Agilent Technologies, Inc. · NYSE:A
Agilent Technologies — Technical Presentation (2011)
44 slides from Agilent Technologies's technical presentation, 2011
Slide 1: Low Thermal Mass (LTM) GC Technology Revealed: A Practical Guide
Low Thermal Mass (LTM) GC Technology Revealed: A Practical Guide Roger L Firor Agilent Technologies Wilmington, DE Gulf Coast Conference 2011 Page 1
Slide 2: “LTM” (Low Thermal Mass) Technology (Patented)
“LTM” (Low Thermal Mass) Technology (Patented) Directly heat/cool fused silica GC columns Gulf Coast Conference 2011 Page 2
Slide 3: LTM - Low Thermal Mass Technology
LTM - Low Thermal Mass Technology “Fast Cool-Down” “Fast Temperature Ramps” “Spec” 1800oC/min, Typical <400oC/min LTM Cooldown Times (Standard Size) Temperature Range 120 V Oven Fast Ramps Insert ** 400 (°C) (°C/min) > 200 V, 15A > 200 V, 15A 350 300 50 to 70 75 120 120 2m LTM Temp (oC) 250 70 to 11
Slide 4: LTM Column Module
LTM Column Module Installed external to main GC oven Lead Torus Lead FANS Gulf Coast Conference 2011 Page 4
Slide 5: Connecting an LTM Column Module to Inlet and Detector
Connecting an LTM Column Module to Inlet and Detector • Option 1: Use CFT unions and deactivated fused silica leads of same diameter as column > Column module protected by retention gap tubing > Users need to learn how to make CFT connections • Option 2: Use module with long column leads > Avoids us
Slide 6: Module to Retention Gap Connection
Module to Retention Gap Connection Old New Gulf Coast Conference 2011 Page 6
Slide 7: 2010: Valco Unions → Unions Based on Capillary Flow Technology (CFT)
2010: Valco Unions Unions Based on Capillary Flow Technology (CFT) Metal Ferrules Easy to use, do not loosen or leak with oven cycling to 350 C Metal Deactivation Gulf Coast Conference 2011 Page 7
Slide 8: Transfer Line Assembly
Transfer Line Assembly Heated column guide Brackets attach to rails Gulf Coast Conference 2011 Page 8
Slide 9: 5 inch Column Module Installed on Transfer line
5 inch Column Module Installed on Transfer line Gulf Coast Conference 2011 Page 9
Slide 10: 2011: LTM II
2011: LTM II LTM Integrated w/ 7890 GC - Hardware - Firmware - Software Gulf Coast Conference 2011 Page 10
Slide 11: LTM II: Electronics/Firmware Integration
LTM II: Electronics/Firmware Integration LTM PCB – Direct digital communication w/ 7890 GC FW/UI: - PCB has “GC” performance/reliability - Improved thermal control (now digital). Temperature control/display - Confirms cable connections - Diagnostics, thermal fault detection - Added “GC” Press/Flow c
Slide 12: Configuring an LTM II Module in ChemStation
Configuring an LTM II Module in ChemStation LTM Series II IN Segment Column Segment Out Segment Segment 2 GC Oven GC Oven MSD GC Oven is set isothermal at a temperature at or close to maximum LTM module programmed temperature Gulf Coast Conference 2011 12
Slide 13: What are the Best Uses for LTM Technology?
What are the Best Uses for LTM Technology? • Speed up an analysis where overall throughput is important > Simulated Distillation > Total Petroleum Hydrocarbons > Solvent analysis • Multi-dimensional separations where an independent oven is needed to operate under a different temperature program comp
Slide 14: The LTM Advantage
The LTM Advantage • Total Cycle time for an analysis can be cut by a factor of three or more (compared to same columns in an air oven) • Single or dual column configurations (5 inch format) • Dual column configurations allow simultaneous injection • With dual column modules, two different phases (i.
Slide 15: Setting Column Flow with an LTM Module (First Generation)
Setting Column Flow with an LTM Module (First Generation) •The 7890A or 6890 Series GC’s did not have knowledge of LTM column temperature •Constant flow mode could not be set from the GC keypad or software •Options for setting flow in an LTM Module - constant pressure - ramped flow For approximate c
Slide 16: Setting Column Flow with an LTM Module (Second Generation: LTM II)
Setting Column Flow with an LTM Module (Second Generation: LTM II) •The 7890A GC has knowledge of LTM column module temperature •Constant flow mode integrated •Options for setting flow in an LTM II Module > constant pressure > constant flow > ramped flow •LTM II control completely integrated in GC C
Slide 17: Comparison of Cycle Times: Conventional Air Bath vs. LTM
Comparison of Cycle Times: Conventional Air Bath vs. LTM Heating Column Program Cool Down Cycle Time 7890A (120V) 30M x 0.53mm x 40 C(20 min) to 240 6 min 50 sec with 67 min 3.0um DB624 C (20 min) @ 10 3 min oven equil. C/min 7890A (120V) 7M x 0.25mm x 35 C (5 min) to 240 8 min 25 sec 25 min 1.4um D
Slide 18: Fast Chromatography
Fast Chromatography • Users typically choose columns that are longer than needed for a given application • Optimal oven program rates will be around 10 °C/void time • Consider column flow rates that are 2 to 3 times optimum • When translating a method from air-bath to LTM: - consider changing both c
Slide 19: Method Translate: Long to Short Column of Same Diameter
Method Translate: Long to Short Column of Same Diameter [column rows] Flow Rate Column ID 10M 5M 4M ml/min um (°C/min) (°C/min) (°C/min) 12 530 15 31 (2X) 40 (2.6X) 6 320 15 34 (2X) 44 (3X) 3 250 15 35 (2X) 45 (3X) 2 180 15 34 (2X) 50 (3X) Gulf Coast Conference 2011 Page 19
Slide 20: Simplest Calculator: Agilent Pressure/Flow
Simplest Calculator: Agilent Pressure/Flow Typically used to find inlet pressure and/or flows Lengths and diameters are found by iteration Gulf Coast Conference 2011 Page 20
Slide 21: Agilent Method Translator
Agilent Method Translator Find conditions to get same elution order and precisely scale method to new speed or new outlet pressure Speed up factor Constant phase ratio New inlet pressure New flow Gulf Coast Conference 2011 Page 21
Slide 22: Translation from 10M to 5M: D2887
Translation from 10M to 5M: D2887 Column ID and Phase ratio maintained Gulf Coast Conference 2011 Page 22
Slide 23: Translation from 530 to 320
Translation from 530 to 320 Phase ratio maintained 320 column available with 1.50um film – close enough Gulf Coast Conference 2011 Page 23
Slide 24: Translation to LTM: D2887 SimDis
Translation to LTM: D2887 SimDis 530u to 320u column Gulf Coast Conference 2011 Page 24
Slide 25: Interfacing LTM II to a Deans Switch
Interfacing LTM II to a Deans Switch Gulf Coast Conference 2011 Page 25
Slide 26: Deans Switch Calculator
Deans Switch Calculator Primary column: 1.3 ml/min, LTM: 2.5 ml/min LTM Series II/ Deans Switch/5975C 26 September 22, 2011
Slide 27: System Diagram: LTM II/Deans/FID-MSD
System Diagram: LTM ll/Deans/FID-MSD NC PCM 2 1 7 m x 0.25 mm x 0.25 um NO 3 HP-INNOWax LTM II Split 5975C Inlet MSD FID Primary column restrictor 30 m x 0.25 mm x 0.25 um DB5ms Deans Switch Gulf Coast Conference 2011 27
Slide 28: System Diagram: LTM II/Deans/FID-FID
System Diagram: LTM ll/Deans/FID-FID NC PCM 2 1 NO 3 FID LTM II Split Inlet FID restrictor Primary column Deans Switch Gulf Coast Conference 2011 28
Slide 29: 4,6-Dimethyl dibenzothiophene in Road Diesel
4,6-Dimethyl dibenzothiophene in Road Diesel Oven Programs Primary: 80 °C (0) to 340 °C (5) @ 10 °C/min Ovens offset by 30° C LTM II: 50 °C (3) to 240 °C (5) @ 8 °C/min TIC SIM 7.2 ppm FID Gulf Coast Conference 2011 Page 29
Slide 30: 10.6 ppb 4,6-Dimethy dibenzothiophene
10.6 ppb 4,6-Dimethy dibenzothiophene Standard SIM Gulf Coast Conference 2011 Page 30
Slide 31: 1.8 ppm of 4,6-Dimethyl dibenzothiophene in Marine Diesel
1.8 ppm of 4,6-Dimethyl dibenzothiophene in Marine Diesel TIC SIM FID Gulf Coast Conference 2011 Page 31
Slide 32: Calibration
Calibration 4,6-Dimethyldibenzothiophene 1400000 y = 125764x - 17928 1200000 R² = 0.9995 1000000 800000 600000 400000 200000 0 0 2 4 6 8 10 12 ppm 120000 100000 y = 91849x + 806.33 R² = 0.9999 80000 60000 40000 20000 0 0 0.2 0.4 ppm0.6 0.8 1 1.2 Gulf Coast Conference 2011 Page 32
Slide 33: Fuel Ethanol
Primary oven: 30 m x 0.25 mm x 0.25 um DB-5ms Fuel Ethanol LTM: 7 m x 0.25 mm x 0.25 um INNOwax Methanol level is 0.01% 1. Butane 2. Acetaldehyde 3 4 3. Iso-pentane 4. Pentane EtOH 5. 2-Pentene 6. Methanol 1 2 5 6 Cut: 1.80 min to 2.00 min Primary oven: 50 °C (5 min) to 280 °C (5 min) @ 20 °C/min Ov
Slide 34: LTM II/Deans Switch for Analysis of Natural Oils
LTM II/Deans Switch for Analysis of Natural Oils Primary column: 30 m x 0.25 mm x 0.25 um DB5ms LTM II column: 30 m x 0.25 mm Cyclodex Oven Programs 4 6 Primary:70 °C (1) to 280 °C (17) @ 10 °C/min 2 Geranium, cuts at: 8.25 to 8.38 LTM II: 75 °C (7) to 130 °C (5) @ 2 °C/min (linalool), 9.3 to 9.5 Me
Slide 35: Fast GC Applications
Fast GC Applications Gulf Coast Conference 2011 Page 35
Slide 36: Parameters: Hydrocarbon Oil Index
Parameters: Hydrocarbon Oil Index Injection 1 µL, splitless (0.4 min purge delay), 350°C Inlet liner split/splitless P/N 5183 - 4647 (bottom taper, glass wool near top, 4 mm i.d., ) Carrier gas 9 mL/min He constant flow LTM Column 10 m x 0.32 mm i.d. x 0.1 µm DB-5HT LTM Retention gap leads 0.5 m x 0
Slide 37: Calibration Sample of Diesel Plus Motor Oil
400 mg/L Calibration Sample of Diesel Plus Motor Oil Diesel 4500000 4000000 Motor oil 3500000 3000000 Response 2500000 2000000 1500000 1000000 500000 0 0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 Time (min) Gulf Coast Conference 2011 Page 37
Slide 38: Comparison of Sensitivity Gain from Standard Oven Program to Fast LTM Program
Comparison of Sensitivity Gain from Standard Oven Program to Fast LTM Program 4500000 4000000 Response 3500000 3000000 2500000 LTM, 3 min run 2000000 1500000 1000000 500000 0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 4500000 4000000 Response 3500000 3000000 Standard, 21 min run 2500
Slide 39: D2887 SimDis
D2887 SimDis 5 m x 0.32 mm x 0.5 um DB1 LTM Module: 35°C to 350°C (30 s) @ 100°C/min Multimode inlet: 325°C (0 min) to 355°C (2 min) @ 200°C/min Constant Flow: 12 ml/min Split: 20 to 1 7890A oven: 300°C C5 to C40 Calibration in under 3 min. RGO Gulf Coast Conference 2011 Page 39
Slide 40: PW 500: LTM II System
PW 500: LTM II System Column: 5M x 0.53mm x 0.15um DB-HT SimDis LTM Temp Program: 40°C (0 sec) to 400°C (30 sec) @ 50°C/min 7890A Oven: 325°C Isothermal 7890A Carrier: He, constant flow Injection: 2 ul of PW500 in toluene PTV: 210°C (0 min) to 400°C (2 min) @ 300°C/min C20 C70 0 1 2 3 4 5 6 7 8 Gulf
Slide 41: GCxGC: Dual LTM II System
GCxGC: Dual LTM II System S/S inlet:: constant flow mode Three Independent temperature programs possible PCM: Pressure control mode, LTM columns in constant flow S/S Inlet Column 2 Column 1 LTM FID FID PCM Micro Valve Modulator FID Column 3 LTM FID FID LTM = Low Thermal Mass Splitter Gulf Coast Conf
Slide 42: Dual LTM: DB17HT and INNOwax
Dual LTM: DB17HT and INNOwax Paraffin/aromatic mix 40 °C (0 min) to 200 °C @ 3 °C/min DB17HT 5 m x 0.25 mm x 0.15 um •Faster method development •Complimentary results depending on application 30 °C (5 min) to 240 °C @ 2 °C/min INNOwax •Allows wider range of columns (phase ratio’s) to be used 5 m x 0
Slide 43: LTM Series II
LTM Series II • System part # : G6680A, 5 inch format with 2 power supplies • 7890A firmware requirement: A.01.12.1 or greater • GC ChemStation: B.04.03 DSP1, includes LTM II control software • MSD ChemStation: E.02.02 Gulf Coast Conference 2011 43
Slide 44: Summary
Summary • LTM series II incorporates a number of new features including full control integrated in ChemStation, and operation in true constant flow mode that assists the analyst with development of new methods. This is especially true with more complex configurations involving the Deans switch and 5