Professional Documents
Culture Documents
Ion Source
Operator's
Manual
Part Number: 1017901 A
April 2005
LC/MS/MS System
This document is provided to customers who have purchased MDS Sciex equipment to use
in the operation of such MDS Sciex equipment. This document is copyright protected and
any reproduction of this document or any part of this document is strictly prohibited, except
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Portions of this document may make reference to other manufacturers’ products, which may
contain parts that are patented and may contain parts whose names are registered as
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those manufacturers’ products as supplied by Applied Biosystems/MDS SCIEX for
incorporation into its equipment and does not imply any right and/or license to use or permit
others to use such product names as trademarks.
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ISO
Applied Biosystems/MDS SCIEX makes no warranties or representations as to the fitness of
this equipment for any particular purpose and assumes no responsibility or contingent
9001
REGISTERED
liability, including indirect or consequential damages, for any use to which the purchaser COMPANY
may put the equipment described herein, or for any adverse circumstances arising therefrom.
Applied Biosystems/MDS SCIEX is a joint venture between Applera Corporation and MDS
Sciex, the instrument technology division of MDS Inc.
One or more of the following trademarks or registered trademarks may be found in this document:
API 150EX™, API 2000™, API 3000™, API 4000™, API 5000™, BIOANALYST™, BIOSPECTROMETRY™,
BIOTOOLBOX™, CURTAIN GAS™, EXPLORER™, INTERROGATOR™, IONSPRAY™, MASSCHROM™, NANOLINK™,
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ANALYST®, DATA EXPLORER®, DELAYED EXTRACTION®, MICROIONSPRAY®, QSTAR®, SYMBIOT®, and
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3200 QTRAP®, 4000 Q TRAP®, MICROIONSPRAY®, NANOSPRAY®, PHOTOSPRAY®, and QTRAP® are registered
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All product and company names mentioned herein may be the trademark of their respective owners.
iii
TurboIonSpray Software Optimization . . . . . . . . . . . . . . . . . . . . . . . .30
APCI Optimization. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
APCI Hardware Optimization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .31
APCI Software Optimization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .33
Exchanging Probes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Stopping the Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34
Removing the Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .34
Removing the Probe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .35
Installing the Probe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .35
Chapter 4: Performance Test Procedures . . . . . . . . . . . . . . .39
System Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
Instrument Setup. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .39
Injector Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .40
Materials Required . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
Mobile Phase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .40
Preparing the Test Solution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .40
Equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .41
Gas Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .41
Instrument Performance Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
Testing the Source in TurboIonSpray Mode . . . . . . . . . . . . . . . . . . . .42
Testing the Source in APCI Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . .44
Chapter 5: Source Maintenance . . . . . . . . . . . . . . . . . . . . . . .47
Preparation for Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
Removing the Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .47
Source Component Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
Cleaning the Electrode. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .48
Setting the Electrode Extension . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .50
Source Component Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . 51
Replacing the Corona Discharge Needle. . . . . . . . . . . . . . . . . . . . . . .51
Appendix A: Source Parameters . . . . . . . . . . . . . . . . . . . . . . .53
Descriptions and Typical Values for Source-Dependent Parameters .53
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Turbo V Ion Source Operator’s Manual
Appendix B: Troubleshooting. . . . . . . . . . . . . . . . . . . . . . . . . 57
Appendix C: Parts List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
Appendix D: Principles of Operation. . . . . . . . . . . . . . . . . . . 61
Ion Evaporation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
Ionization Modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 62
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
v
vi
Foreword
The foreword contains information about the manual and the hardware
regulatory compliance certification.
vii
Foreword
Conventions
Within the scope of this manual, the following typographical
conventions are used:
viii
Turbo V Ion Source Operator’s Manual
Related Documentation
The customer documentation for the LC/MS/MS system includes the
site planning guide, the operator’s manual, the qualified maintenance
person’s manual, the safety manual, the peripheral devices manual, the
laboratory director’s guide, and the following optional documents:
SQ/IQ/OQ (site, instrument, and operator’s qualifications), and the IPV
(instrument performance validation). Online Help is available in the
Analyst® software and can be activated by pressing F1.
To download the latest versions of these documents, visit
http://docs.appliedbiosystems.com/search.taf.
Regulatory Compliance
Certification
This source, and its components, meet or exceed the requirements of the
following regulatory agencies. Applicable labels for these qualifications
have been affixed to the instrument.
ix
Foreword
International Compliance
See the Declaration of Conformance included with the instrument.
Contact Us
Your opinion is important to us. To provide feedback about this manual,
send an e-mail message to: techpubs@sciex.com
x
1
Introducing the Source
The Turbo V™ source gives you the option of using either the
TurboIonSpray® or APCI (atmospheric pressure chemical ionization)
probe in the same source housing.
This topic contains the following:
• “Why Use the Source” on page 11
• “Parts of the Source” on page 12
11
Introducing the Source
Rapid Sample Introduction: The source can be used for rapid sample
introduction by flow injection with or without an LC column.
Source Housing
The source housing mounts onto the vacuum interface and is held in
position by two guide pins that are rotated with latch handles. The
source probe and the source housing can be quickly and easily removed
without tools. If a probe is not properly installed in the source housing,
or the source housing itself is not properly installed on the instrument,
the high-voltage power will not be enabled. For more information, see
“Source Safety Interlocks” on page 16.
Gas and high-voltage electrical connections enter through the front
plate of the interface and connect internally through the source housing.
When the source is installed onto the mass spectrometer, most of the
electrical and gas connections are made. The sample delivery lines are
connected manually to the splitter and probe. The probe position can be
adjusted vertically and horizontally for optimal performance.
An exhaust system removes source gases through a source exhaust port
in the bottom of the source housing. The source exhaust port connects
through a drain chamber and a source exhaust pump to a drain vessel,
and from there to a customer-supplied exhaust ventilation system. For
more information on the source exhaust system see the illustration
“Source exhaust system” on page 16.
Tempered glass windows on the side and at the end of the source
housing allow you to see the probes and nebulized sample stream.
The source housing includes the following parts:
12
Turbo V Ion Source Operator’s Manual
Probe Tower
Horizontal
Probe Adjustment
Turbo Heater
Splitter
Window Port
Guide Pin
Latch Handle
13
Introducing the Source
Electrode Tip
14
Turbo V Ion Source Operator’s Manual
(Gas 1) flows around the electrode tip to disperse the sample as a mist
of fine particles. It moves through the ceramic vaporization heater into
the reaction region of the source past the corona discharge needle where
the sample molecules are ionized as they pass through the ion source
housing. For more information see, “Principles of Operation” on page
61.
The probe consists of the following parts:
• Retaining ring to fasten the probe to the probe tower on the source
housing.
• Electrode adjustment nut (black collar) to set the length of electrode
tip extension. This is a critical adjustment for the optimizing of a
compound.
• Electrode tip through which samples are spayed into the sample
inlet area of the source. This tip extension is adjustable by turning
the electrode adjustment nut.
Electrode Tip
15
Introducing the Source
Ion Source
B A B A
Pressure Switch
Exhaust Supply
BACKING PUMP
GAS 1 / GAS 2
EXHAUST SUPPLY
MIN 55 PSIG EXHAUST WASTE OUT
Venturi Pump
MAX105 PSIG MAX 60 PSIG
A filtered nitrogen or zero air gas supply (oil free) is delivered to the
source exhaust pump at pressures indicated on the gas panel at the back
of the instrument. The previous figure shows an example of the exhaust
supply connection points for an instrument.
16
Turbo V Ion Source Operator’s Manual
Temperature Controller
The temperature controller monitors and maintains the temperature of
the ceramic heaters in both the APCI and TurboIonSpray probes and
supplies power to the two turbo heaters. A thermal sensor senses the
actual heater temperature and transmits it to the temperature controller
board. The TCB (temperature control board) adjusts the flow of power
to the heater element as a function of the difference between the actual
heater temperature and the temperature setting at the computer.
The temperature controller system consists of a heating element in the
source housing, the TCB, and a transformer that provides the power for
both the heater and the TCB. A thermocouple attached to the heating
element returns the actual heater temperature signal to the TCB.
Sample Introduction
This topic describes how the sample is introduced to the source. It also
describes the sample inlet operational requirements.
Method
The liquid sample stream is pumped to the source by an LC pump or by
a syringe pump. If introduced by an LC pump, the sample may be
injected directly into the mobile phase using flow injection analysis
(FIA) or through a separation column (LC/MS) using a loop injector or
autosampler. If introduced by a syringe pump, the sample is directly
injected into the source.
Sample Inlet Operational Requirements
The sample inlet is specifically designed to transfer the liquid sample to
the source inlet without sample loss and with minimal dead volume.
It is important to apply appropriate analytical procedures and practices
to minimize external dead volumes. Proper procedures help ensure
chromatographic integrity and analytical reproducibility. It is also
important that samples are sufficiently prefiltered so that the capillary
tubing in the inlets is not blocked by particles, precipitated samples, or
salts.
17
Introducing the Source
18
2
Source Installation
This topic describes the procedure for installing the Turbo V™ source.
The source housing and probes are removable for maintenance and
service.
Probe Selection
The Turbo V source accepts either the TurboIonSpray® or the APCI
source probe.The system recognizes which probe is installed and
enables the corresponding specific user controls.
The Analyst software provides the capability to select either of the two
probes, on a per experiment basis. All of the data acquired using the
source is identified by the probe used to acquire the data.
APCI Probe
TurboIonSpray Probe
APCI and TurboIonSpray probes
19
Source Installation
polar compounds. The sensitivity gains that are achieved with this
technique are both flow rate and analyte dependent. For more
information on using the probe, see “Descriptions and Typical Values
for Source-Dependent Parameters” on page 53.
The following list outlines the features of the TurboIonSpray probe:
• Functions as conventional IonSpray source when the heater is
turned off.
• Functions with flow rates from 5 to 3000 µL/min.
• Vaporizes 100% aqueous to 100% organic solvents.
Features of the APCI probe
The APCI probe is ideally suited for creating spectra for MS/MS
experiments compounds that do not readily form ions in solution. These
are usually non-polar compounds. It is also good for rapid sample
introduction by flow injection with or without an LC column. For more
information on using the probe, see “Descriptions and Typical Values
for Source-Dependent Parameters” on page 53.
The following list outlines the features of the APCI probe:
• Functions with flow rates of 50 to 3000 µL/min. and can handle the
entire flow from a wide bore column without splitting.
• Vaporizes a 100% aqueous mobile phase.
• Handles volatile mobile phase buffers.
• Vaporizes volatile and labile compounds with minimal thermal
decomposition.
20
Turbo V Ion Source Operator’s Manual
3. Ensure that the sample inlet line is the appropriate length to connect
to the source with enough slack to move the fully connected source
housing from the bench to the vacuum interface of the instrument.
4. Check the probe to ensure that the electrode tip is adjusted to
specification. For optimum stability and performance, the electrode
should extend between 0.5 and 1.0 mm from the end of the probe
and is compound dependent. This distance affects the shape of the
sprayed cone which affects instrument sensitivity. For more
information on adjusting the electrode extension, see “Electrode
extension adjustment” on page 51.
21
Source Installation
22
Turbo V Ion Source Operator’s Manual
Sample Inlet
Line
Probe
Splitter
23
Source Installation
Interface
Surface
Guide
Pin
Guide
Pin
Source latches
24
3
Source Operation
This topic describes procedures and concepts for operating the
Turbo V™ source.
25
Source Operation
1. Install the probe and source housing on the instrument. For more
information, see “To install the probe and source housing” on page
22.
2. Ensure that the Analyst® software is running.
3. If the hose is connected to a forced ventilation system, disconnect
the hose from the drain bottle.
4. Turn off, or remove, the gas supply line connected to the exhaust
supply fitting located on the instrument bulkhead. For more
information, see the following figure, Source exhaust system
Fault messages should appear on the monitor indicating the source
exhaust gas is off. This verifies that the pressure switch is working.
If the fault messages do not appear, the pressure switch is defective
and the source must not be used. Call your Customer Service
Representative for service.
26
Turbo V Ion Source Operator’s Manual
Ion Source
B A B A
Pressure Switch
Exhaust Supply
BACKING PUMP
GAS 1 / GAS 2
EXHAUST SUPPLY
MIN 55 PSIG EXHAUST WASTE OUT
Venturi Pump
MAX105 PSIG MAX 60 PSIG
5. Turn on, or reconnect, the gas supply line connected to the exhaust
supply fitting located on the instrument rear bulkhead, and then
reconnect the hose to the drain bottle.
The Analyst software instrument status panel should indicate that
the source exhaust gas is on.
6. To acquire data refer to the operator’s manual for your instrument.
To optimize the source see one of the following:
For more information on optimizing the source for
TurboIonSpray mode, see “TurboIonSpray Optimization” on
page 28.
For more information on optimizing the source for APCI mode,
see “APCI Optimization” on page 30.
27
Source Operation
TurboIonSpray Optimization
This topic contains parameter details and procedures for optimizing the
TurboIonSpray mode performance. Overall, optimization consists of:
• Hardware optimization parameters which consist of probe position
and electrode tip adjustments.
• Software optimization parameters which are configured to further
optimize the source performance after the probe adjustments are
completed.
Note: Before starting the liquid sample flow, allow the source to warm
up for 30 minutes or until the housing is warm to the touch. Warming
the probe before use eliminates the possibility that solvent vapors may
condense inside a cold source housing. When using the APCI probe, the
ceramic heater must be warmed slowly to avoid thermal shock to the
heating element.
Operational
LC Flow rate
range
5 to 50 5 to
Parameter 200 µL/min 1000 µL/min
µL/min 3000 µL/min
Probe vertical- 5 to 10 mm 0 to 5mm 0 to 5mm 0 to 13 mm
axis position
Probe 3 to 8 mm 5 to 8 mm 5 to 8 mm 0 to 10 mm
horizontal-axis
position
28
Turbo V Ion Source Operator’s Manual
29
Source Operation
APCI Optimization
This topic contains parameter details and procedures for optimizing the
APCI mode performance. Overall optimization consists of:
• Hardware optimization parameters which consist of probe position
and electrode tip adjustments.
• Software optimization parameters which are configured to further
optimize the source performance after the probe adjustments are
completed.
Note: Before starting the liquid sample flow, allow the source to warm
up for 30 minutes or until the housing is warm to the touch. Warming
30
Turbo V Ion Source Operator’s Manual
the probe before use eliminates the possibility that solvent vapors may
condense inside a cold source housing. When using the APCI probe, the
ceramic heater must be warmed slowly to avoid thermal shock to the
heating element.
31
Source Operation
Look through the window of the source housing to view the position of
the probe.
Tip: The curtain plate orifice should remain clear of solvent or solvent
drops at all times.
1. Set the horizontal axis to 5 and the vertical axis to 5.
2. Infuse or inject the sample.
3. Using the Analyst software, in Q1 or MRM mode, monitor the ion
intensity.
4. Using small increments, move the probe vertical position away
from or towards the curtain plate orifice until optimal sensitivity is
achieved. The APCI probe optimizes toward the orifice plate.
Note: The probe’s vertical position depends on flow rate. At low
flow rates, the probe may need to be closer to the orifice, while at
higher flow rates, the probe should be farther away.
5. Using small increments, move the probe horizontal position
towards, and then past, the curtain plate orifice while monitoring
the signal intensity.
6. Adjust the black electrode adjustment nut on the probe to move the
electrode tube situated inside of the probe. For optimum stability
and performance, the electrode should extend between 0.5 and
1.0 mm from the end of the probe. This adjustment is compound
and flow rate dependent. For more information, see “Electrode
extension adjustment” on page 51.
Repeat this optimization procedure if the analyte, flow rate, or solvent
composition changes. However, the optimal settings will remain
constant for any given combination of the preceding. Once the probe is
optimized it needs only minor adjusting or tuning. If you remove the
probe, you should repeat the optimizing procedure after reinstallation.
32
Turbo V Ion Source Operator’s Manual
Exchanging Probes
Follow this procedure when you need to exchange probes
This topic contains the following:
• “Stopping the Source” on page 34
• “Removing the Source” on page 34
• “Removing the Probe” on page 35
• “Installing the Probe” on page 35
33
Source Operation
34
Turbo V Ion Source Operator’s Manual
1. Remove the source from the instrument. For more information, see
“To remove the source” on page 34.
2. Unscrew and remove the sample supply line from the source probe.
3. Unscrew the probe’s bronze retaining ring from the source probe
tower.
4. Gently pull the source probe straight up out of the housing. Do not
allow the tip of the probe to touch anything as you remove it. Place
the probe on a secure, clean area.
35
Source Operation
36
Turbo V Ion Source Operator’s Manual
Sample Inlet
Line
Probe
Splitter
37
Source Operation
38
4
Performance Test
Procedures
This topic describes the performance tests used to demonstrate the
performance level of the Turbo V™ source.
Meeting the test specifications ensures that the source is operating at an
optimal performance level. These tests should be run in any of the
following situations:
• After the source is first installed.
• After performing major maintenance to the source or to the
instrument.
• Whenever the operator is required to reassess the performance of
the source, that is before starting a project or as part of a standard
operating procedure).
System Setup
This topic contains the information that explains how to prepare the
instrument for the source performance tests.
Instrument Setup
Ensure that the host instrument has passed all specifications for Q1 PPG
and Reserpine (Q1 and MS/MS) testing and that it is fully optimized for
sensitivity. For more information, refer to the instrument’s installation
guide.
The initial setup and verification procedures, detector optimization,
verifying peak width with mass calibration and ion spray must be
39
Performance Test Procedures
Injector Setup
The test solution requires a dedicated injector with a 5 µL loop and a
10 µL syringe. Perform a blank injection before starting the test to clean
the loop and avoid potential contamination from previous injections. To
minimize cross contamination, use a different syringe for each sample
Materials Required
You must prepare the following materials to complete the source
performance tests.
Mobile Phase
Required solvent: 70% acetonitrile (HPLC grade) and 30% deionized
distilled water.
The reserpine solution for the TurboIonSpray and APCI tests consists of
10 pg/µL of reserpine dissolved in the mobile phase of 70:30
acetonitrile:water and 2 mM ammonium acetate and 0.1% formic acid.
40
Turbo V Ion Source Operator’s Manual
Equipment
You will need the following equipment to perform the test procedures:
• PE 250/HP LC pump or equivalent with 8125 Rheodyne injector
(5 µL loop).
• PEEK tubing 1/16" o.d. 0.005" i.d.
• Source (with TurboIonSpray and APCI probes)
• Syringe 250–1000 µL
Gas Requirements
Verify the following gas connections to the instrument:
• Curtain Gas supply is UHP nitrogen at 60 psi
• Source exhaust is Zero Air at 55–60 psi
• Gas 1 is Zero Air at 105 psi, or UHP nitrogen (preferred).
• Gas 2 is Zero Air at 105 psi, or UHP nitrogen (preferred).
Note: Using UHP nitrogen for the nebulizer gas provides
improved sensitivity compared to zero air.
41
Performance Test Procedures
42
Turbo V Ion Source Operator’s Manual
Scan Parameters
Parameter Value
Scan Mode MRM
Q1 609.2
Q3 195.1
Scan Time 200 ms
Duration 10 minutes
Note: Do not introduce any solvent flow before verifying that the
source has reached the temperature setting.
To test the TurboIonSpray mode performance
1. In the Analyst software, select the Method file optimized for
reserpine MS/MS.
2. Set the HPLC pump to deliver 0.2 mL/min of the mobile phase.
3. Connect the pump to the source through an injector equipped with a
5 µL loop.
4. Over-fill the 5 µL loop with 30–40 µL of 10 pg/µL reserpine
solution and perform several injections, while optimizing the
nebulizer gas (Gas1), turbo heater gas (Gas2), Curtain Gas, and
needle current for maximum signal intensity and stability.
5. Optimize the electrode extension through the tube, as well as the
vertical and horizontal position of the probe.
6. Once the source is optimized, inject 30–40 µL of 10 pg/µL of
reserpine solution while monitoring m/z 609/195.
7. Perform three consecutive injections and record the average
intensity.
8. Print a copy of the results.
To analyze the TurboIonSpray mode test results
1. Review the printed copy of the results.
2. Verify that the three injections of the 10 pg/µL solution of reserpine
have intensities greater than the required minimum specifications
for your specific instrument. Refer to the Installation Guide for
your instrument for these specifications.
3. If the source does not meet this specification, verify the following:
43
Performance Test Procedures
Parameter Value
Scan Mode MRM
Q1 609.2
Q3 195.1
Scan Time 100 ms
Duration 10 minutes
Note: Do not introduce any solvent flow before verifying that the
source has reached the temperature setting.
44
Turbo V Ion Source Operator’s Manual
45
Performance Test Procedures
46
5
Source Maintenance
This topic describes the procedures for maintaining the Turbo V™
source and replacing consumable items.
47
Source Maintenance
48
Turbo V Ion Source Operator’s Manual
1. Remove the source from the instrument. For more information, see
“To remove the source” on page 47.
2. Unscrew and remove the sample supply line from the source probe.
3. Unscrew the probe’s bronze retaining ring from the source housing.
4. Gently pull the source probe straight up out of the housing. Do not
allow the tip of the probe to touch anything as you remove it. Place
the probe on a secure, clean area.
Peek Union
Probe - expanded view
49
Source Maintenance
Note: Ensure that the electrode is placed as far into the PEEK
union fitting as it will go. A dead sample volume may be created if
there is a gap between the electrode and its seat inside the union
fitting.
11. Align the electrode with the narrow opening in the sprayer tube,
and then slide the PEEK union fitting and attached electrode into
the probe. Use care not to kink or bend the electrode.
Note: Ensure that the spring is still inside the probe. The spring is
essential for adjusting the electrode’s position with respect to the tip
of the sprayer tube.
12. Tighten the electrode nut onto the probe assembly.
13. Adjust the electrode tip extension to specification. For more
information see,“Setting the Electrode Extension” on page 50
14. Slide the source probe straight down into the housing, taking care
not to allow the tip of the probe to touch any part of the housing.
15. Push down the bronze retaining ring to engage its thread with the
thread on the housing and then screw the ring down all the way.
16. Install the sample inlet line in the top of the probe. Thread the
sample inlet line nut into the fitting at the top of the probe. Tighten
the sample tube nut finger-tight then tighten it one-quarter turn.
17. Install the source onto the mass spectrometer. For more information
about installing the source, see the topic “Installing the Source
Housing on the Instrument” on page 23.
50
Turbo V Ion Source Operator’s Manual
should extend between 0.5 and 1.0 mm from the end of the probe.
See the following figure for more details.
Probe
0.5 - 1 mm Electrode
51
Source Maintenance
52
A
Source Parameters
This topic describes the operating parameters for the Turbo V™ source.
The tables in this topic contain information about individual parameters
that can be optimized. The parameters listed here are generally the only
ones that need to be optimized. For more information see,“Source-
Dependent Parameters” on page 54
Depending on the source installed on the instrument, different source-
dependent parameters will be available to optimize. The default
parameters available for each probe are listed in the following table.
Default Source-Dependent Parameters
53
Source Parameters
The Analyst software provides the capability to select either of the two
probes, on a per experiment basis. All of the data acquired using the
source is identified by the probe used to acquire the data.
The positioning of the probe in the source can have a significant impact
on the sensitivity of the analysis. For more information on how to
optimize the position of the probe, see “TurboIonSpray Optimization”
on page 28 and “APCI Optimization” on page 30.
Source-Dependent Parameters
Param Access
Name Range Typical value
ID ID
GS1 GS1 Gas 1 0 to 90 psi 20 to 60 psi
The GS1 parameter controls the nebulizer gas for the TurboIonSpray probe and
the auxiliary gas for the APCI probe. It helps generate small droplets of sample
flow and affects spray stability and sensitivity. For more information on
optimization steps, see “To optimize Gas 1 (nebulizer gas) using FIA” in the
Tuning, Calibrating, and Optimizing Guide for your instrument. or “To optimize
Gas 1 (auxiliary gas) using FIA” in the Tuning, Calibrating, and Optimizing
Guide for your instrument.
GS2 GS2 Gas 2 0 to 90 psi 30 to 70 psi
The GS2 parameter controls the auxiliary, or turbo, gas for the TurboIonSpray
probe. It is used to help evaporate the spray droplets. GS2 works in conjunction
with the TEM parameter. The best sensitivity is achieved when the combination
of temperature (TEM) and turbo-gas (GS2) flow rate causes the LC solvent to
reach a point at which it is nearly all vaporized. To optimize GS2, increase the
flow until you obtain the best signal-to-noise ratio. If you see a significant
increase in background noise, reduce the value. Too high a temperature can cause
premature vaporization of the solvent at the TurboIonSpray probe tip, especially
if the probe is set too low (5 to 13 mm). Too high gas flow could produce a noisy
or unstable signal. For more information on optimization steps, see “To optimize
Gas 2 (Turbo gas) Flow using FIA” in the Tuning, Calibrating, and Optimizing
Guide for your instrument.
This information does not apply to the APCI probe.
TEM TEM Temperature 0 to 750 600
54
Turbo V Ion Source Operator’s Manual
Param Access
Name Range Typical value
ID ID
The TEM parameter controls the temperature of the turbo gas in the
TurboIonSpray® probe, or the temperature of the APCI probe. It is used to help
evaporate the solvent to produce gas phase sample ions. TEM works in
conjunction with the GS2 parameter used for the TurboIonSpray probe. The best
sensitivity is achieved when the combination of temperature (TEM) and turbo gas
(GS2) flow rate causes the LC solvent to reach a point at which it is nearly all
vaporized. When optimizing the temperature, use a step size of 25 °C and leave
time between steps to allow the source to stabilize. For more information on
optimization steps, see “To optimize TurboIonSpray probe temperature using
FIA” in the Tuning, Calibrating, and Optimizing Guide for your instrument or
“To optimize the APCI probe temperature using FIA” in the Tuning, Calibrating,
and Optimizing Guide for your instrument.
CUR CUR Curtain Gas 10 to 50 psi 10 psi
The CUR parameter controls the gas flow of the Curtain Gas™ interface. The
Curtain Gas interface is located between the curtain plate and the orifice. It
prevents solvent droplets from entering and contaminating the ion optics. The gas
flow should be maintained as high as possible without losing sensitivity. For more
information on optimization steps, see “To optimize the Curtain Gas interface” in
the Tuning, Calibrating, and Optimizing Guide for your instrument.
NC NC Nebulizer, or –5 to 5 –2 in negative mode
Needle Current 2 in positive mode
The NC parameter controls the current applied to the corona discharge needle in
the APCI probe. The discharge ionizes solvent molecules, which in turn ionize
the sample molecules. For the APCI probe the current applied to the corona
discharge needle (NC) usually optimizes over a broad range (about 1 to 5 µA). To
optimize, start at a value of 1 and increase until you achieve the best signal-to-
noise ratio. If, on increasing the current, you observe no changes in signal, leave
the current at the lowest setting that provides the best sensitivity (for example, 2
µA). For more information on optimization steps, see “To optimize the NC
(nebulizer or needle current)” in the Tuning, Calibrating, and Optimizing Guide
for your instrument.
IS IS IonSpray Voltage –4500 to 5500V –4000V in negative
mode, 5000 in
positive mode
55
Source Parameters
Param Access
Name Range Typical value
ID ID
The IS parameter controls the voltage applied to the needle that ionizes the
sample in the ion source. It depends on the polarity, and affects the stability of the
spray and the sensitivity. For more information on optimization procedures, see
“To optimize TurboIonSpray probe voltage using FIA” in the Tuning, Calibrating,
and Optimizing Guide for your instrument.
ihe ihe `Interface Heater off; on on
The ihe parameter switches the interface heater on and off. Heating the interface
helps maximize the ion signal and prevents contamination of the ion optics.
Unless the compound you are analyzing is extremely fragile, it is recommended
to heat the interface. With the Turbo V™ source, the interface plate is heated to
100 °C.
56
B
Troubleshooting
This appendix contains troubleshooting tips for the Turbo V™ source.
Turbo V Troubleshooting
57
Troubleshooting
58
C
Parts List
The following table lists the orderable parts for the Turbo V™ source.
Turbo V Consumables Kit
Turbo V Spares
59
Parts List
60
D
Principles of Operation
This appendix contains information that explains how the Turbo V™
source generates ions.
Ion Evaporation
Only compounds that ionize in the liquid solvent can be generated as
gas phase ions in the source. The efficiency and rate of ion generation
depends on the solvation energies of the specific ions. Ions with lower
solvation energies are more likely to evaporate than ions with higher
solvation energies.
Droplet contains As the solvent At some critical Non-volatile residue
ions of both polarities evaporates the field value, ions remains as a dry
with one polarity electrical field increases are emitted from particle
being predominant and the ions move the droplets
to the surface
+ +
- -
+ +- + + ++ --
+
-- + ++++-
+ +-+ + + ++
- + -+
-+- + +
-+ +
+ +
- +
+
Ion evaporation
Each charged droplet contains solvent and both positive and negative
ions, but with ions of one predominant polarity. As a conducting
medium, excess charges reside at the droplet’s surface. As the solvent
evaporates, the electrical field at the surface of the droplet increases due
to the decreasing radius of the droplet.
If the droplet contains excess ions and enough solvent evaporates from
the droplet, a critical field is reached at which ions are emitted from the
surface. Eventually, all of the solvent will evaporate from the droplet,
leaving a dry particle consisting of the nonvolatile components of the
sample solution.
Given that the solvation energies for most organic molecules are
unknown, the sensitivities of any given organic ion to ion evaporation is
difficult to predict. The importance of solvation energy is evident
61
Principles of Operation
Ionization Modes
The following paragraphs explain the differences between
TurboIonSpray and APCI modes.
APCI mode
The following figure shows the general location of the ion-molecule
reactor of the API probe.
Ceramic
Tube Curtain Gas
Curtain Plate
Wall-less Orifice
Reactor
Curtain
Gas
Curtain Gas
Sample Flow
62
Turbo V Ion Source Operator’s Manual
influence of the electric field in the direction of the curtain plate and
through the gas curtain into the mass analyzer. The whole ion formation
process is collision dominated because of the relatively high
atmospheric pressure of the APCI probe. Except in the immediate
vicinity of the discharge needle tip, where the strength of the electric
field is greatest, the energy imparted to an ion by the electric field is
small in comparison with the ion’s own thermal energy.
Through collisions, an equal distribution of certain ions (for example,
protonated water cluster ions) is maintained. Any excess energy that an
ion may acquire in the ion-molecule reaction process is thermalized.
Through the process known as collisional stabilization, many of the
product ions are fixed, even though many subsequent collisions occur.
Both product ion and reactant ion formation are governed by
equilibrium conditions at 760 torr (atmospheric) operating pressure.
The APCI probe functions as a wall-less reactor since the ions that pass
from the source to the vacuum chamber and eventually to the CEM ion
detector never experience collisions with a wall-only collisions with
other molecules. Ions are also formed outside the designated API
source, but are not detected and are eventually neutralized by
interacting with a wall surface.
The temperature of the probe is an important factor for APCI probe
operation. The temperature must be set high enough to ensure a rapid
evaporation. At a sufficiently high operating temperature, the droplets
are vaporized quickly so that organic molecules are desorbed from the
droplets with minimal thermal degradation. If, however, the
temperature is set too low, the evaporation process is slower and
pyrolysis, or decomposition, may occur before vaporization is
complete. To preserve the molecular identity, the temperature of the
probe must be set to ensure rapid evaporation. Operating the APCI
probe at temperatures above the optimal temperature may cause thermal
decomposition of the sample.
The previous figure, APCI ionization region, shows the reaction flow of
the atmospheric pressure chemical ionization (APCI) process for
reactant positive ions (the proton hydrates, H3O+[H2O]n). This
sequence is derived from experimental results summarized by Huertas
and Fontan (Huertas, M.L. and J. Fontan 1975 “Evolution Times of
Tropospheric Positive Ions,” Atmospheric Environ. 9, 1018.).
The major primary ions N2+, O2+, H2O+, and NO+ are formed by the
electron impact of corona-created electrons on the major neutral
63
Principles of Operation
64
Turbo V Ion Source Operator’s Manual
65
Principles of Operation
66
Turbo V Ion Source Operator’s Manual
Index
A flow injection analysis 17
APCI mode
described 62 G
source testing 44
APCI probe GS1 (Gas 1) 54
cleaning 48 GS2 (Gas 2) 54
features 20
functions of, described 63
inlet description 14 H
optimizing 30
optimizing the source 31 heated nebulizer. See APCI probe
probe selection 19
source testing 44
I
injector setup for source testing 40
C introducing the sample 17
components ionization modes, described 62
corona discharge needle 51 ions, overview of ion generation 61
electrode, maintaining 48 IS (IonSpray voltage) 55
corona discharge needle
optimizing 31
CUR (Curtain Gas interface) 55 L
LC/MS, sample introduction 17
E loop injector 17
electrode
adjusting 50 M
maintaining 48
exhaust pressure switch, testing 25 maintenance schedule 47
exhaust system 15
N
F NC (nebulizer or needle current) 55
features
APCI probe 20
TIS probe 20
FIA 17
67
Index
O maintenance of 47
parameters 30, 33, 53
optimizing preparing for installation 20
APCI probe 30 preparing for operation 25
automatic optimizing 30, 33, 53 removing 34, 47
corona discharge needle 31 source exhaust system, and interlocks
source for APCI probe 31 16
TurboIonSpray probe 28 source housing
TurboIonSpray probe, typical described 12
values 28 installing 21, 35
safety interlocks, function of 16
source testing
P APCI mode 44
parameters criteria for 39
source specific 30, 33, 53 injector setup 40
source testing in APCI mode 44 instrument setup 39
source testing in TIS mode 42 TIS mode 42
source-dependent source-dependent parameters. See
CUR (Curtain Gas interface) parameters
55
GS1 (Gas 1) 54
GS2 (Gas 2) 54 T
IS (IonSpray voltage) 55 TEM (temperature) 54
NC (nebulizer or needle temperature control, operating tips 17
current) 55
TIS mode
TEM (temperature) 54 described 64
parts list 59 source testing 42
prefiltered samples 17 TIS probe
probe cleaning 48
installing 21 features 20
function of, described 64
functionality described 14
S inlet description 14
parts, describe 14
sample introduction 17 probe selection 19
separation column 17 source testing 42
source TIS. See TurboIonSpray probe
cleaning 48 troubleshooting 57
corona discharge needle, TurboIonSpray probe
replacing 51 optimizing 28
electrode, cleaning 48 typical values for optimizing 28
exhaust system 15
features of 11
68