topic 8 low thermal mass and capillary flow technology … · low thermal mass and capillary flow...
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Welcome toNEW “Chromatography Tips & Trick” India Seminar tour
Low Thermal Mass and Capillary Flow Technology for Faster Cycle Times
Abhijit PalMarketing Program Manager , India Chemical Analysis Solution
Life Sciences and Chemical Analysis Agilent Technologies , India
Goa 4 th May , 2010
Group/Presentation TitleAgilent Restricted
Month ##, 200X
AgendaSignificantly Reduce Analysis Times:
• Avoiding Bake-Out of HeavyComponents Beyond Your Peaks of Interest
• Rapid Heating and Cooling
GC, GC/MS News
… Using Agilent’s Technologies:
“Backflush” via Capillary Flow Devices
Low Thermal Mass (LTM) System
Both sold with new 7890 GC, GC/MS…but existing 7890/6890 systems canalso be upgraded to utilize these “productivity” technologies
Agilent’s Newest Technologies:
• Blos bead for GC/NPD
• Triple-axis detector for GC/MSD
• Agilent 7010 GC/MS/MS
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Defining Productivity
• More analyses per unit time . . .
– Faster and more efficient separations– Shorter analysis cycle time (time from injection to injection) – Reduced requirement for sample preparation
• with consistently better results . . .
– Quantitative: accuracy, precision, detection limits, linear range– Qualitative: response ratios, confirmatory retention times, library
searches (eliminate false negatives and false positives)
• while using less operator time for each analysis.
– Less time performing maintenance– Extensive computer control and data processing– Simplified operator review/approval
Productivity: the Sum of Many Technologies
• Low Thermal Mass GC
• Capillary Flow Technology - Backflush
• Hydrogen carrier gas for GC and GC/MS
• Retention Time Locking (RTL) Editor (& Methods)
– With more RTL Databases
• Trace Ion Detection
• Fast Electronic - Synchronous SIM/Scan
• Method Translator
• High signal-to-noise Triple-Axis Detector
– Gain Normalization of the EM
– EM Saver
• 2nd Generation Deconvolution Reporting Software (DRS)
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Jan 2007
Capillary Flow Technology
• Proprietary technology for GC IN OVEN flow manipulation
• Benefits
• Examples
– Backflush
– QuickSwap
– Deans Switch (Heart-cutting)
– Splitters
•
Capillary FlowTechnology Suite
Jan 2007
Significance of Capillary Flow Technology
• Customer survey
#1 in customer ranking• Customer comment
“Change the way we do chromatography, this is a lock-out for Agilent…Emphasize how simple it is:
- Agilent = Plate,- Shimadzu/Thermo = 30 parts”
• Agilent GC Field Advisory Team
Agilent 7890A’s key contribution
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Jan 2007
Improvements with Agilent 7890A GC
• Proven in Agilent 6890 GC
• Improvements in Agilent 7890 GC
– New capabilities
– Easier to set-up and operate
– Backflush user interface in software
• Improvements in support
– Application notes
– AE training
– CE training
GOAL: Widespread lockout for Agilent GC and GC/MS
Jan 2007
Capillary Flow Technology – Many Capabilities
QuickSwap (GC/MS)- Inlet maintenance, change GC column, without venting MS** Shorten/eliminate GC/MS downtime
Solvent Bypass - Eliminate early peaks** Lower detector maintenance costs
Heart Cut- Cut peaks to another column** Find trace levels in a complex matrix
Backflush- Eliminate later/post-run peaks** Shorten cycle times, eliminate sample carryover, less
column usage & lower detector maintenance costs
Split- Send all peaks to multiple detectors** Obtain more information during each run.
Find peaks of interest in unknowns
Modulate (New)- Send faction of effluence to 2nd column few seconds a time** Extra dimension separation during each run
obtain much rich information for complex sample
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Group/Presentation TitleAgilent Restricted
Month ##, 200X
Obtaining Faster GC, GC/MS Analytical Cycle Times – A Variety of Approaches to Fit Your Lab and Your N eeds
Post-RunBake-Out
ChromatographicRun
Post-RunCool-Down
Pre-RunALS Set-Up
Group/Presentation TitleAgilent Restricted
Month ##, 200X
Obtaining Faster GC, GC/MS Analytical Cycle Times – A Variety of Approaches to Fit Your Lab and Your N eeds
Post-RunBake-Out
ChromatographicRun
Post-RunCool-Down
Pre-RunALS Set-Up
Included “ALS Sample Overlap” 7890 GCin in ChemStation SW Faster Cool-down
HW/SW
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Group/Presentation TitleAgilent Restricted
Month ##, 200X
Obtaining Faster GC, GC/MS Analytical Cycle Times – A Variety of Approaches to Fit Your Lab and Your N eeds
Post-RunBake-Out
ChromatographicRun
Post-RunCool-Down
Pre-RunALS Set-Up
Included “ALS Sample Overlap” 7890 GCin in ChemStation SW Faster Cool-down
HW/SW
Faster GC Column Selection,Analyses Method Translation
Group/Presentation TitleAgilent Restricted
Month ##, 200X
Obtaining Faster GC, GC/MS Analytical Cycle Times – A Variety of Approaches to Fit Your Lab and Your N eeds
Post-RunBake-Out
ChromatographicRun
Post-RunCool-Down
Pre-RunALS Set-Up
Included “ALS Sample Overlap” 7890 GCin in ChemStation SW Faster Cool-down
HW/SW
Faster GC Column Selection,Analyses Method Translation
GC Add-Ons Capillary Flow TechnologySignficantly Faster GC (Backflush)Analytical Cycle Times
LTM Technology LTM Technology(Rapid Heating) (Rapid Cooling )
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Group/Presentation TitleAgilent Restricted
Month ##, 200X
5 10 15 20 25 30 35 40 45 50 55 60 65 70
It took additional 33 minsand column to 320oC to remove these high boilers.
min
Milk Extract
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Month ##, 200X
Backflush During GC Run
S/S Inlet
Purged CFTDeviceColumn
25 psi
4 psi
MSD
Aux EPCSplit Vent Trap
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Group/Presentation TitleAgilent Restricted
Month ##, 200X
Backflush
S/S Inlet
Purged CFTDeviceColumn
1 psi
45 psi
MSD
Aux EPCSplit Vent Trap
During GC Run
After GC Run
S/S Inlet
Purged CFTDeviceColumn
25 psi
4 psi
MSD
Aux EPCSplit Vent Trap
Group/Presentation TitleAgilent Restricted
Month ##, 200X
5 10 15 20 25 30 35 40 45 50 55 60 65 70
Run stopped at 42 min and backflushed at 280oC for 7 mins.
It took additional 33 minsand column to 320oC to remove these high boilers.
Blank run after backflushing
min
showing the column was clean.
Milk Extract
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Month ##, 200X
Benefits of Backflushing
– More samples/day/instrument
– Better quality data
– Lower operating costs
– Less frequent and faster GC & MSD maintenance
– Longer column life
– Less chemical background
– Available for Agilent 6890/7890
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GC and GC/MS Productivity Gains with Backflush
Industry Application Cap Flow Device
Back-flush Time
Saved
Cool-Down Time
Saved
FoodSafety
Pesticides inMilk Extract
Splitter 26 min(30%)
1 min
Enviro Fast 8270 QuickSwap 20 min (50%)
3 min
Forensics Fast Drugs of Abuse
Splitter 13 min
(20%)
1 min
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Group/Presentation TitleAgilent Restricted
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Each Purged Capillary Flow Device Has Dual Use
Backflushing
– Removes heavies from column
- Plus -
QuickSwap - Remove column w/o venting
– Air & H 2O blocked
– Safe disconnection of column from inlet for inlet maintenance
– Reversed flow through column during inlet maintenance
– Maintain constant flow to MSD
(flow rates exceeding 2 mL/min require an MSD with Performance Turbo)
MSD TransferLine
Aux EPC In
Column Effluent
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Other Purged Capillary Flow Devices AlsoProvide Dual Use (including Backflush Capability)
22--Way Splitter with Way Splitter with MakeupMakeup
33--Way Splitter with Way Splitter with MakeupMakeup
Deans SwitchDeans Switch
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Group/Presentation TitleAgilent Restricted
Month ##, 200X
Pesticides: Three Way Splitter with Makeup
1X method with 1:1:0.1 split FPD:MSD:ECD
3-Way Splitter with Makeup
Auto-sampler
7890GC
Column
Phosphorus FPD
30 m X 0.25 mm id X 0.25 um HP-5MS
5975C MSD
uECDAUX EPC3.8 psig
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Full scan TIC
SIM
µECD
5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00
FPD(P)
Milk Extract (1 injection)
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“LTM” (L ow Thermal M ass) Technology (Patented)
Directly heat/cool fused silica GC columns
“LTM” (L ow Thermal M ass) Technology
•Direct heating of fused silica GC columns
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Interfacing LTM GC to an Agilent 7890 or 6890 GC
GC oven door replaced with LTM-ready GC oven door (easy) Use same GC injectors, detectors, autosamplers, software, …
Column Modules mount outside isothermal GC oven for fast heating and cooling
Independent and simultaneous temperature programming of 1-4 column modules
Note: Front thermal shield removed to show LTM column modulesEntire thermal shield should always be in place during operation
LTM Column Modules
LTM Control System w/ Keypad User Interface(LTM Control SW for ChemStationAvailable from Agilent Nov/Dec’08)
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LTM Heating Speeds
Heating speeds can be set up to1800oC/min
- achievable rates depend on columnmass, configuration and column void times
- … also includeing practical trade-offsof speed vs resolution
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Typical Cooling Times for a LTM Column (Standard Si ze)
oC 2 m 5 m 10 m 15 m 30 m350->300 3 5 6 7 9300->250 3 5 7 7 13250->200 4 7 8 10 17200->150 4 8 11 13 22150->100 7 13 17 19 36100->50 13 27 34 41 75
Column Length
Type Time350oC � 50C LTM (2m Column) 34 seconds (= 3+3+4+4+7+13)Equilibration 3 seconds
350oC � 50C 7890 GC 3-4 minutesEquilibration 2-3 minutes
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Some Practical Uses of LTM Rapid Heating/Cooling
EnvironmentalNeed for high through-put, especially for low margin samples (eg. Total Petroleum Hydrocarbon (TPH)), where analytical cycle times are a critical element in making a profit
Hydrocarbon ProcessingCertain process control analyses (eg. Simulated Distillation) lend themselves to batch analysis. Shorter analytical cycle times get data back to operations faster, or allow more samples/shift
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Group/Presentation TitleAgilent Restricted
Month ##, 200XAgilent Restricted
Developing Faster GC Run Times for TPH Analysis(C10�C44 Standard Shown)
2x Faster,7890
min5 10 15 20 25 30 35
pApApApA
020
40
60
80
100n-
C10
n-C
12
n-C
14
n-C
16
n-C
18
n-C
20
n-C
22n-
C23
n-C
24
n-C
26
n-C
28
n-C
30
n-C
32
n-C
36
n-C
40
n-C
44
min2 4 6 8 10 12 14 16 18 20
pApApApA
20
40
60
80
100
120
n-C
10
n-C
12
n-C
14
n-C
16
n-C
18
n-C
20
n-C
22n-
C23
n-C
24
n-C
26
n-C
28
n-C
30
n-C
32
n-C
36
n-C
40
n-C
44
min0.5 1 1.5 2 2.5 3
pApApApA
0
200
400
600
800
1000
n-C
10
n-C
12
n-C
14n-
C16
n-C
18
n-C
20n-
C22
n-C
23n-
C24
n-C
26n-
C28
n-C
30n-
C32
n-C
36
n-C
40 n-C
44
10oC/min30m Column - 7890
20oC/min15m Column - 7890
200oC/min5m Column –LTM/7890 10x Faster,
LTM/7890
StandardGC RunTime
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LTM Also Greatly Reduces Cool-Down Times,� 9x Faster Heating/Cooling Cycle Times
Agilent Restricted
40 min + 5.4 min
20 min + 5.4 min
3 min + 2 min
GC Run Time Cool Down
9x Faster Cycle Time LTM/7890
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Soil Sample by TPH Analysis using LTM/7890Reliable Calculated Results, <3 minute run time
Agilent Restricted
Concentration*
Original Method (30 m) 1097 µg/mL
2X Method (15 m) 920 µg/mL
LTM Method (5 m) 909 µg/mL
*Calculated by Area Sum and Peak Grouping
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pA
0
1000
2000
3000
4000
5000
6000
min0.25 0.5 0.75 1 1.25 1.5 1.75 2 2.25
C5
C6 C
7
C8 C 9
C10
C11
C12
C14
C15
C16
C17
C18
C20
C24
C28 C
32
C36
C40
pA
min0.25 0.5 0.75 1 1.25 1.5 1.75 20
500
1000
1500
2000
Fast Simulated Distillation Under 3 Minutes by Use of Low Thermal Mass (LTM) Technologies… 6x faster compared to conventional ASTM D2887 proc edure
ASTM D2887 Reference Oil
LTM Module : 45ºC to 350ºC at 150ºC/min
Calibration sample C5-C44
LTM Module : 45ºC to 350ºC at 150ºC/min
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LTM System Technology - Summary
• High efficiency temperature programmingfast heatingfast cooling (< 1 min in some configurations)high throughputfast method development
• High performance chromatographyutilize commercially available columns (up to 30m length)very good retention time repeatability
• Easily integrates with conventional Agilent GC utilize existing injectors, detectors
• Multicolumn temperature control (1-4 modules)simultaneous, independent operation multidimensional GChigh throughput parallel systemsstrong synergy with Agilent’s Capillary Flow Technology
• Available for Agilent 6890/7890
ISCC User Meeting
May, 2008Page 34
GC, GC/MS News - Agilent GC/MS Portfolio
Smallest footprint, single GC column
Power of MRM
Industry leading GC/MS System
5975C with 7890GC
7000A GC/MS/MS
5975VL with 6850GC
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Group/Presentation TitleAgilent Restricted
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High Performance Triple-Axis Detector
Ultra low neutrals noise
Long life and high linearity
“Gain Normalization” corrects tune file for detector aging to allow repeatable, long term method sensitivity
hyperbolic quartztransmission
quadrupoleanalyzer
triple channelelectron multiplier
high energy dynode
steering rod
ion beam
X
Y
OffsetZ
shield for secondary particles
triple channelelectron multiplier
high energy dynode
steering rod
ion beam
XX
YY
OffsetZ
OffsetZ
shield for secondary particles
Group/Presentation TitleAgilent Restricted
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Agilent 7000 GC/MS/MS
The best 5975C GC/MS technology: • Heated monolithic gold plated quartz quadrupole
• Proven reliable high performance ion source design
• Low Noise Triple-Axis Detector
The best 6400 LC/MS/MS technology:• Linear acceleration enhanced hexapole collision cell
• MassHunter software
And new helium seeded collision cell technologyFor outstanding performance:
• 100 fg of OFN on column at 100:1 S/N RMS in MS/MS mode
• 500 MRM/sec Speed
Inert, high temp source (same as 5975C)
Triple-Axis Detector(as same 5975)
Gold plated quartz, hyperbolic quadrupole(same as 5975C)
Split Flow Turbo
New high performance hexapole collision cell (proprietary design)