lcq deca_duo hardware troubleshooting_8601

7/29/2019 LCQ Deca_Duo Hardware Troubleshooting_8601

1/111


2/111

LCQ Deca/Duo HardwareTroubleshooting

Ed Gonzalez

Product Support


3/111

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


4/111

Mass SpectrometerMass SpectrometerSimplified Schematic

MakeIons

TransferIons

FilterIons

DetectIons

SampleIn

DataOut

Ion Optics SystemIon Optics System


5/111

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


6/111

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


7/111

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


8/111

ESI Ionization ProcessESI Ionization ProcessSimplified Schematic


9/111

ESI Spray Cross SectionESI Spray Cross Section

Gas SheathGas Sheath

Liquid SheathLiquid Sheath

NozzleNozzle

NeedleNeedle

Ion PlumeIon Plume

55kVkV


10/111

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)


11/111

APIAPI--1 / ESI Probe Assembly1 / ESI Probe Assembly(LCQ Classic)


12/111

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


13/111

LCQ Deca Tune Plus WindowLCQ Deca Tune Plus WindowESI Source dialog and Status Panel


14/111

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


15/111

APIAPI--1 / ESI Probe Cross Section1 / ESI Probe Cross Section


16/111

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


17/111

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


18/111

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


19/111

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


20/111

Xcalibur Instrument SetupXcalibur Instrument SetupDivert Valve Dialog


21/111

APIAPI--2 / ESI Probe Assembly2 / ESI Probe Assembly(LCQ Deca / LCQ Duo)


22/111

API-2 / ESI Probe Positions

4 3 2 14 3 2 1

ProbeProbePositionsPositions


23/111

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


24/111

APIAPI--2 / ESI Probe2 / ESI Probe

Exploded Pictorial

C l iC l Mi T P t


25/111

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


26/111

LCQ Deca Tune Plus WindowLCQ Deca Tune Plus Window(ESI Source dialog and Status Panel)


27/111

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


28/111

API 2 / ESI Probe Assembly/ S obe sse b yCross Section


29/111

APIAPI--2 / Off Axis ESI Probe2 / Off Axis ESI Probe

(LCQ Deca / LCQ Duo / LCQ Classic)


30/111

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


31/111

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


32/111

APCI Ionization ProcessAPCI Ionization Process


33/111

LCQ Classic APCI ProbeLCQ Classic APCI Probe

b


34/111

LCQ Deca / LCQ Duo APCI ProbeLCQ Deca / LCQ Duo APCI Probe

Typical APCI TuneParametersTypical APCI TuneParameters


35/111

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


36/111

APCI Source dialog and Status Panel

T bl h ti th APCI P bT bl h ti th APCI P b


37/111

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


38/111

APIAPI--1 / API1 / API--2 APCI Probe2 APCI Probe

Cross Section

I T f / D l ti PI T f / D l ti P


39/111

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


40/111

Peek Holder

Tube lens

skimmerskimmer1 Torr1 Torr

1010--33 TorrTorr

LCQ API Stack AssemblyLCQ API Stack AssemblyCross Section


41/111

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


42/111

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


43/111

CQ eca u e us doQVacuum dialog and Status Panel

Troubleshooting the API StackTroubleshooting the API Stack


44/111

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


45/111

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


46/111

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


47/111

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


48/111

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


49/111

Particle Noise Spectrum of Cal mix


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


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


50/111

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


51/111

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


52/111

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


53/111

Cal Mix Tune ParametersCal Mix Tune ParametersLCQ I O i


54/111

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


55/111

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


56/111

QQ ppTypical Operating Pressures/Comparison to LCQ Classic


3.5x10

-3

torr He220 L/sec100 L/sec30 m3/hr

LCQLCQ DecaDeca OpticsOptics


57/111

QQ ppTypical Operating Pressures/Comparison to LCQ Classic


3.5x10-3 torr He

220 L/sec100 L/sec60 m3/hr

Potential Energy DiagramPotential Energy DiagramLCQ and LCQ Duo


58/111

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


59/111

4000

-15000

Potential 20

50

0

-5-7 -10

0

-20

-50

RF Tune Diagnostic DialogRF Tune Diagnostic DialogLCQ Deca


60/111

Tune Multipole RFTune Multipole RFLCQ Deca


61/111

Multipole RF Tunein Calibration Process


62/111

in Calibration Process

Multipole RF Tuneverification performedprior to calibration.

LCQ Deca Ion OpticsLCQ Deca Ion OpticsSpecifics Features


63/111

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


64/111

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


65/111

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


66/111

Pulsed lens

+DC-DC

No Split

Split DC on Scan out

LCQ

DECA

Overview of Ion SeparationOverview of Ion SeparationQ d l I T


67/111

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


68/111

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


69/111

Filter Ions

Quadrupole Ion TrapQuadrupole Ion TrapOperational Parameters


70/111

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


71/111

Troubleshooting the Ion Trap


72/111

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


73/111

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


74/111

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


75/111

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


76/111

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


77/111

Electron MultiplierElectron MultiplierDetection System

2-Particles

enter the Two particles formed when an ion


78/111

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


79/111

Detection System ParametersDetection System Parameters


80/111

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


81/111

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


82/111

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


83/111

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.



84/111

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.



85/111

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.



86/111

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.



87/111

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


88/111

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


89/111

Static Results from Status TestStatic Results from Status Test


90/111

+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


91/111

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: 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



16:18:57: Start scan readback test on device Multipole RF DAC(V) -- 0 to 1000



Dynamic TestDynamic TestGraphical Output


92/111

Dynamic ResultsDynamic ResultsLenses Test


93/111


16:19:04: Start scan readback test on device Multipole 1 offset (V) -- -132 to 132


16:19:11: Start scan readback test on device Multipole 2 offset (V) -- -132 to 132



16:19:17: Start scan readback test on device Multipole lens (V) -- -132 to 132



16:19:24: Start scan readback test on device Multipole det. RF amp. (Vp-p) -- 0 to 1000


Dynamic ResultsDynamic ResultsIon Detection Test


94/111


16:19:31: Start scan readback test on device Trap Offset (V) -- -132 to 132


16:19:38: Start scan readback test on device Tube gate(V) -- -200 to 198.01



16:19:45: Start scan readback test on device Multiplier(V) -- 0 to -2200



Dynamic ResultsDynamic ResultsAPI Source Test


95/111


16:20:00: Start scan readback test on deviceAuxiliary gas flow(arb) -- 0 to 60


16:21:37: Start scan readback test on device Sheath gas flow(arb) -- 20 to 100


16:23:22: Result: PASSED16:23:22: Start scan readback test on device Capillary Voltage(V) -- -132 to 132



16:23:28: Final result: PASSED

Power SuppliesPower SuppliesStatic Diagnostic


96/111

API and TemperatureAPI and TemperatureStatic Diagnostic


97/111

LensesLensesStatic Diagnostic


98/111

RFRF--11Static Diagnostic


99/111

RFRF--22Static Diagnostic


100/111

CalibrationCalibrationDiagnostic Tool


101/111

Toggles/DetectorToggles/DetectorDiagnostic Tool


102/111

Instrument SettingsInstrument SettingsDiagnostic Tool


103/111

GraphsGraphsPlotting Conversion Dynode Voltage


104/111

GraphsGraphsPlot Tube Lens Calibration


105/111

TriggersTriggersResearch Tool


106/111

Front Panel LEDsFront Panel LEDsClassic/Deca


107/111

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.


108/111

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


109/111

LCQ Duo Front Panel LEDsLCQ Duo Front Panel LEDsDefinition

Power: Indication of the digital power


110/111

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.


111/111

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.

lcq deca_duo hardware troubleshooting_8601

Documents