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Table of Contents
About This Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
TurboIonSpray Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Ion Source Temperature Range. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Liquid Chromatography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
TurboIonSpray Nebulizer (Gas 1) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Heater Gas (Gas 2) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Ion Source Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Sprayer Probe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
Transfer Line and Grounded Union/Splitter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
Heater Probe. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
Exhaust Pump. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
Optimizing the TurboIonSpray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
TurboIonSpray Probe Position. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
TurboIonSpray Voltage (IS) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Nebulizer Gas (GS1) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Curtain Gas (CUR). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Heater Gas (GS2) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Turbo Temperature (TEM) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Declustering Potential (DP) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Solvent Composition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Source Exhaust Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Operating Tips . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Changing the PEEK Tubing Transfer Line . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Changing the Stainless Steel Sprayer Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
Changing the Grounded Union/Splitter Fitting . . . . . . . . . . . . . . . . . . . . . . . . 21
Appendix A: Consumable Parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Appendix B: Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
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Table of Contents Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
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Q Trap LC/MS/MS TurboIonSpray Ion Source Manual About This Manual
Conventions
Within this manual, the following conventions are used:
WARNING! Indicates an operation that may cause personal injury if precautions are
not followed.
WARNING! This symbol indicates a warning of electrical shock hazard. You should
read the warning before attempting any procedure described in this manual. Failure
to do so can result in serious injury.
WARNING! Indicates an operation that may cause injury if precautions are not
followed. Handle after allowing the unit time to cool, or use appropriate insulating
gloves to avoid burns.
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About This Manual Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
2
Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Introduction
Introduction
The TurboIonSpray is an atmospheric pressure ion source in which pre-formed ions in
solution are emitted into the gas phase with or without the application of heat. In this way,
quasi-molecular ions can be generated from very labile and high molecular weight
compounds with no thermal degradation.
TurboIonSpray is the technique by which a liquid sample is pumped by a liquid
chromatograph (LC) pump or syringe drive through a sprayer probe, which is maintained
at a high voltage, and is nebulized into the ion source creating a mist of highly charged
droplets. Once inside the ion source, the droplets evaporate causing the ions to enter the
gas phase by a low energy process called ion evaporation.
The use of heated gas extends the rugged and versatile technique of the TurboIonSpray to
accept higher flow rates with improved sensitivities. The TurboIonSpray will accept flows
from 5 to 1000 L/min of solvent compositions from 100% aqueous to 100% organic,
such as acetonitrile, without splitting. This allows the use of 300 m, 1 mm, 2 mm, and
4.6 mm analytical columns with or without splitting.
A heater probe directs a jet of heated dry gas (up to a maximum of 500 C) at the mist
produced by the sprayer. The gas is sprayed across the orifice at an angle of approximately
45 with respect to the curtain plate. The liquid spray emerging from the TurboIonSpray is
directed at an angle of about 45 from the opposite direction (or 135 from the curtain
plate). The TurboIonSpray effluent and the heated dry gas intersect at an angle of
approximately 90 near the orifice. This interaction helps focus the TurboIonSpray stream
and increases the rate of droplet evaporation resulting in an increased ion signal.
TurboIonSpray setup
TurboIonSpray is ideally suited for LC/MS/MS quantitative analyses. The sensitivity
increases that are achieved with this technique are both flow rate and analyte dependent.
In the conventional IonSpray, source sensitivity decreases with increased flow rate, while
the heated TurboIonSpray process increases ionization efficiency, especially at the higher
flow rates; this results in improved sensitivity. Sensitivity is compound dependent and
compounds of extremely high polarity and low surface activity usually show the greatest
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Introduction Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
sensitivity increases. The TurboIonSpray technique is mild enough to be used with labile
compounds such as peptides, proteins, and thermally labile pharmaceuticals.
Note: The difference between conventional IonSpray and TurboIonSpray is that in the
TurboIonSpray, the ionization of the sample is achieved with additional heater gas
delivered to aid in the desolvation of the spray. Typically, the TurboIonSpray is used at
higher flow rates (greater than or equal to 40 L/min).
Features
The following list outlines the features of the TurboIonSpray ion source:
Able to function as a conventional IonSpray source when the heater gas is turned off.
Able to function with flow rates from 1 L/min to 1000 L/min.
Able to vaporize 100% aqueous to 100% organic solvents.
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Q Trap LC/MS/MS TurboIonSpray Ion Source Manual TurboIonSpray Components
TurboIonSpray Components
Specifications
Ion Source Temperature Range
Probe temperature from 0500 C
Liquid Chromatography
Interfaces to any liquid chromatography system
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TurboIonSpray Components Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
Sprayer Probe
The TurboIonSpray source contains a fixed angle adjustable sprayer probe. The sprayer
probe is adjustable in two directions: toward the orifice from a scale of 0 to 12 (adjusted
by the horizontal adjusting ring mounted on the TurboIonSpray probe), and up and down
toward the orifice from 0 to 12 by the lateral adjustment control on the top of the ion
source.
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Q Trap LC/MS/MS TurboIonSpray Ion Source Manual TurboIonSpray Components
PEEK Tubing
Grounded Union/Splitter
WARNING! The use of the PEEK tubing transfer line connected to the grounded
fitting is mandatory because it prevents any exposed peripherals connected to the
source from floating at high voltage.
WARNING! PEEK tubing (or fused silica) with PEEK fittings must be used as the
transfer line. Metal tubing or fittings must not be used. The use of metal may result
in the exposure of the operator to high voltage.
Refer to the procedure for changing the grounded fitting from a union connection to a
splitter described later in this document.
Heater Probe
The heater probe temperature is set in the applications computer software by modifying
the TEM parameter. There is a direct correlation between the TEM parameter value and
the actual heater temperature (for example, TEM 350 is equal to 350 C at the heater). The
heater gas (Gas 2) is also set in the applications computer software. The connections for
the heater and the gas are made automatically once the source is locked to the interface.
The heater probe temperature is maintained by the temperature control board (TCB)
mounted behind the ion source panel (below the ion source housing). The TCB adjusts the
flow of power to the heater element as a function of the difference between the actual
heater temperature and the temperature setting in the applications computer. The probe
temperature is monitored by a thermocouple connected directly to the heater element that
maintains the temperature within 5 degrees of the applications computer setting. The
operating range for the probe is approximately 100500 C.
Note: The temperature is controlled by monitoring the output of a thermocouple
connected to the heater surrounding the metal tube. At the temperature control board the
thermocouple output is compared with the temperature setting, the difference determines
the power flow to the heater.
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TurboIonSpray Components Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
Exhaust Pump
The TurboIonSpray source requires that the source exhaust system is properly connected
and functioning. See "Source Exhaust Pump" on page 15. A filtered nitrogen or air gas
supply (free from pump oil) is delivered to the source exhaust pump at 60 psi pressure at a
flow of at least 4 L per minute. The source exhaust pump is used to vent solvent vapors
that develop in the ion source plenum.
It is recommended that these vapors be passed through a trap vented to a fume hood or
outside port.
WARNING! Failure to provide proper ventilation of the ion source can result in
hazardous vapors being released into the laboratory environment.
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Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Installation
Installation
The TurboIonSpray source connects to the vacuum interface housing. Two latches
mounted on the source housing secure the TurboIonSpray against the vacuum interface.
WARNING! Some surfaces on the TurboIonSpray source will become hot during
operation. Use caution when installing or removing the source.
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Installation Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
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Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Optimizing the TurboIonSpray
CAUTION! When optimizing the sprayer position, make certain not to spray directly
down the orifice. Spraying down the orifice may contaminate the vacuum interface
and vacuum chamber ion optics and could impact instrument performance.
CAUTION! To avoid possible damage to the instrument, always view the sprayer tip
through the side port when adjusting its position.
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Optimizing the TurboIonSpray Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
repositioned further away from the orifice to prevent solvent penetration through the
orifice into the mass spectrometer.
Orifice
40 L/min
200 L/min
1 mL/min
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Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Optimizing the TurboIonSpray
1000 475 8 90 50 6 10
(450500) (48) (4090) (2055)
V = vertical position
H = horizontal position
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Optimizing the TurboIonSpray Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
CAUTION! Do not operate the TurboIonSpray with probe temperatures greater than
500 C.
Solvent Composition
Commonly used solvents and modifiers are acetonitrile, methanol, propanol, water, acetic
acid, formic acid, ammonium formate, and ammonium acetate. The modifiers such as
triethyl amine (TEA), sodium phosphate, trifluoroacetic acid (TFA), and sodium dodecyl
sulfate are not commonly used because they complicate the spectrum with their ion
mixtures and cluster combinations. They may also suppress the strength of the target
compound ion signal. The standard concentration of ammonium formate or ammonium
acetate is from 2 to 10 millimole per liter for positive ions and 2 to 50 millimole per liter
for negative ions. The concentration of the organic acids is 0.01% to 0.5% by volume.
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Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Optimizing the TurboIonSpray
The source exhaust system is required for TurboIonSpray operation. The exhaust pump
draws the solvent vapors from the enclosed source chamber and delivers them to a trap at
the rear of the instrument chassis where they can be collected. The source exhaust system
is interlocked to the system electronics, such that if the source exhaust pump is not
operating to specification, the instrument electronics are disabled.
The exhaust system lowers the pressure in the source slightly below atmospheric pressure.
If the pressure in the source rises beyond a preset trip point, the instrument high voltage
power supply is disabled.
WARNING! The source exhaust pump must be vented to either an external fume
hood, or external exhaust source.
The pressure switch for the exhaust line must be tested before each use by shutting off the
source exhaust gas supply. If the hose is connected to a forced ventilation system,
disconnect the hose from the drain bottle. Fault messages will be displayed on the monitor
indicating the source exhaust gas is off, which verifies that the pressure switch is working.
If the fault messages are not displayed the pressure switch is defective and the APCI
source must not be used. A service call is mandatory. If the above procedure is not
followed, the ion source pressure sensor may inadvertently allow the system to operate
when the ion source is not being properly exhausted. When the source is not properly
exhausted, vapor can escape through the heated nebulizer probe and condense within the
probe's electrical wiring. This could cause a short circuit and the possibility of a fire if
flammable solvents are used.
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Optimizing the TurboIonSpray Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
Operating Tips
1. When running the TurboIonSpray, with or without the heater probe on, run the curtain
gas at as high a flow rate as possible without decreasing the signal. This will help to:
a) Prevent penetration of the curtain gas, which can produce a noisy signal.
b) Prevent contamination of the orifice.
c) Increase the overall signal to noise ratio.
2. The liquid spray from the TurboIonSpray should be directed away from the orifice in
order to:
a) Prevent contamination of the orifice.
b) Prevent piercing of the curtain gas, which can create an unstable signal.
c) Prevent electrical shorting due to the presence of the liquid.
3. The higher the liquid flow, or the higher the aqueous composition of the solvent, the
higher the temperature and heater gas (Gas 2) flow required. However, too high a
temperature can cause thermal degradation of the compound, and result in a high
chemical background noise, while too high a heater gas flow can produce a noisy, or
unstable signal.
16
Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Changing the PEEK Tubing Transfer Line
WARNING! The use of the PEEK tubing transfer line connected to the grounded
fitting is mandatory because it prevents any exposed peripherals connected to the
source from floating at high voltage.
PEEK tubing
3. Obtain a new piece of 0.0025" PEEK tubing (it must be at least 30 cm [12"] long) and
place PEEK connection fittings on each end.
WARNING! PEEK tubing (or fused silica) with PEEK fittings must be used as the
transfer line. Metal tubing or fittings must not be used. The use of metal may
expose the operator to high voltage.
4. Connect the PEEK tubing to the probe inlet and the grounded union/splitter fitting.
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Changing the PEEK Tubing Transfer Line Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
18
Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Changing the Stainless Steel Sprayer Tube
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Changing the Stainless Steel Sprayer Tube Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
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Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Changing the Grounded Union/Splitter Fitting
WARNING! The use of the PEEK tubing transfer line connected to the grounded
fitting is mandatory because it prevents any exposed peripherals connected to the
source from floating at high voltage.
WARNING! PEEK tubing (or fused silica) with PEEK fittings must be used as the
transfer line. Metal tubing or fittings must not be used. The use of metal may result
in the exposure of the operator to high voltage.
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Changing the Grounded Union/Splitter Fitting Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
22
Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Appendix A: Consumable Parts
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Appendix A: Consumable Parts Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
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Q Trap LC/MS/MS TurboIonSpray Ion Source Manual Appendix B: Troubleshooting
Appendix B: Troubleshooting
Introduction
This troubleshooting section is suitable for use by operators who have access to an ohm
meter and are familiar with its use. Diagnosis does not require removal of the instrument
covers and does not expose the operator to hazardous voltages.
The heater control circuits are protected by a fuse that can be reset. This device may be
tripped by excessive heater current, or by failure to approach the desired operating
temperature within about 5 minutes. When tripped, the device will remove power from the
heater. To reset the protective device, power off the system for about one minute or
remove the ionizer from the system for about one minute.
Diagnosis of the nature of the fault is done by means of ohm meter readings taken across
the pins of the 24-pin connector on the ionizer shown in the following figure.
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Appendix B: Troubleshooting Q Trap LC/MS/MS TurboIonSpray Ion Source Manual
26