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Finnigan

TRACE MS
[Including Voyager and MD Series]

Solids & DCI Probe


Manual

Revision A
FM101890
Xcalibur™ and TRACE™ are trademarks of ThermoQuest Corporation. Microsoft® and Windows NT® are registered trademarks
of Microsoft Corporation. Tygon® is a registered trademark of Norton Industrial Plastics.

Technical information contained in this publication is for reference purposes only and is subject to change
without notice. Every effort has been made to supply complete and accurate information; however,
ThermoQuest Corporation assumes no responsibility and will not be liable for any errors, omissions,
damage, or loss that might result from any use of this manual or the information contained therein (even if
this information is properly followed and problems still arise).
This publication is not part of the Agreement of Sale between ThermoQuest Corporation and the purchaser
of a ThermoQuest system. In the event of any conflict between the provisions of this document and those
contained in ThermoQuest Corporation’s Terms and Conditions, the provisions of the Terms and
Conditions shall govern.
Reference to System Configurations and Specifications supersede all previous information and are subject
to change without notice.

Printing History: Revision A, printed in August 1999.

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Published by Technical Publications, ThermoQuest, Manchester, UK.


Copyright© 1999 ThermoQuest Corporation, a public subsidiary of Thermo Instrument Systems, Inc., a member of the Thermo Electron family of
companies. All rights reserved. Printed in the UK.
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Revision A
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The EU Directives covered by this Declaration

89/336/EEC Electromagnetic Compatibility Directive, amended by 92/31/EEC & 93/68/EEC


73/23/EEC Low Voltage Equipment Directive, amended by 93/68/EEC
93/68/EEC CE Marking Directive

The Products covered by this Declaration

The Finnigan TRACE MS series (formerly MD series) of mass spectrometers for GC/MS.

The Basis on which Conformity is being Declared

The products identified above comply with the EU directive 89/336/EEC by meeting the following standards:

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_________________________________________________________________________ Contents

Contents

1. Read This First ........................................................................................................................... iii

Changes to the Manual and Online Help ...............................................................................................iv

Abbreviations..........................................................................................................................................v

Typographical Conventions...................................................................................................................ix
Data Input ............................................................................................................................ix
Notes, Cautions, and Warnings.............................................................................................x
Topic Headings ....................................................................................................................xi

Reply Card ........................................................................................................................................... xii

1. Installing and Using Probes.........................................................................................................1

1. Introduction........................................................................................................................................2
Probe Source Voltage Requirements ....................................................................................2

2. Installing the Control Unit .................................................................................................................3

3. The Probe Vacuum Lock ...................................................................................................................5

4. The Probe Source...............................................................................................................................6


Changing the Source Exit Plate ............................................................................................7
Reassembling the Source ......................................................................................................9
Source Installation ..............................................................................................................10

5. Configuring Xcalibur for Probe Support .........................................................................................11

6. Solids Probe Installation ..................................................................................................................12


Installing the Solids Probe ..................................................................................................12

7. DCI Probe Installation .....................................................................................................................14


Installing the DCI Probe .....................................................................................................14

8. Using Probes ....................................................................................................................................16


Sample Loading ..................................................................................................................16
Inserting the Probe ..............................................................................................................18
Withdrawing the Probe .......................................................................................................21

9. Probe Control and Data Acquisition using the Solids or DCI Probe ...............................................22
Solids Probe Control ...........................................................................................................22
DCI Probe Control ..............................................................................................................24

_________________Finnigan TRACE MS Solids & DCI Probe Manual_____________________ i


Contents _________________________________________________________________________

10. Troubleshooting ........................................................................................................................ 27

11. Solids and DCI Probes Parts List.............................................................................................. 28


Source and Probe Lock Assembly...................................................................................... 28
Solids Probe Assembly....................................................................................................... 30
DCI Probe Assembly.......................................................................................................... 30
Rotary Pump and Control Unit........................................................................................... 30

ii ___________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


1. Read This First

Welcome to the Finnigan TRACE MS system!


The Finnigan TRACE MS Solids & DCI Probes Manual provides you
with the information you need to install and use a Solids or a DCI probe.
This manual is intended for users who have purchased the probe option for
their Finnigan TRACE MS. It describes the installation of the probe
hardware, operation of the probe, a troubleshooting guide, and a spare parts
list.

Note. The information contained within this manual can also be applied to
the Voyager and MD Series of mass spectrometers. However, the reader
should be aware that all text, examples and Figures refer only to the
Finnigan TRACE MS for the purpose of simplification.

WARNING. Both probes can quickly reach red heat, even when out of the
vacuum lock. Exercise extreme caution at all times whilst using the system.

WARNING. Removal of covers may expose hazardous voltages and


should only be carried out by suitably trained and competent persons.

Caution. If the equipment is used in a manner not described in this


manual, the protection provided by the equipment may be impaired.

_________________Finnigan TRACE MS Solids & DCI Probe Manual____________________ iii


Read This First
Changes to the Manual and Online Help_________________________________________________

Changes to the Manual and


Online Help
To suggest changes to this manual or the online Help, please send your
comments to:
Marketing Manager
ThermoQuest
Crewe Road
Wythenshawe
Manchester
M23 9BE
UK

You are encouraged to report errors or omissions in the text or index.


Thank you!

iv ___________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Read This First
_____________________________________________________________________ Abbreviations

Abbreviations
The following abbreviations are used in this and other TRACE MS manuals
and in the online Help.
A ampere
ac alternating current
ADC analog-to-digital converter
amu atomic mass unit
AP acquisition processor
APCI atmospheric pressure chemical ionization
API atmospheric pressure ionization
ASCII American Standard Code for Information Interchange
b bit
B byte (8 b)
baud rate data transmission speed in events per second
°C degrees Celsius
cfm cubic feet per minute
CD compact disc
CD-ROM compact disc read-only memory
CI chemical ionization
CIF Carriage, Insurance and Freight Paid to
CIP Carriage and Insurance Paid to
cm centimeter
cm3 cubic centimeter
CPU central processing unit (of a computer)
CRM consecutive reaction monitoring
CSE customer support engineer
<Ctrl> control key on the terminal keyboard
d depth
Da dalton
DAC digital-to-analog converter
dc direct current
DCI desorption chemical ionization
DDS direct digital synthesizer
DS data system

_________________Finnigan TRACE MS Solids & DCI Probe Manual____________________ v


Read This First
Abbreviations______________________________________________________________________

DSP digital signal processor


EI electron ionization
<Enter> <Enter> key on the terminal keyboard
EMC electromagnetic compatibility
ESD electrostatic discharge
ESI electrospray ionization
eV electron volt
f femto (10-15)
°F degrees Fahrenheit
FID Flame Ionization Detector
FOB Free on Board
FPD Flame Photometric Detector
ft foot
FTP file transfer protocol
g gram
G giga (109)
GC gas chromatograph
GC/MS gas chromatograph / mass spectrometer
GND electrical ground
GPIB general-purpose interface bus
GUI graphical user interface
h height
h hour
HPLC high-performance liquid chromatograph
HV high voltage
Hz hertz (cycles per second)
ICISä Interactive Chemical Information System
ICLä Instrument Control Languageä
IEC International Electrotechnical Commission
IEEE Institute of Electrical and Electronics Engineers
in. inch
I/O input/output
k kilo (103, 1000)
K kilo (210, 1024)

vi ___________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Read This First
_____________________________________________________________________ Abbreviations

kg kilogram
l length
L liter
LAN local area network
lb pound
LC liquid chromatograph
LC/MS liquid chromatograph / mass spectrometer
LED light-emitting diode
m meter
m milli (10-3)
M mega (106)
M+ molecular ion
µ micro (10-6)
min minute
mL milliliter
mm millimeter
MS scan power: MS1
MS/MS scan power: MS2
MSn scan power: MSn, n = 1 through 10
m/z mass-to-charge ratio
n nano (10-9)
NCBI National Center for Biotechnology Information (USA)
NIST National Institute of Standards and Technology
Ω ohm
p pico (10-12)
Pa pascal
PC personal computer
PCB printed circuit board
PID Photo Ionization Detector
PMD Photo Multiplier Detector
PMT Photo Multiplier Tube
P/N part number
P/P peak-to-peak voltage
ppm parts per million

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ vii


Read This First
Abbreviations______________________________________________________________________

psig pounds per square inch, gauge


RAM random access memory
<Return> <Return> key on the terminal keyboard
RF radio frequency
RMS root mean square
ROM read-only memory
RS232 industry standard for serial communications
s second
SCSI small computer system interface
SIM selected ion monitoring
solids probe direct insertion probe
TIC total ion current
TCP/IP transmission control protocol / Internet protocol
Torr torr
u atomic mass unit
URL uniform resource locator
V volt
V ac volts alternating current
V dc volts direct current
VGA Video Graphics Array
w width
W Watt
WWW World Wide Web

Note. Exponents are written as superscripts. In the corresponding online


Help, exponents are written with a caret (^) or with e notation because of
design constraints in the online Help. For example:

MSn (in this manual) MS^n (in the online Help)

105 (in this manual) 10^5 (in the online Help)

viii __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________
Read This First
___________________________________________________________Typographical Conventions

Typographical Conventions
Typographical conventions have been established for ThermoQuest manuals
for the following:
• Data input
• Notes, Cautions, and WARNINGS
• Topic headings

Data Input
Throughout this manual, the following conventions indicate data input and
output via the computer:
• Prompts and messages displayed on the screen are represented in this
manual by capitalizing the initial letter of each word and italicizing each
word.
• Input that is to be entered by keyboard or buttons that are to be clicked
on by the mouse is represented in bold face letters. (Titles of topics,
chapters, and manuals also appear in bold face letters.)
• For brevity, expressions such as “choose File | Directories” are used
rather than “pull down the File menu and choose Directories.”
• Any command enclosed in angle brackets < > represents a single
keystroke. For example, “press <F1>” means press the key labeled F1.
• Any command that requires pressing two or more keys simultaneously
is shown with a hyphen connecting the keys. For example, “press
<Shift>-<F1>” means depress and hold the <Shift> key and then press
the <F1> key.

_________________Finnigan TRACE MS Solids & DCI Probe Manual____________________ ix


Read This First
Typographical Conventions ___________________________________________________________

Notes, Cautions, and Warnings


Notes, Cautions, and WARNINGS are displayed in boxes such as the one
below.

Note. Boxes such as this are used to display Notes, Cautions, and
WARNINGS.

A Note contains information that can affect the quality of your data. In
addition, notes often contain information that you may need if you are
having trouble.
A Caution contains information necessary to protect your instrument from
damage.
A WARNING describes hazards to human beings.

x ___________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Read This First
___________________________________________________________Typographical Conventions

Topic Headings
The following headings are used to show the organization of topics within a
chapter:

Chapter 1
Chapter Name

1.1 Second Level Topics

Third Level Topics

Fourth Level Topics

Fifth Level Topics

_________________Finnigan TRACE MS Solids & DCI Probe Manual____________________ xi


Read This First
Reply Card _______________________________________________________________________

Reply Card
TRACE MS manuals contain a Reader Survey card located at the front of
each manual.
A message on the Reader Survey card asks the user to fill out and return the
card after he or she has had an opportunity to use the manual. The Reader
Survey card has two functions. Firstly, it allows the user to tell
ThermoQuest what he or she does and doesn’t like about the manual.
Secondly, when the user returns the card, he or she is registered and placed
on the ThermoQuest mailing list. Once registered, the user will receive
ThermoQuest's newsletter Analytical News and will be notified of events of
interest, such as user meetings.

xii __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________
1. Installing and Using Probes

Many samples submitted for evaluation by mass spectrometry are too


involatile or have too low a thermal stability to be introduced into the mass
spectrometer via a GC, and must therefore be introduced directly into the
ion source. Both the Solids and DCI probes allow a quick and easy method
to analyze both solids and liquids falling into this category. The probes
admit the sample directly into the ion source through a vacuum lock. Probes
can also be used as a quick method of pre-screening for the presence of a
particular compound.
The Solids probe is used for solid samples (as its name suggests) or less
volatile liquid samples. The sample is loaded into a sample cup, which is
located at the end of the probe. A thin strip of tungsten foil is used to hold
the sample cup firmly in position.
A heating element and thermocouple assembly is located at the end of the
probe close to the sample cup. The probe may be heated by passing a current
through the heater to evaporate the sample into the electron beam. The
thermocouple monitors the temperature and the heating current is controlled
using the MS data system, Xcalibur™, to maintain the required program rate
and final temperature.
DCI (Desorption Chemical Ionization) is a ‘soft’ ionization technique in
which thermally labile samples can be ionized with reduced fragmentation
compared to EI or even Solids probe CI. The DCI probe permits the
vaporization of samples by the application of an electrical current through a
platinum filament to which the sample is applied.
The sample is loaded by syringe onto the platinum filament situated at the
tip of the DCI probe. With the probe inserted, the sample is desorbed into
the ion source assisted (if necessary) by a controlled heating current passed
through the coil. The DCI filament current is programmable using the
Xcalibur data system.

_________________Finnigan TRACE MS Solids & DCI Probe Manual____________________ 1


Installing and Using Probes
Introduction _______________________________________________________________________

1. Introduction
The TRACE MS can be supplied with two different probes: Solids and DCI.
A probe consists of four elements:
• Control Unit
• Vacuum Lock
• Probe Source
• Probe
The sections that follow in this manual describe each of the above.

Probe Source Voltage Requirements


The probe source requires the following voltage:

Supply voltage 100-120 V 60 Hz


220-240 V 50 Hz
Maximum VA rating 360 V ac

A Power lead is connected to the control unit. Before plugging it in, carry
out the following:
• Select the correct voltage for your power supply. The voltage selector is
on the rear of the control unit.
• Ensure that the correct fuse is fitted to the control unit. The fuse is
located on the rear of the unit, marked as PUMP FUSE (see Figure 1 on
page 4). Two packs of fuses are supplied with the control unit. The table
below shows fuse types and part numbers.
• Ensure that the equipment is earthed.

Voltage Rating Fuse Part Number


110 V Rotary Pump T10A PDM00117
240 V Rotary Pump T6.3A PDM00118

Caution. Ensure that the rotary pump fitted is of the correct voltage rating.

2 ___________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
____________________________________________________________ Installing the Control Unit

2. Installing the Control Unit


The control unit allows you to control the probe’s operation. To install the
control unit:
1. Vent and switch off the TRACE MS (see the relevant section of your
Hardware Manual for details of this procedure).
2. Exit Xcalibur and turn off the controlling PC.
3. Position the probe control unit next to the TRACE MS.
4. Connect the water tubes to the rear of the probe control unit (see Figure
1).

Caution. The maximum water pressure allowable on the water inlet is


15 psig.

5. Locate the probe control unit’s communication cable. Connect one end
to the port marked Control Input on the rear of the control unit.
Connect the other end to the port marked Analog I/O on the rear of the
TRACE MS.
6. Connect the Tygon® tube that exits the rear of the control unit to the
exhaust outlet on the rotary pump.
7. Ensure that the pump has any transit covers removed (especially the
outlet connection) and that it contains the correct amount of oil (refer to
the manufacturer’s handbook or your Hardware Manual).
8. Connect the vacuum pump power cable to the IEC connector on the rear
of the control unit.
9. Select the mains voltage supply rating at the switch on the rear of the
control unit.

Caution. Ensure the correct voltage is selected on the rear of the control
unit or severe damage may be done to the instrument.

10. Connect the control unit to the mains power supply.

Caution. Do not switch the controller on until the TRACE MS is on and


the TRACE MS Server is running.

_________________Finnigan TRACE MS Solids & DCI Probe Manual____________________ 3


Installing and Using Probes
Installing the Control Unit ____________________________________________________________

Control Unit (rear)

To CONTROL
CONTROL VOLTAGE MAINS
SELECTOR SOLIDS ON/OFF
PROBE

PART No 3 AMP
240V
SERIAL No
ADDRESS
DCI
PUMP
FUSE PROBE
3 AMP

RATING LABEL PUMP


MAINS
IN

Pump inlet
To ANALOG I/O on
the mass detector
Rotary pump Water
to/from
supply

Mains

Pump power lead

Figure 1. Connections to the rear of the control unit

4 ___________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
_____________________________________________________________The Probe Vacuum Lock

3. The Probe Vacuum Lock


The probe vacuum lock allows you to insert either of the two sample probes
into the ion source without breaking vacuum. The main component of the
lock is a 90°-rotation ball valve that isolates the system from atmosphere
when the probes are not in use. An outer O-ring seal allows evacuation of
the lock prior to opening the ball valve and fully inserting the probe.

Control unit (front)

Probe
Controller

WATER

VACUUM >50°C PROBE

quick release
valves
vacuum pumping
connection rotary pump connection
to probe lock

probe lock
(underside view)

water to the solids probe (if fitted)

Figure 2. Probe vacuum lock showing connection to rotary pump


via the control unit

Caution. Moving the probe through the vacuum lock with a high probe
temperature or current setting will damage seals in the lock and may also
lead to system contamination. Always allow the probes to cool before
inserting or removing.

Caution. Failure to observe correct operating procedures whilst using the


probe vacuum lock may cause irreparable damage to the pumping system.

_________________Finnigan TRACE MS Solids & DCI Probe Manual____________________ 5


Installing and Using Probes
The Probe Source __________________________________________________________________

4. The Probe Source


The probe source is a combination source that allows data acquisition in all
three ionization modes. The combination source also allows high sensitivity
CI- acquisition. The source comes equipped with two dedicated ion exit
plates to achieve high sensitivity acquisition in EI and CI+ if required.
Details of how to change the source exit plate are given in the following
section, Changing the Source Exit Plate.
The only difference between the exit plates is the size of the central hole.
The table below shows what hole size is appropriate for each acquisition
mode.
Large exit hole EI
Medium exit hole CI- and combination
Small exit hole CI+

The size of the hole alters the pressure inside the source block. A low
pressure favors EI ionization whereas a relatively high pressure favors CI+
ionization. If flexibility is required to acquire samples using different
ionization modes without having to vent the instrument, then the
combination exit plate should be fitted. This will give reasonable sensitivity
in all ionization modes. However, if only EI or CI+ acquisitions are required
then the relevant dedicated exit plate should be fitted. This will increase the
sensitivity in the chosen ionization mode. Similarly, when acquiring in CI-
only, fit the combination exit plate that has already been optimized for CI-
acquisition.

6 ___________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
__________________________________________________________________The Probe Source

Changing the Source Exit Plate


Four exit plates allow configuration of the source for different ionization
modes. To change the exit plate:
1. Remove the source from the mass detector. (The probe lock can remain
attached to the source during this procedure.)
2. Disconnect the source wires from the wires attached to the flange and
remove the two circlips.
3. Pull the source and lenses away from the flange, holding the source
mounting plate.

Source wires Mounting plate

Remove these two circlips

The wires from the source


connect to wires attached to
this part of the flange. Disconnect
all the source wires from those
attached here.

Figure 3. The source showing removal of source wires and circlips

_________________Finnigan TRACE MS Solids & DCI Probe Manual____________________ 7


Installing and Using Probes
The Probe Source __________________________________________________________________

After removing the source block, remove the lenses and magnets in order to
gain access to the exit plate. Carry out this procedure as follows:
1. Hold the source by the mounting plate with the four nuts visible as
shown in Figure 4.
2. Remove the four nuts.
3. Lift the ion lock and exit plate away from the lenses and magnets.

Caution. Hold the exit plate at the edges and avoid touching the flat faces.

4. Change the exit plate.

Remove these four nuts


to lift the ion block and
exit plate away from
lenses and magnets.

Figure 4. Removing the source block from the lens stack

8 ___________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
__________________________________________________________________The Probe Source

Reassembling the Source


To reassemble the source, carry out the dismantling procedure in reverse.
Figure 5 may help with this.

Caution. When fitting the four nuts illustrated in Figure 4, only tighten
them until they are finger-tight. Over-tightening may cause the source
ceramic spacers to crack.

Source block

CI- and combination


exit plate

EI exit plate CI+ exit plate

Undo these four screws Mounting plate


to remove the currently
fitted exit plate.

Figure 5. Removal of the exit plate

_________________Finnigan TRACE MS Solids & DCI Probe Manual____________________ 9


Installing and Using Probes
The Probe Source __________________________________________________________________

Source Installation
To install the source and vacuum lock:
1. Remove any source already in the TRACE MS, remembering to retract
the GC Interface.
2. Ensure that the wires connecting the source will not interfere with the
passage of the probe during operation. Also, ensure that when the source
is moved on its springs, the wires do not move to block the path of the
probe.
3. The probe source has no hole for a GC Interface to enter the source,
therefore withdraw the GC interface a suitable distance back into the
GC.
4. Withdraw the column about 6 cm into the GC interface and tighten the
interfaces-locking nut. It is not necessary to remove the column but
reduce the column head pressure to 20 kPa to conserve helium.
5. Fit the probe source and vacuum lock into the TRACE MS system,
taking care not to trap any wires in the flange seal, and secure with the
two black finger nuts.
6. Move the lock fully to the left to close the lock. Do not insert the probe
at this stage.
7. Connect the Tygon tube from the front of the control box to the 6 mm
stainless steel tube on the lower part of the probe lock. This connects the
lock to the inlet of the rotary pump via the control unit.

Figure 6. Probe lock and source installed on vacuum housing

10 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
_________________________________________________ Configuring Xcalibur for Probe Support

5. Configuring Xcalibur for Probe


Support
In order to configure Xcalibur for Solids or DCI Probe support you must set
the correct Source Type for your TRACE MS. This can be done using the
Instrument Configuration program or alternatively via the TRACE MS
Server.

Using Instrument Configuration

1. Start the Instrument Configuration program by double-clicking on the


Instrument Configuration shortcut icon on the Windows® desktop.
Alternatively, click on the Start button in the Windows Taskbar and
choose Programs I Xcalibur I Instrument Configuration.
2. Configure the TRACE MS. Refer to the online Help or TRACE MS
Getting Connected for more detailed information on how to do this.
• To enable Solids Probe support, set the TRACE MS Source Type to
EICI (Solids Probe).
• To enable DCI Probe support, set the TRACE MS Source Type to
EICI (DCI Probe).
3. Click on Done to exit the Instrument Configuration program.

Using the TRACE MS Server

1. Start Xcalibur by double-clicking on the Xcalibur shortcut icon on the


Windows desktop. Alternatively, click on the Start button in the
Windows Taskbar and choose Programs I Xcalibur I Xcalibur.
2. Right-click on the TRACE MS Server icon displayed on the right of the
Windows Taskbar (Figure 7)to display a menu:
• To enable Solids Probe support, choose
Source Type I EICI (Solids Probe).
• To enable DCI Probe support, choose
Source Type I EICI (DCI Probe).

Figure 7. The taskbar showing Xcalibur Home Page and Server

For more detailed information on the TRACE MS Server, refer to TRACE


MS Getting Started.

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 11


Installing and Using Probes
Solids Probe Installation _____________________________________________________________

6. Solids Probe Installation


The section describes how to install the Solids probe. Before installing the
Solids probe hardware, you will need to correctly configure Xcalibur to
enable Solids probe support. See the previous section Configuring
Xcalibur for Probe Support for details of how to do this.

Installing the Solids Probe


To install the Solids probe:
1. Position the probe securely on its stand.
2. Connect the probe to the front of the control box with the cable supplied
(P/N. TPRC001).

Note. There is a different cable for the DCI and Solids probes.

3. Connect the water lines from the probe to the outlets on the box and
ensure that the water supply is ON. Check the system for water leaks
now.
In the TRACE MS Tune window (Xcalibur), make sure the Solids probe
temperature is set to 20 °C, which is the default value. Refer to the section
on the Tune window (Solids Probe control) for more information on this
(page 22).

WARNING. Beware of hot parts! The probe can heat up very quickly
(800 °C/min).

Caution. The maximum water pressure allowable on the water inlet is


15 psig.

12 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
_____________________________________________________________ Solids Probe Installation

Probe
Controller

WATER

VACUUM >50°C PROBE

Control unit
(front view)

Water cooling
Probe IN/OUT
sample cup

Power connection

Water cooling Heater and


IN/OUT thermocouple

Figure 8. Solids probe showing probe tip detail and connection to


control unit

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 13


Installing and Using Probes
DCI Probe Installation _______________________________________________________________

7. DCI Probe Installation


The section describes how to install the DCI probe. Before installing the
DCI probe hardware, you will need to correctly configure Xcalibur to enable
DCI probe support. See the section Configuring Xcalibur for Probe
Support for details of how to do this.

Installing the DCI Probe


DCI probes require a CI environment to operate in. Ensure that a suitable
exit plate is fitted to the source. To install the DCI probe:
1. Position the probe securely on its stand.
2. Install a DCI probe tip (P/N TPRB009) into the end of the probe,
observing the following guidelines:
a. Align the holes in the back of the tip with the pins in the end of the
probe.
b. Push the tip firmly into the DCI probe.

Caution. Ensure the tip is fully inserted before using it to prevent


damaging the element in the probe lock during use.

3. Connect the DCI probe to the control box with the appropriate cable,
(P/N TPRC002).

Caution. Do not switch on while the probe is removed from the mass
detector because the filament will deteriorate in atmosphere.

In the TRACE MS Tune window (Xcalibur), make sure the DCI current is
set to zero (0 mA), which is the default value. Refer to the section on the
Tune window (DCI Probe control) for more information on this (page 24).

WARNING. Beware of hot parts! The filament becomes hot during


operation.

14 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
_______________________________________________________________ DCI Probe Installation

Probe
Controller

WATER

VACUUM >50°C PROBE

Control unit
(front view)

Platinum filament

Power connection

Figure 9. DCI probe showing probe tip detail and connection to


control

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 15


Installing and Using Probes
Using Probes______________________________________________________________________

8. Using Probes
The following pages describe how you use the TRACE MS Solids and DCI
probes.

Sample Loading
The procedure for loading a sample depends upon the type of probe you are
using, as described below.

Solids Probe
Two types of sample cup are available for use with the Solids probe (see
Figure 10).

Shallow sample cup Deep sample cup

Figure 10. Solids probe sample cups

For non-volatile samples, the shallow cup is recommended. With this type
of cup the sample is close to the heated ion source, aiding evaporation of the
sample.
Use a deep cup for more volatile samples. With this type of cup the sample
is deposited at the bottom, so that it is remote from the heating affect of the
ion source. The sample is then evaporated into the ion source, in a controlled
fashion, using the probe heater.
Load solid samples into the cups using a thin piece of wire, or a drawn-out
length of glass rod. Make sure that the sample is deposited at the bottom of
the cup and not around the neck. Liquid samples in solution are best loaded
using a microsyringe taking care not to leave any air pockets. Allow the
solvent to evaporate from the cup before inserting the probe into the
instrument by standing the holder in a warm place, for example on top of the
GC oven. Take care not to heat the holder too quickly, so as to avoid
blowing the sample out of the cup with solvent vapor.
A common mistake is to overload the probe. A few micrograms are
sufficient. If the sample is easily visible, there is probably too much present.

16 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
_____________________________________________________________________ Using Probes

Caution. The TRACE MS is very sensitive. Overloading the probe will


increase maintenance frequency and compromise spectral accuracy. Never
touch probe parts with fingers; this will lead to immediate background
contamination. Use clean tweezers.

If you have a number of samples to run sequentially, load all the cups and
stand them in the holder provided.
Hold the sample cups firmly in place using a strip of tungsten foil and push
them firmly into the holder at the end of the probe so as to give good
thermal contact with the heater element.
Coil the foil round and insert it into the end of the probe. Fully insert the
probe cup so that the foil forms a spring between the cup and probe tip. The
foil should allow the cups to be inserted easily but held firmly in the probe
tip once they are in place.
Always insert the probe cups fully, so that less than 2 mm of glass protrudes
(see Figure 11).

Caution. Always use the tungsten foil in the Solids probe to hold the
sample in place, and always fully insert the probe cups so that less than
2mm of glass protrudes Failure to do this will risk the probe cups becoming
entangled in the probe lock rotary valve, causing irreparable damage.

tungsten foil

Probe tip

Figure 11. End view of probe tip showing the foil in place

DCI Probe
Load samples onto the platinum filament as a liquid or in solution using a
microsyringe; any solvent is then evaporated prior to probe insertion. As
with the Solids probe, care must be taken not to overload the probe; a few
microliters are sufficient. To achieve reproducible spectra the sample must
be deposited as an even film.

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 17


Installing and Using Probes
Using Probes______________________________________________________________________

DCI is a CI technique. Ammonia has been found to be preferable to methane


due to the lower tendency of the (M+NH4)+ ions to decompose.

sample probe and sample holder assembly


holder

control unit assembly (side view)

Figure 12. Side view of probe and sample holder

Inserting the Probe


The procedure is the same for both Solids and DCI probes.
1. Connect the probe to the front of the control unit in the socket marked
PROBE using the 10-pin lead.

Note. There is a different cable for the DCI and Solids probes. The Solids
probe cable part number is TPRC001 and the DCI probe cable part number
is TPRC002.

2. Ensure that the probe is set to its lowest setting: 20 °C for Solids and
0 mA for DCI. Refer to the relevant section on the Tune window for
more information on this (Solids probe, see page 22; DCI Probe, see
page 24).
3. When the probe has been prepared for use, insert it into the introduction
lock until the interlock fingers reach the guide on the lock handle (see
Figure 13 and Figure 14). You will feel resistance for the last few
millimeters of travel as the probe makes contact with the first seal.

18 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
_____________________________________________________________________ Using Probes

Figure 13. Inserting the probe into the introduction lock (1)

Figure 14. Inserting the probe into the introduction lock (2)

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 19


Installing and Using Probes
Using Probes______________________________________________________________________

4. Pump out the introduction lock by pressing the green VACUUM button
on the front of the control unit. The light will begin flashing and then
stop.
5. When the vacuum light stops flashing, rotate the probe lock valve 90° to
the right (see Figure 15).

Figure 15. Rotating the probe lock valve

6. Carefully push the probe fully into place (see Figure 16).

Figure 16. Pushing the probe fully into place

20 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
_____________________________________________________________________ Using Probes

The probe lock allows either the DCI or the Solids probes to be inserted
while the mass detector remains under vacuum. The lock is equipped with a
series of seals, as well as a rotary valve and a vacuum connection. This
combination allows the probe to be inserted and removed without subjecting
the vacuum system to any pressure fluctuations.

Withdrawing the Probe


The procedure for withdrawing the probe is the reverse of the procedure for
inserting it:
1. Allow the probe to cool to less than 50 °C. This is confirmed by the red
light marked >50 °C on the front of the control unit turning green.

WARNING. This light is for indication only. Exercise caution and check
the actual temperature before handling the probe.

2. Slightly withdraw the probe back from the source, as the source will
keep the probe hot.
3. Withdraw the probe carefully from the system until the fingers on the
interlock meet the valve handle.
4. Rotate the valve fully to the left (90°) using a gentle action, feeling for
any unusual resistance.

Caution. If resistance is felt, the probe cup may have slipped out from the
end of the probe and be fouling the lock. To prevent damage to the cup,
probe or the lock, vent the instrument and withdraw the probe from the
vented system without closing the lock (by springing the fingers of the
interlock system out of the way). Locate and remedy the cause of the
resistance, and pump down after closing the lock securely.

5. Press the VACUUM button on the front of the control unit to stop
pumping of the valve area and then fully withdraw the probe from the
lock.

WARNING. The probe may still be very hot at the tip, from heat
transferred by the hot source.

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 21


Installing and Using Probes
Probe Control and Data Acquisition using the Solids or DCI Probe ____________________________

9. Probe Control and Data


Acquisition using the Solids or DCI
Probe
Data acquisition with the Solids or DCI probe is controlled using Xcalibur.
Before you acquire data, ensure that both Xcalibur and the probe hardware
are set up correctly according to the information supplied in the previous
sections of this manual.
Use the information given in this section in conjunction with your TRACE
MS Getting Started manual, which provides introductory information on
data acquisition using Xcalibur.

Solids Probe Control


The Solids probe temperature is controlled using the Tune window and the
TRACE MS Probe Control page:

Tune Window

Refer to TRACE MS Getting Started for information on opening and


general use of the Tune window.

When the TRACE MS is configured for Solids probe support, the TRACE
MS Controls area of the Tune window displays a Solids probe temperature
text box and readback in its top left corner (see Figure 17). You can use this
text box to set a value for the temperature of the Solids probe (between 20
and 750 °C) in real time. The adjacent readback shows the actual measured
temperature.

Figure 17. TRACE MS Controls displaying Solids probe temperature


and readback

22 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
____________________________ Probe Control and Data Acquisition using the Solids or DCI Probe

Probe Control Page

When Solids probe support is enabled for the TRACE MS, you can use the
Probe Control page in the Instrument Setup window to set temperature
ramping parameters for the Solids probe. To access the Probe Control page,
do the following:
1. Start Xcalibur by double-clicking on the Xcalibur shortcut icon on the
Windows desktop. Alternatively, click on the Start button in the
Windows Taskbar and choose Programs I Xcalibur I Xcalibur.
2. To open the Instrument Setup window, click on the Instrument Setup
button on the Xcalibur Home page, or choose GoTo I Instrument
Setup.
3. To display the Probe Control page, click on the TRACE MS button in
the Viewbar of the Instrument Setup window, then click on the Probe
Control tab (see Figure 18).

Note. The Probe Control page only displays for the TRACE MS method
editor within Instrument Setup when Xcalibur is configured for probe
support.

Figure 18. The TRACE MS Probe Control page in Instrument Setup

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 23


Installing and Using Probes
Probe Control and Data Acquisition using the Solids or DCI Probe ____________________________

When the Solids probe is configured, the Probe Control page displays the
Set Solids Probe control group box (Figure 18). This group box contains a
ramp table for setting the temperature ramping parameters and also displays
a graphical representation of the ramp settings. You can enter values in the
ramp table to set up a ramp that defines the Temperature (°C) of the probe
against Time (min). This allows you to control the temperature of the Solids
probe during an acquisition.
The ramp table allows you to set up to five ramps. For each ramp you can
define a start Temperature (°C), a Time (min) during which the probe will
be held at that temperature, and a Rate (°C/min) at which the probe will be
heated to reach the start Temperature of the next defined ramp.
The ramp display graphically depicts the temperature ramp settings. The
number that appears on the right-hand side of the graph’s Time axis (x-axis)
is equivalent to the overall run time.
You can use the File I Save command to save any set ramping parameters
as part of your method.
When you have set ramping parameters for an acquisition, refer to TRACE
MS Getting Started for further information relating to setting up and
running your experiment.

DCI Probe Control


The DCI probe current is controlled using the Tune window and the TRACE
MS Probe Control page:

Tune Window

Refer to TRACE MS Getting Started for information on opening and


general use of the Tune window.

When the TRACE MS is configured for DCI probe support, the TRACE MS
Controls area of the Tune window displays a DCI probe current text box and
readback in its top left corner (see Figure 19). You can use this text box to
set a value for the current of the DCI probe (between 0 and 1500 mA) in real
time. The adjacent readback shows the actual measured temperature.

24 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
____________________________ Probe Control and Data Acquisition using the Solids or DCI Probe

Figure 19. TRACE MS Controls displaying DCI probe current and


readback

Probe Control Page

When DCI probe support is enabled for the TRACE MS, you can use the
Probe Control page in the Instrument Setup window to set current ramping
parameters for the DCI probe. To access the Probe Control page, do the
following:
1. Start Xcalibur by double-clicking on the Xcalibur shortcut icon on the
Windows desktop. Alternatively, click on the Start button in the
Windows Taskbar and choose Programs I Xcalibur I Xcalibur.
2. To open the Instrument Setup window, click on the Instrument Setup
button on the Xcalibur Home page, or choose GoTo I Instrument
Setup.
3. To display the Probe Control page, click on the TRACE MS button in
the Viewbar of the Instrument Setup window, then click on the Probe
Control tab (see Figure 20).

Note. The Probe Control page only displays for the TRACE MS method
editor within Instrument Setup when Xcalibur is configured for probe
support.

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 25


Installing and Using Probes
Probe Control and Data Acquisition using the Solids or DCI Probe ____________________________

Figure 20. The TRACE MS Probe Control page in Instrument Setup

When the DCI probe is configured, the Probe Control page displays the Set
DCI Control Ramp group box (Figure 20). This group box contains a ramp
table for setting the current ramping parameters and also displays a
graphical representation of the current ramp settings. You can enter values
in the ramp table to set up a ramp that defines the Current (mA) at the probe
filament against Time (min). This allows you to control the current on the
DCI probe filament during an acquisition.
The ramp table allows you to set up to five ramps. For each ramp you can
define a start Current (mA), a Time (min) during which the probe filament
will be held at that current, and a Rate (mA/min) at which current will be
passed through the probe to reach the start Current of the next defined ramp.
The ramp display graphically depicts the current ramp settings. The number
that appears on the right-hand side of the graph’s Time axis (x-axis) is
equivalent to the overall run time.
You can use the File I Save command to save any set ramping parameters
as part of your method.
When you have set ramping parameters for an acquisition, refer to TRACE
MS Getting Started for further information relating to setting up and
running your experiment.

26 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
___________________________________________________________________ Troubleshooting

10. Troubleshooting

Symptom Likely Cause Remedy


TRACE MS fails to achieve The probe lock is not closed. Check and close
vacuum.

The GC interface is leaking. Check the GC column has


been installed properly.

Check the ferrules on the GC


interface.
The probe source is not Re-insert the probe.
inserted properly.
The seal on the probe lock is Check and replace, if
damaged. necessary.

The CI gas pressure is too Reduce the gas pressure.


high.

TRACE MS vents during You are not correctly following See the section Inserting the
insertion of probe. the insertion procedure. Probe on page 18 for details.

Rotary pump is not working See the user documentation


properly (probably a blown supplied with the rotary pump.
fuse).
One or both of the probe lock Check and replace if
O-rings are faulty. necessary.
Solids probe will not cool down. No water supply to Solids Check water supply. Turn on.
probe.
Solids probe readback Probe cable disconnected. Check the cable connection.
temperature continually reads
maximum (750 °C).
Source problems. Probe not inserted fully. See the section Inserting the
Probe on page 18 for details.

Note. All troubleshooting tips for standard EI and CI sources also apply to
probes. See your Hardware Manual for details.

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 27


Installing and Using Probes
Solids and DCI Probes Parts List ______________________________________________________

11. Solids and DCI Probes Parts List

Source and Probe Lock Assembly

Part Number Description


C692A Insertion Lock Assembly
C890A Insertion Lock Spares Kit
5314013 M3×12 mm Long CH HD ST STL Screw
5314018 M3×16 mm Long CH HD ST STL Screw
5711013 O-Ring BS013 Viton
5711018 O-Ring BS011 Viton
5711035 O-Ring BS018 Viton
C851M Insertion Lock Bush
6366308 E-Type Clip 9.5
7024602 Compression Spring
C713A Source Sub-Assembly (Solids Probe)
C030A Filament Assembly
C046M Spacer (3.5 mm thick)
C119M Focus Plate
C306A Source Guide Plate Sub-Assembly
C309M Connection Segment
C318M Magnet Housing (top)
C319M Magnet Housing (filament)
C711A Probe Source Mounting Assembly
1150705 M2 Flat Washer
5312006 M2×6 mm Long CH HD ST STL Screw
5312012 M2×12 mm Long CH HD ST STL Screw
5316005 M1.6×5 mm Long CH HD ST STL Screw
5316033 M1.6×3 mm Long CH HD ST STL Screw
5321011 M1.6 ST STL Nut

28 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________


Installing and Using Probes
______________________________________________________ Solids and DCI Probes Parts List

Part Number Description


C037A Source Heater Assembly
C308M Gas Inlet Tube
C320M Gas Inlet Tube
C589M Mounting Plate
C590M Trap Plate
C591M Trap Insulator
C698A Ion Block Sub-Assembly (probe)
C712M Source Extraction Plate (probe)
TTDC001 Thermocouple Assembly
TMAG051 Source Magnet
TSLI050 Source Lens Insulator

O-ring BS013 viton


part no. 5711013

M3 x 16LG CH HD ST STL
part no. 5314018

O-ring BS011 viton


part no. 5711018

Insertion lock bush


Insertion lock shaft seal part no.C851M
part no. M401006A O-ring BS018 viton
part no. 5711035

Figure 21. Cross-section of probe lock

Note. Parts M401006A, 5711035, 5711018, 5711013 and C851A are all
part of the Insertion lock spares kit which has a part number of C890A.

_________________Finnigan TRACE MS Solids & DCI Probe Manual___________________ 29


Installing and Using Probes
Solids and DCI Probes Parts List ______________________________________________________

Solids Probe Assembly

Part Number Description


ML10-005BD1 Sample Cup Grip
TPRB057 Probe Tip - Earthed Source
TPRB058 Probe Sample Holder (deep)
TPRB059 Probe Sample Holder (shallow)
TPRC001 Water-Cooled Probe Cable Assembly

DCI Probe Assembly

Part Number Description


TPRB009 DCI Probe Tip Assembly
TPRC002 Probe Cable Assembly

Rotary Pump and Control Unit

Part Number Description


TRPK001 E2M1.5 Rotary Pump 240 V
TRPK001C2 E2M1.5 Rotary Pump 110 V
5560010 Rotary Pump Oil - Ultragrade 19
PDM00117 T10 A fuse for 110 V Rotary Pump (20 mm slow blow
fuse)
PDM00118 T6.3 A fuse for 230-240 V Rotary Pump (20 mm slow
blow fuse)

30 __________________ Finnigan TRACE MS Solids & DCI Probe Manual ________________