advances in capillary column backflushing - · pdf file•no unpurged volumes ... fitting,...
TRANSCRIPT
![Page 1: Advances in Capillary Column Backflushing - · PDF file•No unpurged volumes ... fitting, with tubing extending fully into union ... 1/16” Swagelok tee. ISCCE 2010 15 Bleed OFF](https://reader031.vdocuments.us/reader031/viewer/2022011723/5a9bfdeb7f8b9a9c5b8e4efa/html5/thumbnails/1.jpg)
ISCCE 2010ISCCE 2010 1
Advances in Capillary Column Backflushing
Matthew S. Klee, Ph.D.
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ISCCE 2010ISCCE 2010 2
Capillary Flow Technology Traits
•Ease of use - ruggedness•Inertness•Usability to > 350 oC•Excellent exclusion of air •No unpurged volumes •No porous materials into which compounds can dissolve ( peak tailing)
•Fast thermal response •No outgassing or shedding of particles
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ISCCE 2010ISCCE 2010 3
FS Tubing Connections – The Magic
Column 1 In
Restrictor 1
out to vent
Plate
Ferrule
Nut
Restrictor 2
or Column 2
Channel
Unique design provides rugged, reliable connections with minimal unswept volume and high inertness
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ISCCE 2010ISCCE 2010 4
Ferrule Sealing
Seal region
Square cut is not critical
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ISCCE 2010ISCCE 2010 5
Backflush Setup
1. Start with working method and reference sample/chromatogram2. Extract pertinent method information from current method 3. Select BF configuration4. Prepare hardware (next slide)5. Install columns 6. Determine pressure/flow settings, download and test stability7. Screen standard on new configuration8. Lock with migrated RTL calibration if RTL method9. Pick last peak of interest using graphical tool, from which BF timing
and conditions are recommended10. Verify BF works11. Fine tune BF conditions if necessary
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ISCCE 2010ISCCE 2010 6
Preparing hardware during setup
Assemble necessary HW & SW (e.g. PCM/EPC, CFT, Instrument Utilities SW)
Install any needed modules and accessory kits
Check frit (recommend “open/zero” frit)
Check/update PIDs (using instrument utilities SW)
Zero all used pressure control zones (inlet, EPC)
Decide if you need a split purge and install preferred version
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ISCCE 2010ISCCE 2010 7
EPC/PCM instability at low P or flow
•EPC and PCM modules were designed for most accurate and precise control at flows > 1 mL/min−Proportioning valve duty cycle should never be 0%−Symptoms are: long stabilization time, cycling P
•Some backflush configurations require flows of < 1 mL/min
•Adding a bleed ensures stable pressure control−Fixed bleed−Variable bleed
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ISCCE 2010ISCCE 2010 8
Basic Bleed Configuration
Purged Purged UnionUnionColumn 1 Column 2
Det
He supply
EPC1P2
IN
Oven
1/16” Swagelok tee
vent
restrictor
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ISCCE 2010ISCCE 2010 9
Purged 1/16” Union
For purged splitting, in-oven connections
Eliminates air infiltration and stagnant lines
Provides bleed path for EPC stabilization and dumping excess column flow
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ISCCE 2010ISCCE 2010 10
Fixed restrictor configuration using G2855-80582 This is inside oven, replacing
old Swagelok union
These are outside oven on top
Big one goes to Aux EPC
Use 1/16” straight Swagelok union with Vespel ferrules
Small one goes to vent (room, vacuum vent, split vent trap, etc.)
Let hang loose or vent using whatever connectors necessary according to user requirements
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ISCCE 2010ISCCE 2010 11
Cut off and remake the QuickSwap in-oven fitting, with tubing extending fully into union (past the purge point)
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ISCCE 2010ISCCE 2010 12
Fixed split with purged tube fitting
Column
MSDRestrictor
CFT
P1
S/S Inlet
Inlet EPC
P2
AuxEPC
Purged Tube Fitting
Outside oven
Use Vespel ferrules here
vent
Inside Oven
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ISCCE 2010ISCCE 2010 13
Variable split bleed saves the day
Provides necessary bleed to allow pressure control solenoids to operate well (> 1 mL/min)Maintains low flow even during high-pressure backflushUses normally unused pressure channel (EPC, Backpressure channel on PCM)Allows split flow to be turned OFF for leak checkingProvides the opportunity to program bleed flow for custom applications
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ISCCE 2010ISCCE 2010 14
Using 2nd EPC for Bleed During Run
Set P3 < P2
2 mL/min independent
of P2
Purged Purged UnionUnionColumn 1 Column 2
Det
SV Trap
He supply
EPC1P2
IN
Oven
IN
EPC2P3
atmosphere1/16” Swagelok tee
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ISCCE 2010ISCCE 2010 15
Bleed OFF During Leak Check
0 mL/min
Purged Purged UnionUnionColumn 1 Column 2
Det
SV Trap
He supply
EPC1P2
IN
Oven
IN
EPC2OFF
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ISCCE 2010ISCCE 2010 16
Variable restrictor configuration using G2855-80581 This is inside oven, replacing
old Swagelok union
These are outside oven on top
From Aux EPC 1 (purge feed line)
Use 1/16” straight Swagelok union with Vespel ferrules
Vent to split vent trap then to input of EPC 2
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ISCCE 2010ISCCE 2010 17
Post-Column BF with Variable Split
Column
MSDRestrictor
QuickSwap
P1
S/S Inlet
Inlet EPC
P2
AuxEPC 1
Purged Tube Fitting
Outside oven
Use Vespel ferrules here
AuxEPC 2
vent
trap
P3
Inside oven
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ISCCE 2010ISCCE 2010 18
Large-Volume Injection, Cool On-Column Solvent Vapor Exit
Not for the novice!
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ISCCE 2010ISCCE 2010 19
LVI COC SVE with Pre-Column Backflush to Vent 1
Vent
G3186B Purged Ultimate Union
COC
ColumnCoated
Vent
G3180B Purged 2-Way Splitter
EPC
Det
Pre-Columns
Uncoated
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ISCCE 2010ISCCE 2010 20
LVI COC SVE with Backflush of the column to Vent 2
EPCmakeup
G3180APurged Splitter
Column
COC
Retention Gap
Pre Column
G3182B Ultimate Union Det 1
Det 2
Vent
Purged Ultimate Union G3186,
G1472A
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ISCCE 2010ISCCE 2010 21
Conclusion
Capillary column backflushing has a large potential return – but requires some attention to detail to set up
Cost to implement backflushing is relatively low and is greatly facilitated by readily available instrument parts and accessories