, VB-WAX, ZB-WAX Polyethylene Glycol BP20 (Wax) DB-FFAP, HP-FFAP, Stabilwax-DA, CP Wax 58CB, VB-FFAP, ZB-FFAP Polyethylene Glycol (TPA treated) BP21 (FFAP) DB-1701, Rtx-1701, HP-1701, SPB-7, CP-Sil 19CB, VB-1701, ZB-1701 14% Cyanopropylphenyl Polysiloxane BP10 (1701) HP-225, DB-225, Rtx-225 50% Cyanopropylphenyl Polysiloxane BP225 DB-624, HP-VOC, Rtx Volatiles, VOCOL, VB-624, ZB-624 Cyanopropylphenyl Polysiloxane BP624, BPX-Volatiles Cyclodex-B, Rt-BDEXm Permethylated Beta Cyclodextrin CYDEX-B Unique highly polar phase 90% Cynopropyl Polysilphenylene-siloxane BPX90 GC Column Replacement Guide 39 For further information on our full range of products, please visit www.sge.com
  • 43. GC Troubleshooting and Maintenance Symptom Possible cause Solution High baseline level Septum bleed and/or contaminated liner Replace septa and insert a new inlet liner. Poor carrier gas quality causing phase decomposition Ensure gas traps are installed correctly to remove moisture, organics and oxygen. Ensure high purity carrier gas is used. Maximum temperature of the phase has been exceeded Lower maximum program temperature. Highly acid or alkaline samples Neutralize sample before injecting Dirty samples Filter sample. Use a FocusLiner™. Dilute sample. Contaminated solvent Use a high purity solvent. Split peaks Poor manual injection technique Increase the plunger depression speed. Mixed solvent Change to a single solvent Compound degradation Can happen with some pesticides. Lower injector temperature. Recondition capillary column and re-inject sample. Column inserted too far into injector Reposition column according to manufacturer’s instructions. Fronting peaks Too much sample injected on to column Dilute sample. Use a thicker film. Increase the split ratio. Tailing peaks Column contamination Cut 50cm off the front of the column and re-install in the injector. Recondition column. Sample not suitable for phase polarity Choose a more polar column. Poorly deactivated inlet liner Replace with a new fully deactivated inlet liner. Graphite ferrule contamination in the start of the column Cut 5cm off the front of the column and re-install in the injector Broad peaks Make-up gas flow rate for atmospheric detectors is low Increase make up gas flow according to manufacturer’s instructions. Carrier gas flow is low Check carrier gas flow. Split gas flow is too low Increase split flow or use the ‘solvent effect’ to focus peaks. Column contamination Cut 50cm off the front of the column and re-install in the injector. Co-elution of peaks Change column polarity or lower temp. program ramp rate to separate peaks. Change in sample concentration Check injector conditions are reproducible e.g. temperature and split ratio. Mass spectrometer sampling rate is too low causing Increase sampling rate or reduce number of ions detected in SIM mode. triangular-looking peaks Shifting Leaking septum Tighten septum cap or replace with new septum. retention times Carrier gas velocity has changed Verify carrier gas flow rate. Check inlet pressure on GC. Ensure pressure in gas line and gas cylinder is OK Method temperature has changed Re-check temperature method conditions Column dimensions and film thickness have changed after Re-check dimensions on column tag against column description. installing a new column Sample concentration has changed – more has been Dilute sample or increase split ratio. injected on column Dirty column. Extra non-volatile material deposited on Cut 50cm off the front of the column and re-install in the injector the column has caused a change in column polarity Recondition column. Loss of Aging column has resulted in a substantial loss of phase Replace column. peak resolution causing a loss in column resolving power Method temperature has changed Re-check temperature method conditions Carrier gas velocity has changed Re-check carrier gas velocity and optimize to Van Deemter optima. Dirty column. Extra non-volatile material deposited on Cut 50cm off the front of the column and re-install in the injector. the column has caused a change in column polarity Manual injection technique or operator has changed Ensure technique is consistent. No peaks GC incorrectly wired Check all connections from GC to computer / integrator. Wrong detector is being monitored Check injector number is consistent with detector number being monitored. FID flame is out If using water, reduce injection volume. Water can extinguish the flame. Check flame gas pressures Syringe is blocked or leaking around plunger Use a known good syringe to confirm this is the problem. Massive leak in system Check all column and injector connections. Check column for breakage. This can sometimes be difficult to locate as the fused silica can break leaving the polyimide outer coating intact. Column is blocked Cut 5cm off the front and back ends of the column and re-install. Loss of sensitivity Concentration of sample has changed Re-confirm with a known standard concentration injection. Flame gas flow rates and/or make-up gas flow have changed Check flame gas pressures System has become active Replace inlet liner with a new deactivated liner. Cut 50cm off the front of the column, re-install in the injector and re-condition the column Splitless conditions have changed Re-check solvent and method temperatures. Ghost peaks Syringe has become contaminated from previous sample Ensure syringe has been thoroughly washed with solvent between injections. Sometimes this can involve 20 solvent rinses. New standards have impurities Confirm by using a different source of primary standards. Impurities in solvent Use a different type of solvent or confirm by using a different source of the same solvent. Septum bleed Can appear as discrete peaks in temperature program runs. Will disappear with isothermal analysis. Replace septum. Could also be from sample vial septa Peaks are still eluting from previous run Peaks will appear broader for that part of the chromatogram. Confirm by extending run time and ensuring all peaks have eluted from sample. Flashback has happened Inject twice the amount of pure solvent (this may need to be repeated). Carrier gas lines may also need to be cleaned 40For further information on our full range of products, please visit www.sge.com
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