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Presentation Topics
Overview of the LCQ Ion Optic System Tour of the LCQ Ion Optic System
Making Ions Transferring Ions Filtering Ions (Quadrupole Ion Trap) Detecting Ions
Mass Spectrometer
Simplified Schematic
Sample In
Make Ions
Transfer Ions
Filter Ions
Detect Ions
Data Out
APCI
Molecular Weight
GC
TSP PBI
FAB
Non Polar
Polar
Detect Ions
Mechanical Pump Auxiliary Gas Turbo Pump Turbo Pump +15 kV Ring Conversion Dynode Electrode
Make Ions
Desolvate Ions
Filter Ions
Nozzle
Needle Ion Plume Liquid Sheath
Aerosol Formation
Relative velocity between the sheath gas flow and the liquid flow causes a shearing effect on the emanating large droplet, and results in rapid droplet size reduction (spray)
Sheath Gas
Sample Tube
Heated Capillary
Field lines
Applied high voltage activates the coulombic explosion process
Infusion Flow Rate (L/min.): 3-5 Spray Voltage (kV): Spray Current (A): Sheath Gas Flow Rate (arb): Aux. Gas Flow Rate (arb): Capillary Temperature: Probe Position : 4-6 0.1-0.75 30-60 0 200-250C
Sample
Polyimide Sheath Liquid
Fused Silica
Elongation of polyimide occurs when specific solvents are adsorbed into the sample tube. The sample tube must be cut to ensure good spray.
ESI Needle
ESI Needle
Sheath Liquid
Sample
Polyimide Sheath Liquid
Fused Silica
Best results can be achieved by making the sample tube flush with the ESI Needle.
ESI Needle
Sample
Polyimide Sheath Liquid
Fused Silica
The polyimide can be flamed to avoid elongation; however, make sure the end of the fused silica is cut square.
ESI Needle
ESI Needle
Sheath Liquid ESI Needle Polyimide
Fused Silica
Sample
Polyimide Sheath Liquid
Fused Silica
Again, make sure the end of the fused silica is cut square. In this case, the fused silica is cut on an angle. This will produce poor spray.
ESI Needle
L oa d De t e ct or
I nj e ct W ast e
1 5
S HEATH G AS
SYRINGE PORT
4
6
A U X IL I A RY GAS SAMPLE HIG H V O LTA G E
WASTE LINE
2 1
PUMP
2 1
TO ION SOURCE
3 5
TO ION SOURCE
3 5
6
WASTE
6
WASTE
TO MS
TO WASTE
321
Probe Positions
LC Flow Rate
Infusion or LC at flow rates of <10 L/min LC at flow rates from 50 to 100 L/min
Sheath Gas
Required Typical setting: 20 to 40 units Required Typical setting: 80+ units
Auxiliary Gas
Not required Typical setting: 0 units Not required, but might help depending on conditions Typical setting: 0 units
1 mm ID
2 to 3 mm ID
Required
Not required, but usually helps to reduce solvent Typical setting: background ions 80+ units Typical setting: 20 units Required Typical setting: 80 to 100 units Required Typical setting: 20 units
4.6 mm ID
3-4
Infusion Flow Rate (L/min.): 3-5 Spray Voltage (kV): Spray Current (A): Sheath Gas Flow Rate (arb): Aux. Gas Flow Rate (arb): Capillary Temperature: Probe Position : 4-6 0.1-0.75 20-40 0 200-250C 2
Ion flow
Heated Capillary
Tangential Movement
matrix flow
LC Flow Rates
Sheath Gas
Required Typical setting: 10 to 30 units Required Typical setting: 80+ units Required Typical setting: 80+ units
Auxiliary Gas
Not required Typical setting: 0 units Required Typical setting: 10 to 20 units Required Typical setting: 10 to 20 units
Top
Top
Vaporizer Temp (C): Discharge Current (A): Discharge Voltage (kV): Sheath Gas Flow Rate (arb): Aux. Gas Flow Rate (arb): Capillary Temp (C): Capillary Voltage (V): Tube Lens Offset (V):
400-550 (600 max.) 5 (10A max.) 4-6kV (read back) 50-80 0-20 125-250 10-40 30-60 50L/min. - 2mL/min.
Spray current should not exceed 20A Once 20A level is reached, the spray voltage will be lowered to compensate for the 20A threshold
Problematic mixture of solvents/sample/etc. Bake out the probe for 10-60 minutes at 50C above desired Vaporizer Temperature Make sure the corona needle is seated and is not deformed
Solvent/Buffer
+ ++ + +
ESI Nozzle
( 8 kV)
Heated Capillary
Ion Stream
1 Torr
Peek Holder
10-3 Torr
Capillary must be flush with the Tube lens and Skimmer Mount. Kalrez OO- Ring
Manifold
Manifold
Peek Bushing Capillary Sleeve
Capillary Temp (C)*: Capillary Voltage (V): Tube Lens Offset (V):
* Heated Capillary I.D.: LCQ Classic / LCQ Duo: LCQ Deca: 400m 500m
Caution:
Periodically empty the waste bottle to avoid potential back streaming of waste solvent into the source region.
LC Flow Rate
Infusion or LC at flow rates of <10 L/min LC at flow rates from 50 to 200 L/min
Suggested Probe Heated Column Position Capillary Sheath Gas Auxiliary Gas Size (2 to 4) Temperature
Capillary 3 Typical setting: 300 C Typical setting: 350 C Required Typical setting: 10 to 30 units Required Typical setting: 80 units Not required Typical setting: 0 units Required Typical setting: 10 to 20 units
1 to 2 mm ID
Spray Cap
Configuration
Spray Shield
O-Ring
ESI Probe
Capillary Sleeve
Heated capillary
Spray Cap
Peek Bushing
Spray Shield
335.6
524.4
1122.1 1821.8
+ + + ++ + + +
++ + + + + + + + +
Heated Capillary
Bent Capillary Tip
Tube Lens
Skimmer
Avoid bending the tip of the heated capillary. The tip of the capillary must remain off axis to the skimmer; otherwise, spiky noise or reduced sensitivity can occur. The distance between the end of the capillary and the skimmer opening must remain fixed.
Fixed distance
Fundamental RF on Ring
Ion Trap
Ion Optics
Gating Ions into the Ion Trap
Multipole RF
Troubleshooting:
Loss of Sensitivity: Octapole Diagnostic errors: * Clean octapoles(multipoles) and lens * Tune multipole RF prior to running diagnostics.
* Multipole RF tune now performed in calibration for all LCQs run with Xcalibur.
3.5x10-3 torr He
220 L/sec
3.5x10-3 torr He
220 L/sec
3.5x10-3 torr He
220 L/sec
4000 50
Potential
20 0
4000 50
Potential
20 0
Tune Multipole RF
LCQ Deca
Multipole RF Tune
in Calibration Process
Square Quadrupole
Split Multipole
No Split Multipole
600
700
800
900
DECA
No Split LCQ
Ion Trap
Fundamental (Ring Electrode) and Resonance Ejection (End Caps) RF potential are ramped to sequentially eject ions from the Ion Trap
qz= k v
z
0.3 1.0 0 0.8 0.1 0.7 0.6 0.2 0.4 0.5 0.3 0.4 0.5 0.6
(m/z)
0 - 0.1 - 0.2 - 0.3 - 0.4 - 0.5 - 0.6 - 0.7 0.2 0.4 0.6 0.8 1.0
r
0.7 0.8 0.9 1.0
q z-edge = 0.908
1.2 1.4 1.6
qz
Notes:
Full scan target:
-Set to 5X10e7 for best sensitivity in the positive ion mode. -For best mass stability results, set to 2X10e7. -Set (2-3) times less in the negative ion mode. A typical value of 1X10e7 should be used. Positive/Negative switching: -Xcalibur allows for separate tune files. Pos/Neg scan segments can be used. ZoomScan target: -Set to (1-3)X10e6 for compounds with multiple charge. -Singly charged compounds will exhibit a slightly higher target. -For calibration with Cal Mix, set to 1X10e7.
Tune RF Frequency
LCQ Deca
Measure RF Frequency Detected RF RF Frequency Well Standing Wave Ratio Switch Status
Tune RF Modulation
LCQ Deca
Standing Wave Ratio Switch Status Detected RF Highest Mass
RF Modulation Upper and Lower Ranges
RF Modulation
High Mass noise due to a RF electrical discharge from inside the manifold.
Ion Detection
Electron Multiplier
Detection System
2-Particles enter the multiplier
Two particles formed when an ion ejected from the Ion Trap hits the dynode. Dynode particles enter the multiplier. Each particle hits the surface of the multiplier resulting in the ejection of two more particles.
Cathode Applied High Voltage
The cascading effect of this process will produce a charge on the anode cup. This charge represents the signal produced by the ion.
Anode cup
Note:
Multiplier voltage is a calibrated parameter. For best results, the multiplier should not be set manually.
Troubleshooting:
No peaks on Classic:
Check multiplier voltage Switch dynode polarity Check for ions
No peaks on Deca/Duo: Check Multiplier and Dynode Voltages. Noisy spectra with heated capillary capped off:
Potential Dynode noise Clean Dynode Cup
Dynode Noise
Dynode noise occurs over time. A noisy baseline with the heated capillary capped off is the symptom. This is due to an accumulation of material that can build up in the dynode cup over time. The cup should be cleaned when this occurs.
Voltage
Time
The voltage needed to produce gain on the multiplier should show a linear increase with time.
Daily:
Morning Recommendations:
Check the convectron and ion gauge pressures. Make sure the vacuum system is operational. Check the fused silica sample tube. Make sure the fused silica has not elongated. Remove the septum cap. Check the convectron and ion gauges pressure again. Make sure the vacuum pressures are still OK. Start your analysis.
Daily:
Evening Recommendations:
Put the system in the stand-by mode. Turn off the Ion Gauge and rinse the Heated Capillary with methanol or an appropriate solvent. When finished, turn Ion Gauge back on. Cap off the heated capillary with the septum cap. Secure the API probe to the API stack. Make sure the solvent waste bottle is empty. Open the mechanical pump ballast for roughly 0.5 hour. While the pump is ballasting, maintain (move, delete, and/or copy) files at the LCQ computer. If bottled nitrogen gas is being used, check the nitrogen gas. After 0.5 hour, close the ballast valve.
Weekly:
Check the mech. pump oil level. Fill the mech. pump as needed. If through put is high (running 24 hours a day), schedule one day a week to: - Change the mech. pump oil.
- Clean the skimmer and tube lens.
Check the LCQ calibration. Check the air filter. Clean if necessary. Possibly, change the mech. pump oil.
6 months to a year:
Change the turbo pump oil.
Notes
- The API stack and analyzer should be clean as needed. - If the sensitivity starts to drop off and can not be restored, clean the API stack (and analyzer) as needed.
Overview of Diagnostics
Tests and Tools provided:
Static Tests Dynamic Tests Diagnostic Tools Research Tools
Limitations:
Provides status of electronics components Does not provide readbacks from the actual source element Can not detect a broken or loose connection.
Dynamic Results
RF Test
Starting All Diagnostics Scan Tests 16:18:30: 16:18:35: 16:18:37: 16:18:37: 16:18:42: 16:18:44: 16:18:44: 16:18:48: 16:18:50: 16:18:50: 16:18:55: 16:18:57: 16:18:57: 16:19:02: 16:19:04: Start scan readback test on device Auxiliary amplitude (V) -- 0 to 83.2 Scan readback test ended Result: PASSED Start scan readback test on device Main RF DAC (16-bit) -- 0 to 65535 Scan readback test ended Result: PASSED Start scan readback test on device Vernier det. RF amp. (V) -- 0 to 65535 Scan readback test ended Result: PASSED Start scan readback test on device Vernier RF DAC (16-bit) -- 0 to 65535 Scan readback test ended Result: PASSED Start scan readback test on device Multipole RF DAC (V) -- 0 to 1000 Scan readback test ended Result: PASSED
Dynamic Test
Graphical Output
Dynamic Results
Lenses Test
Starting All Diagnostics Scan Tests 16:19:04: 16:19:09: 16:19:11: 16:19:11: 16:19:16: 16:19:17: 16:19:17: 16:19:22: 16:19:24: 16:19:24: 16:19:29: 16:19:31: Start scan readback test on device Multipole 1 offset (V) -- -132 to 132 Scan readback test ended Result: PASSED Start scan readback test on device Multipole 2 offset (V) -- -132 to 132 Scan readback test ended Result: PASSED Start scan readback test on device Multipole lens (V) -- -132 to 132 Scan readback test ended Result: PASSED Start scan readback test on device Multipole det. RF amp. (Vp-p) -- 0 to 1000 Scan readback test ended Result: PASSED
Dynamic Results
Ion Detection Test
Starting All Diagnostics Scan Tests 16:19:31: 16:19:36: 16:19:38: 16:19:38: 16:19:43: 16:19:45: 16:19:45: 16:19:58: 16:20:00: Start scan readback test on device Trap Offset (V) -- -132 to 132 Scan readback test ended Result: PASSED Start scan readback test on device Tube gate (V) -- -200 to 198.01 Scan readback test ended Result: PASSED Start scan readback test on device Multiplier (V) -- 0 to -2200 Scan readback test ended Result: PASSED
Dynamic Results
API Source Test
Starting All Diagnostics Scan Tests 16:20:00: 16:21:35: 16:21:37: 16:21:37: 16:23:20: 16:23:22: 16:23:22: 16:23:27: 16:23:28: 16:23:28: Start scan readback test on device Auxiliary gas flow (arb) -- 0 to 60 Scan readback test ended Result: PASSED Start scan readback test on device Sheath gas flow (arb) -- 20 to 100 Scan readback test ended Result: PASSED Start scan readback test on device Capillary Voltage (V) -- -132 to 132 Scan readback test ended Result: PASSED Final result: PASSED
Power Supplies
Static Diagnostic
Static Diagnostic
Lenses
Static Diagnostic
RF-1
Static Diagnostic
RF-2
Calibration
Diagnostic Tool
Toggles/Detector
Diagnostic Tool
Instrument Settings
Diagnostic Tool
Graphs
Graphs
Triggers
Research Tool
Communication:
computer. Will be green if the two computers are communicating. Will be yellow if the on-board AT is active but not communicating with the NT computer. Will be off if the LCQ is off or if a failure has occurred.
Communication: Indicates communication between the LCQ AT CPU and the NT computer.
Will be green if the two computers are communicating. Will be yellow if the on-board AT is active but not communicating with the NT computer. Will be off if the LCQ is off or if a failure has occurred.