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Chromatograms

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Chromatograms GC Chromatograms

LC Chromatograms

GC Chromatograms by Column Phase..........571–572 Clinical .........................................................................573–582

LC Chromatograms by Column Phase ....................691 Biotechnology..........................................................692–693

Amphetamines, Barbiturates, Basic Drugs, Benzodiazepines, Cannabinoids, Cocaine, Cold Medications, Opiates, Phenothiazines, Sympathomimetic Amines

Environmental .........................................................583–625 Air, Brominated Flame Retardants, Dioxins/Furans, Explosives, Gasoline Range Organics (GRO), Glycols, Haloacetic Acids, Herbicides, PCB Mixtures, Pesticides, Semivolatiles, Volatiles

Food Safety ...............................................................626–631 Food Contaminants, Packaging Volatiles, PAHs

Foods, Flavors, & Fragrances .............................632–647 Cholesterols, Dietary Supplements, Essential Oils, FAMEs, Fatty Acids, Flavors, Food Testing, Fragrances, Preservatives

Forensics ....................................................................648–653 Arson Accelerants, Blood Alcohols, GHB/GBL, Glycols, Inhalants

Amino Acids, Oxytocin, Peptides, Proteins

Clinical .........................................................................694–699 Benzodiazepines, Cannabinoids, Drugs of Abuse, Drug Monitoring, Steroids

Environmental .........................................................700–707 Aldehydes, Explosives, Herbicides, Ketones, Pesticides, Polycyclic Aromatic Hydrocarbons (PAHs)

Food Quality .............................................................708–710 Dietary Supplements, Flavor Compounds, Preservatives, Vitamins

Food Safety ...............................................................711–717 Drug Residues, Food Contaminants

Pharmaceutical........................................................718–721 Chemistry, Manufacturing & Control (CMC) Compounds

Petroleum & Petrochemical ...............................654–679 Fuels, Hydrocarbon Gases, Hydrocarbons, Hydrocarbons (High-Temperature), Hydrocarbons (Simulated Distillation), Permanent Gases, Sulfur Compounds

Pharmaceutical........................................................680–684 Organic Volatile Impurities/Residual Solvents

Solvents & Chemicals............................................685–689 Aldehydes, Amines, Ketones, Solvents

Compound Index GC .................................................................................722–726 LC ..................................................................................728–729


GC Chromatograms GC Chromatograms by Column Phase..........571–572 Clinical .........................................................................573–582 Amphetamines.................................................................................. 573 Barbiturates ..............................................................................573–574 Basic Drugs................................................................................575–576 Benzodiazepines ......................................................................576–577 Cannabinoids .................................................................................... 577 Cocaine ............................................................................................... 578 Cold Medications.....................................................................578–579 Opiates ................................................................................................ 579 Phenothiazines ................................................................................. 580 Sympathomimetic Amines ..................................................580–582

Environmental .........................................................583–625 Air ................................................................................................583–585 Brominated Flame Retardants ...................................586, 603–604 Dioxins/Furans .........................................................................587–589 Explosives ........................................................................................... 590 Gasoline Range Organics (GRO)................................................... 591 Glycols ........................................................................................592–593 Haloacetic Acids ............................................................................... 594 Herbicides .................................................................................. 595, 610 PAHs ..................................................................................................... 596 PCB Mixtures .............................................................................596–604 Pesticides ...................................................................................605–611 Semivolatiles.............................................................................612–619 Volatiles......................................................................................620–625

Food Safety ...............................................................626–631 Food Contaminants................................................................626–628 Packaging Volatiles ................................................................629–630 PAHs .................................................................................................... 631

Foods, Flavors, & Fragrances .............................632–647 Cholesterols........................................................................................ 632 Dietary Supplements ....................................................................... 633 Essential Oils .............................................................................634–635 FAMEs .........................................................................................636–640 Fatty Acids .......................................................................................... 641 Flavors ........................................................................................642–644 Food Testing ...................................................................................... 645 Fragrances.................................................................................645–646 Preservatives ..................................................................................... 647

Forensics ....................................................................648–653 Arson Accelerants ....................................................................648–649 Blood Alcohols................................................................................... 650 GHB/GBL ............................................................................................. 651 Glycols ................................................................................................. 652 Inhalants............................................................................................. 653

Petroleum & Petrochemical ...............................654–679 Fuels ............................................................................................654–656 Hydrocarbon Gases ................................................................657–665 Hydrocarbons ...........................................................................666–670 Hydrocarbons (High-Temperature) ....................................671–674 Hydrocarbons (Simulated Distillation) ..............................675–676 Permanent Gases ....................................................................677–679 Sulfur Compounds ........................................................................... 679

Pharmaceutical........................................................680–684 Organic Volatile Impurities/Residual Solvents ................680–684

Solvents & Chemicals............................................685–689 Aldehydes ........................................................................................... 685 Amines........................................................................................685–687 Ketones................................................................................................ 687 Solvents ......................................................................................688–689

Compound Index ...................................................722–726


GC CHROMATOGRAMS

GC Chromatograms by Column Phase GC Chromatograms by Column Phase

FUSED SILICA FAMEWAX

Rtx®-5/MXT®-5

Rxi®-17

FAMEs .............................................................. 638, 640

fragrance allergens ...............................................646

simulated distillation ...........................................675

essential oils ............................................................634 pharmaceuticals (basic) ...................575, 580, 582 sympathomimetic amines .................................582

MXT®-1HT Sim Dist

Rtx®-5MS

MXT®-1 Sim Dist

hydrocarbons (high temp.) ......................666–667

MXT®-Biodiesel TG biodiesel .........................................................654–655

Rt®-2330 FAMEs ........................................................................639

Rt®-2560 FAMEs .................................................... 636–637, 640

Rt®-TCEP aromatics ..................................................................670

food contaminants ...............................................626 volatiles (food packaging)........................629–630

Rtx®-624 semivolatiles ...........................................................616

Rtx®-65TG food testing .............................................................645

Rtx®-BAC Plus 1/Rtx®-BAC Plus 2 blood alcohol ..........................................................650 GHB, GBL...................................................................651 glycols........................................................................652 inhalants ...................................................................653

Rxi®-17Sil MS brominated flame retardants ..................603–604 PAHs ....................................................... 614–615, 626 PCBs..................................................................603–604

Rxi®-5HT C10–C40 alkanes ...................................................671 crude oil .......................................................... 671, 674 diesel ..........................................................................671 gasoline.....................................................................671 kerosene ...................................................................671

Rxi®-5ms cholesterols .............................................................632

Rxi®-5Sil MS

Rtx®-1614

haloacetic acids......................................................594 herbicides.................................................................595 organochlorine pesticides .......................605–608 PCBs..................................................................598–599 pesticides & herbicides .............................609–610

amphetamines .......................................................573 benzodiazepines ...................................................577 cannabinoids ..........................................................577 cocaine & metabolites .........................................578 dietary supplements ............................................633 dioxins & furans............................................588–589 food contaminants .....................................627–628 opiates, extracted from blood ..........................579 polycyclic aromatic hydrocarbons ..................613 semivolatile organics .................................617–619

brominated flame retardants ............................586

Rtx®-DHA-100

Rxi®-624Sil MS

Rtx®-1701

hydrocarbons (detailed gasoline analysis)...................668–669

residual solvents ..........................................680–682 semivolatiles ................................................. 612, 616 TO-15 VOCs ..............................................................583 volatile organics .....................................................622

Rtx®-1/MXT®-1 essential oils ............................................................635 flavor volatiles.........................................................642 hydrocarbons ..........................................................666 hydrocarbons (gases)...........................................657 sulfur compounds .................................................679

Rtx®-1301 flavor volatiles.........................................................643

barbiturates .............................................................574 fragrances.................................................................645

Rtx®-Biodiesel TG biodiesel ...................................................................654

Rtx®-CLPesticides/Rtx®-CLPesticides2

Rtx®-Dioxin2

antioxidants.............................................................647

dioxins .......................................................................587 furans .........................................................................587

Rtx®-200

Rtx®-Mineral Oil

PAHs ...........................................................................631

benzodiazepines ...................................................576 dietary supplements ............................................633 explosives .................................................................590 fatty acids (free) .....................................................641 food contaminants .....................................627–628 glycols........................................................................592 pharmaceuticals (basic) .................. 575–576, 581 sympathomimetic amines .................................581

C10–C40 alkanes ...................................................673 diesel ................................................................672–673 mineral oil ................................................................672 motor oil .........................................................672–673

Rxi®-XLB

Rtx®-OPPesticides/ Rtx®-OPPesticides2

Stabilwax®

Rtx®-20

Rtx®-2887 simulated distillation ...........................................675

Rtx®-35 barbiturates ...................................................573–574 pharmaceuticals (acidic, neutral)...........573–574 pharmaceuticals (basic) ......................................576

volatiles ...........................................................623–625

Rtx®-Volatile Amines

Stabilwax®-DA

Rtx®-PCB PCBs..................................................................600–602

Rtx®-VMS

amines .......................................................................686

Rtx®-WAX/MXT®-WAX

amines .......................................................................686 cold medications ...................................................579 pharmaceuticals (basic) ............................579–580 sympathomimetic amines .................................580

FAMEs .............................................................. 637, 639 glycols........................................................................592

amines .......................................................................685 cold medications ...................................................578 pharmaceuticals (basic) ............................ 578, 581 sympathomimetic amines .................................581

brominated flame retardants ..................603–604 PAHs ...........................................................................596 PCBs...............................................596–597, 603–604 acrylamide ...............................................................628 essential oils ..................................................634–635 FAMEs .............................................................. 639, 656 flavor volatiles.........................................................642 food contaminants ...............................................628 glycols........................................................................593 residual solvents ..........................................680–682

organophosphorus pesticides..........................611

Rtx®-35 Amine

Rtx®-5 Amine

Rxi®-PAH

fatty acids (free) .....................................................641 flavor volatiles.........................................................644

Rxi®-1ms diesel, motor oil ........................................... 591, 649 food contaminants ...............................................626 fragrance allergens ...............................................646 hydrocarbons (accelerants) .....................648–649 Mass APH ..................................................................585 petroleum hydrocarbons ...................................591 sulfur compounds .................................................679 TO-15 VOCs ..............................................................584

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GC CHROMATOGRAMS

GC Chromatograms by Column Phase, EPA Methods Chart GC Chromatograms by Column Phase, cont'd

PACKED D3606 Application Column hydrocarbons ..........................................................670

Molesieve 13X permanent gases ...................................................677

Molesieve 5A permanent gases ...................................................677

Refinery Gas Column Set hydrocarbon gases ...............................................664

Rtx®-1 SimDist 2887 simulated distillation ...........................................676

PACKED/MICROPACKED

EPA Methods Chart Method # 504.1 505 508.1 521 522 524.2 552.2 8081B 8141A 8260 8270 8270 (Appendix IX) TO-15

Method Title .............................................................Page # 1,2-Dibromoethane & 1,2-Dibromo-3-Chloropropane ..... 605 Organohalide Pesticides & PCBs ............................................... 609 Chlorinated Pesticides .................................................................. 610 Nitrosamines..................................................................................... 612 1,4-Dioxane ....................................................................................... 616 Volatile Organics ............................................................................. 625 Haloacetic Acids .............................................................................. 594 Chlorinated Pesticides ....................................................................... 608 Organophosphorus Pesticides .................................................. 611 Volatile Organics ................................................................... 622–624 Semivolatile Organics ......................................................... 617–618 Semivolatile Organics ................................................................................619 Toxic Organic Compounds in Air .................................... 583–584

Rt®-XLSulfur sulfurs in beverages..............................................643

ShinCarbon ST hydrocarbon gases ..................................... 659, 677 permanent gases ...................................................677

PLOT MXT®-Msieve 5A permanent gases ...................................................679

MXT®-Q-BOND solvents .....................................................................689

Rt®-Alumina BOND/CFC chlorinated fluorocarbons .................................687 hydrocarbon gases ...............................................658

Chromatogram Search Tool Search by compound name, synonym, CAS #, or keyword

Rt®-Alumina BOND/KCl hydrocarbon gases ............................657, 660, 664

Rt®-Alumina BOND/MAPD hydrocarbon gases ........................... 658, 661–662

Rt®-Alumina BOND/Na2SO4 hydrocarbon gases ........................... 659–661, 663 natural gas ...............................................................660

Rt®-Msieve 5A permanent gases ...................................................678

Rt®-Q-BOND solvents .....................................................................689

Rt®-QS-BOND hydrocarbon gases ..................................... 659, 665 ketones......................................................................687 solvents .....................................................................688

Rt®-S-BOND solvents .....................................................................688

Rt®-U-BOND aldehydes .................................................................685

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GC CHROMATOGRAMS | CLINICAL

Amphetamines, Barbiturates Derivatized Amphetamines (500 ng/mL) on Rxi®-5Sil MS Rxi® Technology! 1. 2. 3. 4. 5.

Exceptionally inert, ultra low-bleed capillary columns.

2 1

Excellent peak shape with short run time.

Column

5 3

7.0

8.0

Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623)

Sample Diluent: Conc.: Injection Inj. Vol.: Liner:

4

9.0

Butyl chloride 500 ng/mL HFAA derivatives

Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Transfer Line Temp.: Analyzer Type: Source Temp.: Electron Energy: Solvent Delay Time: Tune Type: Ionization Mode: Scan Range: Scan Rate: Instrument

C

6.0

Peaks Amphetamine Methamphetamine MDA MDMA MDEA c = contaminant

10.0 Time (min) GC_CF1144

1 μL splitless (hold 1 min) 3.5 mm splitless taper w/wool (cat.# 22286-200.1) 250 °C 28 mL/min 75 °C to 300 °C at 15 °C/min He, constant linear velocity 45 cm/sec, 13.5 psi, 93.1 kPa @ 75 °C MS Scan 250 °C Quadrupole 200 °C 70 eV 4 min PFTBA EI 40-300 amu 5 scans/sec Shimadzu 2010 GC & QP2010+ MS

Underivatized Barbiturates (Acidic/Neutral Drugs) on Rtx®-35 Separation optimized using Pro ezGC!

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

Peaks Barbital Aprobarbital Butalbital Amobarbital Talbutal Pentobarbital Methohexital Secobarbital Thiopental Hexobarbital Mephobarbital Phenobarbital

Column Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rtx®-35, 30 m, 0.32 mm ID, 0.50 μm (cat.# 10439) Barbiturates 1.0 μL split (split ratio 30:1) 300 °C 210 °C (hold 2 min) to 300 °C at 7 °C/min (hold 2 min) He, constant pressure 35 cm/sec @ 210 °C FID @ 300 °C FID sensitivity: 5.12 x 10-10 AFS

GC_PH00267

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GC CHROMATOGRAMS | CLINICAL

Barbiturates Underivatized Barbiturates (Acidic/Neutral Drugs) on Rtx®-35

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.

Peaks Ethosuximide Barbital Methyprylon Aprobarbital Butalbital Amobarbital Pentobarbital Secobarbital Meprobamate Carisoprodal Glutethimide Phenobarbital Methaqualone Primidone Carbamazepine Diphenylhydantoin

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rtx®-35, 30 m, 0.53 mm ID, 1.00 μm (cat.# 10455) Acidic/neutral drugs 50 μg/mL 1.0 μL splitless (hold 0.5 min) 250 °C 100 °C to 280 °C at 10 °C/min (hold 5 min) He, constant pressure 40 cm/sec @ 100 °C FID @ 250 °C FID sensitivity: 5.12 x 10-10 AFS

GC_PH00262

Underivatized Barbiturates (Acidic/Neutral Drugs) on Rtx®-1701

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.

Peaks Ethosuximide Barbital Methyprylon Aprobarbital Butalbital Amobarbital Pentobarbital Secobarbital Meprobamate Carisoprodal Glutethimide Phenobarbital Methaqualone Primidone Carbamazepine Diphenylhydantoin

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

GC_PH00263

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Rtx®-1701, 15 m, 0.53 mm ID, 0.50 μm (cat.# 12037) Acidic/neutral drugs 50 μg/mL 1.0 μL splitless (hold 0.5 min) 250 °C 100 °C to 280 °C at 7 °C/min He, constant pressure 40 cm/sec @ 100 °C FID @ 275 °C FID sensitivity: 5.12 x 10-10 AFS


GC CHROMATOGRAMS | CLINICAL

Basic Drugs Underivatized Mixed Basic Drugs on Rtx®-200 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

Peaks Nicotine Benzocaine Cotinine Meperidine Caffeine Benzphetamine Ketamine Diphenhydramine Lidocaine Phenyltoloxamine Tripelennamine Phenothiazine Dextromethorphan Methadone Amitriptyline Trimipramine Tetracaine Pyrilamine Medazepam

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

Bupivacaine Scopolamine Codeine Morphine Diazepam Chlorpromazine Temazepam Flunitrazepam Bromazepam Prazepam Acetopromazine Flurazepam Papaverine Clonazepam Haloperidol Alprazolam Triazolam Thioridazine Trazodone

Rtx®-200, 30 m, 0.25 mm ID, 0.25 μm (cat.# 15023) Basic drug sample 1,000 ng/μL 1.0 μL split (split ratio 50:1) 250 °C 100 °C to 325 °C at 4 °C/min (hold 10 min) He, constant pressure 30 cm/sec @ 100 °C FID @ 320 °C FID sensitivity: 1.28 x 10-10 AFS

GC_PH00237

Underivatized Mixed Basic Drugs on Rtx®-5 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

GC_PH00235

Peaks Nicotine Benzocaine Cotinine Meperidine Caffeine Benzphetamine Ketamine Diphenhydramine Lidocaine Phenyltoloxamine Tripelennamine Phenothiazine Dextromethorphan Methadone Amitriptyline Trimipramine Tetracaine Pyrilamine Medazepam

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

Bupivacaine Scopolamine Codeine Morphine Diazepam Chlorpromazine Temazepam Flunitrazepam Bromazepam Prazepam Acetopromazine Flurazepam Papaverine Clonazepam Haloperidol Alprazolam Triazolam Thioridazine Trazodone

Rtx®-5, 30 m, 0.25 mm ID, 0.25 μm (cat.# 10223) Basic drug sample 1,000 ng/μL 1.0 μL split (split ratio 50:1) 250 °C 100 °C to 325 °C at 4 °C/min (hold 10 min) He, constant pressure 30 cm/sec @ 100 °C FID @ 320 °C FID sensitivity: 1.28 x 10-10 AFS

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GC CHROMATOGRAMS | CLINICAL

Basic Drugs, Benzodiazepines Underivatized Mixed Basic Drugs on Rtx®-35 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

Peaks Nicotine Benzocaine Cotinine Meperidine Caffeine Benzphetamine Ketamine Diphenhydramine Lidocaine Phenyltoloxamine Tripelennamine Phenothiazine Dextromethorphan Methadone Amitriptyline Trimipramine Tetracaine Pyrilamine Medazepam

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

Bupivacaine Scopolamine Codeine Morphine Diazepam Chlorpromazine Temazepam Flunitrazepam Bromazepam Prazepam Acetopromazine Flurazepam Papaverine Clonazepam Haloperidol Alprazolam Triazolam Thioridazine Trazodone

Rtx®-35, 30 m, 0.25 mm ID, 0.25 μm (cat.# 10423) Basic drug sample 1,000 ng/μL 1.0 μL split (split ratio 50:1) 250 °C 100 °C to 325 °C at 4 °C/min (hold 10 min) He, constant pressure 30 cm/sec @ 100 °C FID @ 320 °C FID sensitivity: 1.28 x 10-10 AFS

GC_PH00236

Benzodiazepines (Underivatized) on Rtx®-200 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

Peaks Medazepam Lorazepam Diazepam Desmethyldiazepam Bromazepam Prazepam Temazepam Flurazepam Clobazam Flunitrazepam Clonazepam Alprazolam Triazolam

Looking for more? Visit our online technical library for chromatograms based on ASTM methods, USP procedures, and other applications. www.restek.com/chromatograms

GC_PH00268 Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rtx®-200, 15 m, 0.32 mm ID, 0.25 μm (cat.# 15021) Benzodiazepines 15 ng each component 1.0 μL split (split ratio 60:1) 250 °C 225 °C to 325 °C at 8 °C/min He, constant pressure 35 cm/sec @ 225 °C FID @ 320 °C FID sensitivity: 5.12 x 10-10 AFS

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GC CHROMATOGRAMS | CLINICAL

Benzodiazepines, Cannabinoids Benzodiazepines (15 μg/mL) on Rxi®-5Sil MS

Rxi® Technology! 1. 2. 3. 4. 5. 6. 7.

Exceptionally inert, ultra low-bleed capillary columns.

Peaks Oxazepam Lorazepam Diazepam Flunitrazepam Prazepam Clonazepam Alprazolam

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Transfer Line Temp.: Analyzer Type: Source Temp.: Electron Energy: Solvent Delay Time: Tune Type: Ionization Mode: Scan Range: Scan Rate: Instrument

Good peak shape with a fast elution time of <8 min

Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) Butyl chloride 15 μg/mL 1 μL splitless (hold 1 min) 3.5 mm splitless taper w/wool (cat.# 22286-200.1) 280 °C 32.2 (20:1 split) mL/min 200 °C to 330 °C at 15 °C/min (hold 3 min) He, constant linear velocity 50 cm/sec, 23.7 psi, 163.4 kPa @ 200 °C MS Scan 280 °C Quadrupole 200 °C 70 eV 4 min PFTBA EI 50-350 amu 5 scans/sec Shimadzu 2010 GC & QP2010+ MS

GC_CF1148

Derivatized Cannabinoids (5 μg/mL) on Rxi®-5Sil MS Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

1. 2. 3. 4.

3

Excellent peak shape with short run time.

1

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner:

4 2

8.0

9.0

10.0

Peaks Cannabidiol delta 9 THC Cannabinol THC-COOH; THCA

11.0

12.0 Time (min) GC_CF1145

Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Transfer Line Temp.: Analyzer Type: Source Temp.: Electron Energy: Solvent Delay Time: Tune Type: Ionization Mode: Scan Range: Scan Rate: Instrument

Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) Ethyl acetate 5 μg/mL TMS derivatives 1 μL splitless (hold 1 min) 3.5 mm splitless taper w/wool (cat.# 22286-200.1) 250 °C 21.4 mL/min 150 °C to 330 °C at 15 °C/min (hold 3 min) He, constant linear velocity 40 cm/sec, 13.8 psi, 95.1 kPa @ 150 °C MS Scan 280 °C Quadrupole 200 °C 70 eV 4 min PFTBA EI 200-500 amu 5 scans/sec Shimadzu 2010 GC & QP2010+ MS

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GC CHROMATOGRAMS | CLINICAL

Cocaine, Cold Medications Cocaine and Metabolites (TMS Derivatives) on Rxi®-5Sil MS (100 ng/mL)

1. 2. 3. 4. 5. 6.

Peaks Ecgonine methyl ester Ecgonine Cocaine Cocaethylene Benzoylecgonine Cannabinol*

m/z 1 82 82 82 82 82 409

m/z 2 96 96 182 196 96 --

m/z 3 256 356 303 317 346 --

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Transfer Line Temp.: Source Temp.: Solvent Delay Time: Tune Type: Ionization Mode: Instrument Notes

Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) Butyl chloride 100 ng/mL 1 μL splitless (hold 1 min) Single taper w/wool (cat.# 22286-200.1) 250 °C 20 mL/min 100 °C to 200 °C at 30 °C/min to 300 °C at 15 °C/min He, constant linear velocity 40 cm/sec, 12.5 psi, 86.2 kPa @ 100 °C MS SIM 310 °C 250 °C 4 min PFTBA EI Shimadzu 2010 GC & QP2010+ MS Samples were prepared as follows: Standards brought to dryness under nitrogen, then 50 μL BSTFA + 1% TMCS (cat.# 35606) were added. 50 μL pyridine was then added, and samples were incubated at 70 °C for 30 min. After incubation, samples were diluted with butyl chloride. * Cannabinol was used as a derivatization check.

GC_CF1149

Underivatized Cold Medications (Basic Drugs) on Rtx®-5 Amine 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

GC_PH00469 Column Injection Inj. Vol.: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

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Rtx®-5 Amine, 30 m, 0.53 mm ID, 1.00 μm (cat.# 12355) 1 μL split (split ratio 20:1) 250 °C 88 mL/min 175 °C to 280 °C at 10 °C/min (hold 5.5 min) He, constant flow 40 cm/sec FID @ 280 °C

Peaks Phenylpropanolamine Phenylephrine Guaifenesin Pheniramine Phenyltoloxamine Chlorpheniramine Brompheniramine Dextromethorphan Pyrilamine Codeine Hydrocodone


GC CHROMATOGRAMS | CLINICAL

Cold Medications, Opiates Underivatized Cold Medications (Basic Drugs) on Rtx®-35 Amine 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

4 2 7 8 6 5 3

9

Peaks Guaifenesin Pheniramine Phenyltoloxamine Chlorpheniramine Brompheniramine Dextromethorphan Pyrilamine Triprolidine Codeine Hydrocodone

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Ionization Mode: Scan Range:

Rtx®-35 Amine, 30 m, 0.25 mm ID, 0.50 μm (cat.# 11338) 1,000 ng/μL 1.0 μL split 250 °C 250 °C to 300 °C at 7 °C/min (hold 7 min) He, constant flow 30 cm/sec MS Scan EI 40-450 amu

10

1

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

11.0

12.0

13.0

14.0 GC_PH00575

Time (min)

Extracted Opiates from Blood on Rxi®-5Sil MS Peaks 1. Hydrocodone 2. Codeine 3. Oxycodone 4. Hydromorphone 5. 6-Monoacetylmorphine 6. Morphine * Matrix

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Mode: Transfer Line Temp.: Analyzer Type: Solvent Delay Time: Tune Type: Ionization Mode: Notes

Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) Ethyl acetate 100 ng/mL propionic anhydride derivatives 1 μL splitless (hold 1 min) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C 100 mL/min 65 °C (hold 1 min) to 315 °C at 15 °C/min He, constant flow 1 mL/min 35 cm/sec @ 65 °C MS SIM 250 °C Quadrupole

7 min PFTBA EI Opiates were spiked into a blood sample and extracted by SPE, then derivatized with propionic anhydride. Acknowledgement Data courtesy of Miami Dade County Medical Examiner Department GC_CF1150

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579


GC CHROMATOGRAMS | CLINICAL

Phenothiazines, Sympathomimetic Amines Underivatized Phenothiazines (Basic Drugs) on Rtx®-5 Separation optimized using Pro ezGC!

Peaks Phenothiazine Promethazine Trimeprazine Promazine Chlorprothixene Chlorpromazine Trifluoperazine Acetopromazine Prochlorperazine Thioridazine

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

Looking for more? Visit our online technical library for chromatograms based on ASTM methods, USP procedures, and other applications. www.restek.com/chromatograms

GC_PH00269 Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rtx®-5, 15 m, 0.32 mm ID, 0.50 μm (cat.# 10236) 2,000 ng/μL 1.0 μL split (split ratio 30:1) 250 °C 200 °C to 325 °C at 5 °C/min He, constant pressure 25 cm/sec @ 200 °C FID @ 315 °C FID sensitivity: 2.56 x 10-10 AFS

Underivatized Sympathomimetic Amines (Basic Drugs) on Rtx®-35 Amine 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

2

5 1 8

3

Peaks Amphetamine Methamphetamine N-Ethylamphetamine p-Methoxyamphetamine (PMA) p-Methoxymethamphetamine (PMMA) Methylenedioxyamphetamine (MDA) Methylenedioxymethamphetamine (MDMA) Methylenedioxyethylamphetamine (MDEA) HMMA MBDB

10 Column

4 6

Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Ionization Mode: Scan Range:

7

Rtx®-35 Amine, 30 m, 0.25 mm ID, 0.50 μm (cat.# 11338) Underivatized sympathomimetic amines 1,000 ng/μL 1.0 μL split 250 °C 150 °C to 240 °C at 7 °C/min He, constant flow 30 cm/sec MS Scan EI 40-450 amu

9

3.00

4.00

5.00

6.00

7.00 Time (min)

580 www.restek.com

8.00

9.00

10.00

11.00

12.00

13.00 GC_PH00574


GC CHROMATOGRAMS | CLINICAL

Sympathomimetic Amines Underivatized Sympathomimetic Amines (Basic Drugs) on Rtx®-5 Amine 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

Peaks Phenylethylamine Amphetamine Phentermine Methamphetamine Fenfluramine Mephentermine Cathinone Phenylpropanolamine Methcathinone Nicotine Ephedrine

Pseudoephedrine Phenmetrazine Phendimetrazine Methylenedioxyamphetamine Diethylpropion Methylenedioxymethamphetamine Methylenedioxyethylamphetamine 4-Methyl-2,5-dimethoxyamphetamine Phenylephrine Caffeine Benzphetamine

22

Column

16 14 2 5 6 18

10 13

4

19

3 9 1 7

5

21

17

1 μL split 250 °C 45 mL/min 100 °C to 310 °C at 10 °C/min He MS Scan 40-600 amu Varian 3400 coupled with with Varian Saturn 2000 MS detector

Ionization performed in the EI Auto mode.

15

11,12

Rtx®-5 Amine, 30 m, 0.25 mm ID, 0.50 μm (cat.# 12338)

Injection Inj. Vol.: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Detector Mode: Scan Range: Instrument

8

7.5

10

12.5

15

Time (min) 20 GC_PH00438

17.5

Sympathomimetic Amines (Basic Drugs) (HFBA Derivatives) on Rtx®-200 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

Peaks Phenylethylamine - HFBA Amphetamine - HFBA Phentermine - HFBA Methamphetamine - HFBA Fenfluramine - HFBA Mephentermine - HFBA Cathinone - HFBA Phenylpropanolamine - HFBA Methcathinone - HFBA Nicotine - HFBA Ephedrine - HFBA

Pseudoephedrine - HFBA Phenmetrazine - HFBA Phendimetrazine - HFBA Methylenedioxyamphetamine - HFBA Diethylpropion - HFBA Methylene dioxymethamphetamine - HFBA Methylene dioxyethylamphetamine - HFBA 4-Methyl-2,5-dimethoxyamphetamine - HFBA Phenylephrine - HFBA Caffeine - HFBA Benzphetamine - HFBA Column

1,2 15,20

Injection Inj. Vol.: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Detector Mode: Ionization Mode: Scan Range: Instrument

4 11

3 8

12 9

14

16

7.5

45 mL/min 100 °C to 310 °C at 10 °C/min He MS Scan EI 40-600 amu Varian 3400 coupled with with Varian Saturn 2000 MS detector

21 5

5

1 μL split 250 °C

22

7 10

19 17

13

Rtx®-200, 30 m, 0.25 mm ID, 0.50 μm (cat.# 15038)

10

18

12.5

15

17.5 Time (min) GC_PH00439

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581


GC CHROMATOGRAMS | CLINICAL

Sympathomimetic Amines Sympathomimetic Amines (TFAA Derivatives) (Basic Drugs) on Rtx®-5

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

Peaks Amphetamine - TFAA Phentermine - TFAA Phenylpropanolamine - TFAA Ephedrine - TFAA Methamphetamine - TFAA Fenfluramine - TFAA Pseudoephedrine - TFAA Methylenedioxyamphetamine - TFAA Methylenedioxymethamphetamine - TFAA Methylphenidate - TFAA

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Transfer Line Temp.: Ionization Mode:

Rtx®-5, 30 m, 0.25 mm ID, 0.25 μm (cat.# 10223) Derivatized sympathomimetic amines Approximately 2.5 ng/μL 1.0 μL splitless (hold 1.0 min) 225 °C 40 °C (hold 1 min) to 150 °C at 30 °C/min to 300 °C at 5 °C/min He, constant pressure 20 cm/sec @ 100 °C MS Scan 275 °C EI

GC_PH00251

Sympathomimetic Amines (HFBA Derivatives) (Basic Drugs) on Rtx®-5 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

Peaks Amphetamine - HFBA Phentermine - HFBA Phenylpropanolamine - HFBA Ephedrine - HFBA Methamphetamine - HFBA Fenfluramine - HFBA Pseudoephedrine - HFBA Methylenedioxyamphetamine - HFBA Methylenedioxymethamphetamine - HFBA Methylphenidate - HFBA

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Transfer Line Temp.: Ionization Mode:

Rtx®-5, 30 m, 0.25 mm ID, 0.25 μm (cat.# 10223) Derivatized sympathomimetic amines Approximately 2.5 ng/μL 1.0 μL splitless (hold 1.0 min) 225 °C 40 °C (hold 1 min) to 150 °C at 30 °C/min to 300 °C at 5 °C/min He, constant pressure 20 cm/sec @ 100 °C MS Scan 275 °C EI

GC_PH00252

582 www.restek.com


GC CHROMATOGRAMS | ENVIRONMENTAL

Air TO-15 65 Component Mix on Rxi®-624Sil MS (30 m) 54,55

58

NEW!

53

56 57

61 62

19,20 34

47

44

52

63

24,25 36

39,40

32

21

67

43 49

38 48

22,23

13,14 15 12

41 28 27 26 29 33 35 30 31

18

64 65

60

46

45

51

50

42

66 59

69

16 68

6 7 1 45 3 2

8

70

11

9 10

2.00

Column Sample

Diluent: Conc.: Injection Oven Oven Temp.: Carrier Gas Flow Rate: Linear Velocity: Detector Mode: Transfer Line Temp.: Analyzer Type: Source Temp.: Quad Temp.: Electron Energy: Solvent Delay Time: Tune Type: Ionization Mode: Scan Range: Scan Rate: Preconcentrator Trap 1 Settings Type/Sorbent : Cooling temp: Preheat temp: Preheat time: Desorb temp: Desorb flow: Desorb time: Bakeout temp: Flush flow: Flush time: Sweep flow:

17

3.00

37 4.00

Rxi®-624Sil MS, 30 m, 0.32 mm ID, 1.80 μm (cat.# 13870) TO-15 65 component mix (cat.# 34436) TO-14A internal standard/ tuning mix (cat.# 34408) Nitrogen 10.0 ppbv 200 cc injection Direct 32 °C (hold 1 min) to 150 °C at 11 °C/min to 230 °C at 33 °C/min He, constant flow 2.0 mL/min 51 cm/sec @ 32 °C MS Scan 230 °C Quadrupole 230 °C 150 °C 69.9 eV 1.0 min BFB EI 35 - 250 amu 3.32 scans/sec Nutech 8900DS Glass Beads -155 °C 5 °C 0 sec 20 °C 5 mL/min 360 sec 200 °C 120 mL/min 60 sec 120 mL/min

5.00

6.00

Sweep time: Trap 2 Settings Type/Sorbent: Cooling temp: Desorb temp: Desorb time: Bakeout temp: Bakeout time: Cryofocuser Cooling temp: Inject time: Internal Standard Purge flow: Purge time: Vol.: ISTD flow: Standard Size: Purge flow: Purge time: Sample flow: Instrument Acknowledgement

7.00

60 sec Tenax® -35 °C 190 °C 30 sec 200 °C 10 sec -160 °C 140 sec 100 mL/min 6 sec 20 mL 100 mL/min 200 mL 100 mL/min 6 sec 100 mL/min HP6890 GC & 5973 MSD Nutech

8.00

9.00

10.00

11.00

Peaks tR (min) 1. Propylene 1.42 2. Dichlorodifluoromethane (Freon® 12) 1.46 3. 1,2-Dichlorotetrafluoroethane (Freon® 114) 1.58 4. Chloromethane 1.62 5. Vinyl chloride 1.73 6. 1,3-Butadiene 1.77 7. Bromomethane 2.02 8. Chloroethane 2.12 9. Trichlorofluoromethane (Freon® 11) 2.34 10. Ethanol 2.54 11. Acrolein 2.71 12. 1,1-Dichloroethene 2.78 13. 1,1,2-Trichlorotrifluoroethane (Freon® 113) 2.80 14. Acetone 2.82 15. Carbon disulfide 2.95 16. Isopropyl alcohol 2.99 17. Acetonitrile (contaminant) 3.05 18. Methylene chloride 3.20 19. trans-1,2-Dichloroethene 3.43 20. Methyl tert-butyl ether (MTBE) 3.44 21. Hexane 3.67 22. 1,1-Dichloroethane 3.80 23. Vinyl acetate 3.82 24. 2-Butanone (MEK) 4.29 25. cis-1,2-Dichloroethene 4.29 26. Ethyl acetate 4.34 27. Bromochloromethane (IS) 4.50 28. Tetrahydrofuran 4.52 29. Chloroform 4.60 30. 1,1,1-Trichloroethane 4.74 31. Cyclohexane 4.80 32. Carbon tetrachloride 4.88 33. Benzene 5.06 34. 1,2-Dichloroethane 5.12 35. Heptane 5.35

12.00

13.00

Time (min) GC_AR1148

Peaks tR (min) 36. 1,4-Difluorobenzene (IS) 5.47 37. Trichloroethylene 5.69 38. 1,2-Dichloropropane 5.94 39. Methyl methacrylate 6.01 40. 1,4-Dioxane 6.02 41. Bromodichloromethane 6.20 42. cis-1,3-Dichloropropene 6.64 43. 4-Methyl-2-pentanone (MIBK) 6.80 44. Toluene 6.99 45. trans-1,3-Dichloropropene 7.26 46. 1,1,2-Trichloroethane 7.47 47. Tetrachloroethene 7.55 48. 2-Hexanone (MBK) 7.72 49. Dibromochloromethane 7.88 50. 1,2-Dibromoethane 8.01 51. Chlorobenzene-d5 (IS) 8.54 52. Chlorobenzene 8.58 53. Ethylbenzene 8.71 54. m-Xylene 8.87 55. p-Xylene 8.87 56. o-Xylene 9.32 57. Styrene 9.35 58. Bromoform 9.56 59. 4-Bromofluorobenzene* 9.99 60. 1,1,2,2-Tetrachloroethane 10.18 61. 4-Ethyltoluene 10.47 62. 1,3,5-Trimethylbenzene 10.55 63. 1,2,4-Trimethylbenzene 11.02 64. 1,3-Dichlorobenzene 11.35 65. 1,4-Dichlorobenzene 11.49 66. Benzyl chloride 11.65 67. 1,2-Dichlorobenzene 11.93 68. 1,2,4-Trichlorobenzene 13.47 69. Hexachlorobutadiene 13.59 70. Naphthalene 13.67 *Tunings tandard

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583


GC CHROMATOGRAMS | ENVIRONMENTAL

Air TO-15 65 Component Mix on Rxi®-1ms (30 m) 54,55,56 6

NEW!

7

5

2 3

4

8

11 50

1 10 9

41

28

53

38 21

25,26,27

16

30

13

36

64,65 48

45 33

42 40 43

20

15 12

51,52

46

37

31 32

17,18 19 24

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

58,59

61 62 57

63

44 66

49 34 22 23

67

29

47

70

35 60 39

14 1.00

Column Sample

Diluent: Conc.: Injection Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Mode: Transfer Line Temp.: Analyzer Type: Source Temp.: Quad Temp.: Electron Energy: Solvent Delay Time: Tune Type: Ionization Mode: Scan Range: Scan Rate: Preconcentrator Trap 1 Settings Type/Sorbent : Cooling temp: Preheat temp: Preheat time: Desorb temp: Desorb flow: Desorb time: Bakeout temp: Flush flow: Flush time: Sweep flow: Sweep time:

2.00

Rxi®-1ms, 30 m, 0.32 mm ID, 1.00 μm (cat.# 13354) TO-15 65 component mix (cat.# 34436) TO-14A internal standard/ tuning mix (cat.# 34408) Nitrogen 10.0 ppbv 250 cc injection Direct 35 °C (hold 1 min) to 230 °C at 11 °C/min He, constant flow 2.0 mL/min 51 cm/sec @ 35 °C MS Scan 230 °C Quadrupole 230 °C 150 °C 69.9 eV 1.0 min BFB EI 35 - 250 amu 3.32 scans/sec Nutech 8900DS Glass Beads -155 °C 5 °C 0 sec 20 °C 5 mL/min 360 sec 200 °C 120 mL/min 60 sec 120 mL/min 60 sec

584 www.restek.com

3.00

4.00

Trap 2 Settings Type/Sorbent: Cooling temp: Desorb temp: Desorb time: Bakeout temp: Bakeout time: Cryofocuser Cooling temp: Inject time: Internal Standard Purge flow: Purge time: Vol.: ISTD flow: Standard Size: Purge flow: Purge time: Sample flow: Instrument Acknowledgement

68 69 5.00

6.00

Tenax® -35 °C 190 °C 30 sec 200 °C 10 sec -160 °C 140 sec 100 mL/min 6 sec 20 mL 100 mL/min 200 mL 100 mL/min 6 sec 100 mL/min HP6890 GC & 5973 MSD Nutech Instruments

7.00 Time (min)

8.00

9.00

Peaks tR (min) 1. Propylene 1.37 2. Dichlorodifluoromethane (Freon® 12) 1.39 3. Chloromethane 1.44 4. 1,2-Dichlorotetrafluoroethane (Freon® 114) 1.49 5. Vinyl chloride 1.51 6. 1,3-Butadiene 1.56 7. Bromomethane 1.64 8. Chloroethane 1.70 9. Ethanol 1.80 10. Acetonitrile (contaminant) 1.83 11. Acrolein 1.86 12. Acetone 1.90 13. Trichlorofluoromethane (Freon® 11) 1.93 14. Isopropyl alcohol 2.03 15. 1,1-Dichloroethene 2.13 16. Methylene chloride 2.17 17. Carbon disulfide 2.26 18. 1,1,2-Trichlorotrifluoroethane (Freon® 113) 2.27 19. trans-1,2-Dichloroethene 2.49 20. 1,1-Dichloroethane 2.57 21. Methyl tert-butyl ether (MTBE) 2.60 22. Vinyl acetate 2.64 23. 2-Butanone (MEK) 2.74 24. cis-1,2-Dichloroethene 2.88 25. Bromochloromethane (IS) 2.94 26. Hexane* 2.97 27. Ethyl acetate* 2.99 28. Chloroform 3.00 29. Tetrahydrofuran 3.17 30. 1,2-Dichloroethane 3.32 31. 1,1,1-Trichloroethane 3.42 32. Benzene 3.63 33. Carbon tetrachloride 3.70 34. Cyclohexane 3.76

10.00

11.00

12.00

13.00

GC_AR1147

Peaks tR (min) 35. 1,4-Difluorobenzene (IS) 3.82 36. 1,2-Dichloropropane 4.05 37. Bromodichloromethane 4.14 38. Trichloroethylene 4.17 39. 1,4-Dioxane 4.21 40. Methyl methacrylate 4.31 41. Heptane 4.35 42. cis-1,3-Dichloropropene 4.65 43. 4-Methyl-2-pentanone (MIBK) 4.71 44. trans-1,3-Dichloropropene 4.98 45. 1,1,2-Trichloroethane 5.07 46. Toluene 5.25 47. 2-Hexanone (MBK) 5.47 48. Dibromochloromethane 5.51 49. 1,2-Dibromoethane 5.67 50. Tetrachloroethene 6.01 51. Chlorobenzene-d5 (IS) 6.48 52. Chlorobenzene 6.51 53. Ethylbenzene 6.83 54. m-Xylene 6.98 55. p-Xylene 6.98 56. Bromoform 6.98 57. Styrene 7.26 58. 1,1,2,2-Tetrachloroethane 7.35 59. o-Xylene 7.35 60. 4-Bromofluorobenzene** 7.74 61. 4-Ethyltoluene 8.52 62. 1,3,5-Trimethylbenzene 8.61 63. 1,2,4-Trimethylbenzene 9.01 64. Benzyl chloride 9.11 65. 1,3-Dichlorobenzene 9.11 66. 1,4-Dichlorobenzene 9.19 67. 1,2-Dichlorobenzene 9.55 68. 1,2,4-Trichlorobenzene 11.68 69. Naphthalene 11.79 70. Hexachlorobutadiene 12.38 *Peaks 26 and 27 share ion m/z 43; **Tuning standard


GC CHROMATOGRAMS | ENVIRONMENTAL

Air Mass APH on Rxi®-1ms 28 26

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

24 23 25 18

15

12

20 19

21 22

13 14 8 9

10

17 11 27

5

7 6

3

16

4

2

1

4

5

6

7

8

9

10

11

12

13 14 15 Time (min)

16

17

18 19 20

21 22

23

GC_AR1145

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

Peaks 1,3-Butadiene iso-Pentane Methyl tert-butyl ether Bromochloromethane n-Hexane Benzene Cyclohexane 1,4-Difluorobenzene 2,3-Dimethylpentane n-Heptane Toluene n-Octane Chlorobenzene-d5 Ethylbenzene 2,3-Dimethylheptane m-Xylene/p-Xylene o-Xylene n-Nonane 4-Bromofluorobenzene Isopropylbenzene 1-Ethyl-3-methylbenzene 1,3,5-Trimethylbenzene n-Decane 1,2,3-Trimethylbenzene/p-Isopropyltoluene Butylcyclohexane n-Undecane Naphthalene n-Dodecane

NEW!

Column Rxi®-1ms, 60 m, 0.32 mm ID, 1.00 μm (cat.# 13357) Injection Splitless Oven Oven Temp: 35 °C (hold 5 min) to 220 °C at 7 °C/min (hold 2 min) Carrier Gas He, constant flow Flow Rate: 1.2 mL/min Detector MS Mode: Scan Transfer Line Temp.: 240 °C Analyzer Type: Quadrupole Source Temp.: 230 °C Quad Temp.: 150 °C Solvent Delay Time: 4.0 min Ionization Mode: EI Scan Range: 35-250 amu Preconcentrator Entech 7100 Instrument HP6890 GC & 5973 MSD Acknowledgement Courtesy of Mass DEP, Northeast Region

How can we help you today? Contact us... customer service: 1-814-353-1300, ext. 3 | e-mail: csreps@restek.com technical service: 1-814-353-1300, ext. 4 | e-mail: support@restek.com sales representatives: 1-814-353-1300, ext. 3 | e-mail: salesreps@restek.com 4 ways to order: 1. CALL: 1-800-356-1688, ext. 3 or 1-814-353-1300, ext. 3 Monday–Friday 8:00 a.m.–6:30 p.m. Eastern Time 2. FAX: 1-814-353-1309 24 hours a day 3. ONLINE: www.restek.com 24 hours a day 4. E-MAIL: csreps@restek.com 24 hours a day Outside the U.S.? Find a distributor at

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585


GC CHROMATOGRAMS | ENVIRONMENTAL

Brominated Flame Retardants Brominated Flame Retardants on Rtx®-1614 1. 2. 3. 4. 5. 6. 7. 8.

Get results 3 times faster with a short column method!

Peaks BDE-10 BDE-7 BDE-8 BDE-11 BDE-12 BDE-13 BDE-15 BDE-30

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

9. 10. 11. 12. 13. 14. 15. 16. 17.

BDE-32 BDE-17 BDE-25 BDE-28 BDE-33 BDE-35 BDE-37 BDE-75 BDE-49

18. 19. 20. 21. 22. 23. 24. 25. 26.

BDE-71 BDE-47 BDE-66 BDE-77 BDE-100 BDE-119 BDE-99 BDE-116 BDE-118

27. 28. 29. 30. 31. 32. 33. 34. 35.

BDE-85 BDE-155 BDE-126 BDE-154 BDE-153 BDE-138 BDE-166 BDE-183 BDE-181

36. 37. 38. 39. 40.

BDE-190 BDE-208 BDE-207 BDE-206 BDE-209

Rtx®-1614, 15 m, 0.25 mm ID, 0.10 μm (cat.# 10296) 100 - 300 ppb PBDE PAR solution (#EO-5113, Cambridge Isotope Laboratories Inc.) 500 ppb decabromodiphenyl ether (#BDE-209, Wellington Laboratories) 1 μL splitless (hold 1 min) 4 mm cyclo double taper (cat.# 20896) 340 °C 120 °C (hold 1 min) to 275 °C at 15 °C/min to 300 °C at 5 °C/min (hold 5 min) He, constant linear velocity 60 cm/sec @ 120 °C μ-ECD @ 345 °C

Great peak shape for BDE 209!

also see: PCBs and Brominated Flame Retardants

➲ pages 603–604 GC_EV01025

Brominated Flame Retardants on Rtx®-1614 Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rtx®-1614, 30 m, 0.25 mm ID, 0.10 μm (cat.# 10295) 100 - 300 ppb PBDE PAR solution (cat.# EO-5113, Cambridge Isotope Laboratories Inc.) 500 ppb decabromodiphenyl ether (cat.# BDE-209, Wellington Laboratories)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

1 μL splitless (hold 1 min) Cyclo double taper (4 mm) (cat.# 20896) 300 °C 100 °C (hold 3 min) to 320 °C at 5 °C/min (hold 15 min) He, constant linear velocity 20 cm/sec @ 100 °C μ-ECD @ 340 °C

GC_EV01019

586 www.restek.com

Peaks BDE-10 BDE-7 BDE-8 BDE-11 BDE-12 BDE-13 BDE-15 BDE-30 BDE-32 BDE-17 BDE-25 BDE-28 BDE-33 BDE-35 BDE-37 BDE-75 BDE-49 BDE-71 BDE-47 BDE-66

21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40.

BDE-77 BDE-100 BDE-119 BDE-99 BDE-116 BDE-118 BDE-85 BDE-155 BDE-126 BDE-154 BDE-153 BDE-138 BDE-166 BDE-183 BDE-181 BDE-190 BDE-208 BDE-207 BDE-206 BDE-209


GC CHROMATOGRAMS | ENVIRONMENTAL

Dioxins/Furans TCDDs on Rtx®-Dioxin2 Column

1. 2. 3. 4. 5. 6. 7. 8.

Peaks 1,2,3,4-TCDD 1,2,3,7-TCDD 1,2,3,8-TCDD 1,2,3,9-TCDD 2,3,7,8-TCDD 1,2,6,7-TCDD 1,2,7,8-TCDD 1,2,8,9-TCDD

tR (min) 27.92 28.65 28.65 28.78 29.40 29.58 29.58 30.02

NEW!

Column Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp:

Rtx®-Dioxin2, 60 m, 0.25 mm ID, 0.25 μm (cat.# 10758) Laboratory prepared test mix 1.0 μL splitless 290 °C

150 °C (hold 1 min) to 210 °C at 30 °C/min (hold 1 min) to 250 °C at 3 °C/min (hold 12 min) to 330 °C at 70 °C/min (hold 6 min) Carrier Gas He, constant flow Flow Rate: 1.5 mL/min Detector Micromass Autospec Ultima Transfer Line Temp.: 290 °C Analyzer Type: Magnetic sector Source Temp.: 290 °C Tune Type: PFK Ionization Mode: EI Instrument Agilent/HP6890 GC Acknowledgement Courtesy of Maxxam Analytics (Ontario, Canada). GC_EV1239

TCDFs on Rtx®-Dioxin2 Column 1. 2. 3. 4. 5. 6. 7.

Peaks 2,3,4,7-TCDF 2,3,4,8-TCDF 2,3,7,8-TCDF 3,4,6,7-TCDF 2,3,6,7-TCDF 1,2,6,9-TCDF 1,2,3,9-TCDF

tR (min) 18.58 18.58 18.91 19.10 19.24 19.24 19.66

NEW! Column Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp:

Rtx®-Dioxin2, 60 m, 0.25 mm ID, 0.25 μm (cat.# 10758) Laboratory prepared test mix 1.0 μL splitless 290 °C

180 °C (hold 1 min) to 235 °C at 45 °C/min (hold 1 min) to 250 °C at 3 °C/min (hold 15 min) to 300 °C at 50 °C/min (hold 1 min) Carrier Gas He, constant flow Flow Rate: 1.7 mL/min Detector Micromass Autospec Ultima Transfer Line Temp.: 290 °C Analyzer Type: Magnetic sector Source Temp.: 290 °C Tune Type: PFK Ionization Mode: EI Instrument Agilent/HP6890 GC Acknowledgement Courtesy of Maxxam Analytics (Ontario, Canada).

GC_EV1252

Maxxam Analytics HRMS Group Receives Kaizen Award for Productivity Improvements Congratulations to Maxxam Analytics’ Hi-Res Mass Spec Ultra Trace Analysis team, who received a Kaizen award for productivity improvements made using the Rtx®-Dioxin2 column. Shown from left to right are: Owen Cosby, Supervisor HRMS Services; Kay Shaw, HRMS Team Leader and Scientific Specialist; and Angel Guerrero, HRMS Senior Analyst.

According to Owen Cosby of Maxxam Analytics, “Using the Rtx®-Dioxin2 column allowed us to combine EPA 1613 TCDD-only and TCDF confirmation analyses onto one column and one instrument. This resulted in multiple benefits— we shortened run times, reduced instrument downtime and column changes, and increased instrument capacity for our full-list samples.”

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587


GC CHROMATOGRAMS | ENVIRONMENTAL

Dioxins/Furans Dioxins (TCDDs) in Fly Ash on Rxi®-5Sil MS column

NEW! TCDDs Column Sample Diluent: Injection Inj. Vol.: Liner: Oven Oven Temp:

Rxi®-5Sil MS , 60 m, 0.18 mm ID, 0.10 μm (cat.# 43607) Fly ash extract Nonane 1 μL splitless 2 mm splitless liner (cat.# 20712)

120 °C (hold 1 min) to 160 °C at 10 °C/min to 300 °C at 2.5 °C/min Carrier Gas He, constant flow Flow Rate: 1 mL/min Detector Waters AutoSpec Ultima Mass Spectrometer Source Temp.: 280 °C Ionization Mode: EI Notes Electron Ionization at 40eV Acknowledgement Chromatogram courtesy of Karen MacPherson, Li Shen, Terry Kolic, and Eric Reiner at the Ontario Ministry of the Environment

GC_EV1194

Furans (TCDFs) in Fly Ash on Rxi®-5Sil MS

NEW! TCDFs Column Sample Diluent: Injection Inj. Vol.: Liner: Oven Oven Temp:

Rxi®-5Sil MS , 60 m, 0.18 mm ID, 0.10 μm (cat.#43607) Fly ash extract Nonane 1 μL splitless 2 mm splitless liner (cat.# 20712)

120 °C (hold 1 min) to 160 °C at 10 °C/min to 300°C at 2.5°C/min Carrier Gas He, constant flow Flow Rate: 1 mL/min Detector Waters AutoSpec Ultima Mass Spectrometer Source Temp.: 280 °C Ionization Mode: EI Notes Electron Ionization at 40eV Acknowledgement Chromatogram courtesy of Karen MacPherson, Li Shen, Terry Kolic, and Eric Reiner at the Ontario Ministry of the Environment

GC_EV1195

588 www.restek.com


GC CHROMATOGRAMS | ENVIRONMENTAL

Dioxins/Furans Dioxins (PnCDDs) in Fly Ash on Rxi®-5Sil MS

NEW!

PnCDDs in Fly Ash

Column Sample Diluent: Injection Inj. Vol.: Liner: Oven Oven Temp: Carrier Gas Flow Rate: Detector Source Temp.: Ionization Mode: Notes

Rxi®-5Sil MS, 60 m, 0.18 mm ID, 0.10 μm (cat.# 43607) Fly ash extract Nonane 1 μL splitless 2 mm splitless liner (cat.# 20712)

120 °C (hold 1 min) to 160 °C at 10 °C/min to 300 °C at 2.5 °C/min He, constant flow 1 mL/min Waters AutoSpec Ultima Mass Spectrometer 280 °C EI Electron Ionization at 40eV Red indicates toxicity Acknowledgement Chromatogram courtesy of Karen MacPherson, Li Shen, Terry Kolic, and Eric Reiner at the Ontario Ministry of the Environment GC_EV1197

Dioxins (HxCDFs) in Fly Ash on Rxi®-5Sil MS

NEW!

Column Sample Diluent: Injection Inj. Vol.: Liner: Oven Oven Temp: Carrier Gas Flow Rate: Detector Source Temp.: Ionization Mode: Notes

Rxi®-5Sil MS, 60 m, 0.18 mm ID, 0.10 μm (cat.# 43607) Fly ash extract Nonane 1 μL splitless 2 mm splitless liner (cat.# 20712)

120 °C (hold 1 min) to 160 °C at 10 °C/min to 300 °C at 2.5 °C/min He, constant flow 1 mL/min Waters AutoSpec Ultima Mass Spectrometer 280 °C EI Electron Ionization at 40eV Red indicates toxicity Acknowledgement Chromatogram courtesy of Karen MacPherson, Li Shen, Terry Kolic, and Eric Reiner at the Ontario Ministry of the Environment

HxCDFs in Fly Ash

GC_EV1199

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589


GC CHROMATOGRAMS | ENVIRONMENTAL

Explosives Explosives on Rtx®-200 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23.

Peaks 2-Nitrotoluene 3-Nitrotoluene 4-Nitrotoluene 2,3-Diaminotoluene 2,6-Diaminotoluene 2,4-Diaminotoluene 1,4-Dinitrobenzene 2,6-Dinitrotoluene 2-Amino-6-nitrotoluene 1,3-Dinitrobenzene 2,4-Dinitrotoluene 2-Amino-4-nitrotoluene 2,3-Dinitrotoluene 3,4-Dinitrotoluene 3-Nitrobiphenyl 2,4,6-Trinitrotoluene 2,4,5-Trinitrotoluene 4-Amino-2,6-dinitrotoluene 2,3,4-Trinitrotoluene 1,3-Dinitronaphthalene 2,6-Diamino-4-nitrotoluene 2-Amino-4,6-dinitrotoluene 2,2'-Dinitrobiphenyl

GC_EV00060 Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Transfer Line Temp.: Analyzer Type: Ionization Mode:

Rtx®-200, 30 m, 0.25 mm ID, 0.25 μm (cat.# 15023) Explosives sample 20 ng/μL 1 μL splitless (hold 0.6 min) 280 °C 80 °C (hold 2 min) to 260 °C at 3 °C/min (hold 2 min) He, constant pressure 20 cm/sec @ 80 °C MS Scan 300 °C Quadrupole EI

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GC CHROMATOGRAMS | ENVIRONMENTAL

Gasoline Range Organics Petroleum Hydrocarbons (TPH) on Rxi®-1ms 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Peaks C8 C10 C12 C14 C16 C18 C20 C22 C24 C26 C28 C30 C32 C34 C36 C38 C40

GC_EV00886 Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Instrument Acknowledgement

Rxi®-1ms, 20 m, 0.18 mm ID, 0.18 μm (cat.# 13302) Florida TRPH standard (cat.# 31266) Hexane 500 μg/mL 0.5 μL split (split ratio 20:1) 3.5 mm split Precision® liner w/wool (cat.# 21021) 275 °C 40 °C (hold 1 min) to 330 °C at 20 °C/min (hold 10 min) H2, constant pressure 55 cm/sec @ 40 °C FID @ 350 °C Shimadzu 2010 GC GC courtesy of Shimadzu Scientific.

Lubrication Range Organics Diesel Fuel #2/Motor Oil on Rxi®-1ms

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Peaks 1. Diesel fuel #2 composite 2. Motor oil

GC_EV00887

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Instrument

Rxi®-1ms, 20 m, 0.18 mm ID, 0.18 μm (cat.# 13302) Diesel #2/motor oil (cat.# 31682) Hexane 5,000 μg/mL 0.5 μL split (split ratio 20:1) 3.5 mm split Precision® liner w/wool (cat.# 21021) 275 °C 40 °C (hold 1 min) to 330 °C at 20 °C/min (hold 10 min) H2, constant pressure 55 cm/sec @ 40 °C FID @ 350 °C Shimadzu 2010 GC

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591


GC CHROMATOGRAMS | ENVIRONMENTAL

Glycols Glycols on Rtx®-Wax

Peaks 1. Propylene glycol 2. Ethylene glycol

GC_EV00444 Column Sample Conc.: Injection Inj. Temp.: Oven Oven Temp: Detector Notes

Rtx®-Wax, 30 m, 0.53 mm ID, 1.00 μm (cat.# 12455) 100 μg/mL each Direct 220 °C 80 °C (hold 1 min) to 120 °C at 8 °C/min (hold 3 min) FID @ 270 °C 10 psi pressure

Glycols on Rtx®-200 Peaks 1. Ethylene glycol 2. Propylene glycol

GC_EV00445 Column Sample Conc.: Injection Inj. Temp.: Oven Oven Temp: Detector Notes

592 www.restek.com

Rtx®-200, 30 m, 0.53 mm ID, 1.00 μm (cat.# 15055) 100 μg/mL each Direct 220 °C 80 °C (hold 1 min) to 200 °C at 8 °C/min (hold 3 min) FID @ 270 °C 10 psi pressure


GC CHROMATOGRAMS | ENVIRONMENTAL

Glycols Glycols on Stabilwax® 1. 2. 3. 4. 5. 6. 7.

Glycols on Stabilwax®

Peaks 1,2-Propylene glycol Ethylene glycol 1,3-Butylene glycol 1,3-Propylene glycol 1,4-Butylene glycol Diethylene glycol Glycerol

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Make-up Gas Flow Rate: Notes

Peaks 1. Propylene glycol 2. Ethylene glycol Column

Stabilwax®, 30 m, 0.53 mm ID, 1.00 μm (cat.# 10655) Glycol mix Water:methanol (50:50) 150 ppm 1.0 μL direct Open-top Uniliner® liner without wool (cat.# 20843-205) 80 °C to 200 °C at 8 °C/min (hold 10 min) He, constant flow 6.9 mL/min 50 cm/sec FID @ 270 °C

Stabilwax®, 30 m, 0.53 mm ID, 1.0 μm (cat.# 10655) Glycols Water 100 ppm

Sample Diluent: Conc.: Injection Inj. Vol.: Liner:

1.0 μL direct Open-top Uniliner® inlet liner without wool (cat.# 20843-205) 225 °C

Inj. Temp.: Oven Oven Temp:

80 °C (hold 1 min) to 200 °C at 8 °C/ min (hold 5 min) He, constant linear velocity 50 cm/sec FID @ 250 °C Agilent/HP6890 GC Septum Purge: 5.0 cc/min

Carrier Gas Linear Velocity: Detector Instrument Notes

45 mL/min Septa purge = 5.0 cc/min

GC_EV00476

GC_EV00546

Chromatogram Search Tool Search by compound name, synonym, CAS #, or keyword www.restek.com/chromatograms

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593


GC CHROMATOGRAMS | ENVIRONMENTAL

Haloacetic Acids Haloacetic Acids & Dalapon by EPA Method 552.2 on Rtx®-CLPesticides & Rtx®-CLPesticides2 Rtx®-CLPesticides

GC_EV01006

Rtx®-CLPesticides2

GC_EV01007 Columns

Sample

Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

594 www.restek.com

Rtx®-CLPesticides2 30 m, 0.32 mm ID, 0.25 μm (cat.# 11324) and Rtx®-CLPesticides 30 m, 0.32 mm ID, 0.32 μm (cat.# 11141) using Rxi® guard column 5 m, 0.32 mm ID (cat.# 10039) with deactivated universal “Y” Press-Tight® connector (cat.# 20405-261) Haloacetic acid methyl ester mix #2 (cat.# 31647) Dalapon methyl ester (cat.# 32057) Methyl-2,3-dibromopropionate (cat.# 31656) 1,2,3-Trichloropropane (cat.# 31648) Methyl tert-butyl ether (MTBE) 1.0 μL splitless (hold 0.75 min) Cyclo double taper (4 mm) (cat.# 20896) 250 °C 35 °C (hold 4 min) to 250 °C at 15 °C/min (hold 5 min) He, constant flow 25 cm/sec μ-ECD @ 300 °C This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

Peaks Conc. (μg/mL) Methyl monochloroacetate 1.2 Methyl monobromoacetate 0.8 Methyl dichloroacetate 1.2 Dalapon methyl ester 2 Methyl trichloroacetate 0.4 1,2,3-Trichloropropane (IS) 4 Methyl bromo(chloro)acetate 0.8 Methyl bromodichloroacetate 0.8 Methyl dibromoacetate 0.4 Methyl chlorodibromoacetate 2 Methyl 2,3-dibromopropionate (SS) 2 Methyl tribromoacetate 4


GC CHROMATOGRAMS | ENVIRONMENTAL

Herbicides Herbicides on Rtx®-CLPesticides & Rtx®-CLPesticides2

Rtx®-CLPesticides

<13 min chlorophenoxyacid herbicide analysis!

Peaks 1. Dalapon methyl ester 2. 3,5-Dichlorobenzoic acid methyl ester (SS) 3. 4-Nitroanisole 4. DCAA methyl ester (SS) 5. Dicamba methyl ester 6. MCPP methyl ester 7. MCPA Methyl ester 8. Dichlorprop, methyl ester 9. 4,4'-DBOB (IS) 10. 2,4-D methyl ester 11. Pentachloroanisole 12. 2,4,5-TP, methyl ester 13. 2,4,5-T methyl ester 14. Chloramben, methyl ester 15. 2,4-DB methyl ester 16. Dinoseb methyl ester 17. Bentazon methyl ester 18. DCPA 19. Pichloram methyl ester 20. Acifluorfen methyl ester C. contaminant

GC_EV00971 Columns

Rtx®-CLPesticides2

Sample

Fully resolve bentazon and picloram methyl esters

Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Instrument Notes

Rtx®-CLPesticides2 30 m, 0.32 mm ID, 0.25 μm (cat.# 11324) and Rtx®-CLPesticides 30 m, 0.32 mm ID, 0.32 μm (cat.# 11141) using Rxi® deactivated guard column 5 m, 0.32 mm ID (cat.# 10039) with universal “Y” Press-Tight® connector (cat.# 20405-261) 200 ng/mL herbicide mix #1 (cat.# 32055) 1,000 ng/mL dalapon methyl ester (cat.# 32057) 20,000 ng/mL herbicide mix #3 (cat.# 32059) 200 ng/mL herbicide mix #4 (cat.# 32062) 250 ng/mL 4,4’-dibromooctafluorobiphenyl (cat.# 32053) 400 ng/mL 2,4-dichlorophenyl acetic acid methyl ester (cat.# 32050) Hexane 1.0 μL splitless (hold 0.75 min) Cyclo double taper (4 mm) (cat.# 20895) 250 °C 70 °C (hold 0.5 min) to 190 °C at 25 °C/min (hold 1 min) to 300 °C at 11 °C/min (hold 5 min) He, constant pressure 36 cm/sec @ 70 °C μ-ECD @ 325 °C Agilent/HP6890 GC This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

GC_EV00971A

also see: Pesticides & Herbicides

➲ page 610

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595


GC CHROMATOGRAMS | ENVIRONMENTAL

PAH and PCB Mixtures PAHs and PCB Congeners on Rxi®-XLB Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

NEW!

PCB 31 & 28 4 3

8

PCB 180, Benzo[a]anthracene, chrysene, & triphenylene

Benzo[b]fluoranthene & benzo[k]fluoranthene

20

9

5

21 24

19

2

23

9.92 9.97 10.02 10.07 10.12 10.17 10.22 10.27 10.32

1

6 7

18 11

15.66 15.71 15.76 15.81 15.86 15.91 15.96 16.01 16.06

14.90 14.95 15.00 15.05 15.10 15.15 15.20 15.25 15.30

13

20 21

14 19

24

27, 28

25

29

23

26

89 10 15

16

17

18

14.08 Time (min)

15.08

22

12 6.08

7.08

Column Sample

Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Detector Mode: Transfer Line Temp.: Analyzer Type: Source Temp.: Electron Energy: Solvent Delay Time: Tune Type: Ionization Mode: Scan Range: Scan Rate: Instrument

8.08

9.08

10.08

11.08

12.08

13.08

Rxi®-XLB, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13723) SV calibration mix #5 / 610 PAH mix (cat.# 31011) Benzo(e)pyrene (cat.# custom) Triphenylene (cat.# custom) 2-Methylnaphthalene (cat.# 31285) 2-Methylfluoranthene (cat.# custom) PCB congener standard #2 (cat.# 32294) PCB 31 (cat.# custom) Dichloromethane 0.5 μL splitless (hold 1.75 min) 2.0 mm ID straight inlet liner w/wool (cat.# 21718) 300 °C 50 mL/min 40 °C (hold 2 min) to 240 °C at 30 °C/min (hold 2 min) to 340 °C at 10 °C/min (hold 5 min) He, constant flow 1 mL/min MS Scan 300 °C Quadrupole 280 °C 70 eV 4 min manual EI 45-550 amu 5 scans/sec PE Clarus 500 GC & Clarus 500 MS

596 www.restek.com

16.08

17.08

18.08

Peaks 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29.

Naphthalene 2-Methylnaphthalene Acenaphthylene Acenaphthene Fluorene Phenanthrene Anthracene PCB 31 PCB 28 PCB 52 Fluoranthene PCB 101 Pyrene 2-Methylfluoranthene PCB 118 PCB 153 PCB 138 PCB 180 Benzo[a]anthracene Chrysene Triphenylene PCB 194 Benzo[b]fluoranthene Benzo[k]fluoranthene Benzo[e]pyrene Benzo[a]pyrene Dibenzo[a,h]anthracene Indeno[1,2,3-cd]pyrene Benzo[g,h,i]perylene

19.08

Conc. (μg/mL) 5 5 5 5 5 5 5 1 1 1 5 1 5 5 1 1 1 1 5 5 5 1 5 5 5 5 5 5 5

20.08

21.08

22.08 GC_EV1223


GC CHROMATOGRAMS | ENVIRONMENTAL

PCB Mixtures EU PCB Congeners on Rxi®-XLB Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

NEW!

PCB 31 & 28 1

2

2 1

1. 2. 3. 4. 5. 6. 7. 8. 9.

3

Peaks PCB 31 PCB 28 PCB 52 PCB 101 PCB 118 PCB 153 PCB 138 PCB 180 PCB 194

4 6 9.90 9.95 10.00 10.05 10.10 10.15 10.20 10.25 10.30

5 7

8 9

9.35

9.85

10.35

10.85

11.35

11.85

12.35

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Detector Mode: Transfer Line Temp.: Analyzer Type: Source Temp.: Electron Energy: Ionization Mode: Scan Range: Scan Rate: Instrument

12.85

13.35 Time (min)

13.85

14.35

14.85

15.35

15.85

16.35

16.85

17.35

GC_EV1240

Rxi®-XLB, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13723) PCB congener standard #2 (cat.# 32294) PCB 31 (cat.# custom) Dichloromethane 3.5 ppm 0.5 μL splitless (hold 1.75 min) 2.0 mm ID straight inlet liner w/wool (cat.# 21718) 300 °C 50 mL/min 40 °C (hold 2 min) to 240 °C at 30 °C/min (hold 2 min) to 340 °C at 10 °C/min (hold 5 min) He, constant flow 1 mL/min MS Scan 300 °C Quadrupole 280 °C 70 eV EI 45-550 amu 5 scans/sec PE Clarus 500 GC & Clarus 500 MS

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597


GC CHROMATOGRAMS | ENVIRONMENTAL

PCB Mixtures Aroclor PCBs on Rtx®-CLPesticides Rtx®-CLPesticides 30 m, 0.32 mm ID, 0.32 μm (cat.# 11141)

Peaks 1. Decachlorobiphenyl (DCB)

Seven EPA Methods on One Column Pair using a μ-ECD www.restek.com/RtxCLP7

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Pulse Pressure: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

598 www.restek.com

Rtx®-CLPesticides, 30 m, 0.32 mm ID, 0.32 μm (cat.# 11141) PCB kit #1 diluted to 1,000 ppb in hexane (cat.# 32089) Decachlorobiphenyl (BZ #209) diluted to 100 ppb in acetone (cat.# 32029) 1.0 μL pulsed splitless (hold 0.3 min) Cyclo double taper (4 mm) (cat.# 20895) 250 °C 30 psi (206.8 kPa) 120 °C to 200 °C at 45 °C/min to 230 °C at 15 °C/min to 330 °C at 30 °C/min (hold 2 min) He, constant flow 60 cm/sec μ-ECD @ 330 °C This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.


GC CHROMATOGRAMS | ENVIRONMENTAL

PCB Mixtures Aroclor PCBs on Rtx®-CLPesticides2 Rtx®-CLPesticides2 30 m, 0.32 mm ID, 0.25 μm (cat.# 11324)

Peaks 1. Decachlorobiphenyl (DCB)

Sample throughput can be significantly improved by using Rtx®-CLPesticides & Rtx®-CLPesticides2 columns. www.restek.com/RtxCLP7

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Pulse Pressure: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rtx®-CLPesticides2, 30 m, 0.32 mm ID, 0.25 μm (cat.# 11324) PCB kit #1 diluted to 1,000 ppb in hexane (cat.# 32089) Decachlorobiphenyl (BZ #209) diluted to 100 ppb in acetone (cat.# 32029) 1.0 μL pulsed splitless (hold 0.3 min) Cyclo double taper (4 mm) (cat.# 20895) 250 °C 30 psi (206.8 kPa) 120 °C to 200 °C at 45 °C/min to 230 °C at 15 °C/min to 330 °C at 30 °C/min (hold 2 min) He, constant flow 60 cm/sec μ-ECD @ 330 °C This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

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599


GC CHROMATOGRAMS | ENVIRONMENTAL

PCB Mixtures Aroclor 1242/1254/1262 PCBs on Rtx®-PCB

restek innovation! The Rtx®-PCB column offers excellent resolution for PCB congeners.

GC_EV00768

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

600 www.restek.com

Rtx®-PCB, 40 m, 0.18 mm ID, 0.18 μm (cat.# 41303) Aroclor 1242 (cat.# 32009) Aroclor 1254 (cat.# 32011) Aroclor 1262 (cat.# 32409) Hexane 300 ng/mL 1.0 μL splitless (hold 0.75 min) Recessed taper (4 mm) (cat.# 20983) 230 °C 100 °C (hold 1 min) to 200 °C at 30 °C/min to 320 °C at 2 °C/min (hold 1 min) H2, constant pressure 40 cm/sec @ 100 °C ECD @ 330 °C


GC CHROMATOGRAMS | ENVIRONMENTAL

PCB Mixtures Aroclor 1242 PCBs on Rtx®-PCB

GC_EV00752 Column Sample Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rtx®-PCB, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13223) Aroclor 1242 (cat.# 32009) 200 ng/mL 1.0 μL splitless (hold 0.75 min) 3.5 mm ID single taper inlet liner (cat.# 20962) 250 °C 100 °C (hold 1.0 min) to 300 °C at 10 °C/min (hold 4 min) H2, constant pressure 71 cm/sec @ 110 °C ECD @ 310 °C

Aroclor 1254 PCBs on Rtx®-PCB

GC_EV00753 Column Sample Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rtx®-PCB, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13223) Aroclor 1254 (cat.# 32011) 200 ng/mL 1.0 μL splitless (hold 0.75 min) 3.5 mm ID single taper inlet liner (cat.# 20962) 250 °C 100 °C (hold 1.0 min) to 300 °C at 10 °C/min (hold 4 min) H2, constant pressure 71 cm/sec @ 110 °C ECD @ 310 °C

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601


GC CHROMATOGRAMS | ENVIRONMENTAL

PCB Mixtures Aroclor 1260 PCBs on Rtx®-PCB

GC_EV00754 Column Sample Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rtx®-PCB, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13223) Aroclor 1260 (cat.# 32012) 200 ng/mL 1.0 μL splitless (hold 0.75 min) 3.5 mm ID single taper inlet liner (cat.# 20962) 250 °C 100 °C (hold 1.0 min) to 300 °C at 10 °C/min (hold 4 min) H2, constant pressure 71 cm/sec @ 110 °C ECD @ 310 °C

Aroclor PCBs on Rtx®-PCB European indicator PCB congeners resolved from other congeners when using GC-MS.

101 52

Column Sample

153

180

28

Conc.: Injection Inj. Vol.: Liner:

118

138

Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector Mode: Transfer Line Temp.: Ionization Mode: Scan Range:

Rtx®-PCB, 60 m, 0.25 mm ID, 0.25 μm (cat.# 13226) Aroclor 1242 (cat.# 32009) Aroclor 1254 (cat.# 32011) Aroclor 1262 (cat.# 32409) 333 ppm each 1.0 μL splitless (hold 0.75 min) Splitless taper (4 mm) w/wool (cat.# 22405) 280 °C 100 °C (hold 1 min) to 200 °C at 30 °C/ min to 320 °C at 2 °C/min (hold 1 min) He, constant flow 1.1 mL/min MS Scan 280 °C EI 50-550 amu

6.00 8.00 10.00 12.00 14.00 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 52.00 54.00 56.00 58.00 60.00 62.00 64.00 Time (min) GC_EV00767

602 www.restek.com


GC CHROMATOGRAMS | ENVIRONMENTAL

PCBs and Brominated Flame Retardants PCBs and BFRs on Rxi®-XLB and Rxi®-17Sil MS (GCxGC)

NEW!

GC_EV1237

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Modulation Modulator Temp. Offset: Second Dimension Separation Time: Hot Pulse Time: Cool Time between Stages: Detector Data Rate: Instrument Notes

Rxi®-XLB 30 m, 0.25 mm ID, 0.25 μm (cat.# 13723) Rxi®-17Sil MS 1 m, 0.15 mm ID, 0.15 μm (cat.# 43820) with IP deactivated guard column 0.2 m, 0.15 mm ID PBDE mix (cat.# 33098) PCB congener mix, method 8082A (cat.# 32416) Isooctane 250 pg/μL 1.0 μL splitless (hold 1.0 min) Sky® 4 mm single taper w/wool (cat.# 23303.5) 250 °C 20 mL/min Rxi®-XLB: 80 °C (hold 1 min) to 120 °C at 10 °C/min to 300 °C at 3 °C/min Rxi®-17Sil MS: 85 °C (hold 1 min) to 125 °C at 10 °C/min to 305 °C at 3 °C/min He, corrected constant flow (2.0 mL/min) 20 °C 3.5 sec 1.25 sec 0.50 sec μ-ECD @ 325 °C 50 Hz Agilent/HP6890 GC The Rxi®-17Sil MS column (cat.# 43820) is a 10 m column. A 1 m section was used as a second dimension column. Guard column was connected using a Siltek®-treated universal Press-Tight® connector (cat.# 20480).

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603


GC CHROMATOGRAMS | ENVIRONMENTAL

PCBs and Brominated Flame Retardants PCBs and BFRs on Rxi®-XLB and Rxi®-17Sil MS (GCxGC)

NEW!

GC_EV1238 Column Sample Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Modulation Modulator Temp. Offset: Second Dimension Separation Time: Hot Pulse Time: Cool Time between Stages: Detector Data Rate: Instrument Notes

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Rxi®-XLB 30 m, 0.25 mm ID, 0.25 μm (cat.# 13723) Rxi®-17Sil MS 1 m, 0.15 mm ID, 0.15 μm (cat.# 43820) with IP deactivated guard column 0.2 m, 0.15 mm ID Wellington BFR-PAR mix Aroclor Isooctane 1.0 μL splitless (hold 1.0 min) Sky® 4 mm single taper w/wool (cat.# 23303.5) 250 °C 20 mL/min Rxi®-XLB: 80 °C (hold 1 min) to 120 °C at 10 °C/min to 300 °C at 3 °C/min Rxi®-17Sil MS: 85 °C (hold 1 min) to 125 °C at 10 °C/min to 305 °C at 3 °C/min He, corrected constant flow (2.0 mL/min) 20 °C 3.5 sec 1.25 sec 0.50 sec μ-ECD @ 325 °C 50 Hz Agilent/HP6890 GC The Rxi®-17Sil MS column (cat.# 43820) is a 10 m column. A 1 m section was used as a second dimension column. Guard column was connected using a Siltek®-treated universal Press-Tight® connector (cat.# 20480).


GC CHROMATOGRAMS | ENVIRONMENTAL

Pesticides Organochlorine Pesticides on Rtx®-CLPesticides and Rtx®-CLPesticides2 by EPA Method 504.1 (Dual Column Analysis) 1. 2. 3. 4. 5. 6. 7.

Peaks Bromodichloromethane Chlorodibromomethane 1,2-Dibromoethane (EDB) 1,1,1,2-Tetrachloroethane Bromoform 1,2,3-Trichloropropane 1,2-Dibromo-3-chloropropane (DBCP)

CLP tR (min) 2.504 3.239 3.531 3.910 3.935 4.655 5.480

CLP2 tR (min) 2.866 3.740 3.899 4.166 4.505 4.833 5.850

NEW!

Rtx®-CLPesticides

Rtx®-CLPesticides2

GC_EV1227 Columns

Sample

Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: Instrument Notes

Rtx®-CLPesticides2 30 m, 0.32 mm ID, 0.25 μm (cat.# 11324) and Rtx®-CLPesticides 30 m, 0.32 mm ID, 0.32 μm (cat.# 11141) using Rxi® guard column 5 m, 0.32 mm ID (cat.# 10039) with Universal “Y” Press-Tight® connector (cat.# 20405) Dibromochloromethane (chlorodibromochloromethane) (cat.# 30271) Bromodichloromethane (cat.# 30251) 504.1 calibration mix (cat.# 30239) 1,1,1,2-tetrachloroethane (cat.# 30411) Bromoform (cat.# 30252) n-Hexane 10 ng/mL 2 μL splitless (hold 0.50 min) Sky® 4 mm single taper inlet liner w/wool (cat.# 23303.1) 200 °C 50 mL/min 30 °C (hold 2.0 min) to 220 °C at 30 °C/min He, constant flow 5.0 mL/min 60 cm/sec μ-ECD @ 220 °C 50 mL/min He 50 Hz Agilent/HP6890 GC This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual-columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

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605


GC CHROMATOGRAMS | ENVIRONMENTAL

Pesticides Organochlorine Pesticide Mix AB #2 on Rtx®-CLPesticides and Rtx®-CLPesticides2 (0.53 mm ID column set) Rtx®-CLPesticides

Rtx®-CLPesticides2

0.53 mm ID column analysis performed in less than 9 min.

GC_EV00936 Columns

Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

GC_EV00937

Rtx®-CLPesticides 30 m, 0.53 mm ID, 0.50 μm (cat.# 11140) and Rtx®-CLPesticides2 30 m, 0.53 mm ID, 0.42 μm (cat.# 11340) using Rxi® guard column 5 m, 0.53 mm ID (cat.# 10054) with Siltek® treated universal “Y” Press-Tight® connector (cat.# 20486) Organochlorine pesticide mix AB #2 (8-80 μg/mL in hexane/toluene) (cat.# 32292) Pesticide surrogate mix, EPA 8080, 8081 (200 μg/mL in acetone) (cat.# 32000) 1.0 μL splitless (hold 0.3 min) Splitless taper (4 mm) (cat.# 20799) 250 °C 120 °C to 200 °C at 45 °C/min to 230 °C at 12.5 °C/min to 325 °C at 30 °C/min (hold 2 min) He, constant linear velocity 45 cm/sec @ 120 °C μ-ECD @ 330 °C This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

Peaks 2,4,5,6-Tetrachloro-m-xylene (SS) -BHC -BHC -BHC -BHC Heptachlor Aldrin Heptachlor epoxide (isomer B) -Chlordane -Chlordane Endosulfan I

12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

4,4'-DDE Dieldrin Endrin 4,4'-DDD Endosulfan II 4,4'-DDT Endrin aldehyde Endosulfan sulfate Methoxychlor Endrin ketone Decachlorobiphenyl (SS)

Organochlorine Pesticide Mix AB #2 on Rtx®-CLPesticides and Rtx®-CLPesticides2 (0.32 mm ID column set) Rtx®-CLPesticides

Rtx®-CLPesticides2

0.32 mm ID column analysis performed in less than 7 min.

GC_EV00933A

GC_EV00933 Columns

Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Detector Notes

Rtx®-CLPesticides 30 m, 0.32 mm ID, 0.32 μm (cat.# 11141) and Rtx®-CLPesticides2 30 m, 0.32 mm ID, 0.25 μm (cat.# 11324) using Rxi® guard column 5 m, 0.32 mm ID (cat.# 10039) with deactivated universal “Y” Press-Tight® connector (cat.# 20405-261) Organochlorine pesticide mix AB #2 (cat.# 32292) Pesticide surrogate mix, EPA 8080, 8081 (cat.# 32000) 1 μL splitless (hold 0.3 min) Splitless taper (4 mm) (cat.# 20799) 250 °C 120 °C to 200 °C at 45 °C/min to 230 °C at 15 °C/min to 330 °C at 30 °C/min (hold 2 min) He μ-ECD @ 330 °C Instrument was operated in constant flow mode. Linear velocity: 60 cm/sec @ 120 °C. This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual-columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

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1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

Peaks 2,4,5,6-Tetrachloro-m-xylene (SS) -BHC -BHC -BHC -BHC Heptachlor Aldrin Heptachlor epoxide (isomer B) trans-Chlordane cis-Chlordane Endosulfan I

12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

4,4'-DDE Dieldrin Endrin 4,4'-DDD Endosulfan II 4,4'-DDT Endrin aldehyde Endosulfan sulfate Methoxychlor Endrin ketone Decachlorobiphenyl (SS)


GC CHROMATOGRAMS | ENVIRONMENTAL

Pesticides Organochlorine Pesticide Mix AB #2 on Rtx®-CLPesticides and Rtx®-CLPesticides2 (0.25 mm ID column set) Rtx®-CLPesticides

Rtx®-CLPesticides2

GC_EV00940 Columns

Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

GC_EV00941

Rtx®-CLPesticides 30 m, 0.25 mm ID, 0.25 μm (cat.# 11123) and Rtx®-CLPesticides2 30 m, 0.25 mm ID, 0.20 μm (cat.# 11323) using Rxi® guard column 5 m, 0.25 mm ID (cat.# 10029) with Siltek® treated universal “Y” Press-Tight® connector (cat.# 20486) Organochlorine pesticide mix AB #2, 8–80 μg/mL each component in hexane/toluene (cat.# 32292) Pesticide surrogate mix, EPA 8080, 8081 pesticide surrogate mix, 200 μg/mL each component in acetone (cat.# 32000) 0.5 μL splitless (hold 0.5 min) Cyclo double taper (2 mm) (cat.# 20908) 250 °C 125 °C to 200 °C at 45 °C/min to 230 °C at 12.5 °C/min to 330 °C at 30 °C/min (hold 2 min) He, constant linear velocity 41 cm/sec @ 125 °C ECD @ 330 °C This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

Peaks 2,4,5,6-Tetrachloro-mxylene (SS) -BHC -BHC -BHC -BHC Heptachlor Aldrin Heptachlor epoxide (isomer B) -Chlordane -Chlordane

11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

Endosulfan I 4,4'-DDE Dieldrin Endrin 4,4'-DDD Endosulfan II 4,4'-DDT Endrin aldehyde Endosulfan sulfate Methoxychlor Endrin ketone decachlorobiphenyl (SS)

Organochlorine Pesticides on Rtx®-CLPesticides Columns (0.18 mm ID column set) Rtx®-CLPesticides

Rtx®-CLPesticides2

Dual column analysis in less than 8 minutes!

Columns

Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Instrument Notes

GC_EV00892 Rtx®-CLPesticides 20 m, 0.18 mm ID, 0.18 μm (cat.# 42102) and Rtx®-CLPesticides2 20 m, 0.18 mm ID, 0.14 μm (cat.# 42302) using IP deactivated guard column 5 m, 0.53 mm ID (cat.# 10045) with SeCure® “Y” connector kit with universal “Y” Press-Tight® connector (cat.# 20276) Organochlorine pesticide mix AB #2 (cat.# 32292) Pesticide surrogate mix, EPA 8080, 8081 (cat.# 32000) 0.5 μL splitless (hold 0.75 min) Splitless taper (2 mm) (cat.# 20796) 250 °C 140 °C (hold 1 min) to 250 °C at 35 °C/min (hold 1 min) to 330 °C at 35 °C/min (hold 3 min) He, constant linear velocity 20 cm/sec @ 140 °C μ-ECD @ 350 °C Agilent/HP6890 GC cat.# 32292 = 8-80 μg/mL each component in hexane/toluene cat.# 32000 = 200 μg/mL each component in acetone

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

Peaks 2,4,5,6-Tetrachloro-m-xylene (SS) -BHC -BHC -BHC -BHC Heptachlor Aldrin Heptachlor epoxide -Chlordane -Chlordane Endosulfan I

12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

GC_EV00893 4,4'-DDE Dieldrin Endrin 4,4'-DDD Endosulfan II 4,4'-DDT Endrin aldehyde Endosulfan sulfate Methoxychlor Endrin ketone Decachlorobiphenyl (SS)

This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

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607


GC CHROMATOGRAMS | ENVIRONMENTAL

Pesticides Organochlorine Pesticides by EPA Method 8081B on Rtx®-CLPesticides/Rtx®-CLPesticides2 (extended list)

NEW!

Rtx®-CLPesticides

Rtx®-CLPesticides2

GC_EV1193 Columns

Sample

Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Instrument Notes

Rtx®-CLPesticides2 30 m, 0.32 mm ID, 0.25 μm (cat.# 11324) and Rtx®-CLPesticides 30 m, 0.32 mm ID, 0.32 μm (cat.# 11141) using Rxi® guard column 5 m, 0.32 mm ID (cat.# 10039) with deactivated universal “Y” Press-Tight® connector (cat.# 20405-261) Organochlorine pesticide mix AB #2 (cat.# 32292) Organochlorine pesticide mix C #1 (cat.# 32296) 2,4,5,6-Tetrachloro-m-xylene (cat.# 32027) Decachlorobiphenyl (BZ #209) (cat.# 32029) Chlorpyrifos (cat.# 32212) 2,4'-DDE (cat.# 32099) 2,4'-DDD (cat.# 32098) Chlorobenzilate (cat.# 32211) Captan (cat.# custom) cis-Nonachlor (cat.# custom) Mirex (cat.# custom) Oxychlordone (cat.# custom) Diallate (cat.# custom) Hexane 1 μL splitless (hold 0.3 min) Cyclo double taper (4 mm) (cat.# 20896) 250 °C 80 °C to 175 °C at 8 °C/min to 195 °C at 11 °C/min to 235 °C at 7 °C/min to 320 °C at 25 °C/min (hold 3 min) He, constant flow 28 cm/sec μ-ECD @ 330 °C 60 mL/min N2 Agilent/HP6890 GC This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

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Conc. (ng/mL) 1. 1,2-Dibromo-3-chloropropane 100 2. Hexachlorocyclopentadiene 100 3. Tetrachloro-m-xylene (SS) 100 4. cis-Diallate 500 5. Hexachlorobenzene 100 6. trans-Diallate 500 7. -BHC 40 8. -BHC 40 9. -BHC 40 10. -BHC 40 11. Heptachlor 40 12. Aldrin 40 13. Chlorpyrifos 100 14. Isodrin 100 15. Oxychlordane 50 16. Heptachlor epoxide 40 17. -Chlordane 40 18. 2,4'-DDE 100 19. trans-Nonachlor 100

Peaks

Peaks

20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

-Chlordane Endosulfan I Captan 4,4'-DDE Dieldrin 2,4'-DDD Endrin Chlorobenzilate 2,4'-DDT cis-Nonachlor 4,4'-DDD Endosulfan II 4,4'-DDT Endrin aldehyde Endosulfan sulfate Methoxychlor Mirex Endrin ketone Decachlorobiphenyl

Conc. (ng/mL) 40 40 100 100 80 100 80 500 100 100 80 80 80 80 80 400 100 80 100


GC CHROMATOGRAMS | ENVIRONMENTAL

Pesticides Pesticides of U.S. EPA Method 505 on Rtx®-CLPesticides and Rtx®-CLPesticides2 Rtx®-CLPesticides

GC_EV01004

Rtx®-CLPesticides2

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.

Peaks Hexachlorocyclopentadiene Hexachlorobenzene Simazine Atrazine -BHC Heptachlor Alachlor Aldrin Heptachlor epoxide -Chlordane trans-Nonachlor -Chlordane Dieldrin Endrin cis-Nonachlor Methoxychlor

GC_EV01005 Columns

Sample Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Instrument Notes

Rtx®-CLPesticides 30 m, 0.32 mm ID, 0.32 μm (cat.# 11141) and Rtx®-CLPesticides2 30 m, 0.32 mm ID, 0.25 μm (cat.# 11324) using Rxi® guard column 5 m, 0.32 mm ID (cat.# 10039) with deactivated universal “Y” Press-Tight® connector (cat.# 20405-261) 200 ng/mL 505 organohalide pesticide mix (cat.# 32024) 4.2 μg/mL simazine (cat.# 32236) 4.2 μg/mL atrazine (cat.# 32208) Methanol 2 μL splitless (hold 0.75 min) Cyclo double taper (4 mm) (cat.# 20896) 250 °C 90 °C (hold 1 min) to 310 °C at 10 °C/min (hold 5 min) He, constant flow 40 cm/sec μ-ECD @ 325 °C Agilent/HP6890 GC This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

7 EPA Methods on 1 Column Pair! Analyze Pesticides, PCBs, Herbicides, and More on a Single Rtx®-CLPesticides Column Set

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609


GC CHROMATOGRAMS | ENVIRONMENTAL

Pesticides, Herbicides Pesticides & Herbicides US EPA Method 508.1 on Rtx®-CLPesticides & Rtx®-CLPesticides2

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

Rtx®-CLPesticides

GC_EV01022

Rtx®-CLPesticides2

Columns

Sample

Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Peaks Hexachlorocyclopentadiene Etridiazole Chlorneb Propachlor Trifluralin Hexachlorobenzene -BHC Simazine Atrazine Pentachloronitrobenzene (IS) -BHC -BHC -BHC Heptachlor Chlorothalonil Metribuzin Alachlor Aldrin 4,4'-Dibromobiphenyl (SS) Metachlor DCPA Heptachlor epoxide -Chlordane Cyanazine -Chlordane Endosulfan I 4,4'-DDE Dieldrin Endrin Chlorobenzilate 4,4'-DDD Endosulfan II 4,4'-DDT Endrin aldehyde Endosulfan sulfate Methoxychlor cis-Permethrin trans-Permethrin

Rtx®-CLPesticides2 30 m, 0.32 mm ID, 0.25 μm (cat.# 11324) and Rtx®-CLPesticides 30 m, 0.32 mm ID, 0.32 μm (cat.# 11141) using Rxi® guard column 5 m, 0.32 mm ID (cat.# 10039) with deactivated universal “Y” Press-Tight® connector (cat.# 20405-261) 50 ng/mL 508.1 calibration mix #1 (cat.# 32094) 100 ng/mL 508.1 calibration mix #2 (cat.# 32095) 100 ng/mL 508.1 calibration mix #3 (cat.# 32096) 50 ng/mL pentachloronitrobenzene (cat.# 32091) 250 ng/mL 4,4'-dibromobiphenyl (cat.# 32092) 500 ng/mL atrazine (cat.# 32208) 500 ng/mL simazine (cat.# 32236) Ethyl acetate 2 μL splitless (hold 0.75 min) Cyclo double taper (4 mm) (cat.# 20896) 250 °C 80 °C (hold 0.5 min) to 155 °C at 19 °C/min (hold 1 min) to 210 °C at 4 °C/min to 310 °C at 25 °C/min (hold 0.5 min) He, constant flow 26 cm/sec μ-ECD @ 325 °C This chromatogram was obtained using an Agilent μ-ECD. To obtain comparable results, you will need to employ a μ-ECD in addition to confirmational dual columns connected to a 5-meter guard column using a “Y” Press-Tight® connector.

GC_EV01023

For specifications and a competitive column comparison, go to

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GC CHROMATOGRAMS | ENVIRONMENTAL

Pesticides Organophosphorous Pesticides U.S. EPA Method 8141A on Rtx®-OPPesticides & Rtx®-OPPesticides2 Rtx®-OPPesticides 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 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.

Rtx®-OPPesticides2

Columns

Sample

Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Dead Time: Detector Notes

Peaks Dichlorvos Hexamethylphosphoramide Mevinphos Trichlorfon TEPP Demeton-O Tributyl phosphate (SS) Thionazin Ethoprop Naled Sulfotepp Phorate Dicrotophos Monocrotophos Demeton-S Terbufos Dimethoate Diazinon Dioxathion Fonophos Disulfoton Phosphamidon isomer (breakdown product) Dichlorofenthion Phosphamidon Chlorpyrifos methyl Methyl parathion Ronnel Aspon Fenitrothion Malathion Chlorpyrifos Trichloronate Parathion-ethyl Fenthion Merphos Chlorfenvinphos Crotoxyphos Stirofos Tokuthion Merphos oxone (breakdown product) Ethion Fensulfothion Bolstar Carbophenothion Famphur Triphenyl phosphate (SS) EPN Phosmet Leptophos Tri-o-cresyl phosphate Azinphos-methyl Azinphos-ethyl Coumaphos Rtx®-OPPesticides 30 m, 0.32 mm ID, 0.50 μm (cat.# 11239) and Rtx®-OPPesticides2 30 m, 0.32 mm ID, 0.32 μm (cat.# 11241) Triphenylphosphate (cat.# 32281) Tributylphosphate (cat.# 32280) 8140/8141 OP pesticide calibration mix A (cat.# 32277) 8141 OP pesticide calibration mix B (cat.# 32278) 100 ng/mL 1 μL splitless (hold 1 min) Siltek® splitless taper (4 mm) (cat.# 20798-214.1) 200 °C 80 °C (hold 0.5 min) to 280 °C at 12 °C/min (hold 10 min) He 1.03 min @ 80 °C FPD @ 250 °C Constant pressure

GC_EV00394

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611


GC CHROMATOGRAMS | ENVIRONMENTAL

Semivolatiles Nitrosamines in Drinking Water on Rxi®-624Sil MS by Modified EPA Method 521 Utilizing CSR-LVSI 1 5 1. 2. 3. 4. 5. 6. 7. 8. 9.

4 2

3

Peaks N-Nitrosodimethylamine-d6 N-Nitrosodimethylamine N-Nitrosomethylethylamine N-Nitrosodiethylamine N-Nitrosodipropylamine-d14 N-Nitrosodipropylamine N-Nitrosopyrrolidine N-Nitrosopiperidine N-Nitrosodibutylamine

NEW! 6

8 7 9

7. 00

8 . 00

9 .0 0

10 .0 0

11.00

12.00

1 3. 0 0

14 . 0 0

15.00 T im e ( m i n ) GC_EV1286

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Detector SIM Program:

Rxi®-624Sil MS, 30 m, 0.25 mm ID, 1.40 μm (cat.# 13868) using Rxi® guard column 5 m, 0.25 mm ID (cat.# 10029) with universal Press-Tight® connectors (cat.# 20429) N-Nitrosodimethylamine-d6 (cat.# 33910) N-Nitrosodi-n-propylamine-d14 (cat.# 33911) Nitrosamine calibration mix, method 521 (cat.# 31898) Dichloromethane 10 ng/mL 10 μL splitless (hold 1 min) Sky® 4 mm single taper w/wool (cat.# 23303.5) 250 °C 80 mL/min

38 °C (hold 1 min) to 160 °C at 12 °C/min to 200 °C at 5 °C/min (hold 1 min) He, constant flow 1.4 mL/min Agilent 5975C Start Time Group (min) Ion(s) (m/z) Dwell (ms) 1 6.9 80, 74, 46, 43, 42 23 2 7.9 88, 56, 43, 42 30 3 8.9 102, 56, 44, 42 30 4 10 130, 78, 70, 58, 46, 43, 42 15 5 12.05 100, 68, 42, 41 30 6 14.5 158, 116, 84, 57, 41 23 Transfer Line Temp.: 280 °C Analyzer Type: Quadrupole Source Temp.: 230 °C Quad Temp.: 150 °C Solvent Delay Time: 6.9 min Tune Type: BFB Ionization Mode: EI Instrument Agilent 7890A GC & 5975C MSD

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GC CHROMATOGRAMS | ENVIRONMENTAL

Semivolatiles Polycyclic Aromatic Hydrocarbons on Rxi®-5Sil MS

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

Peaks Naphthalene 2-Methylnaphthalene 1-Methylnaphthalene 2-Fluorobiphenyl (SS) Acenaphthylene Acenaphthene Fluorene Phenanthrene Anthracene Fluoranthene Pyrene p-Terphenyl-d14 (IS) Benzo[a]anthracene Chrysene Benzo[b]fluoranthene Benzo[k]fluoranthene Benzo[a]pyrene Perylene-d12 (IS) Indeno[1,2,3-cd]pyrene Dibenzo[a,h]anthracene Benzo[ghi]perylene

tR (min) 4.93 5.58 5.68 5.93 6.45 6.62 7.12 8.06 8.11 9.23 9.45 9.61 10.65 10.69 11.96 12.00 12.42 12.51 14.19 14.23 14.65

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Outstanding response at 5 pg on-column!

GC_EV00970 Column Sample

Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Pulse Pressure: Pulse Time: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Detector Mode: SIM Program:

Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) PAH mix, 1 μL of 0.005 μg/mL (IS 2 μg/mL) SV Calibration mix #5 / 610 PAH Mix (cat.# 31011) 1-Methylnaphthalene (cat.# 31283) 2-Methylnaphthalene (cat.# 31285) 2-Fluorobiphenyl (cat.# 31091) 5 pg on-column 1.0 μL pulsed splitless (hold 0.15 min) Drilled Uniliner® (hole near top) w/wool (cat.# 21055-200.5) 300 °C 20 psi (137.9 kPa) 0.2 min 60 mL/min 50 °C (hold 0.5 min) to 290 °C at 25 °C/min to 320 °C at 5 °C/min He, constant flow 1.4 mL/min MS SIM Start Time Group (min) Ion(s) Dwell (ms) 1 128 m/z 100 2 142 m/z 100 3 172 m/z 100 4 152 m/z 100 5 166 m/z 100 6 178 m/z 100 7 202,244 m/z 100 8 228 m/z 100 9 252,264 m/z 100 10 276,278 m/z 100

Transfer Line Temp.: 290 °C Ionization Mode: EI

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613


GC CHROMATOGRAMS | ENVIRONMENTAL

Semivolatiles Polycyclic Aromatic Hydrocarbons on Rxi®-17Sil MS 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27.

Peaks Naphthalene 2-Methylnaphthalene 1-Methylnaphthalene Acenaphthylene Acenaphthene Fluorene Phenanthrene Anthracene Fluoranthene Pyrene Benz[a]anthracene Chrysene Triphenylene

Benzo[b]fluoranthene Benzo[k]fluoranthene Benzo[j]fluoranthene Benzo[a]pyrene 3-Methylcholanthrene Dibenz[a,h]acridine Dibenz[a,j]acridine Indeno[1,2,3-cd]pyrene Dibenz[a,h]anthracene Benzo[ghi]perylene 7H-Dibenzo[c,g]carbazole Dibenzo[a,e]pyrene Dibenzo[a,i]pyrene Dibenzo[a,h]pyrene

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Excellent resolution and peak shape for PAHs that cannot be resolved by MS. 7 8 16

6 45 2

14 15

3 1

11.8 12.0 12.2 12.4 26.2 26.4 26.6 26.8 27.0 27.2 27.4 27.6 27.8 28.0 28.2 28.4 9 10 12,13 21,22

11 17 18

23 24

20 19

25

26 27

5

10

15

Column Sample

20

25

30

Rxi®-17Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 14123) PAH supplement mix for method 8100 (cat.# 31857) EPA Method 8310 PAH mixture (cat.# 31841) triphenylene (custom) Dichloromethane 10 ppm

35

Diluent: Conc.: Injection Inj. Vol.: 0.5 μL splitless (hold 1.75 min) Liner: Auto SYS XL PSS split/splitless w/wool (cat.# 21718) Inj. Temp.: 320 °C Purge Flow: 75 mL/min Oven Oven Temp: 65 °C (hold 0.5 min) to 220 °C at 15 °C/min to 330 °C at 4 °C/min (hold 15 min) Carrier Gas He, constant flow Flow Rate: 2.0 mL/min Detector FID @ 320 °C Instrument PE Clarus 600 GC Acknowledgement Instrument provided by PerkinElmer

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40

Time (min) GC_EV1160


GC CHROMATOGRAMS | ENVIRONMENTAL

Semivolatiles Polycyclic Aromatic Hydrocarbons on Rxi®-17Sil MS (15 m x 0.25 mm x 0.25 μm) Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15 16. 17. 18. 19. 20.

Peaks Naphthalene 2-Methylnaphthalene 1-Methylnaphthalene Acenaphthylene Acenaphthene Fluorene Phenanthrene Anthracene Fluoranthene Pyrene Benzo[a]anthracene Chrysene Triphenylene Benzo[b]fluoranthene Benzo[k]fluoranthene Benzo[j]fluoranthene Benzo[a]pyrene Indeno[1,2,3-cd]pyrene Dibenz[a,h]anthracene Benzo[ghi]perylene

GC_EV1186

Benzofluoranthenes on Rxi®-17Sil MS (15 m x 0.25 mm x 0.25 μm)

GC_EV1189

Phenanthrene and Anthracene on Rxi®-17Sil MS (15 m x 0.25 mm x 0.25 μm)

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Flow Rate: Detector Constant Column + Constant Make-up: Make-up Gas Type: Data Rate: Instrument

Rxi®-17Sil MS, 15 m, 0.25 mm ID, 0.25 μm (cat.# 14120) Methylene chloride 20 ng/μL 1 μL split (split ratio 20:1) 4 mm split Precision® liner w/wool (cat.# 21022) 275 °C 42 mL/min 80 °C (hold 1 min) to 320 °C at 15 °C/min (hold 2 min) H2, constant flow 2 mL/min FID @ 340 °C 50 mL/min N2 20 Hz Agilent/HP6890 GC

GC_EV1188

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615


GC CHROMATOGRAMS | ENVIRONMENTAL

Semivolatiles EPA 522 Analyte Mix on Rxi®-624Sil MS (30 m x 0.25 mm x 1.4 μm) Column

NEW!

Sample

Peaks 1. Tetrahydrofuran-D8 2. 1,4-Dioxane-d8 3. 1,4-Dioxane

1

tR (min) 5.27 6.19 6.23

2 3

Rxi® Technology!

Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Mode: SIM Program:

Transfer Line Temp.: Analyzer Type: Source Temp.: Quad Temp.: Solvent Delay Time: Tune Type: Ionization Mode: Instrument Notes

Exceptionally inert, ultra low-bleed capillary columns.

Rxi®-624Sil MS, 30 m, 0.25 mm ID, 1.40 μm (cat.# 13868) using Rxi® guard column 5 m, 0.25 mm ID (cat.# 10029) with universal angled Press-Tight® connectors (cat.# 20446-261) Tetrahydrofuran-d8 (cat.# 30112) 1,4-Dioxane-d8 (cat.# 30614) 1,4-Dioxane (cat.# 30287) Dichloromethane 50 ng/mL 10 μL splitless (hold 1 min) Sky® 4 mm single taper w/wool (cat.# 23303.5) 120 °C 80 mL/min 35 °C (hold 1 min) to 120 °C at 12 °C/min (hold 1 min) He, constant flow 1.4 mL/min 30.556 cm/sec @ 35 °C MS SIM Start Time Group (min) Ion(s) Dwell (ms) 1 5.0 46,78,80 m/z 50 2 5.85 96,88,64,62,58 m/z 40 280 °C Quadrupole 230 °C 150 °C

5.0 min BFB EI Agilent 7890A GC & 5975C MSD Large volume splitless injection for EPA Method 522 without a PTV. Acknowledgement M. Misselwitz, J. Cochran

5.10 5.15 5.20 5.25 5.30 5.35 5.40 5.45 5.50 5.55 5.60 5.65 5.70 5.75 5.80 5.85 5.90 5.95 6.00 6.05 6.10 6.15 6.20 6.25 6.30 6.35 6.40 6.45 6.50 6.55 6.60 6.65 6.70 6.75 6.80 Time (min) GC_EV1251

EPA 522 Analyte Mix on Rtx®-624 w/5 m Integra-Guard® (30 m x 0.25 mm x 1.4 μm)

NEW! Column 1

Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Mode: SIM Program:

Transfer Line Temp.: Analyzer Type: Source Temp.: Quad Temp.: Solvent Delay Time: Tune Type: Ionization Mode: Instrument Notes

Rtx®-624 w/5 m Integra-Guard®, 30 m, 0.25 mm ID, 1.40 μm (cat.# 10968-124) Tetrahydrofuran-d8 (cat.# 30112) 1,4-Dioxane-d8 (cat.# 30614) 1,4-Dioxane (cat.# 30287) Dichloromethane 50 ng/mL

Peaks 1. Tetrahydrofuran-D8 2. 1,4-Dioxane-d8 3. 1,4-Dioxane

tR (min) 5.59 6.51 6.55

10 μL splitless (hold 1 min) Sky® 4 mm single taper w/wool (cat.# 23303.5) 120 °C 80 mL/min 35 °C (hold 1 min) to 120 °C at 12 °C/min (hold 1 min) He, constant flow 1.4 mL/min 30.556 cm/sec @ 35 °C MS SIM Start Time Group (min) Ion(s) Dwell (ms) 1 5.2 46,78,80 m/z 50 2 6.3 96,88,64,62,58 m/z 75

2

3

280 °C Quadrupole 230 °C 150 °C

5.2 min BFB EI Agilent 7890A GC & 5975C MSD Large volume splitless injection for EPA Method 522 without a PTV and without a press-fit connector for the retention gap. Acknowledgement M. Misselwitz, J. Cochran 5.55 5.60 5.65

5.70

5.75

5.80 5.85 5.90 5.95

6.00 6.05 6.10

6.15 6.20 6.25 6.30 6.35 Time (min)

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6.40 6.45 6.50 6.55 6.60

6.65 6.70 6.75 GC_EV1250


GC CHROMATOGRAMS | ENVIRONMENTAL

Semivolatiles Semivolatiles on Rxi®-5Sil MS by EPA Method 8270 (Split Injection)

NEW!

60,61,62

63 64 65 59

52 36 37

42 56 45 55 50 39 48 40 51 58 38 41 43 46 47 53 57 54 44

32 15 16 18,19,20 24 2628 30 33 34 12,13 29 14 17 21 23 31 25 11 22 27 3.40

3.80

4.20

49

35

66

4.60

5.00

5.40

5.80

6.20

6.60

84, 85, 86 EIC: m/z 93

8 80,81 9

EIC: m/z 252

75 78

71 72

90 89

73 74 82

87 93 94

EIC: 1 = m/z 96 2 = m/z 88 3 = m/z 74 4 = m/z 79 1

76

67

4

EIC: 93 = m/z 276 94 = m/z 278

77 68 70

3 6,7 10

2

83 79

88

69

91

95 92 5

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

10.00

11.00

12.00

13.00

14.00

Time (min)

GC_EV1248 Column Sample

Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) 8270 MegaMix® (cat.# 31850) 8270 Benzidines mix (cat.# 31852) Benzoic acid (cat.# 31879) 1,4-Dioxane (cat.# 31853) Revised B/N surrogate mix (cat.# 31888) Acid surrogate mix (4/89 SOW) (cat.# 31063) Revised SV internal standard mix (cat.# 31886) Methylene chloride 40 μg/mL (IS/SS 20 μg/mL)

Diluent: Conc.: Injection Inj. Vol.: 1 μL split (split ratio 10:1) Liner: Sky® 4 mm Precision® liner w/wool (cat.# 23305.5) Inj. Temp.: 270 °C Split Vent Flow Rate: 12 mL/min Oven Oven Temp.: 70 °C (hold 1 min) to 285 °C at 28 °C/min to 305 °C at 3 °C/min to 320 °C at 30 °C/min (hold 1 min) Carrier Gas He, constant flow Flow Rate: 1.2 mL/min Detector MS Mode: Scan Transfer Line Temp.: 280 °C Analyzer Type: Quadrupole Source Temp.: 270 °C Quad Temp.: 150 °C Electron Energy: 70 eV Solvent Delay Time: 1.3 min Tune Type: DFTPP Ionization Mode: EI Scan Range: 35-550 amu Scan Rate: 5.36 scans/sec Instrument Agilent 7890A GC & 5975C MSD

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31.

Peaks 1,4-Dioxane-d8 (IS) 1,4-Dioxane N-Nitrosodimethylamine Pyridine 2-Fluorophenol (SS) Phenol-d6 (SS) Phenol Aniline Bis(2-chloroethyl)ether 2-Chlorophenol 1,3-Dichlorobenzene 1,4-Dichlorobenzene-D4 (IS) 1,4-Dichlorobenzene Benzyl alcohol 1,2-Dichlorobenzene 2-Methylphenol Bis(2-chloroisopropyl)ether 4-Methylphenol 3-Methylphenol N-nitroso-di-n-propylamine Hexachloroethane Nitrobenzene-D5 (SS) Nitrobenzene Isophorone 2-Nitrophenol 2,4-Dimethylphenol Benzoic acid Bis(2-chloroethoxy)methane 2,4-Dichlorophenol 1,2,4-Trichlorobenzene Naphthalene-D8 (IS)

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. 57. 58. 59. 60. 61. 62. 63.

Naphthalene 4-Chloroaniline Hexachlorobutadiene 4-Chloro-3-methylphenol 2-Methylnaphthalene 1-Methylnaphthalene Hexachlorocyclopentadiene 2,4,6-Trichlorophenol 2,4,5-Trichlorophenol 2-Fluorobiphenyl (SS) 2-Chloronaphthalene 2-Nitroaniline 1,4-Dinitrobenzene Dimethyl phthalate 1,3-Dinitrobenzene 2,6-Dinitrotoluene 1,2-Dinitrobenzene Acenaphthylene 3-Nitroaniline Acenaphthene-d10 (IS) Acenaphthene 2,4-Dinitrophenol 4-Nitrophenol 2,4-Dinitrotoluene Dibenzofuran 2,3,5,6-Tetrachlorophenol 2,3,4,6-Tetrachlorophenol Diethyl phthalate 4-Chlorophenyl phenyl ether Fluorene 4-Nitroaniline 4,6-Dinitro-2-methylphenol

64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92. 93. 94. 95.

N-nitrosodiphenylamine 1,2-Diphenylhydrazine 2,4,6-Tribromophenol (SS) 4-Bromophenyl phenyl ether Hexachlorobenzene Pentachlorophenol Phenanthrene-D10 (IS) Phenanthrene Anthracene Carbazole di-n-Butyl phthalate Fluoranthene Benzidine Pyrene-D10 (SS) Pyrene p-Terphenyl-d14 (SS) 3,3'-Dimethylbenzidine Butyl benzyl phthalate Bis(2-ethylhexyl)adipate 3,3'-Dichlorobenzidine Benzo[a]anthracene Chrysene-D12 (IS) Bis(2-ethylhexyl)phthalate Chrysene Di-n-octyl phthalate Benzo[b]fluoranthene Benzo[k]fluoranthene Benzo[a]pyrene Perylene-D12 (IS) Indeno[1,2,3-cd]pyrene Dibenz[a,h]anthracene Benzo[ghi]perylene

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617


GC CHROMATOGRAMS | ENVIRONMENTAL

Semivolatiles Semivolatile Organics on Rxi®-5Sil MS by U.S. EPA Method 8270 89

77

NEW!

EIC: 2 = m/z 88 3 = m/z 74 4 = m/z 79

EIC: 93 = m/z 276 94 = m/z 278

90

79 84, 85, 86

94 93

4 3 2 78

92

87 2.50

75

3.00

80

5

Rxi® Technology!

82 81

15.85

13.30

16.00

88 83

Extremely low bleed at 320 °C

76

Exceptionally inert, ultra low-bleed capillary columns.

90 89 91 94 95 93

1 3,4 2 3.00

4.00

5.00

6.00

7.00

8.00

9.00

10.00

11.00

12.00

13.00

14.00

15.00

53 51

41

Column Sample

Diluent: Conc.: Injection Inj. Vol.:

Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) 8270 MegaMix® (cat.# 31850) 8270 Benzidines mix (cat.# 31852) Benzoic acid (cat.# 31879) 1,4-Dioxane (cat.# 31853) Revised B/N surrogate mix (cat.# 31888) Acid surrogate mix (4/89 SOW) (cat.# 31063) Revised SV internal standard mix (cat.# 31886) Dichloromethane 8 μg/mL (IS/SS 20 μg/mL)

1 μL pulsed splitless (hold 0.59 min) Liner: Sky® 4 mm single taper w/wool (cat.# 23303.5) Inj. Temp.: 270 °C Pulse Pressure: 30 psi (206.8kPa) Pulse Time: 0.64 min Purge Flow: 100 mL/min Oven Oven Temp.: 40 °C (hold 1 min) to 280 °C at 25 °C/min to 320 °C at 5 °C/min (hold 1 min) Carrier Gas He, constant flow Flow Rate: 1.2 mL/min Linear Velocity: 39.723 cm/sec @ 40 °C Detector MS Mode: Scan Transfer Line Temp.: 280 °C Analyzer Type: Quadrupole Source Temp.: 276 °C Quad Temp.: 150 °C Solvent Delay Time: 2.19 min Tune Type: DFTPP Ionization Mode: EI Scan Range: 35-550 amu Scan Rate: 5.36 scans/sec Instrument Agilent 7890A GC & 5975C MSD Notes 7890 Siltek®-treated EZ Twist Top split/splitless injection port (cat.# 22178) Gold-plated dual Vespel® ring inlet seal (cat.# 21241)

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16.00 Time (min) 70

EIC: m/z = 184

31 60, 61

7.50

12, 13

7.60

7.70 71

52

6,7

72

22 36

32

37

64 66

49

18, 19, 20 11 8 10 9

15 16 14

21 17

25

35

39 38

40

74

65

59 26 27,28 30 33 34 23 24 29

73

56

42

67 68

45

58 55 57 50 53 47 43 46 48 54 44

62 69 63

4.40 4.60 4.80 5.00 5.20 5.40 5.60 5.80 6.00 6.20 6.40 6.60 6.80 7.00 7.20 7.40 7.60 7.80 8.00 8.20 8.40 8.60 8.80 9.00 9.20 9.40 9.60

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24.

Peaks 1,4-Dioxane-d8 (IS) 1,4-Dioxane N-Nitrosodimethylamine Pyridine 2-Fluorophenol (SS) Phenol-d6 (SS) Phenol Aniline Bis(2-chloroethyl) ether 2-Chlorophenol 1,3-Dichlorobenzene 1,4-Dichlorobenzene-D4 (IS) 1,4-Dichlorobenzene Benzyl alcohol 1,2-Dichlorobenzene 2-Methylphenol Bis(2-Chloroisopropyl)ether 3-Methylphenol 4-Methylphenol N-Nitrosodi-N-propylamine Hexachloroethane Nitrobenzene-D5 (SS) Nitrobenzene Isophorone

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.

2-Nitrophenol 2,4-Dimethylphenol Bis(2-chloroethoxy)methane Benzoic acid 2,4-Dichlorophenol 1,2,4-Trichlorobenzene Naphthalene-D8 (IS) Naphthalene 4-Chloroaniline Hexachlorobutadiene 4-Chloro-3-methylphenol 2-Methylnaphthalene 1-Methylnaphthalene Hexachlorocyclopentadiene 2,4,6-Trichlorophenol 2,4,5-Trichlorophenol 2-Fluorobiphenyl (SS) 2-Chloronaphthalene 2-Nitroaniline 1,4-Dinitrobenzene Dimethyl phthalate 1,3-Dinitrobenzene 2,6-Dinitrotoluene 1,2-Dinitrobenzene Acenaphthylene

50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72.

3-Nitroaniline Acenaphthene-d10 (IS) Acenaphthene 2,4-Dinitrophenol 4-Nitrophenol 2,4-Dinitrotoluene Dibenzofuran 2,3,5,6-Tetrachlorophenol 2,3,4,6-Tetrachlorophenol Diethyl phthalate 4-Chlorophenyl phenyl ether Fluorene 4-Nitroaniline 4,6-Dinitro-2-methylphenol N-nitrosodiphenylamine (as diphenylamine) 1,2-Diphenylhydrazine (as azobenzene) 2,4,6-Tribromophenol (SS) 4-Bromophenyl phenyl ether Hexachlorobenzene Pentachlorophenol Phenanthrene-D10 (IS) Phenanthrene Anthracene

73. 74. 75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92. 93. 94. 95.

GC_EV1245 Carbazole di-n-Butyl phthalate Fluoranthene Benzidine Pyrene-d10 (SS) Pyrene p-Terphenyl-d14 (SS) 3,3'-Dimethylbenzidine Butyl benzyl phthalate Bis(2-ethylhexyl) adipate 3,3'-Dichlorobenzidine Benzo[a]anthracene Chrysene-D12 (IS) Bis(2-ethylhexyl)phthalate Chrysene Di-n-octyl phthalate Benzo[b]fluoranthene Benzo[k]fluoranthene Benzo[a]pyrene Perylene-D12 (IS) Indeno[1,2,3-cd]pyrene Dibenz[a,h]anthracene Benzo[ghi]perylene


GC CHROMATOGRAMS | ENVIRONMENTAL

Semivolatiles Semivolatile Organics w/Appendix IX on Rxi®-5Sil MS by U.S. EPA Method 8270

NEW!

GC_EV1246 Column Sample

Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Pulse Pressure: Pulse Time: Purge Flow: Oven Oven Temp:

Rxi®-5Sil MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) 8270 MegaMix® (cat.# 31850) 8270 Benzidines mix (cat.# 31852) Benzoic acid (cat.# 31879) Revised B/N surrogate mix (cat.# 31888) Acid surrogate mix (4/89 SOW) (cat.# 31063) Revised SV internal standard mix (cat.# 31886) Appendix IX mix #1 (cat.# 31625) Appendix IX mix #2 (cat.# 31806) Dichloromethane 10 μg/mL (1,4-dioxane and IS/SS 20 μg/mL) 1 μL pulsed splitless (hold 0.59 min) Sky® 4 mm single taper w/wool (cat.# 23303.5) 270 °C 30 psi (206.8kPa) 0.64 min 100 mL/min

40 °C (hold 1 min) to 280 °C at 25 °C/min to 320 °C at 5 °C/min (hold 1 min) Carrier Gas He, constant flow Flow Rate: 1.2 mL/min Linear Velocity: 39.723 cm/sec @ 40 °C Detector MS Mode: Scan Transfer Line Temp.: 280 °C Analyzer Type: Quadrupole Source Temp.: 276 °C Quad Temp.: 150 °C Solvent Delay Time: 2.19 min Tune Type: DFTPP Ionization Mode: EI Scan Range: 35-550 amu Scan Rate: 5.36 scans/sec Instrument Agilent 7890A GC & 5975C MSD Notes 7890 Siltek®-treated EZ Twist Top® split/ splitless injection port (cat.# 22178) Flip Seal® dual Vespel® ring inlet seal (cat.# 23411)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

Peaks 1,4-Dioxane-d8 (IS) 1,4-Dioxane N-Nitrosodimethylamine Pyridine Ethyl methacrylate 2-Picoline N-Nitrosomethylethylamine Methyl methanesulfonate 2-Fluorophenol (SS) N-Nitrosodiethylamine Ethyl methanesulfonate Benzaldehyde Phenol-d6 (SS) Phenol Aniline Bis(2-chloroethyl) ether Pentachloroethane 2-Chlorophenol 1,3-Dichlorobenzene 1,4-Dichlorobenzene-D4 (IS) 1,4-Dichlorobenzene Benzyl alcohol 1,2-Dichlorobenzene 2-Methylphenol Bis(2-Chloroisopropyl)ether N-Nitrosopyrrolidine 3-Methylphenol 4-Methylphenol Acetophenone N-Nitrosodipropylamine 4-Nitrosomorpholine o-Toluidine Hexachloroethane Nitrobenzene-D5 (SS) Nitrobenzene N-Nitrosopiperidine Isophorone 2-Nitrophenol

39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77.

2,4-Dimethylphenol Bis(2-chloroethoxy)methane Benzoic acid 2,4-Dichlorophenol ,Dimethylphenethylamine 1,2,4-Trichlorobenzene Naphthalene-D8 (IS) Naphthalene 4-Chloroaniline 2,6-Dichlorophenol Hexachloropropene Hexachlorobutadiene N-Nitrosobutylamine Caprolactam 1,4-Phenylenediamine 4-Chloro-3-methylphenol Isosafrole (isomer) 2-Methylnaphthalene 1-Methylnaphthalene Hexachlorocyclopentadiene 1,2,4,5-Tetrachlorobenzene Isosafrole (isomer) 2,4,6-Trichlorophenol 2,4,5-Trichlorophenol 2-Fluorobiphenyl (SS) Safrole Biphenyl 2-Chloronaphthalene 1-Chloronaphthalene Diphenyl ether 2-Nitroaniline 1,4-Naphthoquinone 1,4-Dinitrobenzene Dimethyl phthalate 1,3-Dinitrobenzene 2,6-Dinitrotoluene 1,2-Dinitrobenzene Acenaphthylene 3-Nitroaniline

78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92. 93. 94. 95. 96. 97. 98. 99. 100. 101. 102. 103. 104. 105. 106. 107. 108. 109. 110. 111. 112. 113. 114.

Acenaphthene-d10 (IS) Acenaphthene 2,4-Dinitrophenol 4-Nitrophenol Pentachlorobenzene 2,4-Dinitrotoluene Dibenzofuran 1-Naphthalamine 2,3,5,6-Tetrachlorophenol 2,3,4,6-Tetrachlorophenol 2-Naphthalamine Diethyl phthalate 4-Chlorophenyl phenyl ether Fluorene 2-Methyl-5-nitroaniline 4-Nitroaniline 4,6-Dinitro-2-methylphenol N-nitrosodiphenylamine (as diphenylamine) 1,2-Diphenylhydrazine (as azobenzene) 2,4,6-Tribromophenol (SS) 1,3,5-Trinitrobenzene Diallate Phenacetin 4-Bromophenyl phenyl ether Hexachlorobenzene Atrazine 4-Aminobiphenyl Pentachlorophenol Pentachloronitrobenzene Propyzamide Phenanthrene-D10( IS) Phenanthrene Anthracene Carbazole di-n-Butyl phthalate 4-Nitroquinoline1 -oxide Methapyriline

115. 116. 117. 118. 119. 120. 121. 122. 123. 124. 125. 126. 127. 128. 129. 130. 131. 132. 133. 134. 135. 136. 137. 138. 139. 140. 141. 142. 143. 144. 145.

Isodrin Fluoranthene Benzidine Pyrene-d10( SS) Pyrene Aramite( isomer) p-Terphenyl-d14 (SS) Aramite( isomer) Dimethylaminoazobenzene Chlorobenzilate 3,3'-Dimethylbenzidine Butyl benzyl phthalate Kepone Bis(2-ethylhexyl) adipate 2-Acetylaminofluorene 3,3'-Dichlorobenzidine Benz[a]anthracene Chrysene-D12( IS) Bis(2-ethylhexyl)phthalate Chrysene Di-n-octyl phthalate 7,12-Dimethylbenzo[a] anthracene Benzo[b]fluoranthene Benzo[k]fluoranthene Benzo[a]pyrene Perylene-D12( IS) 3-Methylcholanthrene Dibenzo[a,j]acridine Indeno[1,2,3-cd]pyrene Dibenz[a,h]anthracene Benzo[ghi]perylene

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619


GC CHROMATOGRAMS | ENVIRONMENTAL

Volatiles Volatile Organic Compounds Retention Time Index: Rtx®-VMS Data collected using a 60 m, 0.25 mm ID, 1.4 μm Rtx®-VMS column; Oven: 40 °C (hold 6 min) to 230 °C @ 14 °C/min (hold 11 min); Carrier gas: helium; Regulation: constant pressure; Flow rate: 1 mL/min; Linear velocity: 21 cm/sec; Dead time: 4.90 min

for more info See pages 623–625 for Rtx®-VMS volatile organics chromatograms.

Compound Dichlorodifluoromethane Chloromethane Vinyl chloride Water Bromomethane Methanol 2-Methylbutane Chloroethane Trichlorofluoromethane n-Pentane Diethylether 1,1-Dichloroethene Carbon disulfide Freon® 113 Ethanol Iodomethane 3-Chlorotrifluoropropane Chloro-methyl-methylether Acrolein 2-Methylpentane Allyl chloride Methylene chloride 3-Methylpentane Acetone trans-1,2-Dichloroethene Methyl tert-butyl ether 2-Propanol tert-Butyl alcohol Methyl acetate Hexane Acetonitrile Chloroprene 1,1-Dichloroethane Acrylonitrile Diisopropyl ether 2,4-Dimethylpentane Vinyl acetate Ethyl-tert-buyl ether 1-Propanol cis-1,2-Dichloroethene Allyl alcohol 2,2-Dichloropropane Bromochloromethane Chloroform Cyclohexane Methyl acrylate Carbon tetrachloride Tetrahydrofuran 1,1,1-Trichloroethane Ethyl acetate 2-Butanone Dibromofluoromethane 1,1-Dichloropropene Propargyl alcohol 1-Chlorobutane 2,2,4-Trimethylpentane Propionitrile Benzene n-Heptane (C7) Methacrylonitrile

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Rtx®-VMS Ret. Time 5.52 6.26 6.54 6.70 7.61 7.93 7.96 8.00 8.41 8.61 9.59 9.64 9.65 9.70 9.74 9.99 10.45 10.54 10.57 10.59 10.72 10.98 11.09 11.24 11.24 11.42 11.52 11.56 11.63 11.64 12.22 12.30 12.42 12.60 12.62 12.68 13.02 13.08 13.18 13.32 13.35 13.48 13.62 13.75 13.84 13.87 13.94 14.03 14.06 14.13 14.18 14.18 14.20 14.35 14.51 14.53 14.59 14.60 14.62 14.64

Compound Benzene-d6 Pentafluorobenzene 1,2-Dichloroethane-d4 1,2-Dichloroethane tert-Amyl-methyl ether Isobutyl alcohol Fluorobenzene Isopropyl acetate Formic acid Trichloroethene 1,4-Difluorobenzene n-Butanol Methyl cyclohexane Acetic acid Dibromomethane 1,2-Dichloropropane Bromodichloromethane Methyl methacrylate α,α,α-Trifluorotoluene 1,4-Dioxane n-Propyl acetate 2-Chloroethyl-vinyl-ether 2-Chloroethanol cis-1,3-Dichloropropene 1-Bromo-2-chloroethane n-Octane Toluene-d8 Toluene Propionic acid Chloroacetonitrile 4-Methyl-2-pentanone 2-Bromo-1-chloropropane 2-Nitropropane Pyridine 1,1-Dichloropropanone trans-1,3-Dichloropropene Tetrachloroethene Ethyl methacrylate 1,1,2-Trichloroethane Dibromochloromethane 1,3-Dichloropropane Isobutyric acid 1,2-Dibromoethane n-Butyl acetate 2-Hexanone Butyric acid 1-Chloro-3-fluorobenzene Ethylbenzene Chlorobenzene 1-Chloro-4-fluorobenzene Ethylbenzene-d10 1-Chlorohexane 1,1,1,2-Tetrachloroethane m-Xylene p-Xylene Chlorobenzene-d5 1-Chloro-2-fluorobenzene o-Xylene Stryrene Isovaleric acid

Rtx®-VMS Ret. Time 14.72 14.75 14.79 14.90 15.00 15.06 15.16 15.34 15.37 15.39 15.58 15.60 15.78 15.93 16.05 16.17 16.23 16.28 16.45 16.49 16.70 16.92 16.93 17.04 17.05 17.17 17.28 17.36 17.61 17.64 17.76 17.81 17.83 17.86 17.88 17.88 17.89 17.92 18.11 18.40 18.49 18.55 18.78 18.80 18.82 19.17 19.17 19.36 19.39 19.39 19.40 19.41 19.44 19.53 19.54 19.55 19.67 20.13 20.17 20.18

Compound Bromoform Isopropylbenzene 1,2-Butanediol Valeric acid 1,4-Dichlorobutane Bromobenzene 4-Bromo-1-fluorobenzene cis-1,4-Dichloro-2-butene n-Decane n-Propylbenzene 1,1,2,2-Tetrachloroethane 1,3,5-Trimethylbenzene 1-Ethyl-4-methylbenzene 1-Ethyl-3-methylbenzene 1,2,3-Trichloropropane trans-1,4-Dichloro-2-butene 2-Chlorotoluene 4-Chlorotoluene Cyclohexane tert-Butylbenzene 1-Ethyl-2-methylbenzene 1,2,4-Trimethylbenzene Pentachloroethane 1,3-Dichloro-2-propanol sec-Butylbenzene Isocaproic acid p-Isopropyltoluene 1,3-Dichlorobenzene Caproic acid 1,4-Dichlorobenzene n-Butylbenzene Malononitrile Benzyl chloride 1,2-Dichlorobenzene-d4 1,2-Dichlorobenzene Hexachloroethane 1-Octanol Bis-(2-chloro-isopropyl) ether 4-Bromo-1-chlorobenzene Benzyl alcohol Heptanoic acid n-Dodecane 3-Bromochlorobenzene 1,2-Dibromo-3-chloropropane 2-Bromochlorobenzene Hexachlorobutadiene Nitrobenzene 1,2,4-Trichlorobenzene Benzyl acetate n-Tridecane Naphthalene 1,2,3-Trichlorobenzene n-Tetradecane 2-Methylnaphthalene 1-Methylnaphthalene n-Pentadecane 2-Chloronaphthalene

Rtx®-VMS Ret. Time 20.30 20.51 20.82 20.89 20.90 20.91 20.95 20.97 21.04 21.07 21.10 21.30 21.33 21.34 21.39 21.40 21.40 21.61 21.78 21.81 21.82 21.88 21.92 22.05 22.06 22.09 22.22 22.53 22.55 22.64 22.88 22.89 23.23 23.36 23.38 23.63 23.70 24.06 24.09 24.23 24.29 24.54 24.61 24.78 25.54 25.99 26.02 26.19 26.29 26.51 27.01 27.46 28.83 30.36 30.96 31.65 33.36


GC CHROMATOGRAMS | ENVIRONMENTAL

Volatiles Volatile Organic Compounds Retention Time Index: Rxi®-624Sil MS* Data collected using a 30 m x 0.25 mm x 1.400 μm Rxi®-624Sil MS column; Oven: 35 °C (hold 5 min) @ 11 °C/min to 60 °C @ 20 °C/min to 220 °C; Carrier gas: helium; Regulation: constant flow; Flow: 1.17 mL/min; GC Temperature: 35 °C; Inlet Pressure: 7.94 psi; Outlet Pressure: 0.00 psi; Dead Time: 1.780 min; Linear Velocity: 32.68 cm/sec; Detector 1: Mass Spectrometer *Modeled by Pro ezGC software.

for more info See page 622 for an Rxi®-624Sil MS volatile organics chromatogram.

Compound Dichlorodifluoromethane Chloromethane Water Vinyl chloride Methanol Ethylene oxide Bromomethane Chloroethane Trichlorofluoromethane n-Pentane Ethanol Diethylether 2-Methylbutane Acrolein 1,1-Dichloroethene Freon® 113 Acetone Iodomethane 2-Propanol Carbon disulfide Acetonitrile Methyl acetate Allyl chloride Methylene chloride 2-Methylpentane tert-Butyl alcohol Acrylonitrile Methyl-d3-tert-butyl-ether

Methyl tert-butyl-ether trans-1,2-Dichloroethene 3-Methylpentane Hexane 1,1-Dichloroethane Allyl alcohol Vinyl acetate Diisopropyl ether Chloroprene 1-Propanol Ethyl tert-buyl ether TB(d9)A cis-1,2-Dichloroethene 2-Butanone 2,2-Dichloropropane Ethyl acetate Propionitrile Methyl acrylate Methacrylonitrile Bromochloromethane Tetrahydrofuran Chloroform Dibromofluoromethane 1,1,1-Trichloroethane Pentafluorobenzene

Rxi®-624Sil MS Ret. Time 2.178 2.438 2.588 2.63 2.985 3.127 3.192 3.395 3.834 4.032 4.199 4.387 4.501 4.677 4.848 4.929 4.971 5.135 5.323 5.323 5.581 5.676 5.693 5.939 6.01 6.19 6.414 6.435 6.477 6.48 6.503 7.023 7.291 7.309 7.33 7.386 7.407 7.431 7.978 8.133 8.204 8.208 8.208 8.283 8.297 8.336 8.499 8.528 8.542 8.678 8.871 8.872 8.937

Compound Cylcohexane 1-Chlorobutane Carbon tetrachloride 1,1-Dichloropropene Benzene-d6 1,2-Dichloroethane-d4 Benzene 1,2-Dichloroethane Isopropyl acetate 2,2,4-Trimethylpentane Isobutyl alcohol tert-Amyl-methyl ether n-Heptane Fluorobenzene 1,4-Difluorobenzene 1-Butanol Trichloroethene Methyl cyclohexane tert-Amyl ethyl ether 1,2-Dichloropropane α,α,α-Trifluorotoluene Methyl methacrylate 1,4-Dioxane n-Propyl acetate Dibromomethane Bromodichloromethane 2-Nitropropane Chloroacetonitrile 2-Chloroethyl-vinyl-ether 1-Bromo-2-chloroethane Epichlorhydrin cis-1,3-Dichloropropene 2,4-Dimethylpentane 4-Methyl-2-pentanone 1,1-Dichloropropanone Pyridine Toluene-d8 Toluene n-Octane trans-1,3-Dichloropropene Ethyl methacrylate 2-Bromo-1-chloropropane 1,1,2-Trichloroethane Tetrachloroethene 1,3-Dichloropropane n-Butyl acetate Dibromochloromethane 1,2-Dibromoethane 1-Chloro-3-fluorobenzene 1-Chloro-4-fluorobenzene Chlorobenzene-D5 Chlorobenzene Ethylbenzene-d10

Rxi®-624Sil MS Ret. Time 8.959 9.032 9.055 9.067 9.255 9.28 9.296 9.365 9.376 9.455 9.456 9.457 9.537 9.636 9.784 9.911 10.013 10.268 10.27 10.28 10.325 10.327 10.379 10.383 10.443 10.532 10.736 10.764 10.792 10.843 10.875 10.938 10.961 11.062 11.105 11.135 11.185 11.246 11.345 11.441 11.471 11.497 11.619 11.699 11.761 11.792 11.82 11.934 12.119 12.338 12.386 12.415 12.44

Compound 1-Chlorohexane 1,1,1,2-Tetrachloroethane Ethylbenzene m-Xylene p-Xylene n-Nonane 1-Chloro-2-fluorobenzene o-Xylene Stryrene n-Amyl acetate Bromoform Isopropylbenzene cis-1,4-Dichloro-2-butene 1,4-Dichlorobutane 4-Bromo-1-fluorobenzene 1,1,2,2-Tetrachloroethane Bromobenzene trans-1,4-Dichloro-2-butene 1,2,3-Trichloropropane n-Propylbenzene 2-Chlorotoluene 1,3,5-Trimethylbenzene n-Decane 4-Chlorotoluene tert-Butylbenzene Pentachloroethane 1,2,4-Trimethylbenzene sec-Butylbenzene n-Butylcyclohexane 1,3-Dichlorobenzene p-Isopropyltoluene 1,4-Dichlorobenzene-d4 1,4-Dichlorobenzene n-Butylbenzene 1,2-Dichlorobenzene-d4 1,2-Dichlorobenzene Hexachloroethane 1-Octanol 4-Bromo-1-chlorobenzene 1,2-Dibromo-3-chloropropane Nitrobenzene Tetraethyl lead 2-Bromochlorobenzene n-Tetradecane n-Dodecane 1,2,4-Trichlorobenzene Hexachlorobutadiene Naphthalene 1,2,3-Trichlorobenzene 2,5-Dibromotoluene 2-Methylnaphthalene 1-Methyl-naphthalene

Rxi®-624Sil MS Ret. Time 12.442 12.503 12.512 12.636 12.636 12.668 12.703 12.99 13.01 13.148 13.177 13.327 13.382 13.439 13.485 13.6 13.612 13.635 13.655 13.698 13.78 13.858 13.867 13.886 14.131 14.16 14.182 14.325 14.4 14.431 14.453 14.497 14.519 14.796 14.814 14.823 15.06 15.07 15.467 15.476 15.638 15.652 15.761 15.783 15.784 16.176 16.293 16.418 16.608 17.488 17.558 17.754

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621


GC CHROMATOGRAMS | ENVIRONMENTAL

Volatiles Volatiles by EPA Method 8260 on Rxi®-624Sil MS (30 m, 0.25 mm ID, 1.40 μm)

Rxi® Technology!

Resolution of critical pairs, low bleed, and high inertness make this a great column for volatiles!

Exceptionally inert, ultra low-bleed capillary columns.

Column Sample

Rxi®-624Sil MS, 30 m, 0.25 mm ID, 1.40 μm (cat.# 13868) 8260A surrogate mix (cat.# 30240) 8260A internal standard mix (cat.# 30241) 8260B MegaMix® calibration mix (cat.# 30633) VOA calibration mix #1 (ketones) (cat.# 30006) 8260B acetate mix (Revised) (cat.# 30489) California oxygenates mix (cat.# 30465) 502.2 calibration mix #1 (gases) (cat.# 30042) 25 ppb in RO water Purge and trap split (split ratio 30:1) 225 °C

Conc.: Injection Inj. Temp.: Purge and Trap Instrument: OI Analytical 4660 Trap Type: 10 Trap Purge: 11 min @ 20 °C Desorb Preheat Temp.: 180 °C Desorb: 0.5 min @ 190 °C Bake: 5 min @ 210 °C Interface Connection: injection port Oven Oven Temp: 35 °C (hold 5 min) to 60 °C at 11 °C/min to 220 °C at 20 °C/ min (hold 2 min) Carrier Gas He, constant flow Flow Rate: 1.0 mL/min Detector MS Mode: Scan Transfer Line Temp.: 230 °C Analyzer Type: Quadrupole Source Temp.: 230 °C Quad Temp.: 150 °C Electron Energy: 70 eV Solvent Delay Time: 1.5 min Tune Type: BFB Ionization Mode: EI Scan Range: 36-260 amu Instrument Agilent 7890A GC & 5975C MSD Notes Other Purge and Trap Conditions: Sample Inlet: 40 °C Sample: 40 °C Water Management: Purge 110 °C, Desorb 0 °C, Bake, 240 °C Acknowledgement Eclipse 4660 purge and trap courtesy of O.I. Analytical, College Station, TX.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26.

Peaks tR (min) Dichlorodifluoromethane (CFC-12) 2.198 Chloromethane 2.459 Vinyl chloride 2.659 Bromomethane 3.226 Chloroethane 3.434 Trichlorofluoromethane (CFC-11) 3.876 Diethyl ether (ethyl ether) 4.440 1,1-Dichloroethene 4.909 1,1,2-Trichlorotrifluoroethane (CFC-113) 4.998 Acetone 5.029 Iodomethane 5.195 Carbon disulfide 5.323 Acetonitrile 5.637 Allyl chloride 5.715 Methyl acetate 5.723 Methylene chloride 5.981 tert-Butyl alcohol 6.234 Acrylonitrile 6.451 Methyl tert-butyl ether (MTBE) 6.509 trans-1,2-Dichloroethene 6.512 1,1-Dichloroethane 7.315 Vinyl acetate 7.359 Diisopropyl ether (DIPE) 7.407 Chloroprene 7.429 Ethyl tert-butyl ether (ETBE) 7.970 2-Butanone (MEK) 8.193

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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.

Peaks cis-1,2-Dichloroethene 2,2-Dichloropropane Ethyl acetate Propionitrile Methyl acrylate Methacrylonitrile Bromochloromethane Tetrahydrofuran Chloroform 1,1,1-Trichloroethane Dibromofluoromethane Carbon tetrachloride 1,1-Dichloropropene 1,2-Dichloroethane-d4 Benzene 1,2-Dichloroethane Isopropyl acetate Isobutyl alcohol tert-Amyl methyl ether (TAME) Fluorobenzene Trichloroethene 1,2-Dichloropropane Methyl methacrylate 1,4-Dioxane (ND) Dibromomethane Propyl acetate 2-Chloroethanol (ND)

tR (min) 8.193 8.193 8.265 8.276 8.318 8.476 8.507 8.521 8.651 8.843 8.848 9.026 9.037 9.246 9.262 9.334 9.340 9.421 9.421 9.598 9.976 10.243 10.290 10.299* 10.326 10.346 10.368*

GC_EV1169

54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78. 79. 80.

Peaks Bromodichloromethane 2-Nitropropane cis-1,3-Dichloropropene 4-Methyl-2-pentanone (MIBK) Toluene-D8 Toluene trans-1,3-Dichloropropene Ethyl methacrylate 1,1,2-Trichloroethane Tetrachloroethene 1,3-Dichloropropane 2-Hexanone Butyl acetate Dibromochloromethane 1,2-Dibromoethane (EDB) Chlorobenzene-d5 Chlorobenzene Ethylbenzene 1,1,1,2-Tetrachloroethane m-Xylene p-Xylene o-Xylene Styrene n-Amyl acetate Bromoform Isopropylbenzene (cumene) cis-1,4-Dichloro-2-butene

tR (min) 10.496 10.698 10.904 11.026 11.148 11.210 11.407 11.435 11.585 11.662 11.729 11.749 11.837 11.921 12.035 12.412 12.440 12.507 12.507 12.612 12.612 12.935 12.949 13.018 13.118 13.226 13.268

Peaks tR (min) 81. 4-Bromofluorobenzene 13.385 82. 1,1,2,2-Tetrachloroethane 13.456 83. trans-1,4-Dichloro-2-butene 13.496 84. Bromobenzene 13.515 85. 1,2,3-Trichloropropane 13.526 86. n-Propylbenzene 13.565 87. 2-Chlorotoluene 13.657 88. 1,3,5-Trimethylbenzene 13.699 89. 4-Chlorotoluene 13.751 90. tert-Butylbenzene 13.965 91. Pentachloroethane 14.007 92. 1,2,4-Trimethylbenzene 14.010 93. sec-Butylbenzene 14.140 94. 4-Isopropyltoluene (p-cymene) 14.254 95. 1,3-Dichlorobenzene 14.263 96. 1,4-Dichlorobenzene-D4 14.321 97. 1,4-Dichlorobenzene 14.340 98. n-Butylbenzene 14.579 99. 1,2-Dichlorobenzene 14.635 100. 1,2-Dibromo-3-chloropropane( DBCP) 15.252 101. Nitrobenzene 15.407 102. 1,2,4-Trichlorobenzene 15.935 103. Hexachloro-1,3-butadiene 16.040 104. Naphthalene 16.196 105. 1,2,3-Trichlorobenzene 16.396 * ND = not detected; retention time determined by wet needle injection


GC CHROMATOGRAMS | ENVIRONMENTAL

Volatiles Volatile Organics by EPA Method 8260 (80 ppb Standard) on Rtx®-VMS

restek innovation! Good choice for alcohols & oxygenates!

87,88

91

79,80 83,84

93,94 92

86

82

95

90

89

96

77

81 85

78 76

18.90 19.00 19.10 19.20 19.30 19.40 19.50 19.60 19.70 19.80 19.90 20.00 20.10 20.20 20.30 GC_EV00686

1.00

Column Sample

Injection Inj. Temp.: Purge and Trap Instrument: Trap Type: Purge: Desorb Preheat Temp.: Desorb: Bake: Transfer Line Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Dead Time: Detector Transfer Line Temp.: Tune Type: Scan Range: Notes

2.00

3.00

4.00

5.00

6.00

7.00

8.00

9.00

Rtx®-VMS, 30 m, 0.25 mm ID, 1.4 μm (cat.# 19915) 8260B MegaMix® calibration mix kit (cat.# 30475) California oxygenates mix (cat.# 30465) VOA calibration mix #1 (ketones) (cat.# 30006) 8260A surrogate mix (cat.# 30240) 8260 internal standard mix (cat.# 30074) Purge and trap split (split ratio 25:1) 250 °C O.I. Analytical 4560 with 4551A Autosampler #10 (Tenax®/silica gel/carbon molecular sieve) 11 min @ 20 °C, flow 38 mL/min 150 °C 1.0 min @ 190 °C, flow 32 mL/min 10 min @ 210 °C 110 °C 35 °C (hold 7 min) to 90 °C at 4 °C/min to 220 °C at 45 °C/min (hold 1 min) He, constant flow 1.3 mL/min 1.47 min @ 35 °C Agilent 5971A GC-MS

280 °C PFTBA/BFB 35-260 amu Sample Size: 10 mL Sample Temp: 40 °C Water Management: 110 °C purge, 0 °C desorb, 240 °C bake 6-Port Valve: 110 °C Sparge Mount: 45 °C Valve Manifold: 50 °C Other Conditions: prepurge, preheat, dry purge OFF Acknowledgement Purge & trap courtesy of O.I. Analytical

10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 20.00 21.00 22.00 GC_EV00685 Time (min)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34.

Peaks Dichlorodifluoromethane Chloromethane Vinyl chloride Bromomethane Chloroethane Trichlorofluoromethane Diethyl ether 1,1-Dichloroethene Carbon disulfide 1,1,2-Trichloro-1,2,2-trifluoroethane Iodomethane Allyl chloride Methylene chloride Acetone trans-1,2-Dichloroethene Methyl-d3-tert-butyl-ether Methyl acetate Methyl tert-butyl ether tert-Butyl alcohol Acetonitrile Diisopropyl ether Chloroprene 1,1-Dichloroethane Acrylonitrile Ethyl tert-butyl ether cis-1,2-Dichloroethene 2,2-Dichloropropane Bromochloromethane Chloroform Carbon tetrachloride Tetrahydrofuran Methyl acrylate 1,1,1-Trichloroethane Dibromofluoromethane

35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70.

1,1-Dichloropropene 2-Butanone Benzene Propionitrile Methacrylonitrile 1,2-Dichloroethane-d4 Pentafluorobenzene tert-Amyl methyl ether 1,2-Dichloroethane Isobutyl alcohol Trichloroethene 1,4-Difluorobenzene Dibromomethane 1,2-Dichloropropane Bromodichloromethane Methyl methacrylate cis-1,3-Dichloropropene 2-Chloroethyl vinyl ether Toluene-d8 Toluene 2-Nitropropane Tetrachloroethene 2-Bromo-1-chloropropane 4-Methyl-2-pentanone trans-1,3-Dichloropropene 1,1,2-Trichloroethane Ethyl methacrylate Dibromochloromethane 1,3-Dichloropropane 1,2-Dibromoethane 2-Hexanone Chlorobenzene-d5 Chlorobenzene Ethylbenzene 1,1,1,2-Tetrachloroethane m-Xylene

71. p-Xylene 72. o-Xylene 73. Bromoform 74. Styrene 75. Isopropylbenzene 76. 4-Bromo-1-fluorobenzene (SS) 77. Bromobenzene 78. cis-1,4-Dichloro-2-butene 79. 1,4-Dichlorobutane 80. n-Propylbenzene 81. 1,1,2,2-Tetrachloroethane 82. 2-Chlorotoluene 83. 1,2,3-Trichloropropane 84. 1,3,5-Trimethylbenzene 85. trans-1,4-Dichloro-2-butene 86. 4-Chlorotoluene 87. tert-Butylbenzene 88. Pentachloroethane 89. 1,2,4-Trimethylbenzene 90. sec-Butylbenzene 91. p-Isopropyltoluene 92. 1,3-Dichlorobenzene 93. 1,4-Dichlorobenzene-D4 94. 1,4-Dichlorobenzene 95. n-Butylbenzene 96. 1,2-Dichlorobenzene 97. 1,2-Dibromo-3-chloropropane 98. Nitrobenzene 99. Hexachlorobutadiene 100. 1,2,4-Trichlorobenzene 101. Naphthalene 102. 1,2,3-Trichlorobenzene *Carbon dioxide

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623


GC CHROMATOGRAMS | ENVIRONMENTAL

Volatiles Volatile Organics by EPA 8260B on Rtx®-VMS

restek innovation! • First choice for use with dual purge & traps1 • EPA recommended surrogate used.

GC_EV00428 Column Sample Diluent: Conc.: Injection Liner: Inj. Temp.: Purge and Trap Instrument: Trap Type: Purge: Dry Purge: Desorb Preheat Temp.: Desorb: Bake: Interface Connection: Transfer Line Tubing: Transfer Line Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector Mode: Transfer Line Temp.: Analyzer Type: Tune Type: Ionization Mode: Scan Range: Instrument Notes

Rtx®-VMS, 20 m, 0.18 mm ID, 1.00 μm (cat.# 49914) Water 10 ppb in 5 mL RO water (unless noted); ketones 2.5X Purge and trap split (split ratio 40:1) 1 mm split (cat.# 20973) 220 °C Tekmar LCS 3100 Vocarb® 3000 11 min @ ambient, flow 40 mL/min 1 min, flow 40 mL/min 245 °C 2 min @ 250 °C, flow 40 mL/min 8 min @ 260 °C Injection port Silcosteel® treated 0.53 mm ID tubing (cat.# 20595) 120 °C 50 °C (hold 4 min) to 100 °C at 18 °C/min (hold 0 min) to 230 °C at 40 °C/min (hold 3 min) He, constant flow 1.0 mL/min MS Scan 280 °C Quadrupole BFB EI 35-300 amu HP6890 GC & 5973 MSD For proper flows, adjust retention time of dichlorodifluoromethane to a retention time of 1.03 min @ 50 °C

¹A.L. Hilling and G. Smith, Environmental Testing & Analysis, 10(3), 15-19, 2001.

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1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 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.

Peaks Dichlorodifluoromethane Chloromethane Vinyl chloride Bromomethane Chloroethane Trichlorofluoromethane Ethanol (2,500 ppb) 1,1-Dichloroethene Carbon disulfide (40 ppb) Allyl chloride Methylene chloride Acetone trans-1,2-Dichloroethene Methyl tert-butyl ether tert-Butyl alcohol (100 ppb) Diisopropyl ether 1,1-Dichloroethane Acrylonitrile Vinyl acetate Allyl alcohol (250 ppb) Ethyl tert-butyl ether cis-1,2-Dichloroethene 2,2-Dichloropropane Bromochloromethane Chloroform Ethyl acetate Carbon tetrachloride Methyl acrylate Propargyl alcohol (500 ppb) Dibromofluoromethane (SMC) Tetrahydrofuran 1,1,1-Trichloroethane 2-Butanone 1,1-Dichloropropene Benzene Pentafluorobenzene (IS) tert-Amyl Methyl ether 1,2-Dichloroethane Isobutyl alcohol (500 ppb) Isopropyl acetate Trichloroethene 1,4-Difluorobenzene (SMC) Dibromomethane 1,2-Dichloropropane Bromodichloromethane Methyl methacrylate n-Propyl acetate 2-Chloroethanol (2,500 ppb)

49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92. 93. 94. 95. 96. 97.

cis-1,3-Dichloropropene Toluene-d8 (SMC) Toluene Pyridine (250 ppb) Tetrachloroethene 4-Methyl-2-pentanone trans-1,3-Dichloropropene 1,1,2-Trichloroethane Ethyl methacrylate Dibromochloromethane 1,3-Dichloropropane 1,2-Dibromoethane n-Butyl acetate 2-Hexanone 2-Picoline (250 ppb) Chlorobenzene-d5 (IS) Chlorobenzene Ethylbenzene 1,1,1,2-Tetrachloroethane m-Xylene p-Xylene o-Xylene Styrene Bromoform Isopropylbenzene 4-Bromofluorobenzene (SMC) Bromobenzene n-Propylbenzene 1,1,2,2-Tetrachloroethane 2-Chlorotoluene 1,3,5-Trimethylbenzene 1,2,3-Trichloropropane 4-Chlorotoluene tert-Butylbenzene Pentachloroethane 1,2,4-Trimethylbenzene sec-Butylbenzene p-Isopropyltoluene 1,3-Dichlorobenzene 1,4-Dichlorobenzene-d4 (IS) 1,4-Dichlorobenzene n-Butylbenzene 1,2-Dichlorobenzene 1,2-Dibromo-3-Chloropropane Nitrobenzene (250 ppb) Hexachlorobutadiene 1,2,4-Trichlorobenzene Naphthalene 1,2,3-Trichlorobenzene


GC CHROMATOGRAMS | ENVIRONMENTAL

Volatiles Volatile Organics by U.S. EPA Method 524.2 Revision IV on Rtx®-VMS 79-81

71,72

62 68,69 74 78 75 64, 66,67 65 73 76 61 77 70 59,60 58 56,57 63 53 54,55

33

29-31

1 2 3

6 4

5

14 15 8,9 1112 13 7 10

22-24 18 2021 27 16, 17 19 25 28 26 32

45, 46 34 36 35 37 38

39

40-41 44 47 50 49 51 48 43 42

84,85

87 86

52

82 83

GC_EV00718

Column Sample

Diluent: Conc.: Injection Liner: Inj. Temp.: Purge and Trap Instrument: Trap Type: Purge: Dry Purge: Desorb Preheat Temp: Desorb: Bake: Interface Connection: Transfer Line Tubing: Oven Oven Temp: Carrier Gas Flow Rate: Dead Time: Detector Mode: Transfer Line Temp.: Tune Type: Ionization Mode: Scan Range: Notes

Rtx®-VMS, 30 m, 0.25 mm ID, 1.4 μm (cat.# 19915) 502.2 calibration mix #1 (gases) (cat.# 30042) Drinking water VOA MegaMix®, 524.2 rev. 4.1 (cat.# 30601) 524 Internal standard/surrogate mix (cat.# 30201) Ketones mix, 524.2 rev. 4.1 (cat.# 30602) RO water Compounds at 20 ppb each in 5 mL RO water (ketones at 50 ppb; internal standards at 40 ppb) Purge and trap split (split ratio 30:1) 1 mm split (cat.# 20972) 250 °C Tekmar LSC-3100 purge and trap Vocarb 3000 (type K) 11 min @ ambient, flow 40 mL/min 1 min, flow 40 mL/min 245 °C 2 min @ 250 °C, flow 33 mL/min 8 min @ 260 °C Injection port Silcosteel® transfer line 40 °C (hold 2 min) to 85 °C at 14 °C/min (hold 2 min) to 220 °C at 30 °C/min (hold 4 min) He, constant flow 1.1 mL/min 1.48 min @ 40 °C MS Scan 280 °C PFTBA/BFB EI 35-300 amu Dry purge: MCS bypassed using Silcosteel® tubing

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44.

Peaks Dichlorodifluoromethane Chloromethane Vinyl chloride Bromomethane Chloroethane Trichlorofluoromethane Diethyl ether 1,1-Dichloroethene Carbon disulfide Iodomethane Allyl chloride Methylene chloride Acetone trans-1,2-Dichloroethene Methyl tert-butyl ether 1,1-Dichloroethane Acrylonitrile cis-1,2-Dichloroethene 2,2-Dichloropropane Bromochloromethane Chloroform Methyl acrylate Carbon tetrachloride Tetrahydrofuran 1,1,1-Trichloroethane 2-Butanone 1,1-Dichloropropene 1-Chlorobutane Propionitrile Methacrylonitrile Benzene 1,2-Dichloroethane Fluorobenzene Trichloroethene Dibromomethane 1,2-Dichloropropane Bromodichloromethane Methyl methacrylate cis-1,3-Dichloropropene Toluene Chloroacetonitrile 2-Nitropropane 1,1-Dichloropropanone 4-Methyl-2-pentanone

45. Tetrachloroethene 46. trans-1,3-Dichloropropene 47. 1,1,2-Trichloroethane 48. Ethyl methacrylate 49. Dibromochloromethane 50. 1,3-Dichloropropane 51. 1,2-Dibromoethane 52. 2-Hexanone 53. Chlorobenzene 54. Ethylbenzene 55. 1,1,1,2-Tetrachloroethane 56. m-Xylene 57. p-Xylene 58. o-Xylene 59. Styrene 60. Bromoform 61. Isopropylbenzene 62. 4-Bromofluorobenzene 63. Bromobenzene 64. n-Propylbenzene 65. 1,1,2,2-Tetrachloroethane 66. 2-Chlorotoluene 67. 1,2,3-Trichloropropane 68. 1,3,5-Trimethylbenzene 69. trans-1,4-Dichloro-2-butene 70. 4-Chlorotoluene 71. tert-Butylbenzene 72. Pentachloroethane 73. 1,2,4-Trimethylbenzene 74. sec-Butylbenzene 75. p-Isopropyltoluene 76. 1,3-Dichlorobenzene 77. 1,4-Dichlorobenzene 78. n-Butylbenzene 79. Hexachloroethane 80. 1,2-Dichlorobenzene-D4 81. 1,2-Dichlorobenzene 82. 1,2-Dibromo-3-Chloropropane 83. Nitrobenzene 84. Hexachlorobutadiene 85. 1,2,4-Trichlorobenzene 86. Naphthalene 87. 1,2,3-Trichlorobenzene * Peaks 42 & 43 share an ion (43)

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GC CHROMATOGRAMS | FOOD SAFETY

Food Contaminants QuEChERS Extract of NIST SRM 2974a Freeze-Dried Mussel Tissue (GCxGC contour plot) Column

Sample Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp:

Carrier Gas

GC_FF1197 1. 2. 3. 4. 5. 6.

Peaks Naphthalene 2-Methylnaphthalene 1-Methylnaphthalene Biphenyl 2,6-Dimethylnaphthalene Acenaphthylene

7. 8. 9. 10. 11. 12. 13.

14. 15. 16. 17. 18. 19. 20.

Acenaphthene 2,3,5-Trimethylnaphthalene Fluorene Phenanthrene Anthracene 1-Methylphenanthrene Fluoranthene

21. 22. 23. 24. 25.

Pyrene Benzo(a)anthracene Chrysene Benzo(b)fluoranthene Benzo(k)fluoranthene Benzo(j)fluoranthene Benzo(e)pyrene

Benzo(a)pyrene Perylene Dibenz(a,h)anthracene Indeno(1,2,3-cd)pyrene Benzo(ghi)perylene

Rxi®-17Sil MS 30 m, 0.25 mm ID, 0.25 μm (cat.# 14123) Rxi®-1ms 1.2 m, 0.15 mm ID, 0.15 μm (cat.# custom) NIST SRM 2974a freeze-dried mussel tissue with incurred residues Acetonitrile 1 μL splitless (hold 1 min) Splitless taper (4 mm) w/semivolatiles wool (cat.# 20798-231.1) 250 °C 40 mL/min Rxi®-17Sil MS: 90 °C (hold 1 min) to 320 °C at 3.75 °C/min (hold 2.67 min) Rxi®-1ms: 95 °C (hold 1 min) to 325 °C at 3.75 °C/min (hold 2.67 min) He, corrected constant flow (2.2 mL/min)

Modulation Modulator Temp. Offset: 20 °C Second Dimension Separation Time: 3 sec Hot Pulse Time: 0.9 sec Cool Time between Stages: 0.6 sec Detector TOFMS Transfer Line Temp.: 300 °C Analyzer Type: TOF Source Temp.: 250 °C Electron Energy: 70 eV Mass Defect: -20 mu/100 u Solvent Delay Time: 5 min Tune Type: PFTBA Ionization Mode: EI Acquisition Range: 45 to 550 amu Spectral Acquisition Rate: 100 spectra/sec Instrument LECO Pegasus 4D GCxGC-TOFMS Notes PAHs (shown in box) elute in a relatively narrow band and are identified by the white peak marker dots.

Melamine Spike in Cat Food on Rtx®-5MS

5

Reliable identifications in matrix.

1. 2. 3. 4. 5.

Peaks Cyanuric acid Ammelide Ammeline Melamine Benzoguanamine

Get More! High Sensitivity Melamine GC-MS Analysis of Cat Food Modified Conditions Save Costs & Reduce Maintenance Read the full article at

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Column Sample 1

2 3

8.5

9.0

9.5

10.0

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4

10.5 11.0 Time (min)

11.5

12.0

12.5

13.0 13.5 GC_FF00977

Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector Mode: Transfer Line Temp.: Ionization Mode:

Rtx®-5MS, 30 m, 0.25 mm ID, 0.25 μm (cat.# 12623) Melamine, cyanuric acid, ammelide, ammeline, benzoguanamine in dry cat food 10 μg/mL prederivatized 1 μL splitless (hold 1 min) 3.5 mm splitless taper (cat.# 22286) 280 °C 75 °C to 320 °C at 15 °C/min (hold 4 min) He, constant flow 1 mL/min MS SIM 290 °C EI

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GC CHROMATOGRAMS | FOOD SAFETY

Food Contaminants Marijuana Pesticides by GCxGC on Rxi®-5Sil MS and Rtx®-200

NEW!

GC_FF1205 Column

Sample Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp:

Carrier Gas Modulation Modulator Temp. Offset: Second Dimension Separation Time: Hot Pulse Time: Cool Time between Stages: Detector Transfer Line Temp.: Analyzer Type: Source Temp.: Electron Energy: Mass Defect: Solvent Delay Time: Tune Type: Ionization Mode: Acquisition Range: Spectral Acquisition Rate: Instrument

Rxi®-5Sil MS 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) Rtx®-200 1.3 m, 0.25 mm ID, 0.25 μm (cat.# 15020) Toluene 1 μL splitless (hold 1 min) Sky® 4 mm single taper w/wool (cat.# 23303.1) 250 °C 40 mL/min Rxi®-5Sil MS: 80 °C (hold 1 min) to 310 °C at 5 °C/min Rtx®-200: 85 °C (hold 1 min) to 315 °C at 5 °C/min He, corrected constant flow (2 mL/min) 20 °C 3 sec 0.9 sec 0.6 sec TOFMS 290 °C TOF 225 °C 70 eV -20 mu/100 u 5 min PFTBA EI 45-550 amu 100 spectra/sec LECO Pegasus 4D GCxGC-TOFMS

1-800-356-1688 or 1-814-353-1300

tR 1 (sec) Methamidophos 480 Dichlorvos 507 1,2,3,5-Tetrachlorobenzene 621 Nicotine 654 Mevinphos 768 Acephate 771 Pentachlorobenzene 885 o-Phenylphenol 888 Tebuthiuron 894 Tetrachloronitrobenzene 984 Omethoate 990 2,3,5,6-Tetrachloroaniline 1029 -BHC 1128 Hexachlorobenzene 1134 Pentachloroanisole 1152 Dimethoate 1164 -BHC 1191 Pentachloronitrobenzene 1197 Pentachlorobenzonitrile 1206 -BHC 1212 Chlorothalonil 1251 Anthracene 1257 Diazinon 1260 -BHC 1281 Pentachloroaniline 1314 Vinclozolin 1371 Carbaryl 1383 Metalaxyl 1398 Peaks

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

Notes

tR 2 (sec) 2.51 2.11 1.12 1.39 2.59 0.17 1.16 1.21 2.06 1.59 0.25 1.28 1.40 1.16 1.26 2.46 1.64 1.52 1.69 1.43 2.56 1.42 1.25 1.49 1.30 2.08 2.06 1.87

Peaks 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.

Pentachlorothioanisole Pirimiphos methyl Methiocarb Dichlofluanid Malathion Chlorpyrifos Fenthion DCPA Parathion Cyprodinil Heptachlor epoxide Thiabendazole Captan Folpet Procymidone Endosulfan I Imazalil 4,4'-DDE Dieldrin Myclobutanil Endrin Endosulfan II 4,4'-DDD Oxadixyl 2,4'-DDT Carfentrazone ethyl Endosulfan sulfate Fenhexamid

tR 1 (sec) 1431 1434 1437 1446 1461 1473 1479 1482 1488 1548 1557 1572 1578 1590 1590 1638 1674 1695 1698 1707 1740 1767 1785 1785 1791 1848 1851 1863

tR 2 (sec) 1.20 1.33 1.59 2.00 1.79 1.38 1.43 1.71 2.10 1.20 1.38 1.47 1.83 1.74 2.24 1.41 1.88 1.17 1.40 2.22 1.44 1.55 1.31 2.94 1.16 1.87 2.08 1.44

Peaks 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78. 79.

4,4'-DDT Propargite Piperonyl butoxide Iprodione Bifenthrin Dicofol Fenpropathrin Phosalone Azinphos methyl cis-Permethrin Coumaphos trans-Permethrin Cypermethrin 1 Cypermethrin 2 Cypermethrin 3 Cypermethrin 4 Pyraclostrobin Fluvalinate 1 Fluvalinate 2 Difenoconazole 1 Difenoconazole 2 Deltamethrin Azoxystrobin

tR 1 (sec) 1869 1911 1926 1962 1986 1995 2004 2046 2049 2190 2196 2205 2292 2304 2310 2316 2400 2409 2418 2439 2445 2478 2496

tR 2 (sec) 1.23 1.31 1.06 1.74 1.17 1.20 1.51 1.86 1.80 1.14 2.33 1.18 1.49 1.54 1.53 1.58 1.42 1.72 1.70 1.55 1.55 1.49 1.70

Rtx®-200 (cat.# 15020) is a 15 m column. A 1.3 m section was used as the second dimension column.

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GC CHROMATOGRAMS | FOOD SAFETY

Food Contaminants Acrylamide (Reference Standard) on Stabilwax®

Acrylamide (Potato Chip Extract) on Stabilwax®

Peaks 1. Acrylamide

Peaks 1. Acrylamide

1

blank 0.5

1.0

1.5

2.0

2.5

3.0

GC_FF00642

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Stabilwax®, 15 m, 0.53 mm ID, 0.50 μm (cat.# 10637) Acrylamide standard Water 25 μg/mL 1 μL splitless (hold 0.5 min) Auto SYS splitless w/wool (2 mm ID) (cat.# 20830) 260 °C 100 °C (hold 0.5 min) to 200 °C at 15 °C/min He, constant pressure 62 cm/sec @ 100 °C FID @ 260 °C

3.5

4.0

4.5

5.0

5.5

Time (min)

Column Sample Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

6.0

6.5

7.0

GC_FF00643

Stabilwax®, 15 m, 0.53 mm ID, 0.50 μm (cat.# 10637) 1 g of potato chips spiked with 100 μg acrylamide 1 μL splitless (hold 0.5 min) Auto SYS splitless w/wool (2 mm ID) (cat.# 20830) 260 °C 100 °C (hold 0.5 min) to 200 °C at 15 °C/min He, constant pressure 62 cm/sec @ 100 °C FID @ 260 °C

Hexachlorocyclohexanes in Sage QuEChERS Extract (Zoom of GCxGC-TOFMS Contour Plot)

NEW!

GCxGC with orthogonal Rxi®-5Sil MS and Rtx®-200 columns is a powerful way to handle complex samples like dietary supplement extracts. Note separation of gamma-HCH from the isobaric interference above. GC_FF1194 Column Sample Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Modulation Modulator Temp. Offset: Second Dimension Separation Time:

Rxi®-5Sil MS 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) Rtx®-200 1.5 m, 0.18 mm ID, 0.20 μm (cat.# 45001) Toluene 1 μL splitless (hold 1 min) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C 40 mL/min Rxi®-5Sil MS: 80 °C (hold 1 min) to 310 °C at 4 °C/min (hold 1.5 min) Rtx®-200: 90 °C (hold 1 min) to 320 °C at 4 °C/min (hold 1.5 min) He, constant flow 1.8 mL/min 25 °C

Hot Pulse Time: Cool Time between Stages: Detector Transfer Line Temp.: Analyzer Type: Source Temp.: Electron Energy: Mass Defect: Solvent Delay Time: Ionization Mode: Acquisition Range: Spectral Acquisition Rate: Instrument Notes

1.2 sec 0.8 sec TOFMS 290 °C TOF 225 °C 70 eV -20 mu/100 u 4 min EI 45 to 550 amu 100 spectra/sec LECO Pegasus 4D GCxGC-TOFMS See application note GNAN1338 for extraction and cleanup details. A 1.5 m length of the Rtx®-200 column was trimmed from a 10 m column. Columns were connected with a universal Press-Tight® connector (cat.# 20429).

4 sec

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GC CHROMATOGRAMS | FOOD SAFETY

Packaging Volatiles Food Packaging Volatiles on Rtx®-5MS 1. 2. 3. 4. 5. 6.

Peaks Isopropanol Methylene chloride 2-Methyl-1-propanol Tetrahydrofuran Benzene Toluene

Column Injection Liner: Inj. Temp.: Purge and Trap Instrument: Trap Type: Purge: Dry Purge: Desorb Preheat Temp.: Desorb: Bake: Interface Connection: Transfer Line Tubing: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Mode: Source Temp.: Electron Energy: Scan Range: Instrument

7. 8. 9. 10. 11. 12.

Hexanal Furfural 4-Heptanone (IS) Butyl ether Styrene Dodecane

Rtx®-5MS, 30 m, 0.25 mm ID, 1.00 μm (cat.# 12653) Purge and trap split (split ratio 20:1) 1 mm ID 250 °C Tekmar LSC-3100 purge & trap Vocarb 3000, type K 10 min @ 60 °C, flow 40 mL/min 3 min, flow 40 mL/min 220 °C 2 min @ 245 °C, flow 40 mL/min 6 min @ 230 °C injection port Siltek®/Sulfinert® tubing (cat.# 22501) 50 °C to 92 °C at 3 °C/min to 220 °C at 20 °C/min (hold 1 min) He, constant flow 1 mL/min 36 cm/sec MS Scan 280 °C EI @ 70 eV 35-260 amu HP6890 GC & 5973 MSD

GC_FF00457

Food Packaging Volatiles by Purge & Trap GC-MS on Rtx®-5MS, Overwrap at the Seam

1. 2. 3. 4. 5. 6. 7. 8.

Peaks Tetrahydrofuran 1-Butanol Toluene Hexanal Ethylbenzene 4-Heptanone Butyl ether Styrene

Column Injection Liner: Inj. Temp.: Purge and Trap Instrument: Trap Type: Purge: Dry Purge: Desorb Preheat Temp.: Desorb: Bake: Interface Connection: Transfer Line Tubing: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Mode: Source Temp.: Electron Energy: Scan Range: Instrument

9. 10. 11. 12. 13. 14. 15.

1-Methylethylbenzene Propylbenzene Benzaldehyde Benzeneacetaldehyde Acetophenone Benzoic acid, methyl ester Decanal

Rtx®-5MS, 30 m, 0.25 mm ID, 1.00 μm (cat.# 12653) Purge and trap split (split ratio 20:1) 1 mm ID 250 °C Tekmar LSC-3100 purge & trap Vocarb 3000, type K 10 min @ 60 °C, flow 40 mL/min 3 min, flow 40 mL/min 220 °C 2 min @ 245 °C, flow 40 mL/min 6 min @ 230 °C Injection port Siltek®/Sulfinert® tubing(cat.# 22501) 50 °C to 92 °C at 3 °C/min to 220 °C at 20 °C/min (hold 1 min) He, constant flow 1 mL/min 36 cm/sec MS Scan 280 °C EI @ 70 eV 35-260 amu HP6890 GC & 5973 MSD

GC_FF00459

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GC CHROMATOGRAMS | FOOD SAFETY

Packaging Volatiles Food Packaging Volatiles by Purge & Trap GC-MS on Rtx®-5MS (Purge & Trap GC-MS)

1. 2. 3. 4. 5. 6.

Peaks Ethyl acetate Toluene 4-Heptanone n-Butyl ether Styrene Alkanes

Column Sample Injection Liner: Inj. Temp.: Purge and Trap Instrument: Trap Type: Purge: Dry Purge: Desorb Preheat Temp.: Desorb: Bake: Interface Connection: Transfer Line Tubing: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Mode: Source Temp.: Electron Energy: Scan Range: Instrument

Rtx®-5MS, 30 m, 0.25 mm ID, 1.00 μm (cat.# 12653) Overwrap, inner bowl Purge and trap split (split ratio 20:1) 1 mm ID 250 °C Tekmar LSC-3100 purge & trap Vocarb 3000, type K 10 min @ 60 °C, flow 40 mL/min 3 min, flow 40 mL/min 220 °C 2 min @ 245 °C, flow 40 mL/min 6 min @ 230 °C Injection port Siltek®/Sulfinert® tubing (cat.# 22501) 50 °C to 92 °C at 3 °C/min to 220 °C at 20 °C/min (hold 1 min) He, constant flow 1 mL/min 36 cm/sec MS Scan 280 °C EI @ 70 eV 35-260 amu HP6890 GC & 5973 MSD

GC_FF00462

Food Packaging Volatiles by Purge & Trap GC-MS on Rtx®-5MS (Purge & Trap GC-MS) 1. 2. 3. 4. 5. 6. 7. 8.

Peaks Tetrahydrofuran Ethylbenzene 4-Heptanone Styrene Benzaldehyde Nonanal Decanal Cinnamaldehyde

Column Sample Injection Liner: Inj. Temp.: Purge and Trap Instrument: Trap Type: Purge: Dry Purge: Desorb Preheat Temp.: Desorb: Bake: Interface Connection: Transfer Line Tubing: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Mode: Source Temp.: Electron Energy: Scan Range: Instrument

Rtx®-5MS, 30 m, 0.25 mm ID, 1.00 μm (cat.# 12653) Overwrap, lid of bowl Purge and trap split (split ratio 20:1) 1 mm ID 250 °C Tekmar LSC-3100 purge & trap Vocarb 3000, type K 10 min @ 60 °C, flow 40 mL/min 3 min, flow 40 mL/min 220 °C 2 min @ 245 °C, flow 40 mL/min 6 min @ 230 °C Injection port Siltek®/Sulfinert® tubing (cat.# 22501) 50 °C to 92 °C at 3 °C/min to 220 °C at 20 °C/min (hold 1 min) He, constant flow 1 mL/min 36 cm/sec MS Scan 280 °C EI @ 70 eV 35-260 amu HP6890 GC & 5973 MSD

GC_FF00461

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GC CHROMATOGRAMS | FOOD SAFETY

PAHs NIST SRM 2260a PAH Mix on Rxi®-PAH

NEW!

GC_FF1223 Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Pulse Pressure: Pulse Time: Purge Flow: Oven Oven Temp.: Carrier Gas Flow Rate: Detector Mode: SIM Program:

Transfer Line Temp.: Analyzer Type: Source Temp.: Quad Temp.: Solvent Delay Time: Tune Type: Ionization Mode: Instrument

Rxi®-PAH, 40 m, 0.18 mm ID, 0.07 μm (cat.# 49316) NIST SRM 2260a PAH mix Toluene 0.2 - 2 μg/mL (SRM 2260a PAH mix was diluted 5x in toluene) 0.5 μL pulsed splitless (hold 0.58 min) Sky® 2 mm single taper w/wool (cat.# 23316.1) 275 °C 80 psi (551.6kPa) 0.6 min 40 mL/min 110 °C (hold 1 min) to 210 °C at 37 °C/min to 260 °C at 3 °C/min to 350 °C at 11 °C/min (hold 4.5 min) He, constant flow 1.4 mL/min MS SIM Start Time Group (min) Ion(s) (m/z) Dwell (ms) 1 3.00 128, 152, 153, 154, 165 40 2 5.50 178, 184, 190, 202 50 3 13.00 226, 228 100 4 20.00 252 200 5 26.00 276, 278 100 6 29.00 300, 302 150 350 °C Quadrupole 350 °C 200 °C 3.00 min PFTBA EI Agilent 7890A GC & 5975C MSD

1-800-356-1688 or 1-814-353-1300

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36.

Peaks Quant Ion (m/z) Naphthalene 128 Biphenyl 154 Acenaphthylene 152 Acenaphthene 153 Fluorene 165 Dibenzothiophene 184 Phenanthrene 178 Anthracene 178 4H-Cyclopenta[def]phenanthrene 190 Fluoranthene 202 Pyrene 202 Benzo[ghi]fluoranthene 226 Benzo[c]phenanthrene 228 Benz[a]anthracene 228 Cyclopenta[cd]pyrene 226 Triphenylene 228 Chrysene 228 Benzo[b]fluoranthene 252 Benzo[k]fluoranthene 252 Benzo[j]fluoranthene 252 Benzo[a]fluoranthene 252 Benzo[e]pyrene 252 Benzo[a]pyrene 252 Perylene 252 Dibenz[a,j]anthracene 278 Dibenz[a,c]anthracene 278 Indeno[1,2,3-cd]pyrene 276 Dibenz[a,h]anthracene 278 Benzo[b]chrysene 278 Picene 278 Benzo[ghi]perylene 276 Anthanthrene 276 Dibenzo[b,k]fluoranthene 302 Dibenzo[a,e]pyrene 302 Coronene 300 Dibenzo[a,h]pyrene 302

SIM Group # 1 1 1 1 1 2 2 2 2 2 2 3 3 3 3 3 3 4 4 4 4 4 4 4 5 5 5 5 5 5 5 5 6 6 6 6

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631


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Cholesterols Underivatized Cholesterol on Rxi®-5ms A. Temperature program conditions. Oven temp.: 200 °C (hold 1 min) to 330 °C @ 20 °C/min (hold 7.5 min)

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Peaks 1. 5--Cholestane (IS) 2. Cholesterol

GC_FF00881

B. Isothermal conditions will maximize sample throughput. Oven temp.: 300 °C (hold 10 min)

One column, many cholesterol methods.

Column Sample

Rxi® -5ms, 15 m, 0.25 mm ID, 0.25 μm (cat.# 13420) 1,000 μg/mL cholesterol in DMF 1,000 μg/mL 5--cholestane in hexane 25 ng cholesterol, 150 ng 5--cholestane on column

Injection Inj. Vol.: Liner: Inj. Temp.: Carrier Gas Linear Velocity: Detector

1 μL split (split ratio 20:1) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C He, constant pressure (9.7 psi, 66.9 kPa) 24 cm/sec @ 200 °C FID @ 340 °C

GC_FF00882

Derivatized Cholesterol on Rxi®-5ms A. Temperature program conditions. Oven temp.: 200 °C (hold 1 min) to 330 °C @ 20 °C/min (hold 7.5 min)

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Peaks 1. 5--Cholestane (IS) 2. Cholesterol

GC_FF00883

B. Isothermal conditions will maximize sample throughput. Oven temp.: 300 °C (hold 10 min)

Column Sample

Rxi®-5ms, 15 m, 0.25 mm ID, 0.25 μm (cat.# 13420) 1,000 μg/mL cholesterol in hexane 1,000 μg/mL 5--cholestane in hexane 50 ng derivatized cholesterol, 150 ng 5--cholestane on column

Injection Inj. Vol.: Liner: Inj. Temp.: Carrier Gas Linear Velocity: Detector

1 μL split (split ratio 20:1) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C He, constant pressure (9.7 psi, 66.9 kPa) 24 cm/sec @ 200 °C FID @ 340 °C

GC_FF00884

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GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Dietary Supplements Dietary Supplement (Finished Product) QuEChERS Extract Cleaned with Cartridge SPE (GCxGC-TOFMS Contour Plot)

NEW!

GCxGC with orthogonal Rxi®-5Sil MS and Rtx®-200 columns is a powerful way to handle complex samples like dietary supplement extracts.

GC_FF1191 Column Sample Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Modulation Modulator Temp. Offset: Second Dimension Separation Time: Hot Pulse Time: Cool Time between Stages: Detector Transfer Line Temp.: Analyzer Type: Source Temp.: Electron Energy: Mass Defect: Solvent Delay Time: Ionization Mode: Acquisition Range: Spectral Acquisition Rate: Instrument Notes

1-800-356-1688 or 1-814-353-1300

Rxi®-5Sil MS 30 m, 0.25 mm ID, 0.25 μm (cat.# 13623) Rtx®-200 1.5 m, 0.18 mm ID, 0.20 μm (cat.# 45001) Toluene 1 μL splitless (hold 1 min) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C 40 mL/min Rxi®-5Sil MS: 80 °C (hold 1 min) to 310 °C at 4 °C/min (hold 1.5 min) Rtx®-200: 90 °C (hold 1 min) to 320 °C at 4 °C/min (hold 1.5 min) He, constant flow 1.8 mL/min 25 °C 4 sec 1.2 sec 0.8 sec TOFMS 290 °C TOF 225 °C 70 eV -20 mu/100 u 4 min EI 45 to 550 amu 100 spectra/sec LECO Pegasus 4D GCxGC-TOFMS See application note GNAN1338 for extraction and cleanup details. A 1.5 m length of the Rtx®-200 column was trimmed from a 10 m column. Columns were connected with a universal Press-Tight® connector (cat.# 20429).

Restek is your complete source for analyzing pesticides in dietary supplements. www.restek.com/dietary

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633


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Essential Oils Lemon Oil on Rtx®-5

GC_FF00138 Column Sample Injection Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Notes

Rtx®-5, 30 m, 0.32 mm ID, 0.25 μm (cat.# 10224) Wet needle split injection of a neat lemon oil Split (split ratio 100:1) 250 °C 75 °C (hold 8 min) to 250 °C at 4 °C/min H2, constant flow 3.2 mL/min 40 cm/sec FID @ 250 °C FID sensitivity: 2 x 10-11 AFS

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

Peaks Heptanol -Thujene -Pinene Camphene Sabinene -Pinene 6-Methyl-5-hepten-2-one Myrcene Octanal -Phellandrene 3-Carene -Terpinene p-Cymene Limonene -Terpinene Octanol Terpinolene Linalool Nonanal Citronellal Terpinene-4-ol -Terpineol Decanol Octyl acetate Nerol Neral Carvone Geraniol Geranial Nonyl acetate Citronellyl acetate Neryl acetate Geranyl acetate Dodecanal -Caryophyllene trans--Bergamotene -Humulene -Bisabolene

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30.

Peaks -Pinene -Pinene Sabinene Myrcene -Terpinene L-Limonene 1,8-Cineole cis-Ocimene -Terpinene p-Cymene Terpinolene 3-Octyl acetate 3-Octanol l-Menthone trans-Sabinenehydrate -Bourbonene Linalool Terpinene-4-ol -Caryophyllene Dihydrocarvone trans-Dihydrocarvyl acetate trans--Farnesene -Terpineol Germacrene- Carvone cis-Carvyl acetate trans-Carveol cis-Carveol cis-Jasmone Viridiflorol

Spearmint Oil (Native ) on Stabilwax®

GC_FF00140 Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

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Stabilwax®, 60 m, 0.25 mm ID, 0.25 μm (cat.# 10626) Spearmint oil Neat 0.2 μL split (split ratio 100:1) 250 °C 75 °C (hold 4 min) to 200 °C at 4 °C/min (hold 10 min) H2, constant pressure 40 cm/sec @ 160 °C FID @ 250 °C FID sensitivity: 4 x 10-11 AFS

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GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Essential Oils Synthetic Essential Oil Mixture on Rtx®-1 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

Peaks Ethyl butyrate trans-2-Hexenol -Pinene Benzaldehyde Camphene Octanol -Myrcene -Pinene -Phellandrene p-Cymene L-Limonene Camphor trans-Sabinene hydrate Linalool Citronellal l-Menthone Menthofuran l-Menthol -Terpineol Linalyl acetate -Citronellol

Column

GC_FF00534

Injection Inj. Vol.: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Source Temp.:

22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42.

Nerol Carveol Anisaldehyde Carvone Geraniol Anethole Cinnamic alcohol Eugenol Neryl acetate Geranyl acetate Vanillin Coumarin -Ionone Ethyl vanillin -Caryophyllene -Caryophyllene -Ionone Valencene Ethyl laurate Amyl cinnamic aldehyde Nootketone

Rtx®-1, 60 m, 0.25 mm ID, 0.25 μm (cat.# 10126) 1 μL split 250 °C 100 mL/min 100 °C to 260 °C at 4 °C/min (hold 1 min) He, constant linear velocity 30 cm/sec @ 50 °C MS Scan 280 °C

Citronella Java Oil on Stabilwax® 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.

Peaks Limonene Citronellal Linalool Borneol -Elemene -Caryophyllene Neryl acetate -Terpineol Germancrene- -Citronellol Geranyl acetate -Cadenene Nerol Geraniol Eugenol -Bergamotene

Column

GC_FF00145

1-800-356-1688 or 1-814-353-1300

Sample Injection Inj. Vol.: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Mode: Source Temp.:

Stabilwax®, 60 m, 0.25 mm ID, 0.25 μm (cat.# 10626) Citronella Java oil 1.0 μL split 250 °C 100 mL/min 100 °C to 260 °C at 4 °C/min (hold 1 min) He, constant pressure 30 cm/sec @ 50 °C MS Scan 280 °C

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635


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

FAMEs FAMEs (AOAC 996.06 Standard) on Rt®-2560

Food industry FAME mix cat.# 35077 12

2 3

4

18

6

8

16

1

21 27 34

5

7

9 10

11

24 29 23 26 30 33 13 14 15 17 19 20 22 25 28 31 36 32 35

37

GC_FF00649 Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

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Peaks C4:0 Methyl butyrate C6:0 Methyl hexanoate C8:0 Methyl octanoate C10:0 Methyl decanoate C11:0 Methyl undecanoate C12:0 Methyl laurate C13:0 Methyl tridecanoate C14:0 Methyl myristate C14:1 Methyl myristoleate (cis-9) C15:0 Methyl pentadecanoate C15:1 Methyl pentadecenoate (cis-10) C16:0 Methyl palmitate C16:1 Methyl palmitoleate (cis-9) C17:0 Methyl heptadecanoate C17:1 Methyl heptadecenoate (cis-10) C18:0 Methyl stearate C18:1 Methyl elaidate (trans-9) C18:1 Methyl oleate (cis-9) C18:2 Methyl linoleaidate (trans-9,12)

Rt®-2560, 100 m, 0.25 mm ID, 0.20 μm (cat.# 13199) Food industry FAME mix (cat.# 35077) Methylene chloride 30 mg/mL total FAMEs 2.0 μL split (split ratio 200:1) Splitless (4 mm ID) (cat.# 20814) 225 °C 100 °C (hold 4 min) to 240 °C at 3 °C/min (hold 10 min) H2, constant flow 1.2 mL/min FID @ 250 °C

% in Mix 4.0 4.0 4.0 4.0 2.0 4.0 2.0 4.0 2.0 2.0 2.0 6.0 2.0 2.0 2.0 4.0 2.0 4.0 2.0

20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37.

Peaks % in Mix C18:2 Methyl linoleate (cis-9,12) 2.0 C20:0 Methyl arachidate 4.0 C18:3 Methyl -linolenate (cis-6,9,12) 2.0 C20:1 Methyl eicosenoate (cis-11) 2.0 C18:3 Methyl linolenate (cis-9,12,15) 2.0 C21:0 Methyl heneicosanoate 2.0 C20:2 Methyl eicosadienoate (cis-11,14) 2.0 C22:0 Methyl behenate 4.0 C20:3 Methyl eicosatrienoate (cis-8,11,14) 2.0 C22:1 Methyl erucate (cis-13) 2.0 C20:3 Methyl eicosatrienoate (cis-11,14,17) 2.0 C20:4 Methyl arachidonate (cis-5,8,11,14) 2.0 C23:0 Methyl tricosanoate 2.0 C22:2 Methyl docosadienoate (cis-13,16) 2.0 C24:0 Methyl lignocerate 4.0 C20:5 Methyl eicosapentaenoate (cis-5,8,11,14,17) 2.0 C24:1 Methyl nervonate (cis-15) 2.0 C22:6 Methyl docosahexaenoate (cis-4,7,10,13,16,19) 2.0

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GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

FAMEs FAMEs (cis/trans isomers) on Rt®-2560

Peaks 1. 2. 3. 4. 5. 6. 7. 8.

C18:0 methyl stearate C18:1 methyl petroselaidate (trans-6) C18:1 methyl elaidate (trans-9) C18:1 methyl transvaccenate (trans-11) C18:1 methyl petroselinate (cis-6) C18:1 methyl oleate (cis-9) C18:1 methyl vaccenate (cis-11) C18:2 methyl linoleate (cis-9,12)

Conc. (wt.%) 20.0 8.0 10.0 12.0 8.0 10.0 12.0 20.0

1

Excellent resolution of cis & trans isomers!

32

33

34

7

4

36

35

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

cis/trans FAME mix cat.# 35079

6

3 2

8

5

37

38

39

40

41

42 GC_FF00652

Rt®-2560, 100 m, 0.25 mm ID, 0.20 μm (cat.# 13199) cis/trans FAME mix (cat.# 35079) Methylene chloride 10 mg/mL total FAMEs 1 μL split (split ratio 20:1) Splitless (4 mm ID) (cat.# 20814) 225 °C 100 °C (hold 4 min) to 240 °C at 3 °C/min (hold 10 min) H2, constant flow 1.2 mL/min FID @ 250 °C

FAMEs (cis/trans isomers) on Rtx®-Wax

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

Peaks C14:0 C14:1n5 cis C14:1n5 trans C16:0 C16:1n7 cis C16:1n7 trans C18:0 C18:1 cis isomers (n12, n9, n7) C18:1 trans isomers (n12, n9, n7) C18:2n6 cis C18:2n6 trans C20:0 C20:1n9 cis C20:1n9 trans

Column Sample Conc.: Injection Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rtx®-Wax, 60 m, 0.25 mm ID, 0.25 μm (cat.# 12426) 40-75 ng split (split ratio 50:1) 220 °C 165 °C to 250 °C at 2 °C/min He, constant pressure 20 cm/sec @ 165 °C FID @ 250 °C

GC_FF00121

1-800-356-1688 or 1-814-353-1300

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637


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

FAMEs FAMEs (Marine Oil Standard) on FAMEWAX FAST analysis of marine oil FAMEs! 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

3 1

15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

Peaks C14:0 C15:0 C16:0 C16:1 C16:2 C17:0 C17:1 C16:4 C18:0 C18:1 (oleate) C18:1 (vaccenate) C18:2n6cis C18:3n3 C18:4n6

C18:4n3 C20:0 C20:1n7 C20:1n9 C20:4n6 C20:4n3 C20:5n3 C22:1n7 C21:5n3 C23:0 (IS) C22:5n6 C22:5n3 C22:6n3 C24:1

Column

FAMEWAX, 30 m, 0.32 mm ID, 0.25 μm (cat.# 12498)

Sample Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

12 mg/mL total FAMEs 0.5 μL split (split ratio 150:1) 3 mm split w/ wool (cat.# 20936-202.1) 250 °C 195 °C to 240 °C at 5 °C/min (hold 1 min) H2, constant flow 62 cm/sec FID @ 250 °C

4 24 21 10 27

2

57 6

8 9 11 12

17 14 13 15 16 18

22 19

20

23

26 25

28

GC_FF00568

FAMEs (Marine Oil Standard) on FAMEWAX Peaks 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

Column engineered for optimal resolution.

C14:0 C14:1 C16:0 C16:1 C18:0 C18:1 (oleate) C18:1 (vaccenate) C18:2 C18:3 C20:0 C20:1 C20:2 C20:4 C20:3 C20:5 C22:0 C22:1 C24:0 C22:6 C24:1

Conc. (μg/mL) 600 100 1,600 500 800 1,300 400 200 200 100 900 100 300 100 1,000 100 300 100 1,200 100

GC_FF00499 Column Sample Diluent: Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

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FAMEWAX, 30 m, 0.32 mm ID, 0.25 μm (cat.# 12498) Marine oil FAME mix (cat.# 35066) Isooctane 10,000 μg/mL (total FAMEs; see breakdown in peak list) 1 μL split (split ratio 100:1) 250 °C 195 °C to 240 °C at 5 °C/min (hold 1 min) H2, constant flow 3 mL/min FID @ 275 °C

1-800-356-1688 or 1-814-353-1300


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

FAMEs FAMEs (Cocoa Butter) on Stabilwax®

FAMEs (Saw Palmetto) on Rtx®-Wax Peaks

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

6

Column Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Peaks C14:0 C16:0 C16:1n7 C17:0 C18:0 C18:1n9 C18:2n6 C18:3n3 C20:0 C20:1n9 C22:0

8 Time (min) GC_FF00120

1.0 μL split (split ratio 45:1) 250 °C 200 °C to 250 °C at 8 °C/min (hold 3 min) H2, constant pressure 31.4 cm/sec @ 200 °C FID @ 250 °C FID sensitivity: 8 x 10-11 AFS

FAMEs (PUFA, Marine Source) on Rt®-2330 Peaks C14:0 C16:0 C16:1n7 C18:1n9 C18:1n7 C18:2n6 C18:3n3 C20:1n11 C20:1n9

10. 11. 12. 13. 14. 15. 16. 17. 18.

GC_FF00538 Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector

Stabilwax®, 30 m, 0.25 mm ID, 0.25 μm (cat.# 10623) FAME reference standard for cocoa butter

1. 2. 3. 4. 5. 6. 7. 8. 9.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

Conc. (mg/mL) Methyl caproate (C6:0) 0.4 Methyl caprylate (C8:0) 0.4 Methyl nonanoate (C9:0) 2.0 Methyl caprate (C10:0) 0.4 Methyl laurate (C12:0) 5.0 Methyl myristate (C14:0) 2.0 Methyl palmitate (C16:0) 2.0 Methyl palmitoleate (C16:1) 0.4 Methyl stearate (C18:0) 0.4 Methyl oleate (C18:1) 5.0 Methyl linoleate (C18:2) 1.0 Methyl linolenate (C18:3) 0.4

Rtx®-Wax, 30 m, 0.25 mm ID, 0.25 μm (cat.# 12423) Saw palmetto standard See peak list 1 μL split (split ratio 100:1) 250 °C 120 °C (hold 3 min) to 220 °C at 20 °C/min (hold 12 min) He, constant flow 1 mL/min 34 cm/sec FID @ 300 °C

FAMEs (Polyunsaturated Fatty Acids, Animal Source) on Rt®-2330 C20:1n7 C18:4n3 C22:1n11 C22:1n9 C20:4n3 C20:5n3 C21:5n3 C22:5n3 C22:6n3

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

Peaks C14:0 C16:0 C16:1n7 C18:0 C18:1n9 C18:1n7 C18:2n6 C18:3n6 C18:3n3 C20:3n6 C20:4n6 C20:5n3 C22:4n6 C22:5n3 C22:6n3

GC_FF00118 Column Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rt®-2330, 30 m, 0.25 mm ID, 0.20 μm (cat.# 10723) PUFA mix 0.5 μL split (split ratio 35:1) 225 °C 160 °C to 225 °C at 2 °C/min H2, constant pressure 45 cm/sec @ 160 °C FID @ 250 °C FID sensitivity: 8 x 10-11 AFS

1-800-356-1688 or 1-814-353-1300

GC_FF00119 Column Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rt®-2330, 30 m, 0.32 mm ID, 0.20 μm (cat.# 10724) PUFA 2 mix 0.1 μL split (split ratio 20:1) 260 °C 160 °C to 250 °C at 2 °C/min (hold 10 min) H2, constant pressure 40 cm/sec FID @ 260 °C FID sensitivity: 8 x 10-11 AFS

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639


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

FAMEs FAMEs (Flax Seed Oil) on FAMEWAX

1. 2. 3. 4. 5. 6.

Looking for more?

Peaks C16:0 C18:0 C18:1n9 C18:2n6 C18:3n6 C18:3n3

Column Sample Injection Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Visit our online technical library for chromatograms based on ASTM methods, USP procedures, and other applications.

FAMEWAX, 30 m, 0.25 mm ID, 0.25 μm (cat.# 12497) Flax seed oil Split 225 °C

www.restek.com/chromatograms

165 °C (hold 30 min) to 220 °C at 1.5 °C/min (hold 15 min) He, constant linear velocity 40 cm/sec FID @ 230 °C

GC_FF00364

FAMEs (NLEA Mix) on Rt®-2560 An Rt®-2560 column provides the resolution of cis & trans FAMEs needed for AOAC Method 996.06. Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp:

NLEA FAME mix cat.# 35078

Carrier Gas Flow Rate: Detector

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

Rt®-2560, 100 m, 0.25 mm ID, 0.20 μm (cat.# 13199) NLEA FAME mix (cat.# 35078) Methylene chloride 30 mg/mL total FAMEs 16 1 μL split (split ratio 100:1) Splitless (4 mm ID) (cat.# 20814) 225 °C 100 °C (hold 4 min) to 240 °C at 3 °C/min (hold 10 min) H2, constant flow 1.2 mL/min FID @ 250 °C

18

11

6

12

21 14

4 3

5 7

8 13

2 1

15 9 10

17

19 20

22

Peaks C4:0 methyl butyrate C6:0 methyl hexanoate C8:0 methyl octanoate C10:0 methyl decanoate C11:0 methyl undecanoate C12:0 methyl laurate C13:0 methyl tridecanoate C14:0 methyl myristate C14:1 methyl myristoleate (cis-9) C15:0 methyl pentadecanoate C16:0 methyl palmitate C16:1 methyl palmitoleate (cis-9) C17:0 methyl heptadecanoate C18:0 methyl stearate C18:1 methyl elaidate (trans-9) C18:1 methyl oleate (cis-9) C18:2 methyl linoelaidate (trans-9,12) C18:2 methyl linoleate (cis-9,12) C20:0 methyl arachidate C20:1 methyl eicosenoate (cis-11) C18:3 methyl linolenate (cis-9,12,15) C22:0 methyl behenate C22:1 methyl erucate (cis-13) C23:0 methyl tricosanoate C24:0 methyl lignocerate C20:5 methyl eicosapentaenoate (cis-5,8,11,14,17) C24:1 methyl nervonate (cis-15) C22:6 methyl docosahexaenoate (cis-4,7,10,13,16,19)

26 27 25

28

23 24

GC_FF00651

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GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Fatty Acids Fatty Acids (Free) on Rtx®-200

1. 2. 3. 4. 5. 6. 7. 8. 9.

Fatty Acids (Free) on Stabilwax®-DA (30 m, 0.25 mm ID, 0.25 μm) No derivatization needed!

Peaks Acetic acid Propionic acid Isobutyric acid n-Butyric acid Isovaleric acid n-Valeric acid Isocaproic acid Caproic acid Heptanoic acid

1. 2. 3. 4. 5. 6. 7. 8. 9.

No derivatization needed!

Peaks Acetic acid Propionic acid Isobutyric acid n-Butyric acid Isovaleric acid n-Valeric acid Isocaproic acid Caproic acid Heptanoic acid

GC_CH00282 Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Notes

GC_CH00280 Column

Rtx®-200, 30 m, 0.25 mm ID, 0.25 μm (cat.# 15023) Free fatty acid standard ~10-20 ng/μL

Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

0.8 μL split 250 °C 40 mL/min 90 °C H2, constant flow 1.4 mL/min 40 cm/sec FID @ 250 °C FID sensitivity: 4 x 10-11 AFS

Stabilwax®-DA, 30 m, 0.25 mm ID, 0.25 μm (cat.# 11023) Free acid standard ~10-20 ng/μL 1.0 μL split (split ratio 50:1) 250 °C 145 °C H2, constant pressure 40 cm/sec FID @ 250 °C FID sensitivity: 2 x 10-11 AFS

Fatty Acids (Free) on Stabilwax®-DA (30 m, 0.32 mm ID, 0.25 μm)

4

2

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

Great for low to high molecular weight fatty acids.

5 6

3

7

1 8 Column 9

Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Purge Flow: Oven Oven Temp: Carrier Gas Flow Rate: Detector

10 11

12

Peaks C4:0 Butyric acid C6:0 Caproic acid C8:0 Caprylic acid C10:0 Capric acid C12:0 Lauric acid C14:0 Myristic acid C16:0 Palmitic acid C18:0 Stearic acid C18:1 Oleic acid C18:2 Linoleic acid C18:3 Linolenic acid C20:0 Arachidic acid C22:0 Behenic acid Stabilwax®-DA, 30 m, 0.32 mm ID, 0.25 μm (cat.# 11024) Free fatty acid mix Methanol 100 ppm 1 μL splitless (hold 0.25 min) Laminar cup splitter 250 °C 75 mL/min 40 °C to 250 °C at 10 °C/min (hold 15 min) H2, constant flow 6 mL/min FID @ 250 °C

13

GC_FF00653

1-800-356-1688 or 1-814-353-1300

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641


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Flavors Flavor Volatiles on Rtx®-1 Column

Rtx®-1, 60 m, 0.53 mm ID, 0.50 μm (cat.# 10143)

Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Flavor volatiles test mix 0.8 μL split (split ratio 20:1) 220 °C 70 °C (hold 15 min) to 190 °C at 2 °C/min (hold 5 min) He, constant linear velocity 20 cm/sec @ 70 °C FID @ 260 °C FID Sensitivity: 64 x 10-11 AFS

GC_FF00536

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

Peaks Methanol Acetaldehyde Ethanol Acetone Isopropyl alcohol Methylene chloride Hexane Ethyl acetate Ethyl propionate n-Hexanal Ethyl butyrate Furfural

13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25.

trans-2-Hexenal -Thujene -Pinene Camphene Sabinene -Pinene Octanal Myrcene -Phellandrene -Terpinene p-Cymene -Limonene -Terpinene

26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

Octanol Terpinolene Nonanal Linalool cis-Limonene monoxide trans-Limonene monoxide Citronellal Terpinene-4-ol -Terpineol Decanal d/l Carveol Neral Carvone

39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50.

Geranial Neryl acetate Geranyl acetate -Ionone -Caryophyllene trans--Bergamotene BHA -Ionone Valencene -Elemene -Bisabolene Nootketone

Flavor Volatiles on Stabilwax® Column

Stabilwax®, 60 m, 0.53 mm ID, 0.50 μm (cat.# 10643)

Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Flavor volatiles test mix 0.8 μL split (split ratio 20:1) 220 °C 70 °C (hold 15 min) to 190 °C at 2 °C/min (hold 5 min) He, constant linear velocity 20 cm/sec @ 70 °C FID @ 260 °C FID Sensitivity: 64 x 10-11 AFS

GC_FF00537

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

Peaks Hexane Acetaldehyde Acetone Methanol Ethyl acetate Isopropyl alcohol Ethanol Methylene chloride Ethyl propionate -Pinene Ethylbutyrate

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12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23.

n-Hexanal -Pinene Sabinene Myrcene -Limonene 1,8-Cineole trans-2-Hexenal -Terpinene p-Cymene Terpinolene Octanal Nonanal

24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35.

cis-Limonene monoxidec trans-Limonene Furfural Citronellal Decanal Linalool Octanol trans--Bergamotene -Caryophyllene Terpinene-4-ol Neral -Terpineol

36. 37. 38. 39. 40. 41. 42. 43. 44.

Neryl acetate Valencene Geranial Carvone Geranyl acetate d/l Carveol -Ionone d/l Carveol -Ionone

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GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Flavors Sulfur Compounds in Headspace Sample of U.S. Beer on Rt®-XLSulfur 1. 2. 3. 4.

Sulfur Compounds in Headspace Sample of Canadian Beer on Rt®-XLSulfur

Peaks Hydrogen sulfide Methyl mercaptan Dimethyl sulfide and/or ethyl mercaptan Unknown

1. 2. 3. 4.

Peaks Hydrogen sulfide Methyl mercaptan Dimethyl sulfide and/or ethyl mercaptan Unknown

Column Column Sample Injection Oven Oven Temp: Carrier Gas Flow Rate: Detector Notes

Rt®-XLSulfur, 100/120 mesh, 1 m, 0.95 mm OD, 0.75 mm ID (cat.# 19806) Headspace of a U.S. beer sample Headspace-loop split

Sample Injection Oven Oven Temp:

60 °C to 260 °C at 15 °C/min (hold 5 min) He, constant flow 10 mL/min SCD @ 800 °C Injection: 1 cc sample loop, 6-port Valco® valve Detector sensitivity: attn. x 1

Carrier Gas Flow Rate: Detector Notes

Rt®-XLSulfur, 100/120 mesh, 1 m, 0.95 mm OD, 0.75 mm ID (cat.# 19806) Headspace of a Canadian beer sample Headspace-loop split 60 °C to 260 °C at 15 °C/min (hold 5 min) He, constant flow 10 mL/min SCD @ 800 °C Injection: 1 cc sample loop, 6-port Valco® valve Detector sensitivity: attn. x 1

GC_FF00494

Sulfur Compounds in Headspace Sample of Mexican Beer on Rt®-XLSulfur

1. 2. 3. 4.

GC_FF00487

Rum on Rtx®-1301

Peaks Hydrogen sulfide Methyl mercaptan Dimethyl sulfide and/or ethyl mercaptan Unknown

Column Sample Injection Oven Oven Temp: Carrier Gas Flow Rate: Detector Notes

Rt®-XLSulfur, 100/120 mesh, 1 m, 0.95 mm OD, 0.75 mm ID (cat.# 19806) Headspace of a Mexican beer sample Headspace-loop split 60 °C to 260 °C at 15 °C/min (hold 5 min) He, constant flow 10 mL/min SCD @ 800 °C Injection: 1 cc sample loop, 6 port Valco® valve Detector sensitivity: attn. x 1

GC_FF00483

1-800-356-1688 or 1-814-353-1300

GC_FF00110 Column Sample Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rtx®-1301, 60 m, 0.25 mm ID, 1.40 μm (cat.# 16016) Neat 1.0 μL split (split ratio 100:1) Cyclosplitter® (cat.# 20706) 150 °C 35 °C (hold 5 min) to 100 °C at 1 °C/min H2, constant pressure 40 cm/sec FID @ 200 °C

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

Peaks Acetaldehyde Methanol Ethanol Acetone Ethyl formate Isopropanol n-Propanol Ethyl acetate sec-Butanol Isobutanol Isoamyl alcohol Active amyl alcohol n-Amyl alcohol

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643


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Flavors Underivatized Alcoholic Beverage Acids and Methyl Esters on Stabilwax®-DA Peaks 6 15

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.

16

13 45 11 7

2

3

4

12 8

5

17

9

3

1

6

7 Column Sample Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Type:

14

10

8

9 10 11 12 Time (min) Stabilwax®-DA, 30 m, 0.18 mm ID, 0.18 μm (cat.# 550752)

13

14

Ethyl octanoate Acetic acid Propionic acid Isobutyric acid 3-Decanol Ethyl decanoate Ethyl laurate cis-Lactone 2-Phenylethanol trans-Lactone Methyl myristate Ethyl myristate Octanoic acid Ethyl palmitate Decanoic acid Dodecanoic acid Vanillin

Conc. (μg/mL) 100 100 100 100 50 50 50 100 50 100 50 50 100 50 100 100 100

15 GC_FF00500

Ethyl acetate 1 μL splitless (hold 0.5 min) Splitless (4 mm ID) w/glass wool (cat.# 20814-202.1) 240 °C 70 °C to 240 °C at 12 °C/min (hold 3 min) H2, constant linear velocity 28 psi, 193.1 kPa @ 240 °C FID N2

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GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Food Testing, Fragrances Egg Pasta Sterols & Glycerides on Rtx®-65TG

1. 2. 3. 4. 5.

Peaks Squalene (IS) Cholesterol -Sitosterol Diglycerides Triglycerides

Column Sample Conc.: Injection Inj. Vol.: Inlet Temp. Program: Oven Oven Temp: Carrier Gas Flow Rate: Detector Acknowledgement

GC_FF01046 Rtx®-65TG, 30 m, 0.25 mm ID, 0.10 μm (cat.# 17008) Fat extract from egg pasta in diethyl ether solution with 3,000 ppm squalene (IS) 50μg /mL 0.5 μL ptv split (split ratio 80:1) 70 °C (hold 12 min) to 370 °C at 99 °C/min (hold 5 min) 220 °C (hold 2 min) to 360 °C at 5 °C/min (hold 5 min) H2, constant flow 1.5 mL/min FID @ 370 °C Daniele Naviglio, Fabiana Pizzolongo; Dipartimento di Scienza degli Alimenti – Università degli Studi di Napoli “Federico II” – Via Università, 100 - 80055 Portici (NA) – Italia

5% Fragrance Materials Association Mix on Rtx®-1701 Peaks Column 1

Rtx®-1701, 60 m, 0.25 mm ID, 0.25 μm (cat.# 12026) Fragrance materials test mix (cat.# 31807) 5% FMA mix in acetone

Sample

2

Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

12

1 μL split (split ratio 40:1) Splitless (4 mm ID) (cat.# 20814) 285 °C 50 °C to 270 °C at 3 °C/min He, constant flow 0.6 mL/min FID @ 300 °C

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

Ethyl butyrate Limonene Eucalyptol Geraniol Benzoic acid Cinnamic aldehyde Hydroxycitronellal Thymol Cinnamyl alcohol Cinnamyl acetate Vanillin Benzyl salicylate

Conc. (wt.%) 35.7 20.0 0.5 0.6 1.0 0.5 5.0 0.3 0.3 0.3 0.1 35.7

7

3

6

4

8

9

10

5 0

5

10

15

1-800-356-1688 or 1-814-353-1300

20

25

30

35

11 40

45

50

55

60

65

Time (min) GC_FF00658

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645


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Fragrances Fragrance Allergens on Rxi®-1ms & Rxi®-17 (GC x GC)

NEW!

GC_FF01010

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

Peaks Limonene 1-Fluoronaphthalene Benzyl alcohol Benzeneacetaldehyde Eucalyptol -Linalool Camphor Methyl 2-octynoate Estragole Citronellol

11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

Citral 1 trans-Cinnamaldehyde Geraniol Citral 2 Anise alcohol Hydroxycitronellol Safrole Cinnamyl alcohol Methyl 2-nonynoate Eugenol Methyleugenol

22. Coumarin 23. Hydroxycitronellol contaminant 24. Iso-eugenol 25. -Isomethyl ionone 1 26. Lilial 27. -Isomethyl ionone 2 28. Amyl cinnamal 29. Lyral 1 30. Lyral 2 31. Amylcinnamyl alcohol 1 Column Sample Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp:

GC_FF01011

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32. 33. 34. 35. 36. 37. 38. 39.

Amylcinnamyl alcohol 2 Farnesol 1 Farnesol 2 Hexyl cinnamal 1 Benzyl benzoate Hexyl cinnamal 2 Benzyl salicylate Benzyl cinnamate

Rxi®-1ms 30 m, 0.25 mm ID, 0.25 μL (cat.# 13323) Rxi®-17 1 m, 0.10 mm ID, 0.10 μm (cat.# 13501) Fragrance allergens MTBE 0.2 μL split (split ratio 200:1) 4 mm laminar cup splitter (cat.# 20801) 250 °C Rxi®-1ms: 40 °C (hold 1 min) to 240 °C at 4 °C/min Rxi®-17: 45 °C (hold 1 min) to 245 °C at 4 °C/min He, corrected constant flow (2 mL/min)

Carrier Gas Modulation Modulator Temp. Offset: 20 °C Second Dimension Separation Time: 3 sec Hot Pulse Time: 0.8 sec Cool Time between Stages: 0.7 sec Detector FID @ 300 °C Constant Column + Constant Make-up: 50 mL/min Data Rate: 200 Hz Notes Additional Detector Conditions: Hydrogen: 40 mL/min Air: 450 mL/min

1-800-356-1688 or 1-814-353-1300


GC CHROMATOGRAMS | FOODS, FLAVORS, & FRAGRANCES

Preservatives Tocopherols and Tocotrienols on Rtx®-20

1

1. 2. 3. 4. 5. 6. 7. 8. 9.

2

3

Peaks -Tocopherol -Tocopherol -Tocopherol dl--Tocotrienol -Tocopherol dl--Tocotrienol dl--Tocotrienol Hexadecyl hexadecanoate dl--Tocotrienol

5 Column

8

Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp:

6

Carrier Gas Flow Rate: Detector

4

7

Rtx®-20, 30 m, 0.53 mm ID, 0.50 μm (cat.# 10340) Isooctane 1,000 μg/mL each component 1 μL split (split ratio 20:1) Splitless (4 mm ID) (cat.# 20814) 320 °C 270 °C to 290 °C at 2 °C/min to 320 °C at 10 °C/min (hold 1 min) H2, constant flow 5.2 mL/min FID @ 320 °C

9

GC_FF00634

Chromatogram Search Tool Search by compound name, synonym, CAS #, or keyword www.restek.com/chromatograms

1-800-356-1688 or 1-814-353-1300

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647


GC CHROMATOGRAMS | FORENSICS

Arson Accelerants Unleaded Gasoline on Rxi®-1ms

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

GC_PC01071 Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rxi®-1ms, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13323) Unleaded gasoline: unweathered (cat.# 30096) Methanol 5,000 μg/mL 1.0 μL split (split ratio 20:1) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C 50 °C (hold 2 min) to 75 °C at 10 °C/min to 300 °C at 20 °C/min (hold 5 min) He, constant flow 28 cm/sec FID @ 300 °C

99% Weathered Unleaded Gasoline on Rxi®-1ms

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

GC_PC01070 Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

648 www.restek.com

Rxi®-1ms, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13323) Unleaded gasoline: 99% weathered (cat.# 30436) Methanol 5,000 μg/mL 1.0 μL split (split ratio 20:1) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C 50 °C (hold 2 min) to 75 °C at 10 °C/min to 300 °C at 20 °C/min (hold 5 min) He, constant flow 28 cm/sec FID @ 300 °C

1-800-356-1688 or 1-814-353-1300


GC CHROMATOGRAMS | FORENSICS

Arson Accelerants Unweathered Kerosene on Rxi®-1ms

Mineral Spirits on Rxi®-1ms Rxi® Technology!

Rxi® Technology!

Exceptionally inert, ultra low-bleed capillary columns.

Exceptionally inert, ultra low-bleed capillary columns.

GC_PC01066

GC_PC01060 Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp:

Rxi®-1ms, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13323) Kerosene: unweathered (cat.# 31229) Methylene chloride 5,000 μg/mL 1 μL split (split ratio 20:1) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C 50 °C (hold 2 min) to 75 °C at 10 °C/min to 300 °C at 20 °C/min (hold 5 min) He, constant linear velocity 28 cm/sec @ 50 °C FID @ 300 °C

Carrier Gas Linear Velocity: Detector

50% Weathered Diesel Fuel #2 on Rxi®-1ms

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rxi®-1ms, 30 m, 0.25 mm ID, 0.25 μm (cat.# 13323) Mineral spirits: unweathered (cat.# 31225) Methylene chloride 5,000 μg/mL 1.0 μL split (split ratio 20:1) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C 50 °C (hold 2 min) to 75 °C at 10 °C/min to 300 °C at 20 °C/min (hold 5 min) He, constant flow 28 cm/sec FID @ 300 °C

Unweathered Diesel Fuel #2 on Rxi®-1ms

Rxi® Technology!

Rxi® Technology!

Exceptionally inert, ultra low-bleed capillary columns.

Exceptionally inert, ultra low-bleed capillary columns.

GC_PC00922

GC_PC00921 Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rxi®-1ms, 30 m, 0.25 mm ID, 0.50 μm (cat.# 13338) Diesel fuel #2: 50% weathered (cat.# 31235) Methylene chloride 5,000 μg/mL 1.0 μL split (split ratio 20:1) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C 50 °C (hold 2 min) to 75 °C at 10 °C/min to 300 °C at 20 °C/min (hold 5 min) He, constant linear velocity 28 cm/sec @ 50 °C FID @ 300 °C

1-800-356-1688 or 1-814-353-1300

Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rxi®-1ms, 30 m, 0.25 mm ID, 0.50 μm (cat.# 13338) Diesel fuel #2: unweathered (cat.# 31233) Methylene chloride 5,000 μg/mL 1.0 μL split (split ratio 20:1) Splitless taper (4 mm) w/wool (cat.# 22405) 250 °C 50 °C (hold 2 min) to 75 °C at 10 °C/min to 300 °C at 20 °C/min (hold 5 min) He, constant linear velocity 28 cm/sec @ 50 °C FID @ 300 °C

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649


GC CHROMATOGRAMS | FORENSICS

Blood Alcohols Blood Alcohol Analysis on Rtx®-BAC Plus 1 • Baseline separation of all compounds. • Symmetrical alcohol peaks.

NEW!

Peaks 1. 2. 3. 4. 5. 6. 7.

2

tR (min)

Methanol Acetaldehyde Ethanol Isopropanol Acetone tert-Butanol 1-Propanol (n-Propanol)

Column Sample Diluent: Conc.:

Conc. (μg/mL) 100 100 100 100 100 50 50

0.912 0.967 1.158 1.420 1.548 1.688 1.969

Injection Liner: Headspace-Loop Inj. Port Temp.: Instrument: Inj. Time: Transfer Line Temp.: Valve Oven Temp.: Standby flow rate: Sample Temp.: Sample Equil. Time: Vial Pressure: Pressurize Time: Loop Pressure: Loop Fill Time: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Instrument Notes

5

4

3 1

6 7

0.5

0.75

1

1.25

1.5

1.75

2

2.25

2.5

2.75

Rtx®-BAC Plus 1, 30 m, 0.32 mm ID, 1.8 μm (cat.# 18004) BAC resolution control standard n-P (cat.# 36010) BAC resolution control standard t-B (cat.# 36011) Water 50 μL of each standard were diluted in 900 μL water in a 20 mL headspace vial. Headspace-loop split (split ratio 50:1) 1 mm ID straight inlet liner (cat.# 20972) 200 °C Tekmar HT3 3 min 125 °C 125 °C 50 mL/min 60 °C 5 min 30 psi 1 min 20 psi 1 min 40 °C (hold 3 min) He, constant flow 80 cm/sec @ 40 °C FID @ 240 °C 30 mL/min N2 Agilent/HP6890 GC Headspace concentrator courtesy of Teledyne Tekmar, Mason, OH.

Time (min) G C_CF1153

Blood Alcohol Analysis on Rtx®-BAC Plus 2 • Narrow, highly symmetrical peaks. • All compounds separated in a fast, 2-minute analysis.

NEW!

tR (min)

Peaks 1. 2. 3. 4. 5. 6. 7.

1

Acetaldehyde Methanol Ethanol Acetone Isopropanol tert-Butanol 1-Propanol (n-Propanol)

Column Sample Diluent: Conc.: Injection Liner: Headspace-Loop Inj. Port Temp.: Instrument: Inj. Time: Transfer Line Temp.: Valve Oven Temp.: Standby flow rate: Sample Temp.: Sample Equil. Time: Vial Pressure: Pressurize Time: Loop Pressure: Loop Fill Time: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Instrument Notes

Conc. (μg/mL) 100 100 100 100 100 50 50

0.809 0.861 1.034 1.119 1.181 1.304 1.658

4

5 6

3 2

Rtx®-BAC Plus 2, 30 m, 0.32 mm ID, 0.6 μm (cat.# 18006) BAC resolution control standard n-P (cat.# 36010) BAC resolution control standard t-B (cat.# 36011) Water 50 μL of each standard were diluted in 900 μL water in a 20 mL headspace vial. Headspace-loop split (split ratio 50:1) 1 mm ID straight inlet liner (cat.# 20972) 200 °C Tekmar HT3 3 min 125 °C 125 °C 50 mL/min 60 °C 5 min 30 psi 1 min 20 psi 1 min 40 °C (hold 3 min) He, constant flow 80 cm/sec @ 40 °C FID @ 240 °C 30 mL/min N2 Agilent/HP6890 GC Headspace concentrator courtesy of Teledyne Tekmar, Mason, OH.

7

0.5

0.75

1

1.25

1.5

1.75

2

2.25

2.5

2.75

Time (min) GC_CF1154

650 www.restek.com

1-800-356-1688 or 1-814-353-1300


GC CHROMATOGRAMS | FORENSICS

GHB/GBL GHB Analysis (GBL and AMGBL) on Rtx®-BAC Plus 1 1

NEW!

Peaks 1. GBL 2. AMGBL Column Sample

2

Injection Liner: Headspace-Loop Inj. Port Temp.: Instrument: Inj. Time: Transfer Line Temp.: Valve Oven Temp.: Sample Temp.: Sample Equil. Time: Vial Pressure: Pressurize Time: Loop Pressure: Loop Fill Time: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Instrument Notes

Rtx®-BAC Plus 1, 30 m, 0.32 mm ID, 1.8 μm (cat.# 18004) Gamma-butyrolactone (GBL) (cat.# 34077) Alpha-methylene-gamma-butyrolactone (AMGBL) (cat.# 34079) Headspace-loop split (split ratio 10:1) 1 mm straight inlet liner (cat.# 20972) 200 °C Tekmar HT3 1 min 125 °C 125 °C 100 °C 10 min 30 psi 2 min 20 psi 1 min 80 °C (hold 0 min) to 180 °C at 10 °C/min (hold 0 min) He, constant flow 48 cm/sec FID @ 240 °C 30 mL/min N2 Agilent/HP6890 GC Sample was prepared by injecting 1 μL of each standard into a capped headspace vial. The mass of each compound inside the headspace vial was 1 μg. Headspace concentrator courtesy of Teledyne Tekmar, Mason, OH.

4.6

4.8

5

5.2

5.4 5.6 Time (min)

5.8

6

Now Online!

6.2

6.4 GC_CF1164

Our EZGC™ Web App Will Kick-Start Your GC Method Development

• EZ to Register – If you have a Restek login, you’re already done! (And if you don’t, you can get one at no charge and with no hassle.) • EZ to Get Started – A quick, 5-minute video will show you everything you need to know. • EZ to Use – Just enter your target compounds, and in seconds, the EZGC™ system gives you a customized method, including column, conditions, and model chromatogram. • EZ to Analyze – Model chromatograms are fully interactive. Zoom in, view chemical structures, and even overlay mass spectra. • EZ to Save – Print your chromatogram and custom settings, or save them for future reference.

Start developing incredible GC methods today!

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651


GC CHROMATOGRAMS | FORENSICS

Glycols Glycols on Rtx®-BAC Plus 1 and 2 Column Set 3

NEW!

Rtx®-BAC Plus 1 Peaks 1. 2. 3. 4.

2 1

Ethylene glycol Propylene glycol 1,3-Propanediol Diethylene glycol

BAC Plus 1 tR (min) 1.983 2.323 3.043 4.380

BAC Plus 2 tR (min) 2.207 2.433 3.278 4.385

4 Columns

1.5

2

2.5

3

3.5 Time (min)

4

4.5

5

3

Rtx®-BAC Plus 2

2 1 4

Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Instrument Notes

Rtx®-BAC Plus 1 30 m, 0.32 mm ID, 1.8 μm (cat.# 18004) and Rtx®-BAC Plus 2 30 m, 0.32 mm ID, 0.6 μm (cat.# 18006) using Rxi® guard column 5 m, 0.32 mm ID (cat.# 10039) with Universal “Y” Press-Tight® connector (cat.# 20405-261) Methanol:water (40:60) 200 μg/mL each glycol 1 μL split (split ratio 20:1) Sky® 4 mm straight inlet liner w/wool (cat.# 23300.1) 260 °C 60 °C (hold 0 min) to 240 °C at 20 °C/min (hold 5 min) He, constant flow 70 cm/sec FID @ 240 °C 30 mL/min N2 Agilent/HP6890 GC The Rtx®-BAC Plus 1 and Plus 2 columns were connected to the injection port using a ~12 inch section of guard column between the injection port and the universal “Y” Press-Tight® connector. Injections were performed manually with a Merlin Microshot injector (cat.# 22229).

1.5

2

2.5

3

3.5 Time (min)

4

4.5

5 GC_CF1163

free literature Rtx®-BAC Plus 1 and Rtx®-BAC Plus 2 Columns: Advanced Technology for Fast, Reliable Measurement of Alcohol in Blood Download your free copy from www.restek.com www.restek.com lit. cat.# CFBR1538-UNV

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GC CHROMATOGRAMS | FORENSICS

Inhalants Inhalants on Rtx®-BAC Plus 1 and Plus 2 Column Set 16

NEW!

Rtx®-BAC Plus 1 15

12

17, 18

4

19 7

6 5 2

1

0

9

3

2

14

13

8 10 11

4

6

8

10

12

Time (min)

16

Rtx®-BAC Plus 2 12

8, 7, 3

15

4

17, 18

6

19 11 10

5

14

13

9 1

2

0

2

4

6

8

10

Columns

Sample Diluent: Conc.: Injection Liner: Headspace-Loop Inj. Port Temp.: Instrument: Inj. Time: Transfer Line Temp.: Valve Oven Temp.: Sample Temp.: Sample Equil. Time: Vial Pressure: Pressurize Time: Loop Pressure: Loop Fill Time: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Instrument Notes

Rtx®-BAC Plus 1 30 m, 0.32 mm ID, 1.8 μm (cat.# 18004) and Rtx®-BAC Plus 2 30 m, 0.32 mm ID, 0.6 μm (cat.# 18006) using Rxi® guard column 5 m, 0.32 mm ID (cat.# 10039) with universal “Y” Press-Tight® connector (cat.# 20405-261) Water 50 μg/mL each inhalant Headspace-loop split (split ratio 50:1) 1 mm straight inlet liner (cat.# 20972) 220 °C Tekmar HT3 3 min 125 °C 125 °C 70 °C 5 min 30 psi 2 min 20 psi 1 min 40 °C (hold 4 min) to 120 °C at 10 °C/min (hold 0 min) He, constant flow 50 cm/sec FID @ 240 °C

12 GC_CF1162

Time (min)

Peaks 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

Methanol Ethanol Isopropanol Diethyl ether Acetone Methylene chloride MTBE Hexane Chloroform MEK Ethyl acetate Benzene Trichloroethylene MIBK Toluene Ethylbenzene m-Xylene p-Xylene o-Xylene

BAC Plus 1 tR (min) 1.340 1.694 2.072 2.149 2.256 2.405 3.185 3.683 3.956 4.210 4.524 5.390 6.306 8.101 8.162 10.286 10.487 10.487 10.990

BAC Plus 2 tR (min) 1.230 1.470 1.660 1.334 1.589 1.703 1.660 1.660 2.667 2.543 2.414 2.883 3.522 5.775 5.440 7.681 7.879 7.879 8.467

30 mL/min N2 Agilent/HP6890 GC The Rtx®-BAC Plus 1 and Plus 2 columns were connected to the injection port using a ~12 inch section of guard column between the injection port and the universal Y Press-Tight® connector. Headspace concentrator courtesy of Teledyne Tekmar, Mason, OH.

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653


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Fuels Total Glycerin in Biodiesel on MXT®-Biodiesel TG

Integra-Gap® Technology • Built-in retention gap • Eliminates connector

The best solution for analyzing total glycerin in biodiesel! Column Sample Diluent: Injection Inj. Vol.: Temp. Program: Oven Oven Temp:

GC_PC00969

Carrier Gas Flow Rate: Detector

Retention Gap

Liquid Phase

MXT®-Biodiesel TG, 14 m w/2 m Integra-Gap® (16 m total length), 0.53 mm ID, 0.16 μm (cat.# 70289) Biodiesel (B100), derivatized Heptane 1 μL cold on-column Oven track 50 °C (hold 1 min) to 180 °C at 15 °C/min to 230 °C at 7 °C/min to 380 °C at 30 °C/min (hold 5 min) H2, constant flow 4 mL/min FID @ 380 °C

Biodiesel Oil (B100) on Rtx®-Biodiesel TG

A. Rtx®-Biodiesel TG with Alumaseal® connector and 2 meters of 0.53 mm ID Hydroguard® tubing

B. Rtx®-Biodiesel TG with universal Press-Tight® connector and 2 meters of 0.53 mm ID Hydroguard® tubing

GC_PC00905 Column Sample Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector

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Rtx®-Biodiesel TG, 10 m, 0.32 mm ID, 0.10 μm (cat.# 10291) using Hydroguard® retention gap 2 m, 0.53 mm ID Biodiesel (B100) with butanetriol 12.5 ppm (12.5 ng on-column) 1.0 μL cold on-column Oven track mode 50 °C (hold 1 min) to 180 °C at 15 °C/min to 230 °C at 7 °C/min to 380 °C at 30 °C/min (hold 5 min) H2, constant flow 4 mL/min 79 cm/sec FID @ 380 °C

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Fuels B100 on MXT®-Biodiesel TG

Column Sample Diluent: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Flow Rate: Detector

MXT®-Biodiesel TG, 15 m, 0.32 mm ID, 0.10 μm (cat.# 70291) with a 2 m x 0.53 mm MXT® retention gap connected with an MXT® low-dead-volume connector (17 m total length) Biodiesel (B100), derivatized Heptane 1 μL cold on-column Oven track 50 °C (hold 1 min) to 180 °C at 15 °C/min to 230 °C at 7 °C/min to 380 °C at 30 °C/min (hold 5 min) H2, constant flow 3 mL/min FID @ 380 °C

GC_PC00968

ASTM D6584 Derivatized B100 and Internal Standards on MXT®-Biodiesel TG

Note perfect solvent peak shape!

GC_PC00935 Column Sample Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Flow Rate: Detector

MXT®-Biodiesel TG w/2 m x 0.53 mm retention gap, 10 m, 0.32 mm ID, 0.10 μm (cat.# 70290) B100 + IS butanetriol & tricaprin derivatized with MSTFA as per ASTM D6584 1.0 μL cold on-column Oven track 50 °C (hold 1 min) to 180 °C at 15 °C/min to 230 °C at 7 °C/min to 430 °C at 30 °C/min (hold 5 min) H2, constant flow 4 mL/min FID @ 430 °C

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655


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Fuels FAMEs in Biodiesel Oils on Stabilwax® Soy FAMEs in Biodiesel Oils on Stabilwax®

1. 2. 3. 4. 5. 6.

Peaks Myristic acid Palmitic acid Palmitoleic acid Stearic acid Oleic acid Linoleic acid

C14:0 C16:0 C16:1 C18:0 C18:1 C18:2

7. Linolenic acid 8. Arachidic acid 9. Gadoleic acid 10. Behenic acid 11. Lignoceric acid IS Methyl heptadecanoate

C18:3 C20:0 C20:1 C22:0 C24:0

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector

Stabilwax®, 30 m, 0.32 mm ID, 0.25 μm (cat.# 10624) Soy source of biodiesel (B100), prepared according to European Method EN 14103 1.0 μL split (split ratio 100:1) Cyclosplitter® (cat.# 20706) 250 °C 210 °C (hold 5 min) to 230 °C at 20 °C/min (hold 5 min) H2, constant flow 3 mL/min 60 cm/sec FID @ 250 °C

GC_PC00915

Tallow FAMEs in Biodiesel Oils on Stabilwax®

1. 2. 3. 4. 5. 6.

Peaks Myristic acid Palmitic acid Palmitoleic acid Stearic acid Oleic acid Linoleic acid

C14:0 C16:0 C16:1 C18:0 C18:1 C18:2

7. Linolenic acid 8. Arachidic acid 9. Gadoleic acid 10. Lignoceric acid 11. Nervonic acid IS Methyl heptadecanoate

C18:3 C20:0 C20:1 C24:0 C24:1

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector

Stabilwax®, 30 m, 0.32 mm ID, 0.25 μm (cat.# 10624) Tallow source of biodiesel (B100), prepared according to European Method EN 14103 1.0 μL split (split ratio 100:1) Cyclosplitter® (cat.# 20706) 250 °C 210 °C (hold 5 min) to 230 °C at 20 °C/min (hold 5 min) H2, constant flow 3 mL/min 60 cm/sec FID @ 250 °C

GC_PC00916

Rapeseed FAMEs in Biodiesel Oils on Stabilwax®

1. 2. 3. 4. 5. 6. 7.

Peaks Myristic acid Palmitic acid Palmitoleic acid Stearic acid Oleic acid Linoleic acid Linolenic acid

C14:0 C16:0 C16:1 C18:0 C18:1 C18:2 C18:3

8. Arachidic acid 9. Gadoleic acid 10. Behenic acid 11. Erucic acid 12. Lignoceric acid 13. Nervonic acid IS Methyl heptadecanoate

C20:0 C20:1 C22:0 C22:1 C24:0 C24:1

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector

Stabilwax®, 30 m, 0.32 mm ID, 0.25 μm (cat.# 10624) Rapeseed source of biodiesel (B100), prepared according to European Method EN 14103 1.0 μL split (split ratio 100:1) Cyclosplitter® (cat.# 20706) 250 °C 210 °C (hold 5 min) to 230 °C at 20 °C/min (hold 5 min) H2, constant flow 3 mL/min 60 cm/sec FID @ 250 °C

GC_PC00917

Yellow Grease FAMEs in Biodiesel Oils on Stabilwax®

1. 2. 3. 4. 5. 6.

Peaks Myristic acid Palmitic acid Palmitoleic acid Stearic acid Oleic acid Linoleic acid

C14:0 C16:0 C16:1 C18:0 C18:1 C18:2

7. Linolenic acid 8. Arachidic acid 9. Gadoleic acid 10. Behenic acid 11. Erucic acid 12. Lignoceric acid IS Methyl heptadecanoate

C18:3 C20:0 C20:1 C22:0 C22:1 C24:0

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector

Stabilwax®, 30 m, 0.32 mm ID, 0.25 μm (cat.# 10624) Yellow grease source of biodiesel (B100), prepared according to European Method EN 14103 1.0 μL split (split ratio 100:1) Cyclosplitter® (cat.# 20706) 250 °C 210 °C (hold 5 min) to 230 °C at 20 °C/min (hold 5 min) H2, constant flow 3 mL/min 60 cm/sec FID @ 250 °C

GC_PC00918

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbon Gases Ethylene and C1-C5 Hydrocarbons by ASTM D6159-97 on Rt®-Alumina BOND/KCI, Rtx®-1 (PLOT)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.

Peaks Methane Ethane Ethylene Propane Cyclopropane Propylene Acetylene Isobutane Propadiene n-Butane trans-2-Butene 1-Butene Isobutylene cis-2-Butene iso-Pentane Methylacetylene n-Pentane 1,3-Butadiene

GC_PC01110

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Instrument Notes

Rt®-Alumina BOND/KCl *, 50 m, 0.53 mm ID, 10 μm (cat.# 19760) Ethylene gas plus C1 through C5 hydrocarbons 1 μL split 2 mm splitless (cat.# 20712) 200 °C 60 mL/min 35 °C (hold 2 min) to 190 °C at 4 °C/min (hold 15 min) He, constant pressure (8.0 psi, 55.2 kPa) 25.4 cm/sec @ 35 °C FID @ 200 °C N2 20 Hz HP5890 GC * Rt®-Alumina BOND/KCl, 50 m, 0.53 mm ID, 10.0 μm (cat.# 19760) in series with an Rtx®-1, 30 m, 0.53 mm ID, 5.0 μm (cat.# 10179) connected using a universal Press-Tight® connector (cat.# 20401) (conditions as per ASTM D6159-97)

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657


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbon Gases Halogenated Hydrocarbons on Rt®-Alumina BOND/CFC (PLOT)

NEW! 1

5

1. 2. 3. 4. 5. 6. 7. 8. 9.

Peaks 1,1-Dichloroethylene Methylene chloride trans-1,2-Dichloroethylene Tetrachloromethane Unknown cis-1,2-Dichloroethylene Trichloroethylene 1,1,1-Trichloroethane Chloroform

8 3

2

6

4

0.0

1.0

7 9

2.0

3.0

4.0

Time (min)

GC_PC1193 Column Injection Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Flow Rate: Detector

Rt®-Alumina BOND/CFC, 30 m, 0.53 mm ID, 10 μm (cat.# 19763) Split (split ratio 20:1) 170 mL/min 135 °C H2, constant flow 8 mL/min @ 135 °C FID @ 220 °C

Light Hydrocarbons on Rt®-Alumina BOND/MAPD 1. 2. 3. 4. 5. 6. 7. 8. 7 6 1

5

Peaks Isobutane n-Butane trans-2-Butene 1-Butene Isobutylene cis-2-Butene 1,2-Butadiene n-Hexane

Column Sample Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: Instrument

NEW!

Rt®-Alumina BOND/MAPD, 50 m, 0.32 mm ID, 5.0 μm (cat.# 19780) Crude 1,2-butadiene none 1 μL split 2.0 mm ID straight inlet liner (cat.# 20712) 200 °C 80 mL/min 100 °C (hold 31 min) H2, constant linear velocity 17.40 psi, 120.0 kPa @ 100 °C FID @ 200 °C 30 mL/min N2 20 Hz HP5890 GC

4 3

8

2 5

10

15

20 Time (min)

658 www.restek.com

25

30 G C_PC1201

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbon Gases Butane Lighter Fluid on Rt®-Alumina BOND/Na2SO4

Propane Camping Fuel on Rt®-Alumina BOND/Na2SO4

(PLOT)

(PLOT) 1. 2. 3. 4. 5. 6. 7. 8.

Peaks Methane Ethane Propane Isobutane n-Butane trans-2-Butene 1-Butene Isobutylene

Column

1. 2. 3. 4. 5. 6. 7.

Column

Rt®-Alumina BOND/Na2SO4, 50 m, 0.53 mm ID, 10 μm (cat.# 19756) Butane lighter fluid

Sample Injection Inj. Vol.: Liner:

Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp:

100 μL split Splitless taper (2 mm) (cat.# 20795) 200 °C

Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp:

400 mL/min 45 °C (hold 1 min) to 200 °C at 10 °C/min (hold 3.5 min) H2, constant pressure (8.0 psi, 55.2 kPa) 74 cm/sec @ 45 °C FID @ 200 °C

Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Instrument Notes

Peaks Methane Ethane Ethylene Propane Propylene Isobutane n-Butane

Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Instrument Notes

N2 20 Hz HP5890 GC 100 μL sample loop on gas sampling valve, split

Rt®-Alumina BOND/Na2SO4, 50 m, 0.53 mm ID, 10 μm (cat.# 19756) Propane camping fuel 100 μL split Splitless taper (2 mm) (cat.# 20795) 200 °C 400 mL/min 45 °C (hold 1 min) to 200 °C at 10 °C/min (hold 3.5 min) H2, constant pressure (8.0 psi, 55.2 kPa) 74 cm/sec @ 45 °C FID @ 200 °C N2 20 Hz HP5890 GC 100 μL sample loop on gas sampling valve, split

GC_PC01084

GC_PC01083

Natural Gas on ShinCarbon ST

Natural Gas #2 on Rt®-QS-BOND

(micropacked)

(PLOT)

1. 2. 3. 4. 5. 6. 7. 8.

1 2

Peaks C1 C2 C3 iC4-isobutane C4 iC5-isopentane nC5 Hexanes

Column Sample Conc.: Injection Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

3

1. 2. 3. 4. 5. 6. 7. 8.

SilcoSmooth® tubing, 100/120 mesh on Shincarbon ST, 1 m, 1/16 OD, 1.0 mm ID (cat.# 19809) C1-C6 hydrocarbons 0.5-8% varied Packed on-column 200 °C

Peaks Methane Ethane Propane Isobutane n-Butane Isopentane n-Pentane Hexanes & hexenes

125 °C to 250 °C at 16 °C/min He, constant flow 10 mL/min FID @ 250 °C

45 GC_PC01013

8

67 0

10

20 Time (min)

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30 GC_PC00672

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

Rt®-QS-BOND, 30 m, 0.53 mm ID, 20 μm (cat.# 19738) Natural gas mix (mole%) 20 μL split (split ratio 10:1) Siltek® splitless taper (4 mm) (cat.# 20798-214.1) 240 °C 40 °C (hold 2 min) to 225 °C at 20 °C/min (hold 5 min) He, constant flow 5.7 mL/min FID @ 240 °C

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659


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbon Gases Natural Gas on Rt®-Alumina BOND/KCl (PLOT)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

Peaks Methane Ethane Propane Isobutane n-Butane neo-Pentane iso-Pentane n-Pentane Hexane isomers Heptane isomers Benzene Octane isomers

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Instrument

Rt®-Alumina BOND/KCl, 50 m, 0.53 mm ID, 10 μm (cat.# 19760) Natural gas 500 μL split 2.0 mm ID single taper (cat.# 20795) 200 °C 50 mL/min 45 °C (hold 1 min) to 200 °C at 10 °C/min (hold 8.5 min) H2, constant pressure (8.0 psi, 55.2 kPa) 45 cm/sec @ 45 °C FID @ 200 °C N2 20 Hz HP5890 GC

GC_PC01091

Natural Gas on Rt®-Alumina BOND/Na2SO4 (PLOT)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

Peaks Methane Ethane Propane Isobutane n-Butane neo-Pentane iso-Pentane n-Pentane Hexane isomers Heptane isomers Benzene Octane isomers

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Instrument

Rt®-Alumina BOND/Na2SO4, 50 m, 0.53 mm ID, 10 μm (cat.# 19756) Natural gas 500 μL split 2.0 mm ID single taper (cat.# 20795) 200 °C 50 mL/min 45 °C (hold 1 min) to 200 °C at 10 °C/min (hold 8.5 min) H2, constant pressure (8.0 psi, 55.2 kPa) 45 cm/sec @ 45 °C FID @ 200 °C N2 20 Hz HP5890 GC

GC_PC01092

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbon Gases Propylene and C1-C5 Hydrocarbons on Rt®-Alumina BOND/Na2SO4 (PLOT)

1. 2. 3. 4. 5. 6. 7. 8. 9.

Peaks Methane Ethane Ethylene Propane Cyclopropane Propylene Isobutane n-Butane Propadiene

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Instrument

10. 11. 12. 13. 14. 15. 16. 17. 18.

Acetylene trans-2-Butene 1-Butene Isobutylene cis-2-Butene Isopentane n-Pentane 1,3-Butadiene Methylacetylene

Rt®-Alumina BOND/Na2SO4, 50 m, 0.53 mm ID, 10 μm (cat.# 19756) Propylene and C1-C5 hydrocarbons 10 μL split 2 mm splitless (cat.# 20712) 200 °C 35 mL/min 50 °C to 150 °C at 6 °C/min He, constant pressure (10 psi, 68.9 kPa) 47 cm/sec @ 50 °C FID @ 200 °C N2 20 Hz HP5890 GC

GC_PC01142

C1-C5 Hydrocarbons on Rt®-Alumina BOND/MAPD (PLOT)

4

5

9

NEW!

1. 2. 3. 4. 5. 6. 7. 8.

6 2 3

14

10

15

Column

11 12 13

Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Temp.: Detector Instrument

8 7 1

16 17

0

2

4

1-800-356-1688 or 1-814-353-1300

6

Time (min)

8

Peaks Methane Ethane Ethylene Propane Cyclopropane Propylene Acetylene Propadiene

10

12

9. 10. 11. 12. 13. 14. 15. 16. 17.

n-Butane trans-2-Butene 1-Butene Isobutene cis-2-Butene Isopentane n-Pentane 1,3-Butadiene Methyl acetylene

Rt®-Alumina BOND/MAPD, 50 m, 0.53 mm ID, 10 μm (cat.# 19778) DCG custom standard (cat.# 547267) 5 μL split 2 mm single taper (cat.# 20795) 200 °C 80 mL/min 130 °C (hold 8 min) He, constant pressure (4.4 psi, 30.3 kPa) 130 °C FID @ 200 °C HP5890 GC

14 GC_PC1213

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661


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbon Gases 1,3-Butadiene on Rt®-Alumina BOND/MAPD (Purity Analysis) (PLOT)

5

NEW!

11

6

Rt®-Alumina BOND/MAPD PLOT columns are made specifically for the analysis of petrochemicals and downstream products such as ethylene, propylene, butylenes, and butadiene.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

4 2

Peaks Isobutane n-Butane Propadiene trans-2-Butene 1-Butene Isobutene cis-2-Butene Isopentane n-Pentane 1,2-Butadiene 1,3-Butadiene Methyl acetylene

7

12

3 12 6 1 9 3

10 8

0

2

4

6

8

10

12

12

Time (min) Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: Instrument

662 www.restek.com

14

16

18 GC_PC1211

Rt®-Alumina BOND/MAPD, 50 m, 0.53 mm ID, 10.0 μm (cat.# 19778) Crude 1,3-butadiene 10 μL split 2.0 mm ID straight inlet liner (cat.# 20712) 200 °C 100 mL/min 70 °C (hold 5 min) to 200 °C at 10 °C/min (hold 0 min) He, constant pressure (20 psi, 137.9 kPa) FID @ 250 °C 30 mL/min N2 20 Hz HP5890 GC

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbon Gases Refinery Gas on Rt®-Alumina BOND (Na2SO4) (PLOT) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

Peaks Methane Ethane Ethylene Propane Propylene Isobutane n-Butane Propadiene Acetylene trans-2-Butene 1-Butene Isobutylene cis-2-Butene iso-Pentane n-Pentane 1,3-Butadiene trans-2-Pentene 2-Methyl-2-butene 1-Pentene cis-2-Pentene Hexanes

GC_PC01085 Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

Rt®-Alumina BOND/Na2SO4, 50 m, 0.53 mm ID, 10 μm (cat.# 19756) Refinery gas 10 μL split Taper (2 mm) (cat.# 20795) 200 °C 80 mL/min 45 °C (hold 1 min) to 200 °C at 10 °C/min (hold 3.5 min) H2, constant pressure (8.0 psi, 55.2 kPa) 74 cm/sec @ 45 °C FID @ 200 °C

Refinery Gas on MXT®-Alumina BOND/Na2SO4 5

6

7

Inert surface ensures good peak shape and separation.

NEW!

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

4 8

2

9 6

1

7 7.5 10 16

5 11 13

3

12

14 15

18 17 19 20 21

89

2.5

5

7.5

10

12.5

15

17.5

20

Peaks Methane Ethane Ethylene Propane Propylene Isobutane n-Butane Propadiene Acetylene trans-2-Butene 1-Butene Isobutylene cis-2-Butene Isopentane n-Pentane 1,3-Butadiene trans-2-Pentene 2-Methyl-2-butene 1-Pentene cis-2-Pentene Hexanes

Time (min)

GC_PC1183 Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

1-800-356-1688 or 1-814-353-1300

MXT®-Alumina BOND/Na2SO4, 30 m, 0.53 mm ID, 10 μm (cat.# 79714) Refinery gas 10 μL split 2 mm split 45 °C 80 mL/min 45 °C (hold 1 min) to 200 °C at 10 °C/min (hold 8.5 min) He, constant pressure (10 psi, 68.9 kPa) 31 cm/sec @ 45 °C FID @ 200 °C

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663


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbon Gases Refinery Gas Calibration Standard on Refinery Gas Packed Column Set (packed)

1. 2. 3. 4. 5. 6. 7. 8. 9.

10. 11. 12. 13. 14. 15. 16. 17. 18.

Peaks C5-C6+ Methane Ethane Ethylene Propane Acetylene Propylene Cyclopropane Isobutane

Column Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

Propadiene n-Butane 1-Butene Isobutene trans-2-Butene cis-2-Butene 1,3-Butadiene Isopentane n-Pentane

Refinery gas column set (3 columns): 2a 2b 2c , Silcosteel® tubing (cat.# 88000-875) Refinery gas 1,000 μL packed on-column 150 °C 60 °C He, constant flow 30 mL/min FID @ 150 °C

GC_PC00374

Refinery Gas on Rt®-Alumina BOND/KCl (PLOT)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

Peaks Methane Ethane Ethylene Propane Propylene Isobutane n-Butane Propadiene Acetylene trans-2-Butene

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Instrument

11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

1-Butene Isobutylene cis-2-Butene Isopentane n-Pentane 1,3-Butadiene trans-2-Pentene 2-Methyl-2-butene 1-Pentene cis-2-Pentene Hexanes

Rt®-Alumina BOND/KCl, 50 m, 0.53 mm ID, 10 μm (cat.# 19760) Refinery gas standard 10 μL split Taper (2 mm) (cat.# 20795) 200 °C 80 mL/min 45 °C (hold 1 min) to 200 °C at 10 °C/min (hold 3.5 min) H2, constant pressure (8.0 psi, 55.2 kPa) 74 cm/sec @ 45 °C FID @ 200 °C N2 20 Hz HP5890 GC

GC_PC01088

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbon Gases Refinery Gas Mixture on Rt®-QS-BOND (PLOT) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

Peaks Air Methane Carbon dioxide Ethylene Acetylene Ethane Propylene Propane Propadiene Isobutane Isobutylene

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Sensitivity Mode: Instrument

1-Butene 1,3-Butadiene n-Butane cis-2-Butene trans-2-Butene Isopentane 1-Pentene 2-Methyl-2-butene n-Pentane cis-2-Pentene n-Hexane

Rt®-QS-BOND, 30 m, 0.53 mm ID, 20 μm (cat.# 19738) Refinery gas standard 20 μL split 2 mm (cat.# 20712) 200 °C 35 mL/min 40 °C (hold 2 min) to 225 °C at 15 °C/min (hold 5 min) He, constant pressure (11.5 psi, 79.3 kPa) 68 cm/sec @ 40 °C TCD @ 225 °C He 20 Hz He/H2 HP5890 GC

GC_PC1143

free literature Restek’s PLOT Column Family: The New Benchmark For Performance! Download your free copy from

www.restek.com

lit. cat.# PCBR1163B-UNV

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665


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons Hydrocarbons (C7-C42) on Rtx®-1

GC_PC00216 Column Sample Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27.

Peaks C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 C17 C18 C19 C20 C22 C23 C24 C25 C26 C28 C30 C32 C34 C36 C38 C40 C42

Rtx®-1, 30 m, 0.53 mm ID, 0.25 μm (cat.# 10125) Synthetic hydrocarbon mix ~0.1 mg/mL per component 0.2 μL direct Uniliner® 340 °C 40 °C to 340 °C at 5 °C/min H2, constant pressure 40 cm/sec @ 40 °C FID @ 340 °C FID sensitivity: 64 x 10-11 AFS

Hydrocarbons (C5-C106) on MXT®-1HT SimDist at 430 °C

Lowest bleed product on the market!

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

Peaks C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 C17 C18 C20 C22 C24 C26 C28 C30

tR (min) — — — — — — — 0.988 1.677 2.544 3.503 4.484 5.451 6.386 8.15 9.764 11.259 12.645 13.920 15.134

21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40.

Peaks C32 C34 C36 C38 C40 C42 C44 C46 C48 C50 C52 C54 C56 C58 C60 C62 C64 C66 C68 C70

Column

GC_PC1165

666 www.restek.com

Sample Diluent: Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Flow Rate: Detector Make-up Gas Flow Rate: Constant Column + Constant Make-up: Make-up Gas Type: Data Rate: Instrument

tR (min) 16.280 17.364 18.392 19.371 20.363 21.199 22.041 22.843 23.609 24.340 25.041 25.712 26.365 26.990 27.594 28.173 28.733 29.274 29.797 30.303

41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58.

Peaks C72 C74 C76 C78 C80 C82 C84 C86 C88 C90 C92 C94 C96 C98 C100 C102 C104 C106

tR (min) 30.789 31.265 31.725 32.173 32.609 33.033 33.454 33.858 34.256 34.643 35.024 35.395 35.758 36.115 36.460 36.803 37.139 37.465

MXT®-1HT SimDist, 5 m, 0.53 mm ID, 0.10 μm (cat.# 70112) Custom C5-C106 hydrocarbon standard Carbon disulfide 1% 0.5 μL cold on-column 53 °C to 430 °C at 10 °C/min (hold 5 min) 50 °C to 430 °C at 10 °C/min (hold 5 min) He, constant flow 18 mL/min FID @ 430 °C 24 mL/min 42 mL/min N2 20 Hz Shimadzu 2010 GC

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons Hydrocarbons (C5-C106) on MXT®-1HT SimDist at 450 °C 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

Peaks C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 C17 C18 C20 C22 C24 C26 C28 C30

tR (min) — — — — — — — 0.938 1.586 2.425 3.365 4.332 5.290 6.217 7.966 9.566 11.051 12.426 13.689 14.897

21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40.

Peaks C32 C34 C36 C38 C40 C42 C44 C46 C48 C50 C52 C54 C56 C58 C60 C62 C64 C66 C68 C70

Column Sample Diluent: Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Flow Rate: Detector Make-up Gas Flow Rate: Constant Column + Constant Make-up: Make-up Gas Type: Data Rate: Instrument

GC_PC1164

tR (min) 16.035 17.110 18.133 19.108 20.096 20.923 21.759 22.556 23.317 24.051 24.752 25.422 26.079 26.701 27.305 27.878 28.439 28.975 29.499 30.002

41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58.

Peaks C72 C74 C76 C78 C80 C82 C84 C86 C88 C90 C92 C94 C96 C98 C100 C102 C104 C106

tR (min) 30.489 30.906 31.414 31.862 32.294 32.719 33.132 33.529 33.927 34.310 34.689 35.059 35.423 35.773 36.120 36.463 36.793 37.118

MXT®-1HT SimDist, 5 m, 0.53 mm ID, 0.10 μm (cat.# 70112) Custom C5-C106 hydrocarbon standard Carbon disulfide 1% 0.5 μL cold on-column 53 °C to 450 °C at 10 °C/min (hold 5 min) 50 °C to 450 °C at 10 °C/min (hold 5 min) He, constant flow 18 mL/min FID @ 450 °C 24 mL/min 42 mL/min N2 20 Hz Shimadzu 2010 GC

Hydrocarbons (C10-C44) on MXT®-1HT SimDist

Column Sample Diluent: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Notes

C9 C10

MXT®-1HT SimDist, 5 m, 0.53 mm ID, 0.10 μm (cat.# 70100) D2887 calibration mix (cat.# 31222) Carbon disulfide 0.2 μL on-column Track oven 40 °C to 430 °C at 10 °C/min (hold 30 min) He, constant pressure (1.0 psi, 6.9 kPa) 60 cm/sec FID @ 430 °C 40 mL/min Flow rate: 7.8 mL/min

C11

C12 C14 C16

C18 C20

0

5

1-800-356-1688 or 1-814-353-1300

10

C24

15 Time (min)

C28

C32

20

C36

C40

C44

25 GC_PC00529

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667


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons Fast Detailed Hydrocarbons Analysis (DHA) Analyzed Using ASTM Method on Rtx®-DHA-100/Rtx®-5 DHA

Excellent peak shape for alcohols!

GC_PC00774

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Oven Carrier Gas Flow Rate: Linear Velocity: Detector Oven Temp

Notes

Peaks Ethanol C5 tert-Butanol 2-Methylbutene-2 2,3-Dimethylbutane Methyl tert-butyl ether (MTBE) C6 1-Methylcyclopentene Benzene Cyclohexane 3-Ethylpentane 1,2-Dimethylcyclopentane C7 2,2,3-Trimethylpentane 2,3,3-Trimethylpentane

16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30.

Toluene C8 Ethylbenzene p-Xylene 2,3-Dimethylheptane C9 5-Methylnonane 1,2-Methylethylbenzene C10 C11 1,2,3,5-Tetramethylbenzene Naphthalene C12 1-Methylnaphthalene C13

Rtx®-DHA-100, 100 m, 0.25 mm ID, 0.50 μm (cat.# 10148) using Rtx®-5 DHA tuning column 5 m, 0.25 mm ID DHA/oxygenates setup blend (see notes) 0.01 μL split (split ratio 150:1) 4 mm cup splitter inlet liner with Siltek® deactivation (cat.# 20709-214.1) 250 °C H2, constant flow 3.62 mL/min 55 cm/sec FID @ 300 °C A: 35 °C B: 5 °C (hold 8.32 min) (elute C5) to 48 °C at 22 °C/min (hold 26.32 min) (elute ethylbenzene) to 141 °C at 3.20 °C/min (elute C12) to 300 °C at 1 °C/min A: Front end of DHA/oxygenates set-up blend C5 Efficiency: 586,825 plates C5 k': 0.476 tert-Butanol skew: 2.10 Resolution: tert-butanol/2-methylbutene-2: 5.39

Acknowledgement Chromatogram courtesy of Neil Johansen, Inc., Aztec, New Mexico, in association with Envantage Analytical Software, Inc., Cleveland, Ohio.

Approximate analysis time % Time savings (relative to standard method conditions)

Optimized D6730 with hydrogen* 72 min. 51% faster

Optimized D6730 with helium* 98 min. 33% faster

Standard D6730 conditions 146 min. —

* Optimized conditions and chromatographic results for hydrogen shown above; for helium, see next page.

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons Detailed Hydrocarbon Analysis on Rtx®-DHA-100/Rtx®-5 DHA Tuning Column

1 1. 2. 3. 4.

Peaks Ethanol C5 tert-Butanol 2-Methylbutene-2

Column

Sharp, symmetric oxygenate peaks!

4

Sample Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector Notes

2

Rtx®-DHA-100, 100 m, 0.25 mm ID, 0.50 μm (cat.# 10148) using Rtx®-5 DHA tuning column, 2.62 m, 0.25 mm ID, 1.0 μm Custom detailed hydrocarbon analysis (DHA) mix Neat 0.01 μL split (split ratio 150:1) 4 mm cup splitter inlet liner with Siltek® deactivation (cat.# 20709-214.1) 200 °C 35 °C He, constant flow 2.3 mL/min 28 cm/sec FID @ 250 °C C5 efficiency: 613,596 total theoretical plates k' (C5): 0.489 tert-butanol skewness: 1.25 Resolution (tert-butanol/2-methylbutene-2): 5.60

3

9

10

11 Time (min)

12 GC_PC00743A

free literature Detailed Hydrocarbon Analysis Featuring Rtx®-DHA Columns www.restek.com Download your free copy from www.restek.com lit. cat.# PCFL1007B-UNV

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669


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons Aromatics on Rt®-TCEP

1. 2. 3. 4. 5. 6. 7. 8.

Peaks n-Undecane Benzene n-Dodecane Toluene Ethylbenzene p-Xylene m-Xylene Cumene

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

9. 10. 11. 12. 13. 14. 15.

n-Propylbenzene o-Xylene Mesitylene 1-Ethyl-2-methylbenzene m-Diethylbenzene p-Diethylbenzene o-Diethylbenzene

Rt®-TCEP, 60 m, 0.25 mm ID, 0.40 μm (cat.# 10999) 500 ppm, except ethylbenzene @ 1,000 ppm 1.0 μL split 200 °C 46 mL/min 60 °C (hold 5 min) to 100 °C at 5 °C/min (hold 10 min) He, constant pressure 30 cm/sec @ 80 °C FID @ 200 °C FID sensitivity: 6.4 x 10-11 AFS

GC_PC00211

Gasoline Containing Ethanol on D3606 Application Column Set by ASTM D3606-10 (Modified)

free literature 1. 2. 3. 4.

NEW!

Resolve Benzene and Toluene in Spark Ignition Fuels Containing Ethanol

Peaks Ethanol Benzene 2-Butanol (IS) Toluene

1

Cut time = 2.38 minutes

Excellent separation of ethanol and benzene.

Using a Modified ASTM D3606-10 Method D3606 Column Set Download your free copy from

4 3

www.restek.com lit. cat.# PCTS1408-UNV

2

0

2

6

4

8

Time (min)

Column Sample Diluent: Injection Sample Loop Vol.: Valve Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector Notes

670 www.restek.com

10

GC_PC1224

D3606 application column (2 column set). Column 1: 6' (1.8 m), 1/8" OD, 2.0 mm ID, nonpolar Rtx®-1; Column 2: 16' (4.9 m), 1/8" OD, 2.0 mm ID, proprietary packing material (cat.# 83606-800) Ethanol-containing gasoline with internal standard (IS) Sample valve 1.5 μL 150 °C 135 °C (hold 12 min) He, constant flow 20.0 mL/min TCD @ 200 °C 2.38 minute backflush (must be determined for each GC system).

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons (High-Temperature) C10-C40 Alkanes on Rxi®-5HT

Column

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Sample Diluent: Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Linear Velocity: Dead Time: Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: GC_PC1159 Instrument

Rxi®-5HT, 30 m, 0.32 mm ID, 0.25 μm (cat.# 13924) using Rxi® guard column 2 m, 0.53 mm ID (cat.# 10054) System performance test standard mixture of n-alkanes (cat.# 31678) Hexane 50 μg/mL 1 μL cold on-column 53 °C to 300 °C at 10 °C/min (hold 20 min) 50 °C to 300 °C at 10 °C/min (hold 20 min) H2, constant flow 40 cm/sec @ 50 °C 1.25 min @ 50 °C FID @ 330 °C 30 mL/min N2 20 Hz Agilent/HP6890 GC

Diesel on Rxi®-5HT Column

GC_PC1160

Sample Diluent: Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Linear Velocity: Dead Time: Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: Instrument

Rxi®-5HT, 30 m, 0.32 mm ID, 0.25 μm (cat.# 13924) using Rxi® guard column 2 m, 0.53 mm ID (cat.# 10054) Diesel fuel #2 composite (cat.# 31258) Methylene chloride 50,000 μg/mL diluted to 500 ppm and spiked with C10 & C40 1 μL cold on-column 53 °C to 300 °C at 10 °C/min (hold 20 min) 50 °C to 300 °C at 10 °C/min (hold 20 min) H2, constant flow 40 cm/sec @ 50 °C 1.25 min @ 50 °C FID @ 330 °C 30 mL/min N2 20 Hz Agilent/HP6890 GC

Gasoline on Rxi®-5HT Column

GC_PC1161

Sample Diluent: Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Linear Velocity: Dead Time: Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: Instrument

Rxi®-5HT, 30 m, 0.32 mm ID, 0.25 μm (cat.# 13924) using Rxi® guard column 2 m, 0.53 mm ID (cat.# 10054) Unleaded gasoline composite (cat.# 30081) Methanol 2,500 μg/mL diluted to 500 ppm and spiked with C10 & C40 1 μL cold on-column 53 °C to 300 °C at 10 °C/min (hold 20 min) 50 °C to 300 °C at 10 °C/min (hold 20 min) H2, constant flow 40 cm/sec @ 50 °C 1.25 min @ 50 °C FID @ 330 °C 30 mL/min N2 20 Hz Agilent/HP6890 GC

Kerosene on Rxi®-5HT Column

GC_PC1162

1-800-356-1688 or 1-814-353-1300

Sample Diluent: Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Linear Velocity: Dead Time: Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: Instrument

Rxi®-5HT, 30 m, 0.32 mm ID, 0.25 μm (cat.# 13924) using Rxi® guard column 2 m, 0.53 mm ID (cat.# 10054) Kerosene composite (cat.# 31094) Methylene chloride 500 μg/mL spiked with C10 & C40 1 μL cold on-column 53 °C to 300 °C at 10 °C/min (hold 20 min) 50 °C to 300 °C at 10 °C/min (hold 20 min) H2, constant flow 40 cm/sec @ 50 °C 1.25 min @ 50 °C FID @ 330 °C 30 mL/min N2 20 Hz Agilent/HP6890 GC

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671


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons (High-Temperature) Diesel #2/Motor Oil on Rtx®-Mineral Oil

Mineral Oil and Motor Oil on Rtx®-Mineral Oil

NEW!

NEW!

GC_PC1169 GC_PC1168 Column Sample Diluent: Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Linear Velocity: Dead Time: Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: Instrument Notes

Rtx®-Mineral Oil, 15 m, 0.32 mm ID, 0.15 μm (cat.# 18074) using IP deactivated guard column 2 m, 0.53 mm ID (cat.# 10047) Diesel #2/motor oil (cat.# 31682) Hexane 5,000 μg/mL diluted to 500 ppm 0.5 μL cold on-column 53 °C to 300 °C at 10 °C/min (hold 20 min) 50 °C to 300 °C at 10 °C/min (hold 20 min) H2, constant flow 40 cm/sec @ 50 °C 0.625 min @ 50 °C FID @ 330 °C 30 mL/min N2 20 Hz Agilent/HP6890 GC Black trace = diesel/motor oil Red trace = C10-C40 standard

Column Sample Diluent: Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Linear Velocity: Dead Time: Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: Instrument Notes

Rtx®-Mineral Oil, 15 m, 0.32 mm ID, 0.15 μm (cat.# 18074) using IP deactivated guard column 2 m, 0.53 mm ID (cat.# 10047) Custom mineral oil/motor oil mix Hexane 500 μg/mL 0.5 μL cold on-column 53 °C to 300 °C at 10 °C/min (hold 20 min) 50 °C to 300 °C at 10 °C/min (hold 20 min) H2, constant flow 40 cm/sec @ 50 °C 0.625 min @ 50 °C FID @ 330 °C 30 mL/min N2 20 Hz Agilent/HP6890 GC Black trace = mineral oil Green trace = motor oil Red trace = C10-C40 standard

Diesel #2/Mineral Oil on Rtx®-Mineral Oil

NEW!

Looking for more? Visit our online technical library for chromatograms based on ASTM methods, USP procedures, and other applications. www.restek.com/chromatograms GC_PC1170 Column Sample Diluent: Conc.: Injection Inj. Vol.: Temp. Program: Oven Oven Temp: Carrier Gas Linear Velocity: Dead Time: Detector Make-up Gas Flow Rate: Make-up Gas Type: Data Rate: Instrument Notes

Rtx®-Mineral Oil, 15 m, 0.32 mm ID, 0.15 μm (cat.# 18074) using IP deactivated guard column 2 m, 0.53 mm ID (cat.# 10047) Diesel #2/mineral oil (cat.# 31676) Hexane 500 μg/mL 0.5 μL cold on-column 53 °C to 300 °C at 10 °C/min (hold 20 min) 50 °C to 300 °C at 10 °C/min (hold 20 min) H2, constant flow 40 cm/sec @ 50 °C 0.625 min @ 50 °C FID @ 330 °C 30 mL/min N2 20 Hz Agilent/HP6890 GC Black trace = diesel/mineral oil Red trace = C10-C40 standard

672 www.restek.com

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons (High-Temperature) Diesel & Motor Oil on Rtx®-Mineral Oil

1. 2. 3. 4.

Diesel

C10

NEW!

Conc. (μg/mL) 20 500 500 20

Peaks C10 Diesel Motor oil C40

C40 Column Sample Diluent: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Instrument Notes

Motor Oil

4

2

0

6

8

Rtx®-Mineral Oil, 15 m, 0.32 mm ID, 0.10 μm (cat.# 18079) using IP deactivated guard column 10 m, 0.32 mm ID (cat.# 10047) with aluminum connector Diesel #2/motor oil (cat.# 31682) Extraction solvent stock solution #2 (cat.# 31680) Hexane/methylene chloride 1.0 μL direct 58 °C 55 °C (hold 1.0 min) to 380 °C at 100 °C/min (hold 6.0 min) H2, constant flow 40 cm/sec FID @ 380 °C 30 mL/min N2 Agilent/HP6890 GC Direct cool on-column injection, programmed by oven tracking. Actual guard column length used in application was 2 m.

10 GC_PC1180

Time (min.)

n-alkanes (C10-C40) on Rtx®-Mineral Oil

NEW! 1. 2. 3. 4. 5. 6. 7. 8.

2

1

Peaks C10 C12 C14 C16 C18 C20 C22 C24

9. 10. 11. 12. 13. 14. 15. 16.

C26 C28 C30 C32 C34 C36 C38 C40

Column Sample Diluent: Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Flow Rate: Make-up Gas Type: Instrument Notes

3 4 5

6

7

8

9

10

11

12

13

14

15

Rtx®-Mineral Oil, 15 m, 0.32 mm ID, 0.10 μm (cat.# 18079) using IP deactivated guard column 10 m, 0.32 mm ID (cat.# 10047) with aluminum connector System performance test standard mixture of n-alkanes (cat.# 31678) Hexane/methylene chloride 20 μg/mL each 1.0 μL direct 58 °C 55 °C (hold 1.0 min) to 380 °C at 100 °C/min (hold 6.0 min) H2, constant flow 40 cm/sec FID @ 380 °C 30 mL/min N2 Agilent/HP6890 GC Direct cool on-column injection, programmed by oven tracking.

16 Actual guard column length used in application was 2 m.

0

2

4

1-800-356-1688 or 1-814-353-1300

Time (min.)

6

8

10 GC_PC1181

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673


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons (High-Temperature) Mid-range Crude on Rxi®-5HT Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

1. 2. 3. 4.

Peaks C17 Pristane C18 Phytane

Column

Rxi®-5HT, 30 m, 0.32 mm ID, 0.10 μm (cat.# 13909) using retention gap 2 m, 0.53 mm ID Mid-range crude 500 μg/mL

Sample Conc.: Injection Inj. Vol.: 1.0 μL cold on-column Oven Oven Temp: 50 °C to 300 °C at 10 °C/min (hold 10 min) Carrier Gas H2, constant flow Linear Velocity: 40 cm/sec Detector FID @ 330 °C Instrument Agilent/HP6890 GC Acknowledgement Sample courtesy of Exxon Mobil Corporation

GC_PC1172

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons (Simulated Distillation) Simulated Distillation (Standard Calibration) on MXT®-1 SimDist 1. 2. 3. 4. 5. 6. 7. 8.

9. 10. 11. 12. 13. 14. 15. 16. 17.

Peaks C6 C7 C8 C9 C10 C11 C12 C14

Column Sample Conc.: Injection Temp. Program: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

C16 C18 C20 C24 C28 C32 C36 C40 C44

free literature Increase Productivity: Get More Runs from Your SimDist Setup Using Next Generation MXT®-1HT SimDist Columns

MXT®-1 SimDist, 6 m, 0.53 mm ID, 0.15 μm (cat.# 70101) ASTM D2887 standard Wet needle Cold on-column -17 °C to 433 °C

Download your free copy from www.restek.com lit. cat.# PCFL1201A

-12 °C to 430 °C at 20 °C/min H2, constant linear velocity 40 cm/sec FID @ 430 °C FID sensitivity: 128 x 10-11 AFS

GC_PC00224

Simulated Distillation (C5-C44) on Rtx®-2887

1. 2. 3. 4. 5. 6. 7. 8. 9.

Peaks C5 C6 C7 C8 C9 C10 C11 C12 C14

10. 11. 12. 13. 14. 15. 16. 17. 18.

C16 C18 C20 C24 C28 C32 C36 C40 C44

Column Sample Diluent: Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector

Rtx®-2887, 10 m, 0.53 mm ID, 2.65 μm (cat.# 10199) C5 to C44 hydrocarbon standard Carbon disulfide 0.01-0.1 wt. % 1 μL direct 360 °C 35 °C to 360 °C at 15 °C/min (hold 5 min) He, constant flow 15 mL/min 112 cm/sec FID @ 360 °C

GC_PC00750

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675


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Hydrocarbons (Simulated Distillation) Simulated Distillation by ASTM D2887 on Rtx®-1 SimDist 2887 (packed)

1. 2. 3. 4. 5. 6. 7. 8. 9. Column Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector Notes

Peaks Pentane Hexane Heptane Octane Nonane Decane Undecane Dodecane Tetradecane

10. 11. 12. 13. 14. 15. 16. 17. 18.

Hexadecane Octadecane Eicosane Tetracosane Octacosane Dotricontane Hexatriacontane Tetracontane Tetratetracontane

Rtx®-1 SimDist 2887, SilcoSmooth® tubing, 100/120 mesh on Silcoport® W, 25 inches, 1/8 in. OD, 2 mm ID (cat.# 80000-800) 1-12% (w/w) each component ASTM D2887-01 calibration mix (1% each in CS2) (cat.# 31674) ASTM D2887-01 calibration mix (5% each, neat) (cat.# 31675) 1.0 μL packed not on-column 350 °C 35 °C to 350 °C at 10 °C/min (hold 5 min) He, constant flow 25 mL/min FID @ 350 °C FID sensitivity: 256 x 10-11 AFS

GC_PC00228

How can we help you today? Contact us... customer service: 1-814-353-1300, ext. 3 | e-mail: csreps@restek.com technical service: 1-814-353-1300, ext. 4 | e-mail: support@restek.com sales representatives: 1-814-353-1300, ext. 3 | e-mail: salesreps@restek.com 4 ways to order: 1. CALL: 1-800-356-1688, ext. 3 or 1-814-353-1300, ext. 3 Monday–Friday 8:00 a.m.–6:30 p.m. Eastern Time 2. FAX: 1-814-353-1309 24 hours a day 3. ONLINE: www.restek.com 24 hours a day 4. E-MAIL: csreps@restek.com 24 hours a day Outside the U.S.? Find a distributor at

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Permanent Gases Permanent Gases on ShinCarbon ST

Permanent Gases and C1+C2 Hydrocarbons on ShinCarbon ST

(micropacked)

(micropacked) 2

2 34 1. 2. 3. 4. 5. 6.

Peaks Hydrogen Oxygen Nitrogen Carbon monoxide Methane Carbon dioxide

Column

1. 2. 3. 4. 5. 6. 7. 8.

Peaks Oxygen Nitrogen Carbon monoxide Methane Carbon dioxide Acetylene Ethylene Ethane

ShinCarbon ST, 100/120 mesh, 2 m, Column

1/16 in. OD, 1.0 mm ID (cat.# 19808)

Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp:

ShinCarbon ST, 100/120 mesh, 2 m, 1/16 in. OD, 1.0 mm ID (cat.# 19808)

Permanent gases mix, approx. 5 mol % each Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp:

5 μL packed on-column 100 °C 40 °C (hold 3 min) to 250 °C at 8 °C/min (hold 10 min) He, constant flow 10 mL/min HID @ 200 °C

Carrier Gas Flow Rate: Detector

Carrier Gas Flow Rate: Detector

1

Permanent gases-C1+C2 hydrocarbons 5 μL packed on-column 100 °C 40 °C (hold 3 min) to 250 °C at 8 °C/min (hold 10 min) He, constant flow 10 mL/min HID @ 200 °C

5

1 3

6 0

5

10 Time (min)

15

20 GC_PC00666

0

8

4

5

5

6

10 Time (min)

15

7

20 GC_PC00665

Permanent Gases on Molecular Sieve 5A and Molecular Sieve 13X (packed) 1. 2. 3. 4.

Columns

Peaks Oxygen Nitrogen Methane Carbon monoxide

Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

Molecular Sieve 5A: Excellent resolution of oxygen, nitrogen, methane, and carbon monoxide.

Molesieve 5A 1 m, 2 mm ID (cat.# 80440-800) and Molesieve 13X 2 m, 2 mm ID (cat.# 80439-800) 5-10% each component balance helium 10 μL direct 150 °C 50 °C H2, constant flow 30 mL/min TCD @ 200 °C

Molecular Sieve 13X: Rapid analysis and excellent peak symmetry for carbon monoxide.

Excellent peak shape.

GC_PC00166

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677


GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Permanent Gases Permanent Gases on Rt®-Msieve 5A

Permanent Gases on Rt®-MSieve 5A

(PLOT)

(PLOT) Peaks 1. Hydrogen 2. Argon 3. Oxygen

Peaks

1. 2. 3. 4. 5. 6.

Argon resolved from oxygen.

Conc. (μg/mL) Hydrogen 40 Argon 30 Oxygen 50 Nitrogen 50 Methane 40 Carbon monoxide 50

Conc. 29.1 ppm 53.4 ppm 31.3 ppm

Excellent peak shape for carbon monoxide. GC_PC00170

GC_PC00898 Column Sample Injection Sample Loop Vol.: Valve Name: Inj. Temp.: Valve Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

Column

Rt®-Msieve 5A, 30 m, 0.53 mm ID, 50 μm (cat.# 19723) Injection Sample valve Sample Loop Vol.: 500 μL Oven Oven Temp: 27 °C Carrier Gas He, constant flow Linear Velocity: 34 cm/sec Detector Valco® HID Acknowledgement Chromatogram courtesy of Larry McElmurry, Mobile Analytical Labs.

Rt®-Msieve 5A, 30 m, 0.53 mm ID, 50 μm (cat.# 19723) Permanent gases Sample valve 5 μL 6-port Valco® valve 200 °C Ambient 27 °C (hold 5 min) to 100 °C at 10 °C/min (hold 5 min) He, constant flow 5.0 mL/min Valco® helium ionization detector @ 150 °C

Helium/Hydrogen Separation using Rt®-Msieve 5A (PLOT)

Peaks 1. Helium 2. Hydrogen

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Sensitivity Mode: Instrument

Rt®-Msieve 5A, 30 m, 0.53 mm ID, 50 μm (cat.# 19723) Helium/hydrogen gas mixture 25 μL split (split ratio 10:1) 2 mm split Precision® liner w/wool (cat.# 20823) 200 °C 40 mL/min 30 °C N2, constant pressure (7.0 psi, 48.3 kPa) 38 cm/sec @ 30 °C TCD @ 200 °C N2 20 Hz N2/Ar HP5890 GC

GC_MS01136

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GC CHROMATOGRAMS | PETROLEUM & PETROCHEMICAL

Permanent Gases, Sulfur Compounds Permanent Gases on MXT®-Msieve 5A

NEW!

1. 2. 3. 4. 5. 6.

Peaks Helium Argon Oxygen Nitrogen Methane Carbon monoxide

GC_PC1182 Column Sample Conc.: Injection Oven Oven Temp.: Carrier Gas Detector

MXT®-Msieve 5A, 30 m, 0.53 mm ID, 50 μm (cat.# 79723) 1% in hydrogen split (split ratio 50:1) 30 °C H2 μ-TCD

Sulfur Compounds on Rxi®-1ms

Sulfur in Gasoline on Rtx®-1

Rxi® Technology! 1. 2. 3. 4. 5. 6. 7. 8.

Exceptionally inert, ultra low-bleed capillary columns.

Peaks Thiophene 2-Methylthiophene 3-Methylthiophene 2-Ethylthiophene Alkylthiophenes Benzothiophene Methylbenzothiophenes Dimethylbenzothiophenes

1. 2. 3. 4. 5.

Peaks Hydrogen sulfide Carbonyl sulfide Methyl mercaptan Ethyl mercaptan Dimethyl sulfide

GC_AR00861 Column Sample GC_PC00198

Column Sample Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector

Rtx®-1, 30 m, 0.32 mm ID, 4.0 μm (cat.# 10198) Gasoline containing 300 ppm total sulfur 1 μL split (split ratio 10:1) 275 °C 40 °C (hold 3 min) to 275 °C at 10 °C/min (hold 5 min) He, constant flow 2.5 mL/min 70 cm/sec SCD @ 275 °C

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Diluent: Conc.: Injection Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rxi®-1ms, 30 m, 0.32 mm ID, 4.00 μm (cat.# 13396) Hydrogen sulfide, carbonyl sulfide, methyl mercaptan, ethyl mercaptan, dimethyl sulfide helium 100 ppbv Splitless 30 °C 30 °C He, constant pressure 48 cm/sec @ 30 °C SCD @ 800 °C Injection: sample loop (30 °C), 1 mL splitless direct Sample storage & transfer: SilcoCan® air monitoring canister with Siltek®-treated 1/4" valve (cat.# 24182-650); Sulfinert®-treated gas sample loop, 1 cc (cat.# 22848); Sulfinert®-treated gas sample loop, 10 cc (custom order)

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679


GC CHROMATOGRAMS | PHARMACEUTICAL

Organic Volatile Impurities/Residual Solvents Residual Solvents (Class 1) for Water-Soluble Articles on Rxi®-624Sil MS tR (min)

Peaks 1. 1,1-Dichloroethene 2. 1,1,1-Trichloroethane 3. Carbon tetrachloride 4. Benzene 5. 1,2-Dichloroethane * DMSO interference

3.586 8.536 9.042 9.787 10.112

Conc. (μg/mL) 0.07 0.08 0.03 0.02 0.04

Column Sample Diluent: Injection Liner: Headspace-Loop Inj. Port Temp.: Instrument: Inj. Time: Transfer Line Temp.: Valve Oven Temp.: Sample Temp.: Sample Equil. Time: Vial Pressure: Pressurize Time: Pressure Equilibration Time: Loop Pressure: Loop Fill Time: Oven Oven Temp:

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Carrier Gas Linear Velocity: Dead Time: Detector Data Rate: Instrument Acknowledgement

Rxi®-624Sil MS, 30 m, 0.32 mm ID, 1.80 μm (cat.# 13870) Residual solvents - class 1 (cat.# 36279) Water Headspace-loop split (split ratio 5:1) 1 mm split (cat.# 20972) 140 °C Tekmar HT3 1 min 110 °C 110 °C 80 °C 60 min 10 psi 0.5 min 0.05 min 5 psi 0.1 min 40 °C (hold 20 min) to 240 °C at 10 °C/min (hold 20 min) He, constant flow 35 cm/sec 1.45 min @ 40 °C FID @ 250 °C 5 Hz Agilent/HP6890 GC Teledyne Tekmar

GC_PH1144

Residual Solvents (Class 1) on Stabilwax® (G16)

1. 2. 3. 4. 5.

Peaks 1,1-Dichloroethene 1,1,1-Trichloroethane Carbon tetrachloride Benzene 1,2-Dichloroethane

Column Sample

GC_PH00951

680 www.restek.com

Stabilwax®, 30 m, 0.32 mm ID, 0.25 μm (cat.# 10624) Residual solvents - class 1 (cat.# 36279) in 20 mL headspace vial (cat.# 24685) Water

Diluent: Injection Inj. Vol.: 1.0 μL headspace-syringe split (split ratio 5:1) Liner: 2 mm splitless (cat.# 20712) Inj. Temp.: 140 °C Headspace-Syringe Instrument: Overbrook Scientific HT200H Syringe Temp.: 100 °C Sample Temp.: 80 °C Sample Equil. Time: 45 min Inj. Speed: 8 Inj. Dwell: 5 sec Oven Oven Temp: 50 °C (hold 20 min) to 165 °C at 6 °C/min (hold 20 min) Carrier Gas He, constant flow Flow Rate: 2.15 mL/min Linear Velocity: 35.2 cm/sec Detector FID @ 250 °C

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GC CHROMATOGRAMS | PHARMACEUTICAL

Organic Volatile Impurities/Residual Solvents Residual Solvents (Class 2 - Mixture A) for Water-Soluble Articles on Rxi®-624Sil MS Peaks 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

tR (min)

Methanol Acetonitrile Dichloromethane trans-1,2-Dichloroethene cis-1,2-Dichloroethene Tetrahydrofuran Cyclohexane Methylcyclohexane 1,4-Dioxane Toluene Chlorobenzene Ethylbenzene m-Xylene p-Xylene o-Xylene

2.281 4.009 4.313 4.798 7.028 7.706 8.708 14.099 15.054 22.018 26.570 26.837 27.147 27.147 27.927

Conc. (μg/mL) 25.00 3.42 5.00 7.83 7.83 5.75 32.33 9.83 3.17 7.42 3.00 3.07 10.85 2.53 1.63

GC_PH1146 Column Sample Diluent: Injection Liner: Headspace-Loop Inj. Port Temp.: Instrument: Inj. Time: Transfer Line Temp.: Valve Oven Temp.: Sample Temp.: Sample Equil. Time: Vial Pressure: Pressurize Time: Pressure Equilibration Time: Loop Pressure: Loop Fill Time:

Oven Oven Temp:

Rxi®-624Sil MS, 30 m, 0.32 mm ID, 1.80 μm (cat.# 13870) Residual solvents class 2 - mix A (cat.# 36271) Water Headspace-loop split (split ratio 5:1) 1 mm split (cat.# 20972)

40 °C (hold 20 min) to 240 °C at 10 °C/min (hold 20 min) Carrier Gas He, constant flow Linear Velocity: 35 cm/sec Dead Time: 1.45 min @ 40 °C Detector FID @ 250 °C Data Rate: 5 Hz Instrument Agilent/HP6890 GC Acknowledgement Teledyne Tekmar

140 °C Tekmar HT3 1 min. 110 °C 110 °C 80 °C 60 min 10 psi 0.5 min

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

0.05 min 5 psi 0.1 min

Residual Solvents (Class 2 - Mixture A) on Stabilwax® (G16) 1

1. 2. 3. 4. 5. 6. 7. 8.

9

13

Column Sample

10

3.4

3, 4

3.6

3.8

4.0

7 2

11 12 6 5

0

2

15

14 8

10 4

1-800-356-1688 or 1-814-353-1300

6

8

Peaks Cyclohexane Methylcyclohexane trans-1,2-Dichloroethene Tetrahydrofuran Methanol Dichloromethane cis-1,2-Dichloroethene Acetonitrile

Time (min) GC_PH00952

9. 10. 11. 12. 13. 14. 15.

Toluene 1,4-Dioxane Ethyl benzene p-Xylene m-Xylene o-Xylene Chlorobenzene

Stabilwax®, 30 m, 0.32 mm ID, 0.25 μm (cat.# 10624) Residual solvents class 2 - mix A (cat.# 36271) in 20 mL headspace vial (cat.# 24685) Water

Diluent: Injection Inj. Vol.: 1,000 μL headspace-syringe split (split ratio 5:1) Liner: 2 mm splitless (cat.# 20712) Inj. Temp.: 140 °C Headspace-Syringe Instrument: Overbrook Scientific HT200H Syringe Temp.: 100 °C Sample Temp.: 80 °C Sample Equil. Time: 45 min Inj. Speed: 8 Inj. Dwell: 5 sec Oven Oven Temp: 50 °C (hold 20 min) to 165 °C at 6 °C/min (hold 20 min) Carrier Gas He, constant flow Flow Rate: 2.15 mL/min Linear Velocity: 35.2 cm/sec Detector FID @ 250 °C

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681


GC CHROMATOGRAMS | PHARMACEUTICAL

Organic Volatile Impurities/Residual Solvents Residual Solvents (Class 2 - Mixture B) for Water-Soluble Articles on Rxi®-624Sil MS Peaks 1. 2. 3. 4. 5. 6. 7. 8.

Rxi® Technology! Exceptionally inert, ultra low-bleed capillary columns.

Column Rxi®-624Sil MS, 30 m, 0.32 mm ID, 1.80 μm (cat.# 13870) Sample Residual solvents class 2 - mix B (cat.# 36280) Diluent: Water Injection Headspace-loop split (split ratio 5:1) Liner: 1 mm split (cat.# 20972) Headspace-Loop Inj. Port Temp.: 140 °C Instrument: Tekmar HT3 Inj. Time: 1 min Transfer Line Temp.: 110 °C Valve Oven Temp.: 110 °C Sample Temp.: 80 °C Sample Equil. Time: 60 min Vial Pressure: 10 psi Pressurize Time: 0.5 min Pressure Equilibration Time: 0.05 min Loop Pressure: 5 psi Loop Fill Time: 0.1 min

Oven Oven Temp: Carrier Gas Linear Velocity: Dead Time: Detector Data Rate: Instrument Acknowledgement

5.355 6.793 8.092 9.980 12.941 21.303 24.862 33.781

Conc. (μg/mL) 2.42 0.42 0.50 0.83 0.67 1.67 0.42 0.83

GC_PH1148 40 °C (hold 20 min) to 240 °C at 10 °C/min (hold 20 min) He, constant flow 35 cm/sec 1.45 min @ 40 °C FID @ 250 °C 5 Hz Agilent/HP6890 GC Teledyne Tekmar

Residual Solvents (Class 2 - Mixture B) on Stabilwax® (G16) 1. 2. 3. 4. 5. 6. 7. 8.

Peaks Hexane 1,2-Dimethoxyethane Trichloroethylene Chloroform 2-Hexanone Nitromethane Pyridine Tetralin

Column Sample

GC_PH00953

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Hexane Nitromethane Chloroform 1,2-Dimethoxyethane Trichloroethene Pyridine 2-Hexanone Tetralin

tR (min)

Diluent: Injection Inj. Vol.: Liner: Inj. Temp.: Headspace-Syringe Instrument: Syringe Temp.: Sample Temp.: Sample Equil. Time: Inj. Speed: Inj. Dwell: Oven Oven Temp: Carrier Gas Flow Rate: Linear Velocity: Detector

Stabilwax®, 30 m, 0.32 mm ID, 0.25 μm (cat.# 10624) Residual solvents class 2 - mix B (cat.# 36272) in 20 mL headspace vial (cat.# 24685) Water 1,000 μL headspace-syringe split (split ratio 5:1) 2 mm splitless (cat.# 20712) 140 °C Overbrook Scientific HT200H 100 °C 80 °C 45 min 8 5 sec 50 °C (hold 20 min) to 165 °C at 6 °C/min (hold 20 min) He, constant flow 2.15 mL/min 35.2 cm/sec FID @ 250 °C

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GC CHROMATOGRAMS | PHARMACEUTICAL

Organic Volatile Impurities: Retention Time Index Reduce method development time—use a retention time index for column selection. Rxi®-624Sil MS

for more info

20 m x 0.18 mm x 1.0 μm df Dead time 0.81 minutes constant flow Initial 45 °C (hold 5 min) 7 °C/min to 220 °C (hold 5 min) Compound Formaldehyde Methanol Pentane Ethanol Diethylether 2-Chloropropane Acetone Methylal 1,1-Dichloroethene 2-Propanol Ethyl formate Methyl acetate Acetonitrile 2-Methylpentane Methylene chloride Methyl tert-buyl ether trans-1,2-Dichloroethene Hexane Isopropyl ether 1-Propanol Methyl cyclopentane Nitromethane 2-Butanone (MEK) cis-1,2-Dichloroethene Ethyl acetate 2-Butanol Tetrahydrofuran Chloroform 1,1,1-Trichloroethane 2,2-Dimethoxypropane Cyclohexane Carbon tetrachloride Isobutyl alcohol 2-Methoxyethanol 1,2-Dimethoxyethane Benzene

MS ion 29 31 43 31 59 43 43 45 61 45 45 43 41 43 84 73 61 57 45 31 56 61 72 96 43 45 42 83 97 73 56 117 42 45 45 78

char.ion 30,31 29,30,33 41,42,72,57,29 45,46,27 74,45 73,63,80,27 58,27,39 75,29,31 96,61,63 43,27,59 31,29,27,74 74,59,29 40,39,38 42,41,71,86 49,86,51,88 57,41,43,45 96,98,63 41,86,43 43,87,69 42,59,27 41,69,84 46,30 43,57 (use 43) 96,61,98 61,70 59,31 72,71,41 (use 72) 83,85,47,87,118 97,99,61 89,43,42,31 84,41,27 117,119 43,31,41,33 47,76 60,58,90 78

See pages 680–682 for Rxi®-624Sil MS chromatograms.

45(5)7/220(5) 1.16 1.36 1.74 1.76 1.87 1.95 2.06 2.07 2.08 2.15 2.2 2.33 2.33 2.48 2.5 2.7 2.76 3.05 3.22 3.22 3.76 3.83 3.9 3.96 4 4.21 4.34 4.51 4.76 4.81 4.88 5.04 5.31 5.31 5.41 5.41

Compound 1,2-Dichloroethane Isopropyl acetate Isooctane Methyl isopropyl ketone n-Heptane (C7) 1-Butanol Trichloroethene Methyl cyclohexane 1,4-Dioxane Propyl acetate 2-Ethoxyethanol Pyridine Hexanone (MIBK) Isoamyl alcohol Toluene Ethylene glycol Isobutyl acetate 1-Pentanol Formamide 1,1-Diethoxypropane 2-Hexanone (MBK) Butyl acetate Dimethyl formamide (DMF) Chlorobenzene Ethylbenzene p-Xylene m-Xylene Isoamyl acetate o-Xylene Dimethyl sulfoxide N,N-Dimethylacetamide Isopropylbenzene (cumene) Anisole 1-Methyl-2-pyrrolidinone 1,2,3,4-Tetrahydronaphthalene Sulfolane

MS ion 62 43 57 43 43 56 95 83 88 43 59 79 43 55 91 31 43 42 45 59 43 43 73 112 91 106 106 43 106 78 87 105 108 99 104 41

char.ion 62,98 61,87 56,41 41,86 57,71,100 41,43,55 95,97,134,132 55,98 58,43,57 61,73 31,45,72 52,50,51 58,56,85,100 42,41,43,70 92,65,51 33 56,73 55,70,41 29,44 47,87,103 58,57,100 56 44,58 112,77,114 91,106 106,91 106,91 55,70 106,91 63,45 44,43,72 120,77 78,65,51 98,44,42 132,117,91,65 56,55,120

45(5)7/220(5) 5.55 5.59 5.63 6 6.06 6.67 6.73 7.17 7.43 7.61 8.12 9.04 9.17 9.33 9.37 9.69 9.91 10.43 10.49 10.79 10.88 11.31 11.68 12.35 12.64 12.93 12.93 13.28 13.74 14.06 14.45 14.55 14.72 19.54 21.39 24.77

free literature Rxi®-624Sil MS: The “Go To” GC Column for Fast, Effective Volatile Impurities Method Development www.restek.com Download your free copy from www.restek.com lit. cat.# PHFL1245

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683


GC CHROMATOGRAMS | PHARMACEUTICAL

Organic Volatile Impurities: Retention Time Index Reduce method development time—use a retention time index for column selection. Retention time data collected using the following conditions: G16 Stabilwax®: 30 m, 0.25 mm ID, 0.5 μm df, Phase ratio: 125, Oven program: 40 °C, hold 1 min, to 190 °C @ 4 °C/min, hold 15 min, Carrier flow: 1.2 mL/min, Dead time: 1.38 min @ 45 °C G16 Rtx®-WAX: 30 m, 0.25 mm ID, 0.5 μm df, Phase ratio: 125, Oven program: 40 °C, hold 1 min, to 190 °C @ 4 °C/min, hold 15 min, Carrier flow: 1.2 mL/min, Dead time: 1.40 min @ 45 °C G43 Rtx®-1301: 30 m, 0.25 mm ID, 1.0 μm df, Phase ratio: 63, Oven program: 40 °C, hold 1 min, to 190 °C @ 4 °C/min, hold 15 min, Carrier flow: 1.2 mL/min, Dead time: 1.40 min @ 45 °C G27 Rxi®-5ms: 30 m, 0.25 mm ID, 1.0 μm df, Phase ratio: 63, Oven program: 40 °C, hold 1 min, to 190 °C @ 4 °C/min, hold 15 min, Carrier flow: 1.1 mL/min, Dead time: 1.49 min @ 45 °C G1 Rtx®-1: 60 m, 0.53 mm ID, 3.00 μm df, Phase ratio: 43, Oven program: 30 °C, hold 4 min, to 220 °C @ 4 °C/min, Carrier flow: 6.3 mL/min, Dead time: 2.54 min @ 35 °C Rtx®-200: 60 m, 0.53 mm ID, 3.00 μm df, Phase ratio: 43, Oven program: 30 °C, hold 4 min, to 220 °C @ 4 °C/min, Carrier flow: 7.8 mL/min, Dead time: 2.22 min @ 35 °C Carrier gas: helium Compound 1,1,1-Trichloroethane 1,1,2-Trichloroethene 1,1-Dichloroethene 1,2-Dichloroethane cis-1,2-Dichloroethene trans-1,2-Dichloroethene 1,2-Dimethoxyethane 1,4-Dioxane 1-Butanol 1-Pentanol 1-Propanol 2-Butanol 2-Ethoxyethanol 2-Methoxyethanol 2-Methyl-1-propanol 2-Propanol 3-Methyl-1-butanol Acetic acid Acetone Acetonitrile Anisole Benzene Butyl acetate Carbon tetrachloride Chlorobenzene Chloroform Cumene Cyclohexane Dichloromethane Dimethylsulfoxide Ethanol Ethyl acetate Ethyl benzene Ethyl ether Ethyl formate Ethylene glycol Formamide Formic acid Heptane Hexane Isobutyl acetate Isopropyl acetate Methanol Methyl acetate Methylbutyl ketone Methylcyclohexane Methylethyl ketone Methylisobutyl ketone m-Xylene N,N-Dimethylacetamide N,N-Dimethylformamide Nitromethane N-Methylpyrrolidone o-Xylene Pentane Propyl acetate p-Xylene Pyridine Sulfolane tert-Butylmethyl ether Tetrahydrofuran Tetralin Toluene 1,1-Diethoxypropane 2,2-Dimethoxypropane 2-Chloropropane 2-Methylpentane Acetaldehyde Chloroethane Chloromethane Ethylene oxide Formaldehyde Isoamyl acetate Isooctane Isopropyl ether Methyl cyclopentane Methyl isopropyl ketone Methylal Trichloroethene Water * Not determined

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ICH Class 1 2 1 1 2 2 2 2 3 3 3 3 2 2 3 3 3 3 3 2 3 1 3 1 2 2 3 2 2 3 3 3 2 3 3 2 2 3 3 2 3 3 2 3 2 2 3 3 2 2 2 2 2 2 3 3 2 2 2 3 3 2 2 — — — — — — — — — — — — — — — — —

G16 Stabilwax® Retention Time 3.96 15.72 2.23 8.80 6.50 3.63 4.80 8.55 11.13 14.95 7.69 7.25 13.99 12.42 9.32 4.81 13.42 22.47 3.02 6.91 18.65 5.23 8.86 3.96 13.91 7.31 12.36 2.16 5.01 26.47 4.98 4.08 10.72 1.72 3.16 28.06 32.99 24.64 1.98 1.65 6.99 4.26 4.23 3.19 9.10 2.50 4.33 6.84 11.21 20.75 18.04 11.82 29.84 12.79 1.49 5.98 10.98 12.64 47.62 1.94 3.63 25.12 7.86 5.42 3.11 1.96 1.58 2.05 1.83 1.63 2.05 2.25 10.51 1.85 1.86 1.91 4.93 2.26 6.50 8.24

G16 Rtx®-WAX Retention Time 3.49 14.28 2.04 7.68 5.65 3.20 4.18 7.49 10.08 13.75 6.80 6.44 12.70 11.11 8.40 4.25 12.25 20.34 2.64 5.83 17.09 4.54 7.88 3.49 12.54 6.41 11.17 2.01 4.33 24.43 4.37 3.56 9.58 1.63 2.78 26.23 30.93 22.09 1.86 1.58 6.18 3.74 3.64 2.80 8.05 2.30 3.76 5.97 10.04 19.01 16.26 10.31 27.86 11.51 1.45 5.29 9.82 11.24 43.31 1.82 3.19 23.48 6.91 4.84 2.79 1.82 1.52 1.85 1.71 1.55 1.86 1.57 9.43 1.75 1.76 1.79 4.29 2.06 5.70 7.18

G43 Rtx®-1301 Retention Time 5.43 10.99 2.79 6.15 4.79 3.55 6.03 7.86 7.18 11.19 4.20 5.08 8.69 6.02 6.00 3.00 9.86 6.52 2.89 3.28 17.12 5.98 12.12 5.61 13.55 5.23 16.66 5.37 3.31 16.62 2.52 4.87 13.86 2.58 3.00 10.77 11.85 5.19 6.34 3.77 10.39 6.19 1.96 3.17 11.81 7.31 4.90 9.64 14.29 12.95 13.09 4.84 25.09 15.46 2.39 8.03 14.29 9.60 34.02 3.50 5.12 27.49 9.80 11.39 5.48 2.67 3.22 1.86 2.14 1.70 1.89 1.68 14.84 5.84 4.03 4.50 6.58 2.84 7.07 1.74

G27 Rxi®-5ms Retention Time 5.40 9.77 4.41 5.46 2.88 3.54 5.54 7.26 5.76 9.44 3.37 4.16 7.36 5.14 4.79 2.55 8.26 4.61 2.50 2.47 16.28 3.83 11.38 5.90 13.14 4.64 16.69 5.89 3.06 13.01 2.19 4.44 13.81 2.67 2.78 6.63 7.30 2.60 6.98 4.11 9.69 5.71 1.80 2.93 10.50 7.95 4.09 8.49 14.17 13.96 10.23 3.53 21.85 15.26 2.62 7.44 14.17 8.57 28.90 3.59 4.90 27.44 9.66 11.38 5.55 2.66 3.56 1.84 2.10 1.70 2.02 1.58 14.18 6.59 4.23 4.93 5.69 2.82 7.05 1.68

G1 Rtx®-1 Retention Time 10.82 16.75 5.73 10.38 8.71 7.17 10.98 13.54 11.49 16.99 6.81 8.51 13.91 9.83 * 4.91 15.28 8.84 4.64 4.32 25.00 11.63 19.43 11.89 21.56 9.18 25.88 * 5.87 18.81 4.03 9.04 22.54 5.34 5.46 12.59 12.72 5.59 14.18 9.06 17.35 11.47 3.14 5.80 17.94 15.49 7.99 15.35 23.01 21.42 16.52 6.30 29.99 24.23 5.36 * 22.99 15.40 36.76 7.52 9.81 37.27 17.36 19.82 11.37 5.20 7.72 3.14 3.97 3.01 3.59 2.66 22.80 13.66 9.03 10.41 11.04 5.65 13.58 2.75

NA Rtx®-200 Retention Time 8.35 14.94 4.16 9.74 7.11 5.16 10.63 14.34 10.13 14.95 6.13 7.69 13.99 10.74 * 4.69 13.55 8.96 7.68 8.89 22.84 9.17 19.63 7.42 18.48 6.66 20.90 * 4.88 30.95 3.80 10.35 18.18 3.87 6.48 13.86 19.93 5.06 7.84 4.86 18.02 12.38 2.93 7.10 20.81 9.21 11.55 18.41 18.78 30.00 26.19 12.01 38.08 20.33 3.29 * 18.69 16.45 48.67 5.73 9.48 31.72 14.00 15.08 8.67 4.61 4.32 3.90 3.55 2.73 3.92 2.59 22.62 8.07 5.83 5.81 14.47 5.09 9.75 2.57

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GC CHROMATOGRAMS | SOLVENTS & CHEMICALS

Aldehydes, Amines Formaldehyde on Rt®-U-BOND (PLOT)

Excellent peak shape for highly polar analytes!

1. 2. 3. 4. 5.

Peaks Air Carbon dioxide Formaldehyde Water Methanol

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Make-up Gas Type: Data Rate: Sensitivity Mode: Instrument

Rt®-U-BOND, 30 m, 0.53 mm ID, 20 μm (cat.# 19750) Formaldehyde (manual headspace) 10 μL split (split ratio 10:1) 2 mm split Precision® liner w/wool (cat.# 20823) 200 °C 40 mL/min 100 °C (hold 1 min) to 150 °C at 25 °C/min (hold 3 min) He, constant pressure (7.7 psi, 53.1 kPa) 39 cm/sec @ 100 °C TCD @ 200 °C He 20 Hz He/H2 HP5890 GC

GC_CH01137

Ethyleneamines on Rtx®-5 Amine

Ethanolamines on Rtx®-5 Amine

Peaks 1. Monoethanolamine 2. Diethanolamine 3. Triethylene glycol monomethyl ether (IS) 4. Triethanolamine

1. 2. 3. 4. 5. 6. 7.

GC_CH00298

GC_CH00296 Column Sample Diluent: Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rtx®-5 Amine, 15 m, 0.25 mm ID, 0.50 μm (cat.# 12335) Ethanolamine mix Methanol 34 ng on column 1.0 μL split (split ratio 58:1) 280 °C 50 °C (hold 2 min) to 180 °C at 10 °C/min (hold 2 min) H2, constant pressure 43 cm/sec @ 50 °C FID @ 300 °C FID sensitivity: 6.4 x 10-11 AFS

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Peaks Isopropanol Monoethanolamine Ethylenediamine Piperazine Diethylenetriamine Aminoethylethanolamine Aminoethylpiperazine Remaining impurities consist of ethyleneamine and piperazine derivatives.

Column Sample Conc.: Injection Inj. Vol.: Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Notes

Rtx®-5 Amine, 30 m, 0.25 mm ID, 0.50 μm (cat.# 12338) Ethyleneamine industrial sample ~5-80 ng on-column 3.0 μL split (split ratio 20:1) 315 °C 40 °C (hold 4 min) to 315 °C at 10 °C/min (hold 5 min) H2, constant pressure 43 cm/sec @ 40 °C FID @ 315 °C FID sensitivity: 6.4 x 10-11 AFS

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685


GC CHROMATOGRAMS | SOLVENTS & CHEMICALS

Amines Primary Amines on Rtx®-35 Amine 1. 2. 3. 4. 5. 6. 7. 8. 9.

Column

Peaks Methylamine Dimethylamine Trimethylamine Ethylamine Isopropylamine tert-Butylamine n-Propylamine Diethylamine sec-Butylamine

Rtx®-35 Amine, 30 m, 0.53 mm ID, 1.00 μm (cat.# 11355) Primary amines Water 50 ppm on-column

Sample Diluent: Conc.: Injection Inj. Vol.: Liner:

2,3

Inj. Temp.: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

5 4

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1 μL split (split ratio 10:1) Splitless taper (4 mm), base deactivated (cat.# 20798-210.1) 250 °C

Visit our online technical library for chromatograms based on ASTM methods, USP procedures, and other applications.

35 °C (hold 5 min) He, constant pressure 35.7 cm/sec FID @ 300 °C

7 8

6

www.restek.com/chromatograms 9

1

0.5

1.0

1.5

2.0

2.5

3.0

3.5

Time (min)

4.0

4.5 5.0 GC_CH00578

Short Chain Amines in Water on Rtx®-Volatile Amine pA

Peaks 1. Methanol 2. Dimethylamine 3. Trimethylamine 4. Methylethylamine 5. Dimethylethylamine 6. Diethylamine 7. Methyldiethylamine 8. Triethylamine IS = isopropylamine

225

2

200

175

Column Rtx®-Volatile Amine, 60 m, 0.32 mm ID (cat.# 18078) Sample Short chain amines Diluent: Water Conc.: 200-1,000 ppm Injection Inj. Vol.: 1.0 μL split (split ratio 15:1) Inj. Temp.: 220 °C Split Vent Flow Rate: 30 mL/min Oven Oven Temp: 40 °C (hold 10 min) to 250 °C at 20 °C/min (hold 10 min) Carrier Gas H2, constant flow Flow Rate: 2.0 mL/min Linear Velocity: 35 cm/sec @ 40 °C Detector FID @ 250 °C Instrument Agilent/HP6890 GC Acknowledgement Chromatogram courtesy of Mr. Gilbert Baele of Taminco, Belgium

5

150

NEW!

125

100 IS 75

50 6 4

1

25

7

8

3

0 0

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5

10 Time (min)

15

20 GC_GN1154

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GC CHROMATOGRAMS | SOLVENTS & CHEMICALS

Amines, Ketones Impurity Analysis of 1,1,1,2-Tetrafluoroethane (CFC-134a) on Rt®-Alumina BOND/CFC (PLOT)

NEW!

1. 2. 3. 4.

Peaks Chloropentafluoroethane (CFC-115) Dichlorodifluoromethane (CFC-12) Chlorodifluoromethane (CFC-22) 1,1,1,2-Tetrafluoroethane (CFC-134a)

Rt®-Alumina BOND/CFC columns provide the best selectivity for impurity analysis of CFCs.

Column Sample Conc.: Injection Inj. Vol.: Oven Oven Temp: Carrier Gas Detector Notes

Rt®-Alumina BOND/CFC, 30 m, 0.53 mm ID (cat.# 19763) 1,1,1,2-Tetrafluoroethane Neat 500 μL split 80 °C (hold 6 min) to 140 °C at 10 °C/min (hold 2 min) He FID Gas sampling, purity analysis Note that tailing peaks are common in CFC analyses due to overloading normally employed for this type of work.

GC_GN1155

Ketones on Rt®-QS-BOND (PLOT) 1. 2. 3. 4.

Peaks Acetone 2-Butanone 2-Hexanone 4-Methyl-2-pentanone

free literature Restek’s PLOT Column Family: The New Benchmark For Performance! Download your free copy from www.restek.com lit. cat.# PCBR1163B-UNV

GC_PC01015 Column Sample Diluent: Conc.: Injection Inj. Vol.: Liner: Inj. Temp.: Oven Oven Temp: Carrier Gas Flow Rate: Detector

Rt®-QS-BOND, 30 m, 0.53 mm ID, 20 μm (cat.# 19738) VOA calibration mix #1 (ketones) (cat.# 30006) Methanol:water, 90:10 (v/v) 1,000 μg/mL 1 μL split (split ratio 50:1) Siltek® splitless taper (4 mm) (cat.# 20798-214.1) 240 °C 60 °C to 225 °C at 15 °C/min (hold 10 min) He, constant flow 5.7 mL/min FID @ 240 °C

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687


GC CHROMATOGRAMS | SOLVENTS & CHEMICALS

Solvents Solvent Mixture on Rt®-S-BOND (PLOT)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

Peaks Methanol Ethanol Acetonitrile Acetone Dichloromethane 1,1-Dichloroethene Nitromethane trans-1,2-Dichloroethylene cis-1,2-Dichloroethylene Tetrahydrofuran Chloroform Ethyl acetate 1,2-Dichloroethane 1,1,1-Trichloroethane

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

Benzene 1,2-Dimethoxyethane Trichloroethylene 1,4-Dioxane Pyridine Dimethylformamide Methylcyclohexane Toluene 2-Hexanone Chlorobenzene Ethylbenzene m-Xylene p-Xylene o-Xylene

Rt®-S-BOND, 30 m, 0.53 mm ID, 20 μm (cat.# 19746) Solvent mixture 1.0 μL split Taper (4 mm) (cat.# 20798) 200 °C 100 mL/min 120 °C to 220 °C at 5 °C/min (hold 5.0 min) H2, constant pressure (4.2 psi, 29.0 kPa) 40 cm/sec @ 120 °C FID @ 220 °C

GC_PC01080

Solvent Mixture on Rt®-QS-BOND (PLOT)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

Peaks Methanol Ethanol Acetonitrile Acetone Dichloromethane 1,1-Dichloroethene Nitromethane trans-1,2-Dichloroethylene cis-1,2-Dichloroethylene Tetrahydrofuran Chloroform Ethyl acetate 1,2-Dichloroethane 1,1,1-Trichloroethane

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

Benzene 1,2-Dimethoxyethane Trichloroethylene 1,4-Dioxane Pyridine Dimethylformamide Methylcyclohexane Toluene 2-Hexanone Chlorobenzene Ethylbenzene m-Xylene p-Xylene o-Xylene

Rt®-QS-BOND, 30 m, 0.53 mm ID, 20 μm (cat.# 19738) Solvent mixture 1.0 μL split Splitless taper (4 mm) (cat.# 20798) 200 °C 100 mL/min 120 °C to 240 °C at 5 °C/min (hold 5.0 min) H2, constant pressure (4.2 psi, 29.0 kPa) 40 cm/sec @ 120 °C FID @ 240 °C

GC_PC01081

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GC CHROMATOGRAMS | SOLVENTS & CHEMICALS

Solvents Solvent Mixture on Rt®-Q-BOND (PLOT)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

Peaks Methanol Ethanol Acetonitrile Acetone Dichloromethane 1,1-Dichloroethene Nitromethane trans-1,2-Dichloroethylene cis-1,2-Dichloroethylene Tetrahydrofuran Chloroform Ethyl acetate 1,2-Dichloroethane 1,1,1-Trichloroethane

Column Sample Injection Inj. Vol.: Liner: Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector

15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

Benzene 1,2-Dimethoxyethane Trichloroethylene 1,4-Dioxane Pyridine Dimethylformamide Methylcyclohexane Toluene 2-Hexanone Chlorobenzene Ethylbenzene m-Xylene p-Xylene o-Xylene

Rt®-Q-BOND, 30 m, 0.53 mm ID, 20 μm (cat.# 19742) Solvent mixture 1.0 μL split Splitless taper (4 mm) (cat.# 20798) 200 °C 100 mL/min 120 °C to 240 °C at 5 °C/min (hold 5.0 min) H2, constant pressure (4.2 psi, 29.0 kPa) 40 cm/sec @ 120 °C FID @ 240 °C

GC_PC01082

Solvents on MXT®-Q-BOND 1. 2. 3. 4. 5. 6. 7.

Peaks Methane Methanol Ethanol Acetone Diethylether Ethyl acetate Hexane

Column Sample Injection Inj. Temp.: Split Vent Flow Rate: Oven Oven Temp: Carrier Gas Linear Velocity: Detector Instrument

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NEW!

Excellent peak shape for alcohols.

MXT®-Q-BOND, 30 m, 0.53 mm ID, 20 μm (cat.# 79716) Solvent mix Split 250 °C

GC_PC1184

200 mL/min 150 °C H2, constant flow 40 cm/sec FID Agilent/HP6890 GC

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689

Chromatograms  

Chromatograms catalog 2013

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