lcq deca_duo hardware troubleshooting_8601
TRANSCRIPT
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LCQ Deca/Duo HardwareTroubleshooting
Ed Gonzalez
Product Support
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Presentation TopicsPresentation 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
LCQ Maintenance
LCQ Diagnostic Overview
Front Panel LEDs Indications
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Mass SpectrometerMass SpectrometerSimplified Schematic
MakeIons
TransferIons
FilterIons
DetectIons
SampleIn
DataOut
Ion Optics SystemIon Optics System
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ESI
GCPBI
TSPFAB
Molecular
Weight
200,000
15,000
1,000
Non Polar
APCI
Polar
Choice in Making IonsChoice in Making IonsPolarity vs. Molecular WeightPolarity vs. Molecular Weight
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Simplified LCQ SchematicSimplified LCQ Schematic
Sheath Liquid
Sheath Gas
ESI Needle Assembly
Heated Capillary
Tube LensOctapole
EndcapElectron
Multiplier
Auxiliary GasSkimmer
RingElectrode
+15 kVConversion
Dynode
MechanicalPump
TurboPump
TurboPump
APCI Probe
Assembly
Make Ions Filter I ons
DetectIons
Transfer Ions
Desolvate Ions
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LCQ Probes used in Making IonsLCQ Probes used in Making Ions
API-1 / ESI Probe (LCQ Classic) API-2 / ESI Probe (LCQ Deca / LCQ Duo)
API-2 / Off Axis ESI Probe (Classic/Deca/Duo) APCI Probe (Same for API-1 and API-2)
i i
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ESI Ionization ProcessESI Ionization ProcessSimplified Schematic
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ESI Spray Cross SectionESI Spray Cross Section
Gas SheathGas Sheath
Liquid SheathLiquid Sheath
NozzleNozzle
NeedleNeedle
Ion PlumeIon Plume
55kVkV
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Aerosol FormationAerosol Formation
Sample Tube
Sheath GasSheath Gas
HeatedHeated
CapillaryCapillary
Field linesField lines
Applied high voltage activates thecoulombic explosion process
Relative velocity between the sheath gas flow and the liquid flowcauses a shearing effect on the emanating large droplet, and
results in rapid droplet size reduction (spray)
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APIAPI--1 / ESI Probe Assembly1 / ESI Probe Assembly(LCQ Classic)
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Cal Mix Tune ParametersCal Mix Tune ParametersAPI-1 on LCQ Classic
Infusion Flow Rate (L/min.): 3-5
Spray Voltage (kV): 4-6 Spray Current (A): 0.1-0.75
Sheath Gas Flow Rate (arb): 30-60 Aux. Gas Flow Rate (arb): 0
Capillary Temperature: 200-250C Probe Position : Pulled all the way back
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LCQ Deca Tune Plus WindowLCQ Deca Tune Plus WindowESI Source dialog and Status Panel
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Troubleshooting the API1 ProbeTroubleshooting the API1 Probe Spray Current too high: High Voltage (HV) shorting effects:
Leaks within ESI Probe Problematic mixture of solvents/sample/etc.
Erratic Spray Voltage: Shorted HV cableSpay current at maximumBad HV supply
Erratic spray: Sample tubeESI needleSheath gas flow
Contamination: Wipe spray shield around heated capillaryWipe out ESI probe flangeFlush the ESI probeClean ESI probe interior parts
Overall solution for 90% of source related Problems: good maintenance
(especially with the sample tube) use of divert valve
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APIAPI--1 / ESI Probe Cross Section1 / ESI Probe Cross Section
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Sample Tube ElongationSample Tube Elongation
Sheath Liquid
ESI NeedleESI Needle
Sample
Polyimide
Polyimide
Fused Silica
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
ESI Needle
Sample
Polyimide
Polyimide
Fused Silica
Fused Silica
The sample tube must be cut
square to ensure good spray.
Best results can be achieved
by making the sample tube
flush with the ESI Needle.
ESI Needle
ESI Needle
Sheath Liquid
Sheath Liquid
Sheath Liquid
ESI Needle
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Sample Tube Elongation ResolutionSample Tube Elongation Resolution
ESI NeedleESI Needle
Sample
Sheath Liquid
Polyimide
Polyimide
ESI Needle
ESI Needle
Fused Silica
Fused Silica
ESI Needle
Sample
Polyimide
Polyimide
ESI Needle
Fused Silica
Fused Silica
The polyimide can be flamed
to avoid elongation; however,
make sure the end of the
fused silica is cut square.
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
Sheath Liquid
Sheath Liquid
Sheath Liquid
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Divert Valve ConfigurationDivert Valve Configuration
Front Panel Injections
S H E A T H
G A S
3
5
4
2
1
S H E A T H
L I Q U I D
S A M P L EA U X IL I A R Y
G A SH IG H
V O L T A G E
L o a d
Det ec t o r
In j ect
Was t e
6
WASTE
LINE
SAMPLE
LOOP
TRANSFER LINE
FROM LC PUMPDIVERT/
INJECT
VALVE
SYRINGE
PORT
TRANSFER LINE FROM
DIVERT/INJECT VALVE
TRANSFER LINE
FITTING
GROUNDED
FITTING
HOLDERSAMPLE TUBE
ESI SOURCE
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Divert Valve ConfigurationDivert Valve ConfigurationNormal Applications
SHEATHGAS
35
4
2
1
SHEATHLIQUID
SAMPLEAUXILIARYGAS HIGHVOLTAGE
Load
Detector
Inject
Waste
6
WASTELINE
TRANSFER LINEFROM LC PUMP
DIVERT/INJECTVALVE
TRANSFER LINE FROM
DIVERT/INJECT VALVE
TRANSFER LINEFITTING
GROUNDEDFITTINGHOLDER
SAMPLE TUBE
ESI SOURCE
11
2
33
44
55
66
FROM LC
PUMP
TO MS TO WASTE
TO ION
SOURCE
FROM LC
PUMP
TO ION
SOURCE
WASTE WASTE
2
lib
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Xcalibur Instrument SetupXcalibur Instrument SetupDivert Valve Dialog
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APIAPI--2 / ESI Probe Assembly2 / ESI Probe Assembly(LCQ Deca / LCQ Duo)
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API-2 / ESI Probe Positions
4 3 2 14 3 2 1
ProbeProbePositionsPositions
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APIAPI--2 / ESI Guidelines2 / ESI Guidelines
Operational Parameters
LC Flow RateSuggested
Column
Size
ProbePosition
(1 to 4)
HeatedCapillary
Temperature
Sheath
Gas
Auxiliary Gas
Infusion or LC at flow rates of
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APIAPI--2 / ESI Probe2 / ESI Probe
Exploded Pictorial
C l iC l Mi T P t
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Cal Mix Tune ParametersCal Mix Tune ParametersAPI-2 on LCQ Deca / LCQ Duo
Infusion Flow Rate (L/min.): 3-5
Spray Voltage (kV): 4-6 Spray Current (A): 0.1-0.75
Sheath Gas Flow Rate (arb): 20-40 Aux. Gas Flow Rate (arb): 0
Capillary Temperature: 200-250C
Probe Position : 2
LCQ D T Pl Wi dLCQ Deca Tune Plus Window
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LCQ Deca Tune Plus WindowLCQ Deca Tune Plus Window(ESI Source dialog and Status Panel)
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Troubleshooting the API2 ProbeTroubleshooting the API2 Probe
Contamination: Wipe spray shield around heated capillaryWipe out ESI probe flangeFlush the ESI probe
Erratic spray: Sample tubeSheath gas flow
Spray Current too high: Problematic mixture of solvents/sample/etc.
Erratic Spray Voltage: Spray current at maximum
Overall solution for 90% of source related Problems: Good maintenance
(especially with the sample tube) Use of divert valve
APIAPI--2 / ESI Probe Assembly2 / ESI Probe Assembly
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API 2 / ESI Probe Assembly/ S obe sse b yCross Section
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APIAPI--2 / Off Axis ESI Probe2 / Off Axis ESI Probe
(LCQ Deca / LCQ Duo / LCQ Classic)
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APIAPI--2 / Off Axis ESI2 / Off Axis ESI
Probe Geometry
Tangential Movement
ESI probe on a 25 degree slide
HeatedHeated
matrix flowmatrix flow
Ion flowIon flow
CapillaryCapillary
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APIAPI--2 / Off Axis ESI Guidelines2 / Off Axis ESI Guidelines
Operational Parameters
LC Flow RatesSlidePlate
Position
ProbePosition
(1 to 7)
HeatedCapillary
Temperature
Sheath
Gas
Auxiliary
Gas
Infusion or LC at flow
rates of 200 L/min
Top 5 Typical setting:
350 C
Required
Typical setting:80+ units
Required
Typicalsetting:10 to 20 units
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APCI Ionization ProcessAPCI Ionization Process
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LCQ Classic APCI ProbeLCQ Classic APCI Probe
b
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LCQ Deca / LCQ Duo APCI ProbeLCQ Deca / LCQ Duo APCI Probe
Typical APCI TuneParametersTypical APCI TuneParameters
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Typical APCI Tune ParametersTypical APCI Tune ParametersConditions: Reserpine at 1ml/min
Vaporizer Temp (C): 400-550 (600 max.)
Discharge Current (A): 5 (10A max.)
Discharge Voltage (kV): 4-6kV (read back)
Sheath Gas Flow Rate (arb): 50-80
Aux. Gas Flow Rate (arb): 0-20
Capillary Temp (C): 125-250
Capillary Voltage (V): 10-40
Tube Lens Offset (V): 30-60
Flow Rate capability: 50L/min. - 2mL/min.
LCQ Deca Tune Plus WindowLCQ Deca Tune Plus Window
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APCI Source dialog and Status Panel
T bl h ti th APCI P bT bl h ti th APCI P b
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Troubleshooting the APCI ProbeTroubleshooting the APCI Probe
Spray voltage erratic: Spray current should not exceed 20AOnce 20A level is reached, the sprayvoltage will be lowered to compensate
for the 20A threshold
Spray current too high: Problematic mixture of solvents/sample/etc.
Contamination: Bake out the probe for 10-60 minutes at 50Cabove desired Vaporizer Temperature
Lack of sensitivity: Make sure the corona needle is seatedand is not deformed
APIAPI 1 / API1 / API 2APCI P b2APCI P b
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APIAPI--1 / API1 / API--2 APCI Probe2 APCI Probe
Cross Section
I T f / D l ti PI T f / D l ti P
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Ion Transfer / Desolvation ProcessIon Transfer / Desolvation ProcessOverview
Heated CapillaryHeated Capil lary IonIonStreamStream
ESI NozzleESI Nozzle(( 8 kV)8 kV)
Solvent/BufferSolvent/Buffer+
+
+
+
++
+
+
++
LCQ API Stack Gas FlowLCQ API Stack Gas Flow
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Peek Holder
Tube lens
skimmerskimmer1 Torr1 Torr
1010--33 TorrTorr
LCQ API Stack AssemblyLCQ API Stack AssemblyCross Section
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Cross Section
Capillary SleeveCapillary Sleeve
Peek BushingPeek Bushing
Kalrez OKalrez O--RingRing
Capillary must be flush with theCapillary must be flush with the
Tube lens and Skimmer Mount.Tube lens and Skimmer Mount.
ManifoldManifold
ManifoldManifold
Capillary SleeveCapillary Sleeve
Peek BushingPeek Bushing
Kalrez OKalrez O--RingRing
Capillary must be flush with theCapillary must be flush with the
Tube lens and Skimmer Mount.Tube lens and Skimmer Mount.
ManifoldManifold
ManifoldManifold
Heated Capillary Specifications:Heater Resistance: 14Platinum Sensor: 110
Cal Mix Tune ParametersCal Mix Tune Parameters
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Cal Mix Tune ParametersLCQ API Stack
Capillary Temp (C)*: 200-250
Capillary Voltage (V): 10-40
Tube Lens Offset (V): 30-60
* Heated Capillary I.D.:
LCQ Classic / LCQ Duo: 400m
LCQ Deca: 500m
LCQ Deca Tune Plus WindowLCQ Deca Tune Plus Window
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CQ eca u e us doQVacuum dialog and Status Panel
Troubleshooting the API StackTroubleshooting the API Stack
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Troubleshooting the API StackTroubleshooting the API Stack
Loss of Sensitivity: Clean skimmer and tube lens
Low Convectron Gauge Pressure: Heated capillary plugged
Cal Mix Contamination: Clean API probe and heated capillary area
Spiky noise: Bent capillary tip or dirty heated capillary Constant Background: Possible heated capillary contamination
Overall solution for 90% of API Stack related Problems: Good maintenance:
Clean/Rinse the heated capillary regionand spray shield daily.
Use of the divert valve
Use of Spray Cap and OrthogonalSampling Adapter
Caution:
Periodically empty the waste bottle to avoid potential back streaming of wastesolvent into the source region.
Orthogonal Spray AdapterOrthogonal Spray Adapter
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Orthogonal Spray AdapterOrthogonal Spray AdapterConfiguration
Buffer depositionBuffer deposition
Heated capillaryHeated capillary
Focusing ringFocusing ring Liquid drainsLiquid drains
ESI ProbeESI Probe
Orthogonal ion flowOrthogonal ion flow
Orthogonal Spray Adapter GuidelinesOrthogonal Spray Adapter Guidelines
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Orthogonal Spray Adapter GuidelinesOrthogonal Spray Adapter GuidelinesOperational Parameters
LC Flow Rate
Suggested
ColumnSize
Probe
Position(2 to 4)
Heated
CapillaryTemperature
Sheath Gas Auxil iary Gas
Infusion or LC at flow
rates of
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Configuration
Heated capillaryHeated capillary
ESI ProbeESI ProbeCapillary SleeveCapillary Sleeve
OO--RingRing
Spray CapSpray Cap
Spray ShieldSpray Shield
Reduces Cal Mix contaminationReduces Cal Mix contamination
PeekPeek
BushingBushing
Spray ShieldSpray Shield
Spiky Noise CharacteristicsSpiky Noise CharacteristicsSingle Noise Spike
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Single Noise Spike
S#: 4 RT: 0.27 AV: 1 T: +p Full ms NL: 2185325
326 327 328 329 330 331 332 333 334 335
m/z
0
10
20
30
40
50
60
70
80
90
100
RelativeAbundance
330.5
335.6
334.3328.6 330.9326.6 327.6 334.6329.0328.0 331.8
Spiky Noise CharacteristicsSpiky Noise CharacteristicsParticle Noise Spectrum of Cal mix
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Particle Noise Spectrum of Cal mix
S#: 4 RT: 0.27 AV: 1 T: +p Full ms NL: 7692800
200 400 600 800 1000 1200 1400 1600 1800
m/z
0
10
20
30
40
50
60
70
80
90
100
RelativeAbundance
1421.9
1522.0
1621.8
1322.1
1222.11721.9
1122.1524.41821.8
330.5
959.6536.3308.5
872.7 1022.3690.9
195.2
413.3812.2262.7 553.7
Spiky Noise at 10 uscans
S#: 4 RT: 0.27 AV: 1 T: +p Full ms NL: 7692800
200 400 600 800 1000 1200 1400 1600 1800
m/z
0
10
20
30
40
50
60
70
80
90
100
RelativeAbundance
1421.9
1522.0
1621.8
1322.1
1222.11721.9
1122.1524.41821.8
330.5
959.6536.3308.5
872.7 1022.3690.9
195.2
413.3812.2262.7 553.7
Spiky Noise at 10 uscans
Heated Capillary Cross SectionHeated Capillary Cross SectionBent Capillary Tip
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p y p
Fixed
distance
Tube
Lens
Heated
CapillarySkimmer
Bent Capillary Tip
With time, compound will
neutralize out on the skimmer.
This will spot will eventually
need to be cleaned; otherwise,
field affects can reduce
sensitivity.
Avoid bending the tip of the heatedcapillary. 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.
+
+
+++
+
+
++
++
+
++
++
++
+
Ion Transfer OverviewIon Transfer Overview
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Ion Transfer OverviewIon Transfer OverviewDeca Ion Optic System
Ion Trap
Transfer
Array
Fundamental RF
on Ring
Ion Streamfrom skimmer
Ions will be trapped
in stable trajectories
Ion OpticsIon OpticsGating Ions into the Ion Trap
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Gating Ions into the Ion Trap
Octapole 1 Offset: LCQ / LCQ DuoOctapole 1 Offset: LCQ / LCQ Duo
Quadrupole 1 Offset: LCQ DecaQuadrupole 1 Offset: LCQ DecaOctapole 2 Offset:Octapole 2 Offset:
LCQ / LCQ Duo / LCQ DecaLCQ / LCQ Duo / LCQ DecaMultipole RFMultipole RFOctapole 1 Offset: LCQ / LCQ DuoOctapole 1 Offset: LCQ / LCQ Duo
Quadrupole 1 Offset: LCQ DecaQuadrupole 1 Offset: LCQ DecaOctapole 2 Offset:Octapole 2 Offset:
LCQ / LCQ Duo / LCQ DecaLCQ / LCQ Duo / LCQ DecaMultipole RFMultipole RF
LCQ Deca Tune Plus WindowLCQ Deca Tune Plus WindowIon Optics dialog and Status Panel
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Cal Mix Tune ParametersCal Mix Tune ParametersLCQ I O i
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LCQ Ion Optics
Octapole 1 Offset (V) for Classic/Duo: -1 to -5
Octapole 1 Offset (V) for Deca: -4 to -9
Lens Voltage (v): -16 to -50Octapole 2 Offset (V) for Classic / Duo: -5.5 to -10
Octapole 2 Offset (V) for Deca: -7 to -15Octapole RF Amplitude (V p-p): 400
Entrance Lens (V) for the Deca only:Entrance Lens (V) for the Deca only: -35 to -60 V
Troubleshooting:Troubleshooting:Loss of Sensitivity: * Clean octapoles(multipoles) and lens
Octapole Diagnostic errors: * Tune multipole RF prior to running diagnostics.
* Multipole RF tune now performed in calibrationfor all LCQs run with Xcalibur.
LCQLCQ ClassicClassic OpticsOptics
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CQQ Classic Op cspTypical Operating Pressures
1.0 torr 1.7x10-3 torr760 torr 2.0 x10-5 torr (1.0x10-5 torr He)
3.5x10-3 torr He
220 L/sec100 L/sec30 m3/hr
LCQLCQ DuoDuo OpticsOptics
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QQ ppTypical Operating Pressures/Comparison to LCQ Classic
1.0 torr 1.7x10-3 torr760 torr 2.0 x10-5 torr (1.0x10-5 torr He)
3.5x10
-3
torr He220 L/sec100 L/sec30 m3/hr
LCQLCQ DecaDeca OpticsOptics
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QQ ppTypical Operating Pressures/Comparison to LCQ Classic
1.3 torr 1.7x10-3 torr760 torr 2.0 x10-5 torr (1.0x10-5 torr He)
3.5x10-3 torr He
220 L/sec100 L/sec60 m3/hr
Potential Energy DiagramPotential Energy DiagramLCQ and LCQ Duo
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4000
-15000
Potentia
l
20
50
0
-3
-20
-7
-10
0
-23
-40-30
Source CID
= 20%-27
Potential Energy DiagramPotential Energy DiagramLCQ Deca
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4000
-15000
Potential 20
50
0
-5-7 -10
0
-20
-50
RF Tune Diagnostic DialogRF Tune Diagnostic DialogLCQ Deca
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Tune Multipole RFTune Multipole RFLCQ Deca
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Multipole RF Tunein Calibration Process
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in Calibration Process
Multipole RF Tuneverification performedprior to calibration.
LCQ Deca Ion OpticsLCQ Deca Ion OpticsSpecifics Features
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Square QuadrupoleSquare Quadrupole
New InterNew Inter--Octapole LensOctapole Lens
New Endcap ElectrodesNew Endcap Electrodes
New Entrance LensNew Entrance Lens
Square QuadrupoleSquare Quadrupole
New InterNew Inter--Octapole LensOctapole Lens
New Endcap ElectrodesNew Endcap Electrodes
New Entrance LensNew Entrance Lens
Split MultipoleSplit MultipoleDeca / Duo Configurations
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Transmit - both set to Offset Value
Deflection - set to +132
Split Square Quadrupole
LCQ Deca
Split Octopole
LCQ Duo
Deflection - set to -132
Effect of Split MultipoleEffect of Split Multipole
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200 300 400 500 600 700 800 900m/z
0
10
20
30
40
50
60
70
80
90
100
Rela
tiveAbundance
With Split
Multipole
No SplitMultipole
MRFAm/z 524(with isotopes)
MRFA
m/z 524(with isotopes)
200 300 400 500 600 700 800 9000
10
20
30
40
50
60
70
80
90
100
RelativeAbundance
LCQ Deca Noise ReductionLCQ Deca Noise Reduction
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Pulsed lens
+DC-DC
No Split
Split DC on Scan out
LCQ
DECA
Overview of Ion SeparationOverview of Ion SeparationQ d l I T
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Quadrupole Ion Trap
Ion Streamfrom Transfer Array
Ion TrapFundamental (Ring Electrode) and Resonance Ejection (End Caps) RF potential
are ramped to sequentially eject ions from the Ion Trap
Mass Selective InstabilityMass Selective InstabilitySimplified Overview
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qz
a z
0
0.2
0.1
- 0.1
- 0.2
- 0.3
- 0.4
- 0.5
- 0.6
- 0.70.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6
0.2 0.3
0.40.5
0.60.7
0.81.0
0.2
0.3
0.4
0.5
0.6
0.7
0.8
1.0
0.10
0.9
z
r
q z = k v(m/z)
q z-edge = 0.908
Ion Trap Mass AnalyzerIon Trap Mass AnalyzerFilter Ions
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Filter Ions
Quadrupole Ion TrapQuadrupole Ion TrapOperational Parameters
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Main RF: 16.2 kV p-p max.(760kHz)
Resonance Ejection RF: 80 V p-p max.(frequency Varies)
Waveform RF: 160 V p-p max.(Arbitrary)
Trap Offset: 10 V fixed
Exit Lens: at Ground potential
Helium gas consumption: 1 cc/min. undervacuum
LCQ Deca Tune Plus WindowLCQ Deca Tune Plus WindowInjection Control dialog and Status Panel
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Troubleshooting the Ion Trap
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Loss of Sensitivity: Clean End caps and ring electrode High Mass Noise: Clean spacer rings and endcaps.
Lack of sensitivity/resolution/mass stability:Lack of helium or Air leak
Notes:
Full scan target: -Set to 5X10e7 for best sensitivityin 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 withmultiple charge.-Singly charged compounds will exhibit aslightly higher target.-For calibration with Cal Mix, set to 1X10e7.
Tune RF FrequencyTune RF FrequencyLCQ Deca
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Standing WaveStanding Wave
RatioRatio
Switch StatusSwitch Status
Detected RFDetected RF
Measure RFMeasure RF
FrequencyFrequency
RF FrequencyRF FrequencyWellWell
Tune RF ModulationTune RF ModulationLCQ Deca
StandingStanding
WW
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WaveWave
RatioRatio
Switch StatusSwitch Status
Detected RFDetected RF
RF ModulationRF Modulation
RF ModulationRF ModulationUpperUpper
andand
LowerLower
RangesRanges
Highest MassHighest Mass
High Mass NoiseHigh Mass Noise
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S#: 34 RT: 1.11 AV: 1 T: + p ms NL: 10610
200 400 600 800 1000 1200 1400 1600
m/z
0
10
20
30
40
50
60
70
80
90
100
RelativeAbundance
1
1641.4
1628.6
1504.01336.0
1229.1
901.9
951.5 1196.3
High Mass noise due to a RF electrical discharge from inside the manifold.
Affects of Helium on SpectraAffects of Helium on Spectra
S#:1 RT:0.00 AV:1 SM:7G NL:2.50E7
T:+p Full ms
S#:23-32 RT:0.71-1.00AV:10 SM:7G NL:5.61E7
T:+p Full ms
Helium flowing into trapHelium flowing into trap
S#:1 RT:0.00 AV:1 SM:7G NL:2.50E7
T:+p Full ms
S#:23-32 RT:0.71-1.00AV:10 SM:7G NL:5.61E7
T:+p Full ms
Helium flowing into trapHelium flowing into trap
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T:+p Full ms
514 516 518 520 522 524 526 528
m/z
0
20
40
60
80
100
R
elativeAbundance
524.3
525.3
T:+p Full ms
500 1000 1500 2000
m/z
0
20
40
60
80
100
R
elativeAbundance
1522.04
1621.97
1322.061721.89
1222.141821.95524.26
1122.21 1921.88
195.15 1022.09
S#:1 RT:0.02 AV:1 SM:7G NL:9.70E6
T:+p Full ms
514 516 518 520 522 524 526 528
m/z
0
20
40
60
80
100
Relative
Abundance
522.6523.0
521.8
521.2523.9
520.7
S#:23-32 RT:0.39-0.54AV:10 SM:7G NL:2.80E7
T:+p Full ms
500 1000 1500 2000
m/z
0
20
40
60
80
100
Relative
Abundance
1620.791520.26
1720.441320.95
1220.75
523.01 1919.961120.90
192.17
Helium shut off and not flowing into trapHelium shut off and not flowing into trap
T:+p Full ms
514 516 518 520 522 524 526 528
m/z
0
20
40
60
80
100
R
elativeAbundance
524.3
525.3
T:+p Full ms
500 1000 1500 2000
m/z
0
20
40
60
80
100
R
elativeAbundance
1522.04
1621.97
1322.061721.89
1222.141821.95524.26
1122.21 1921.88
195.15 1022.09
S#:1 RT:0.02 AV:1 SM:7G NL:9.70E6
T:+p Full ms
514 516 518 520 522 524 526 528
m/z
0
20
40
60
80
100
Relative
Abundance
522.6523.0
521.8
521.2523.9
520.7
S#:23-32 RT:0.39-0.54AV:10 SM:7G NL:2.80E7
T:+p Full ms
500 1000 1500 2000
m/z
0
20
40
60
80
100
Relative
Abundance
1620.791520.26
1720.441320.95
1220.75
523.01 1919.961120.90
192.17
Helium shut off and not flowing into trapHelium shut off and not flowing into trap
Ion DetectionIon Detection
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Electron MultiplierElectron MultiplierDetection System
2-Particles
enter the Two particles formed when an ion
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multiplier
Applied High
Voltage
Anode cup
Cathode
Two particles formed when an ion
ejected from the Ion Trap hits thedynode. Dynode particles enter themultiplier.
Each particle hits the surface of themultiplier resulting in the ejection oftwo more particles.
The cascading effect of this processwill produce a charge on the anodecup.
This charge represents the signalproduced by the ion.
Signal to Data system.Signal to Data system.~~
LCQ Deca Tune Plus WindowLCQ Deca Tune Plus WindowIon Detection System dialog and Status Panel
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Detection System ParametersDetection System Parameters
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Dynode Voltage: 15kV (fixed) Electron Multiplier: 2500 Volts max.
Note:
Multiplier voltage is a calibrated parameter.
For best results, the multiplier should not be set manually.
Troubleshooting:
No peaks on Classic: Check multiplier voltageSwitch 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 NoiseDynode Noise
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Dynode noise occurs over time.
A noisy baseline with the heatedcapillary capped off is the
symptom. This is due to an accumulation of
material that can build up in thedynode cup over time.
The cup should be cleaned whenthis occurs.
Life Time of theLife Time of the
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Electron MultiplierElectron Multiplier
The voltage needed to produce gain on the multiplier should showThe voltage needed to produce gain on the multiplier should show a linear increase with time.a linear increase with time.
TimeTime
VoltageVoltage
LCQ Recommended Maintenance ScheduleLCQ Recommended Maintenance Schedule
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Daily:Morning Recommendations:
Check the convectron and ion gauge pressures. Make sure thevacuum 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 surethe vacuum pressures are still OK.
Start your analysis.
LCQ Recommended Maintenance ScheduleLCQ Recommended Maintenance Schedule
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Daily:Evening Recommendations: Put the system in the stand-by mode.
Turn off the Ion Gauge and rinse the Heated Capillary with methanolor 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.
LCQ Recommended Maintenance ScheduleLCQ Recommended Maintenance Schedule
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Weekly:For normal operation:
Check the mech. pump oil level.
Fill the mech. pump as needed.
If through put is high (running 24 hours a day), scheduleone day a week to:
- Change the mech. pump oil.- Clean the skimmer and tube lens.
LCQ Recommended Maintenance ScheduleLCQ Recommended Maintenance Schedule
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Monthly:Every Month:
Check the helium gas tank pressure. Replace as needed.
Check the nitrogen gas tank (Dewer) pressure. Replace as needed.
Nitrogen gas consumption:
Typical: 3-6 L/min
Worse case scenario associated with choice of Nitrogen Generator:
15L/min (28SCFH at 100psi and 99% purity) for LCQ Classic
30L/min (56SCFH at 100psi and 99% purity) for Duo / Deca
Check the LCQ calibration. Check the air filter. Clean if necessary.
Possibly, change the mech. pump oil.
LCQ Recommended Maintenance ScheduleLCQ Recommended Maintenance Schedule
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Every 3 months:
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 berestored, clean the API stack (and analyzer) as needed.
Overview of Diagnostics
T t d T l id d
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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.
Prior to running the dynamic diagnostics:
Tune all RF components (Octapole/Multipole and Main RF). Make sure the system in the ON mode.
Make sure the API Probe is bolted to the API stack. This allows thehigh voltage to be activated.
Run All DiagnosticsRun All DiagnosticsDynamic and Static Tests
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Static Results from Status TestStatic Results from Status Test
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+15 V - Pass
+150 V - Pass
+205 V - Pass
+24 V - Pass
+28 V - Pass
+35 V - Pass
+36 V - Pass
+5 V - Pass
-15 V - Pass-150 V - Pass
-205 V - Pass
-28 V - Pass
8 kV PS voltage - Pass
Ambient temp. - Pass
Analyzer temp. - Pass
Aux gas flow - Pass
Capillary temp. - PassCapillary voltage - Pass
Convectron - Pass
Detected RF - Pass
Dynode voltage -PassEntrance lens - Pass
Intermultipole lens - Pass
Ion gauge - Pass
Main RF DAC - Pass
Multiplier setting - Pass
Multiplier voltage - Pass
Multipole 1 offset - Pass
Multipole 2 offset - Pass
Multipole RF mod. - Pass
Multipole det. RF - Pass
Multipole RF amp. out - Pass
RF amp. output - Pass
RF det. temp. - PassRF gen. temp. - Pass
RF modulation - Pass
Sheath gas flow -Pass
Trap DC Offset - PassTube/gate lens -Pass
Dynamic ResultsDynamic ResultsRF Test
Starting All Diagnostics Scan Tests
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16:18:30: Start scan readback test on deviceAuxiliary amplitude(V) -- 0 to 83.2
16:18:35: Scan readback test ended
16:18:37: Result: PASSED
16:18:37: Start scan readback test on device Main RF DAC(16-bit) -- 0 to 6553516:18:42: Scan readback test ended
16:18:44: Result: PASSED
16:18:44: Start scan readback test on device Vernier det. RF amp. (V) -- 0 to 65535
16:18:48: Scan readback test ended16:18:50: Result: PASSED
16:18:50: Start scan readback test on device Vernier RF DAC(16-bit) -- 0 to 65535
16:18:55: Scan readback test ended
16:18:57: Result: PASSED
16:18:57: Start scan readback test on device Multipole RF DAC(V) -- 0 to 1000
16:19:02: Scan readback test ended
16:19:04: Result: PASSED
Dynamic TestDynamic TestGraphical Output
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Dynamic ResultsDynamic ResultsLenses Test
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Starting All Diagnostics Scan Tests
16:19:04: Start scan readback test on device Multipole 1 offset (V) -- -132 to 132
16:19:09: Scan readback test ended16:19:11: Result: PASSED
16:19:11: Start scan readback test on device Multipole 2 offset (V) -- -132 to 132
16:19:16: Scan readback test ended
16:19:17: Result: PASSED
16:19:17: Start scan readback test on device Multipole lens (V) -- -132 to 132
16:19:22: Scan readback test ended
16:19:24: Result: PASSED
16:19:24: Start scan readback test on device Multipole det. RF amp. (Vp-p) -- 0 to 1000
16:19:29: Scan readback test ended16:19:31: Result: PASSED
Dynamic ResultsDynamic ResultsIon Detection Test
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Starting All Diagnostics Scan Tests
16:19:31: Start scan readback test on device Trap Offset (V) -- -132 to 132
16:19:36: Scan readback test ended16:19:38: Result: PASSED
16:19:38: Start scan readback test on device Tube gate(V) -- -200 to 198.01
16:19:43: Scan readback test ended
16:19:45: Result: PASSED
16:19:45: Start scan readback test on device Multiplier(V) -- 0 to -2200
16:19:58: Scan readback test ended
16:20:00: Result: PASSED
Dynamic ResultsDynamic ResultsAPI Source Test
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Starting All Diagnostics Scan Tests
16:20:00: Start scan readback test on deviceAuxiliary gas flow(arb) -- 0 to 60
16:21:35: Scan readback test ended16:21:37: Result: PASSED
16:21:37: Start scan readback test on device Sheath gas flow(arb) -- 20 to 100
16:23:20: Scan readback test ended
16:23:22: Result: PASSED16:23:22: Start scan readback test on device Capillary Voltage(V) -- -132 to 132
16:23:27: Scan readback test ended
16:23:28: Result: PASSED
16:23:28: Final result: PASSED
Power SuppliesPower SuppliesStatic Diagnostic
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API and TemperatureAPI and TemperatureStatic Diagnostic
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LensesLensesStatic Diagnostic
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RFRF--11Static Diagnostic
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RFRF--22Static Diagnostic
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CalibrationCalibrationDiagnostic Tool
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Toggles/DetectorToggles/DetectorDiagnostic Tool
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Instrument SettingsInstrument SettingsDiagnostic Tool
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GraphsGraphsPlotting Conversion Dynode Voltage
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GraphsGraphsPlot Tube Lens Calibration
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TriggersTriggersResearch Tool
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Front Panel LEDsFront Panel LEDsClassic/Deca
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Front Panel LEDsFront Panel LEDsDefinition of Classic/Deca
Power: Indication of the digital power Should be green unless the power to the LCQ is off or there has been a failure.
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Vacuum: Indicates that the vacuum is OK. (Convectron gauge, ion gauge, and external switch are all in the correct state.)
Should be green. If any one of the inter-locks is not logically correct, the LED will be off.
Communication: Indicates communication between the on-board AT CPU and the NTcomputer.
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.
System: Indicates the status of the LCQ. Will be green if the LCQ is in the On mode. High voltage is applied.
Will be yellow if the LCQ is in the standby mode. High voltages are off.
Will be off if the LCQ is in the Off mode. Most of the power supplies are off.
Scan: Indicates that the LCQ is in the On mode and Scanning. Will be blue and flashing when the LCQ is collecting data.
Will be off if the LCQ is either in the On or Standby mode. Also will be off if the LCQ isoff.
Front Panel LEDsFront Panel LEDsLCQ Duo
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LCQ Duo Front Panel LEDsLCQ Duo Front Panel LEDsDefinition
Power: Indication of the digital power
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Should be green unless the power to the LCQ is off or there has been a failure.
Will flash yellow indicating a Warning condition for the on-board CPU temperature .
Will be solid yellow indicating a Fatal condition. The MS will be held in a Reset mode until
the temperature problem has been resolved.
Vacuum: Indicates that the vacuum is OK. (Convectron gauge, ion gauge, and external switch are all in the correct state.)
Should be green. If any one of the inter-locks is not logically correct, the LED will be off.
Communication: Indicates communication between the LCQ ATCPU 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.
LCQ Duo Front Panel LEDsLCQ Duo Front Panel LEDsDefinition
System: Indicates the status of the LCQ.
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System: Indicates the status of the LCQ.
Will be green if the LCQ is in the On mode. High voltage is applied.
Will be yellow if the LCQ is in the standby mode. High voltages are off.
Will be off if the LCQ is in the Off mode. Most of the power supplies are off.
Scan: Indicates that the LCQ is in the On mode and Scanning.
Will be blue and flashing when the LCQ is collecting data.
Will be off if the LCQ is either in the On or Standby mode. Also will be offif the LCQ is off.
Syringe Pump: Indicates the status of the syringe pump.
Will be green if the syringe pump on.
Will be yellow when the pump has reached it end of travel.