7168 2577 PDF
7168 2577 PDF
7168 2577 PDF
Hardware Guide
Release History
Any comments about the documentation for this product should be addressed to:
User Assistance
PerkinElmer, Inc.
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.
Notices
The information contained in this document is subject to change without notice.
Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no
warranty of any kind with regard to this document, including, but not limited to, the
implied warranties of merchantability and fitness for a particular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential
damages in connection with furnishing, performance or use of this material.
Copyright Information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this publication may be reproduced in any form
whatsoever or translated into any language without the prior, written permission of
PerkinElmer, Inc.
Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically marked
as such, are protected by law.
Contents
3
Clarus 600/560 D MS Hardware Guide
Printers................................................................................................... 38
Pre-Installation Checklist.............................................................................. 39
Introduction ...................................................................................... 41
Preface .......................................................................................................... 43
System Overview................................................................................... 43
Summary of this Guide.......................................................................... 44
Related Documentation ......................................................................... 44
About Part Numbers Listed in this Manual ........................................... 45
Maintenance ...................................................................................... 73
Overview ...................................................................................................... 75
Typical Overall Maintenance Schedule........................................................ 77
Daily ...................................................................................................... 77
Weekly................................................................................................... 77
Monthly ................................................................................................. 78
Every Six Months .................................................................................. 78
Yearly .................................................................................................... 78
4
Contents
5
Clarus 600/560 D MS Hardware Guide
6
Warnings and
Safety Information 1
Warnings and Safety Information
All eight digit numbers are PerkinElmer part numbers unless stated otherwise.
Three terms, in the following standard formats, are also used to highlight special
circumstances and warnings.
NOTE: A note indicates additional, significant information that is provided with some
procedures.
Terminology
Caution
We use the term CAUTION to inform you about situations that could
CAUTION result in serious damage to the instrument or other equipment. Details
about these circumstances are in a box like this one.
9
Clarus 600/560 D MS Hardware Guide
D Caution (Achtung)
Bedeutet, daß die genannte Anleitung genau befolgt werden muß, um
einen Geräteschaden zu vermeiden.
DK Caution (Bemærk)
Dette betyder, at den nævnte vejledning skal overholdes nøje for at
undgå en beskadigelse af apparatet.
Caution (Advertencia)
E Utilizamos el término CAUTION (ADVERTENCIA) para advertir
sobre situaciones que pueden provocar averías graves en este equipo o
en otros. En recuadros éste se proporciona información sobre este tipo
de circunstancias.
F Caution (Attention)
Nous utilisons le terme CAUTION (ATTENTION) pour signaler les
situations susceptibles de provoquer de graves détériorations de
l'instrument ou d'autre matériel. Les détails sur ces circonstances
figurent dans un encadré semblable à celui-ci.
I Caution (Attenzione)
Con il termine CAUTION (ATTENZIONE) vengono segnalate
situazioni che potrebbero arrecare gravi danni allo strumento o ad
altra apparecchiatura. Troverete informazioni su tali circostanze in un
riquadro come questo.
NL Caution (Opgelet)
Betekent dat de genoemde handleiding nauwkeurig moet worden
opgevolgd, om beschadiging van het instrument te voorkomen.
P Caution (Atenção)
Significa que a instrução referida tem de ser respeitada para evitar a
danificação do aparelho.
Warning
We use the term WARNING to inform you about situations that could
result in personal injury to yourself or other persons. Details about
these circumstances are in a box like this one.
WARNING
10
Warnings and Safety Information
D Warning (Warnung)
Bedeutet, daß es bei Nichtbeachten der genannten Anweisung zu einer
Verletzung des Benutzers kommen kann
DK Warning (Advarsel)
Betyder, at brugeren kan blive kvæstet, hvis anvisningen ikke
overholdes.
Warning (Peligro)
E Utilizamos el término WARNING (PELIGRO) para informarle sobre
situaciones que pueden provocar daños personales a usted o a otras
personas. En los recuadros como éste se proporciona información
sobre este tipo de circunstancias.
F Warning (Danger)
Nous utilisons la formule WARNING (DANGER) pour avertir des
situations pouvant occasionner des dommages corporels à l'utilisateur
ou à d'autres personnes. Les détails sur ces circonstances sont données
dans un encadré semblable à celui-ci.
I Warning (Pericolo)
Con il termine WARNING (PERICOLO) vengono segnalate situazioni
che potrebbero provocare incidenti alle persone. Troverete
informazioni su tali circostanze in un riquadro come questo.
NL Warning (Waarschuwing)
Betekent dat, wanneer de genoemde aanwijzing niet in acht wordt
genomen, dit kan leiden tot verwondingen van de gebruiker.
P Warning (Aviso)
Significa que a não observância da instrução referida poderá causar
um ferimento ao usuário.
11
Clarus 600/560 D MS Hardware Guide
Customer Service
This instrument is manufactured by:
PerkinElmer Inc.
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.
12
Warnings and Safety Information
Regulatory Information
United States (FCC)
This equipment has been tested and found to comply with the limits for a Class A
digital device, pursuant to part 15 of the FCC Rules. These limits are designed to
provide reasonable protection against harmful interference when the equipment is
operated in a commercial environment. This equipment generates, uses, and can
radiate radio frequency energy and, if not installed and used in accordance with
the instruction manual, may cause harmful interference to radio communications.
Operation of this equipment in a residential area is likely to cause harmful
interference in which user will be required to correct the interference at his own
expense.
NOTE: Changes or modifications not expressly approved by PerkinElmer could cause the
instrument to violate FCC (U.S. Federal Communications Commission) emission
regulations, and because of this violation could void the user’s authority to operate
this equipment.
Europe
13
Clarus 600 GC-MS Hardware Guide
Alternating current.
14
Warnings and Safety Information
Clarus 600
Clarus 600 Mass Spectrom eter
Mass Spectrometer
15
Clarus 600/560 D MS Hardware Guide
Mass Spectrometer
GC Air
Interface Vents PC
Ethernet
Connection
Mass Spectrometer
ETHERNET
Processor
FCC Compliance
Reset
This device complies with Part 15 of the FCC Rules.
Operation is subject to the following two conditions:
S1 Switch
1) this device may not cause harmful interference, and
2) this device must accept any interference received,
Warning
Disconnect AC power cord from oulet Disconnect AC power cord from oulet
before removing any cover or parts.
before removing any cover or parts. Do not operate the instrument with any
cover or parts removed.
Air
Caution Intakes
Do not restrict air intake or exhaust.
Air
Exhaust
ROTARY PUMP
Caution
This unit contains protective circuitry.
15 psi
MAX
5 psi
(103 kPa) (35 kPa)
MAX
50 psi
(345 kPa)
MAX
! Contact PerkinElmer qualified service
personnel before performing any
AC line tests
Caution
This unit contains protective circuitry.
Contact PerkinElmer qualified service
personnel before performing any
AC line tests.
16
Warnings and Safety Information
PerkinElmer
precisely.
Shelton, CT 06484 USA
Clarus 560 D
Mass Spectrometer
Part No. Nx xx xxx x
GC Air
Interface Vents PC
Ethernet Serial No. Xxx xx xx
Connection
FCC Compliance
This devi ce compli es with Part 15 of the FCC Rules.
Operation is subject to the follow ing tw o conditions:
1) this device may not cause harmful interference, and
2) this device must accept any interference r eceived, Processor
including interference that may cause undesi red
operation. FCC Compliance
Reset
S1 Switch
Warning Warning
Disc onnect AC power cord from oulet
before removing any c over or parts .
Do not opera te the instrument with any
!
Caution
cover or parts removed.
Air
Caution Intakes
D o not r estrict air in take o r exhaust.
Air
Exhaust
120 VAC ~ 50/60Hz
ROTA RY PU MP
230 VAC ~ 50/60Hz
MAX POWER 1000 VA
Warning POWER IN EN 55011-Class A, Group 1
!
REMOVE VENT LINE BLANKING CAP
AT INSTALLATION. 2
On/Off Switch
!
Caution
Caution
This unit contains protective circuitry.
Contact PerkinElmer qualified service
personnel before performing any
AC line tests.
17
Clarus 600/560 D MS Hardware Guide
WARNING
WARNING
Generic Warnings
Before installing or operating the MS, read the following topics concerning hazards
and potential hazards. Ensure that anyone involved with installation and/or operation
of the MS is knowledgeable in both general safety practices for the laboratory and
safety practices for this instrument. Get advice from your safety engineer, industrial
hygienist, environmental engineer, or safety manager before you install or use this
instrument.
18
Warnings and Safety Information
Never operate the mass spectrometer with any covers or parts removed.
WARNING
Ensure that the power cord is correctly wired and that the ground leads of all
electrical units (for example, recorders, integrators) are connected together via the
19
Clarus 600/560 D MS Hardware Guide
circuit ground to earth. Use only three-prong outlets with common earth ground
connections.
• Servicing of electrical components within the mass spectrometer should be
performed only by a PerkinElmer Service Representative or similarly trained
and authorized person.
• Servicing of the incoming AC power line components in your laboratory
should be performed only by a licensed electrician.
WARNING
WARNING
20
Warnings and Safety Information
Decontamination
Customers wishing to return instrumentation and/or associated materials to
PerkinElmer for repair, maintenance, warranty or trade-in purposes are
advised that all returned goods must be certified as clean and free from
contamination.
http://las.perkinelmer.com/OneSource/decontamination.htm
If you do not have access to the internet and are located in the U.S., call toll free at
1-800-762-4000 or (+1) 203-925-4602, 8:30 a.m. – 7 p.m. EST and speak to
Customer Support.
If you are located outside of the United States or Canada, please call your local
PerkinElmer sales office for more information.
21
Clarus 600/560 D MS Hardware Guide
Compressed Gases
Avoid banging the valves, and ensure that the correct valves and gauges are
installed. It is recommended that gas cylinders be stored and placed outside the
laboratory and connected to the instrument through specially cleaned copper tubing.
Take care not to kink or stress the gas tubing. For safety, cylinders must be firmly
clamped in an upright position.
Ensure that all hydrogen line couplings are leak-free and do not allow hydrogen to
vent within the oven.
Ventilation
22
Warnings and Safety Information
Heated Zones
WARNING
Heated zones should be treated with caution, for example, the transfer line, injector
caps, and detectors. In addition, the detector cover may get hot, especially if flame
ionization detectors are operated at high temperatures. As a general rule, allow
heated zones to cool before attempting to work in the GC oven, on the transfer line,
on an injector, around the detector areas or inside the mass spectrometer manifold.
Cooling of the transfer line may require a wait of ½ to 1 hour.
23
Clarus 600/560 D MS Hardware Guide
Hazardous gas vapors. When using ammonia gas while running in the
chemical ionization (CI) mode, it is necessary to vent the mass
spectrometer effluent from the forepump exhaust into a fume hood or
outside the building.
WARNING
Hazardous Chemicals
Be aware that the chemicals that you use in conjunction with the mass spectrometer
may be hazardous. Do not store, handle, or work with any chemicals or hazardous
24
Warnings and Safety Information
materials unless you have received appropriate safety training and have read and
understood all related Material Safety Data Sheets (MSDS). MSDSs give
information on physical characteristics, precautions, first aid, spill clean up and
disposal procedures. Familiarize yourself with the information and precautions
contained in these documents before attempting to store, use or dispose of the
reagents. Comply with all federal, state, and local laws related to chemical storage,
handling and disposal.
You must work under a suitable hood when handling and mixing certain chemicals.
The room in which you work must have proper ventilation and a waste collection
system. Always wear appropriate safety attire (full-length laboratory coat, protective
glasses, gloves etc.) as indicated on Material Safety Data Sheets.
When using toxic samples, the mechanical pump oil is toxic waste.
WARNING
25
Clarus 600/560 D MS Hardware Guide
26
Warnings and Safety Information
27
Clarus 600/560 D MS Hardware Guide
Storage Conditions
The mass spectrometer may be stored under the following conditions:
28
Warnings and Safety Information
Your laboratory should have all equipment ordinarily required for the safety of
individuals working with chemicals (fire extinguishers, first-aid equipment, safety
shower and eye-wash fountain, spill cleanup equipment, etc.).
29
Clarus 600/560 D MS Hardware Guide
or
A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that
the product is covered by the Waste Electrical and Electronic Equipment (WEEE)
Directive and is not to be disposed of as unsorted municipal waste. Any products
marked with this symbol must be collected separately, according to the regulatory
guidelines in your area.
The objectives of this program are to preserve, protect and improve the quality of
the environment, protect human health, and utilize natural resources prudently and
rationally. Specific treatment of WEEE is indispensable in order to avoid the
dispersion of pollutants into the recycled material or waste stream. Such treatment is
the most effective means of protecting the customer’s environment.
Requirements for waste collection, reuse, recycling, and recovery programs vary by
regulatory authority at your location. Contact your local responsible body (e.g., your
laboratory manager) or authorized representative for information regarding
applicable disposal regulations. Contact PerkinElmer at the web site listed below for
information specific to PerkinElmer products.
Web address:
http://las.perkinelmer.com/OneSource/Environmental-directives.htm
For Customer Care telephone numbers select “Contact us” on the web page.
Products from other manufacturers may also form a part of your PerkinElmer
system. These other producers are directly responsible for the collection and
processing of their own waste products under the terms of the WEEE Directive.
Please contact these producers directly before discarding any of their products.
Consult the PerkinElmer web site (above) for producer names and web
addresses.
30
Warnings and Safety Information
Pre-Installation Requirements
Laboratory Space Requirements
Size Weight
Forepump 30.5 cm (12 in.) wide x 44 cm (17.3 in.) high 25.9 kg (57 lb)
x 72 cm (28.4 in.) deep.
Autosampler Tower 13 cm (5 in.) wide x 36 cm (14 in.) high x 24 4.5 kg (10 lb)
cm (9.5 in.) deep
Physical Single unit for use on standard laboratory bench that can be interfaced to a computer
Configuration and printer.
Bench Space The laboratory bench should be sturdy enough to support the full weight of the GC/MS
as well as additional equipment (for example, computer and/or printer). Expect the
total weight of the GC/MS and accessory equipment to weigh at least 159 kg (350 lb).
Allow a minimum clearance of 15 cm (6 in.) on each side, 22.9 cm (9 in.) at the rear,
and 137.2 cm (54 in.) at the top of the GC/MS. If this is not possible, install the
GC/MS on a bench that has wheels. The bench requires an area underneath for the
forepump.
Do not position the Clarus 600 MS so that it is difficult to operate the
AC power on/off switch on the lower left side of the instrument in case of a
malfunction of the instrument. For the Clarus 650 D the AC power on/off switch on
the back of the instrument.
Peripherals, Printers Allow at least 94 cm (36 in.) on either side of the instrument to accommodate
etc. additional equipment (for example, the computer).
31
Warnings and Safety Information
Environmental Requirements
Pollution Degree This instrument will operate safely in environments that contain
non-conductive foreign matter up to Pollution Degree 2 as
defined in EN/IEC 61010-1.
32
Clarus 600 GC-MS User’s Guide
Power Requirements
Clarus MS All electrical supplies must be smooth, clean, and free of line transients
greater than 40 V peak to peak, and must meet and remain within the
following tolerances:
120 VAC ±10 % @ 50/60 Hz ±1 % 1000 VA maximum
230 VAC ±10 % @ 50/60 Hz ±1 % 1000 VA maximum
Add 100 VA for the computer and 108 VA for a printer.
Clarus GC All electrical supplies must be smooth, clean, and free of line transients
greater than 40 V peak to peak, and must meet and remain within the
following tolerances:
For GC with slow heating rate as standard;
120 VAC ± 10% @ 50/60 Hz ± 1% @ 20 Amps, 2400 VA maximum
230 VAC ± 10% @ 50/60 Hz ± 1% @ 10 Amps, 2400 VA maximum
33
Clarus 600/560 D MS Hardware Guide
Power Outlets Clarus MS: A minimum requirement of a power line separate from the
GC at 15 amps or greater.
Clarus GC: A minimum of one dedicated 120 VAC outlet at 20 A or
one 230 VAC outlet at 10 A (minimum) is required for the Standard
GC. When the optional oven heater is ordered, the outlets will be as
indicated above.
34
Warnings and Safety Information
Safety Requirements
Gas Delivery Copper tubing that is free of grease, oil and organic material must
Lines always be used with the Clarus 600 MS on all gas lines, except
ammonia reagent gas. Ammonia reagent gas requires stainless steel.
Solvent-washed copper tubing must be used to avoid contamination
of the Gas Chromatograph. Suitable solvents are acetone or
dichloromethane (do not use if negative chemical ionization is
planned) followed by methanol. Clean helium or nitrogen should be
used to blow any residual solvent from the tubing. Cap all unused
tubing.
Care must be taken not to kink or overstress the gas delivery lines.
Strain relief consisting of two one inch coils of tubing should be
installed at every gas line connection.
Gas Cylinders All gas cylinders should be firmly clamped to a suitable surface.
Hydrogen Ensure that all hydrogen lines and connections are leak-free. When
using a hydrogen tank, install an in-line hydrogen snubber (part
number 00090038) between the tank regulator and the delivery
tubing.
35
Clarus 600/560 D MS Hardware Guide
Gas Requirements
Carrier gases used with the mass spectrometer require a minimum purity of
99.999%. Gas cylinders should be located outside of the laboratory whenever
possible, and should always be stored and operated in the vertical position.
For all gases delivered to the mass spectrometer, always use copper tubing
CAUTION that is free of grease, oil, and organic material. If in doubt about the
condition of your tubing, clean it before use.
Gases
GC/MS Carrier Minimum purity of 99.999% for helium or hydrogen. Carrier gas tubing
Gases: should be ultra-clean.
A number 1A (200 ft3) gas cylinder should be used for all carrier gases with a
Helium high-purity, stainless-steel diaphragm, two-stage regulator. Filter through a
moisture filter and/or hydrocarbon trap and de-oxo filter designed for MS.
Gas delivery pressure to the GC should be 70 – 100 psi (483 – 689 kPa). Do
not exceed 100 psi (689 kPa) on the carrier gas inlet.
Reagent Gases: Minimum purity of 99.999% for methane, minimum purity of 99.98% for
isobutane, minimum purity of 99.998% for ammonia. Carrier gas tubing
should be ultra-clean.
The gas delivery pressure required is 15 psi (103 kPa) to the bulkhead fitting
(1/8 in. Swagelok) on the mass spectrometer.
Ammonia If ammonia is used for chemical ionization, all fittings and tubing must be
stainless steel to avoid corrosion. A single-stage regulator is required for
ammonia, rated for corrosive service. Also, the forepump must be vented to a
fume hood or outside the building.
Methane and A high-purity, stainless-steel diaphragm, two-stage regulator is required for
Isobutane methane and isobutane with a final delivery pressure of 15 psi (103 kPa).
Clean tubing must be used. It must be solvent-washed and nitrogen-dried. The
bulkhead connector at the rear of the instrument is a 1/8 in. Swagelok fitting.
The use of commercial gas purifiers for reagent gas is recommended.
36
Warnings and Safety Information
PC Requirements
The TurboMass software is installed at PerkinElmer prior to shipment and tested
using the following minimum PC system specifications. If you need to reinstall the
software, verify that the PC meets the following minimum requirements:
• Dell OptiPlex 745, GX620, GC270, or GX 280
• Intel® Pentium processor
• 512 MB of Random Access Memory (RAM)
• High Color (16 bit) at 1024 x 768 SVGA
• Hard disk with 2.0 GB free space
• 8x speed CD-ROM drive
• 1 RS-232 port
• 2 RJ-45 10/100Base-T ports
• A keyboard and PS/2®-style mouse
Operating System
Windows XP SP2
37
Clarus 600/560 D MS Hardware Guide
Software
TurboMass Software.
Printers
• HP LaserJet 4200 Printer Series (HP 4200, 4210, and 4250)
• HP DeskJet 5650 Color InkJet Printer
NOTE: Using any printers other than the ones recommended above may not correctly
display the Communiqué reports.
38
Warnings and Safety Information
Pre-Installation Checklist
CUSTOMER: __________________________________
SPO#: __________________________________
Requirements OK Needs Prior To Installation
Customer Responsibility
Power Requirements
Gas Requirements
Environmental Requirements
Safety Requirements
Preparation of Samples
(Customer Responsibility)
Computer Configuration
Customer Experience
39
Clarus 600/560 D MS Hardware Guide
40
Introduction 2
Introduction
Preface
The Clarus MS is a benchtop mass spectrometer designed with the user in mind. The
small profile of combination Gas Chromatograph and Mass Spectrometer (GC/MS)
allows it to fit on a standard six foot long laboratory bench. Sophisticated software
controls the GC/MS from a Windows XP SP2 computer.
System Overview
The system consists of:
• Clarus GC.
• Clarus MS.
• Computer.
• TurboMass Software.
• Foreline Pump.
43
Introduction
Chapter 2: Introduction
Provides an instrument overview and the references to related
documentation.
Chapter 4: Maintenance
Contains preventive and routine maintenance procedures that
typical users can perform.
Chapter 5: Troubleshooting
Provides helpful troubleshooting tips and a table to help you
identify and solve typical problems.
Related Documentation
The Clarus 600/560 D family of manuals includes the following:
• Clarus 600/560 D MS Tutorial (part number 09936769): The tutorial provides
a step-by-step guide to performing a number of tasks using the instruments and
software.
44
Warnings and Safety Information
To place an order for supplies and many replacement parts, request a free
e-essentials catalog, or ask for information:
Telephone:
• U.S. only: Call toll free 1-800-762-4000, 8:30 a.m. to 7 p.m. EST. Your order
will be shipped promptly, usually within 24 hours.
Internet: http://www.perkinelmer.com
45
Clarus 600 MS User’s Guide
46
About the
Clarus 600/560 D System 3
About the Clarus 500 System
49
Clarus 600 MS Hardware Guide
The system consists of two major components: Clarus MS and the Clarus GC. Brief
descriptions of each major component follow.
50
About the Clarus 600/560 D System
Clarus 600/560 D GC
51
Clarus 600 MS Hardware Guide
PPC provides real-time digital readouts to simplify setting carrier gas pressures and
flows.
52
About the Clarus 600/560 D System
Do not use metal capillary columns in the transfer line. They may
CAUTION
electrically short-out the source.
53
Clarus 600 MS Hardware Guide
The reference gas inlet system consists of a glass bulb filled with heptacosa (FC43)
connected to tubing which directs it to the ion source. You can switch the reference
gas solenoid valve on and off and also purge the reference gas lines from the Tune
screen.
Figure 7 and 8 shows the components or assemblies that comprise the Clarus
600/560 D MS with the manual vent switch (Clarus 600 D and Clarus 560 D) or the
CI adjustment valve (Clarus 600 C) configuration (see the following two pages).
54
About the Clarus 600/560 D System
RF Generator
Head Amplifier
Wide
Access Door Range
Gauge
Transfer Line
On/Off Switch
Diffusion Pump
Manual Vent Valve
For Diffusion Pump
Phosphor Plate
Conversion
Dynode
Photomultiplier
Tube
Grounding Plate
Lens 2
Exit Aperture
Lens 1
Analytical Quads
Pre-Quads
Outer
Source
Inner
Source
Figure 7 Components of the Clarus 600/560 D MS and a detail of the ion optics
path (manual vent valve for diffusion pump configuration)
55
Clarus 600 MS Hardware Guide
RF Generator
Reference Gas Vial
Head Amplifier
Wide
Access Door Range
Gauge
Forepump Line
Inner Source
Transfer Line
On/Off Switch
Phosphor Plate
Conversion
Dynode
Photomultiplier
Tube
Grounding Plate
Lens 2
Exit Aperture
Lens 1
Analytical Quads
Pre-Quads
Outer
Source
Inner
Source
Figure 8 Components of the Clarus 600 MS and a detail of the ion optics path
(CI needle valve for large turbo pump configuration)
56
About the Clarus 600/560 D System
57
Clarus 600 MS Hardware Guide
58
About the Clarus 600/560 D System
Vacuum System
The source, ion optics, analyzer, and detector are fitted inside a cast aluminum
chamber. Vacuum is applied to the chamber using a rotary pump and a
turbomolecular pump. The vacuum is monitored through a wide range gauge. The
rotary pump sits on the floor and a turbomolecular high vacuum pump or an air-
cooled oil diffusion pump (Clarus 600 D) is mounted under the ion optics chamber:
Rotary Pump
The Clarus 600 MS has a 3 m3/hr computer controlled mechanical pump. The
turbomolecular or diffusion pump is backed by this direct drive rotary pump. The
rotary vane pump rests on the lab floor and may be positioned beneath the
instrument. Care should be taken to avoid mechanically coupling vibrations from
this pump to the mass spectrometer. Operation and maintenance details about these
pumps can be found in the manuals provided with the pump.
The rotary vane pump (also called the forepump) provides the first level of vacuum
to approximately 2 x 10-3 Torr. The pump has a switchable dual voltage.
59
Clarus 600 MS Hardware Guide
Voltage Selection
Switch Under Cover
Handle
TurboMass
Connection Port
Exhaust Port
Max
On/Off Min
Switch
Gas Ballast
Switch
Mode Selection
Switch Drain Plug
Oil Level
Indicator
Figure 9 The rotary (fore) pump
Connect the rotary pump exhaust to a line vented to the atmosphere outside the
laboratory or use an appropriate exhaust line filter.
The AC line cord for the rotary vane pump must be plugged into the
designated receptacle on the back of the Clarus 600 MS. The pump is
CAUTION controlled by the TurboMass software.
60
About the Clarus 600/560 D System
Turbomolecular Pump
Clarus 600 MS has two turbomolecular pump options in three configurations.
Turbomolecular pumps are high-speed turbines which transport the sample and
carrier gas molecules away from the mass spectrometer.
Clarus 600S - The 75 L/sec turbomolecular pump supports Electron Ionization
operation (EI) and has optional water cooling.
Clarus 600 T – All of the functions and options of the 600 S with a 255 L/sec
turbomolecular pump for higher column flow rates, pump-down time under three
minutes, and lower detection limits
Clarus 600 C - All of the functions and options of the 600 T with positive and
negative Chemical Ionization (CI) operation.
Diffusion Pump
Clarus 600 D and the 560 D MS has an air-cooled oil diffusion pump. This pump is
only available for Electrical Ionization (EI) operation.
Pump fluid is heated in the base of the pump to produce a vapor which passes
through the interior of the jet assembly and emerges from the jets as high-velocity
vapor streams. These streams entrain eluting compounds and carrier gas, condense
on the cooled pump body wall, and drain into the base of the pump for recirculation.
The entrained compounds are transferred to the forepump.
The diffusion pump system has a manual vent switch. This manual vacuum venting
is controlled by a push button toggle switch and a pump temperature sensing
switch. When you push the button in, the vent is opened. When the button is up
(not pushed in), the vent is closed. See the following illustration.
The mass spectrometer's vacuum system is controlled from the Tune page. Be sure that
this is done in accordance with the information provided in your Mass Spectrometry
Hardware Guide. The following procedures describe a Turbomolecular Pump system
and a Diffusion Pump system.
61
Clarus 600 MS Hardware Guide
62
About the Clarus 600/560 D System
63
Clarus 600 MS Hardware Guide
Turbomolecular Pump
Pumping Down a Turbomolecular Pump Vacuum System
2. Select Vent/Vacuum System Off from the Options menu on the Tune
page, and confirm that you want to vent the system.
Diffusion Pump
Pumping Down a Diffusion Pump Vacuum System
64
About the Clarus 600/560 D System
CAUTION The software will not prohibit the use of the system prior to reaching
the desired vacuum. The software will monitor the vacuum gauge
pressure to determine when the system has reached the proper
operating vacuum (5 x 10-5 Torr).
2. Select Vent/Vacuum System Off from the Options menu on the Tune
page, and confirm that you want to vent the system.
The system will start its automatic venting sequence. The software monitors
the temperature of the source and the inlet. When the temperatures of both
of the source and the inlet are less than 100 °C, the software turns off the
diffusion pump heater and starts a 20 minute countdown timer.
During the cooling down period, the countdown timer will display the time
remaining in minutes and seconds. When the count down timer reaches 0,
the backing pump turns off.
Once the backing pump has been turned off, the software will display a
message indicating that the system is now cool enough to vent. The message
also reminds you to turn off the carrier gas.
3. Vent the mass spectrometer by pressing the push-button behind the front
door of the mass spectrometer. It will lock in the pressed-in position and
turn red indicating the vent valve is open.
CAUTION If you try to vent a hot diffusion system, oxidation of the pump oil may
occur and cause oil to enter the analyzer tub which will damage the
mass spectrometer.
65
Clarus 600 MS Hardware Guide
Access Door
Source
The depressed push button vent switch lights when venting is allowed. Before
pressing Pump/Vacuum System On, make sure the vent switch is closed (the
button is out and the light is off)
Never vent when:
• The diffusion pump is hot
• During the 20 minute cool-down period
Always check that the front panel vent button is out and the lamp is off when
starting to pump the system down.
66
About the Clarus 600/560 D System
NOTE: The vent valve will operate if the vent switch is pushed in (on) before the diffusion
pump becomes hot. This includes the first few minutes of Pump/Vacuum System
On. Venting during this period may cause a vacuum fault to occur and risk back
streaming the diffusion oil into the analyzer. It is a good reminder to leave the
instrument front door open whenever the push button switch is pushed in (on).
NOTE: When the diffusion pump is hot, the vent switch is deactivated and will not light
when pushed in (on). Since the vent switch may be left in the depressed position at
any time, you should be careful to avoid closing the instrument door and forgetting
that the push button switch is pushed in. (When the diffusion pump cools, the
pushed in push button switch will light and automatically vent the system).
Vacuum Gauge
The single wide range vacuum gauge monitors the system pressure from atmosphere
down to 10-9 Torr using a combined Pirani/Inverted Magnetron ionization sensor.
Normal operating pressure with 1 mL/min helium for the 255 L/sec turbomolecular
pump is between 9x10-6 Torr and 2x10-5 Torr after pump-down and ion source bake-
out. The 75 L/sec turbomolecular and the diffusion pumps will operate at somewhat
higher pressures, typically below 4x10-5 Torr.
67
Clarus 600 MS Hardware Guide
TurboMass Software
TurboMass software is the user interface of the Clarus system. The following
screens show some examples of how you can control Clarus. Interaction is via the
mouse and keyboard using menu-driven commands. Printing, file management and
other routine procedures are performed using the appropriate Microsoft Windows
modules.
68
Clarus 600 GC-MS User’s Guide
Tune Page
The Tune Page allows you to tune the mass spectrometer, control the gases, set the
GC interface temperature, and monitor the instrument vacuum pressure.
69
Clarus 600 MS Hardware Guide
Analytical Column
The analytical column inside the Clarus GC oven provides the sample separation.
Make sure you select the proper column for your analysis. PerkinElmer offers a
wide range of columns in the Gas Chromatography Column Catalog. The
TurboMass Tutorial provides additional column selection tips.
There are several things to consider when choosing an analytical capillary column:
1. Know the types of samples you will be analyzing. Are they volatile, semi-volatile,
pesticides, solvents, etc?
2. Select a stationary phase based on polarity of the sample. A very general rule in
column selection is that like dissolves like. Column polarity has the greatest effect
on how the column separates the compounds of interest as the sample interacts with
the stationary phase. There are different degrees of polarity from non-polar to very
polar. When compounds are separated primarily on their boiling points the phase is
considered to be non-polar. Polar phases typically separate compounds based on the
chemical interactions between the sample components and the stationary phase.
3. The inside diameter of the capillary column has an effect on the column’s resolving
power and its capacity or concentration range. In general, the larger the inside
diameter of the column, the larger the sample capacity. However, the larger the
inside diameter, the higher the flow necessary to achieve good performance.
4. The next parameter is the phase or film thickness. Film thickness will primarily
affect the retentive character and the capacity of the column. Increasing the film
thickness will cause an increase in the retention of the compounds being analyzed.
Thick film columns are primarily used for extremely volatile compounds. The
thicker phases will retain components longer, allowing them to interact longer with
the stationary phase, thereby increasing the separation of closely eluting compounds.
5. The last variable to consider is column length. The effect of column length on a
separation becomes less important as column length increases. Resolution is a
function of the square root of the column length. An example of this relationship is
that, if you want to double the separation between two peaks without changing the
stationary phase, inside diameter, film thickness, or GC conditions, it would take a
four-fold increase in the column length. A 30 meter column is the most common
length and is usually sufficient for analyzing most samples. Typically, users doing
environmental EPA type analysis will use a 30 meter column for semi-volatile
compounds and 60 to 105 meter columns for volatile compounds.
70
About the Clarus 600/560 D System
Pre-Operational Checklist
This checklist provides you with a list of items to check to make sure everything are
in working order before you begin to use Clarus.
Item OK
Is there a GC method?
Did you check the air/water spectrum on the TurboMass Tune screen?
71
Clarus 600 MS Hardware Guide
72
Maintenance 4
Overview
WARNING
Cleanliness and care are of critical importance whenever internal assemblies are
removed from the instrument.
• Make sure that any required tools or spare parts are close at hand.
• Never touch any internal source parts with your bare fingers.
Clarus 600 MS Hardware Guide
• If nylon or cotton gloves are used, prevent leaving fibers in sensitive areas.
NEVER use rubber gloves.
If a fault occurs soon after repairing or disturbing a particular part of the system,
ensure that this part has been correctly refitted and/or adjusted and that any adjacent
components have not been inadvertently disturbed.
76
Maintenance
Performing maintenance tasks on a routine basis can reduce the overall costs of
operation. If a fault occurs, you can correct it with minimum difficulty.
Exterior surfaces may be cleaned with a soft cloth dampened with a mild detergent
and water solution. Do not use abrasive cleaners or solvents.
Factory trained service personnel can assist in any advanced training needs. All
tasks should be logged into a logbook to keep a record of any problems or trends.
Daily
• Make sure all system components are in working order.
• Check and ensure that there are gas supplies to the GC and to the mass
spectrometer.
Weekly
• Check the tune and mass calibration. Tune if necessary.
• If equipped with a water chiller, check the water level and temperature.
• If using CI, at the end of the day gas ballast the forepump lightly for 20
minutes.
77
Clarus 600 MS Hardware Guide
Monthly
• Clean the fan filters on the rear of Clarus MS.
Yearly
• Check lens 1, lens 2, and analyzer prequadrupole. Clean if dirty.
• Check and clean the forepump inlet filter, gas ballast control, and the motor fan
cover and enclosure.
78
Maintenance
Leak Checking
Checking for leaks is actually checking the integrity of the vacuum system. You
observe masses 4 (helium), 18 (water), 28 (nitrogen), and 32 (oxygen).
2. Set the GC split flow to 50 mL/min by pressing the PSSI injector icon on the
Clarus GC touch screen. On the next screen, press the split flow setpoint and use
the up and down arrow or keypad buttons to set the split flow to
50mL. For example, if the capillary injector is in position 1 and you selected split
flow in the PPC configuration software, the following screen is displayed.
The total flow (split vent + septum purge + column) is displayed in the lower left
of the screen. The split vent flow setpoint is displayed in the setpoint box in the
lower right.
3. Start the TurboMass software by clicking on the Windows Start button at the bottom
left of the screen and selects TurboMass under the
Programs/TurboMass/TurboMass path, or double-click on the TurboMass icon if it
is on your Windows desktop.
79
Clarus 600 MS Hardware Guide
80
Maintenance
9. If the nitrogen and oxygen are larger it indicates an air leak, which could damage
the filament. Immediately click Press for Standby to turn off the filament.
81
Clarus 600 MS Hardware Guide
After determining that no leaks exist and before acquiring data, you may need to
check the mass spectrometer tuning conditions and, if necessary, modify one or
more of the tuning parameters. Clarus MS can be tuned either manually or
automatically from the Tune window.
The left side of the page holds the tuning parameters for a selected region of the
mass spectrometer. You can change the region by selecting an item from the
Window menu, or by pressing one of the buttons on the bottom-left of the Tune
page.
The panel in the top right of the Tune page displays the tune peak information and
instrument pressure information.
The tune peak display is located on the right side of the screen and allows you to
view up to four masses. The corresponding check boxes located above the peaks
allow you to control each peak display. Any one of the tune peaks can be zoomed so
that it occupies the entire tune peak area. When a tune peak has been zoomed, the
82
Maintenance
controls for the mass and span for that peak are displayed at the top of the display
window. This enables you to display the pressure information while having control
over the peak display.
2. Turn on the filament and high voltages by clicking Press for Operate at the
bottom right of the window.
The indicator box turns green to indicate that it is on.
4. Click OK.
83
Clarus 600 MS Hardware Guide
5. Select Reference Gas On from the Gas menu to remove the check mark (9),
or click to set it in the up position.
6. Save this new Tune of the instrument by selecting Save As from the File menu
and entering a name for this tune in the File name field.
A way to keep track of the tunes is to use dates for the file names.
7. Click Save.
Your mass spectrometer is now Tuned.
84
Maintenance
To prepare Clarus MS for hardware maintenance, there are several steps that are
common and precursory to all maintenance procedures. They are as follows:
85
Clarus 600 MS Hardware Guide
The transfer line, GC oven, and source are HOT. Touching them can
cause serious burns. To prevent personal injury, wait until the oven and
transfer line reach the lower setpoint temperature before touching
them. Only grab and hold the source by its handle.
WARNING
1. On the left side of the Tune page enter 20 in the Inlet Line Temperature to
cool the GC Interface (transfer line).
If the Clarus GC is off, then the PPC control is off and no gas is
CAUTION flowing through the system.
3. On the Tune page, set the source temperature by entering 20 in the Source
Temp field.
4. Allow the transfer line, column oven, and source to cool before touching them.
Remember, the transfer line was heated and it may take at least
10 to 20 minutes to cool.
WARNING
86
Maintenance
1. Once both the Inlet Line and Source temperatures have dropped below 100 °C,
select Vent/Vacuum System Off from the Options menu.
The Vent Pump dialog appears. All pumps are turned off.
2. Click OK.
The gauge goes to ZERO after the turbopump reaches 50 % speed and the vent
valve is opened.
NOTE: Mass Spectrometer venting may take several minutes depending on the helium flow
and/or vent gas flow into the manifold.
Turn off helium carrier gas flow to the MS if you do not have a purge
flow of high purity nitrogen.
CAUTION
Do not allow the vented mass spectrometer to fill with helium for more
than 5 hours.
Failure to do so can damage the photomultiplier detector and require
a service call not covered by warrantee or contract.
Set all temperatures to ambient. Once the GC column oven, source, and transfer line
are cool you may then turn off the GC carrier gas.
87
Clarus 600 MS Hardware Guide
Changing a Column
Removing a Column
1. Prepare the mass spectrometer for hardware maintenance (see Preparing
Clarus 600/560 D MS for
Hardware Maintenance on page 85).
2. Using a ¼-inch open-end wrench, loosen the 1/16-inch column nut attached to
the injector fitting and slide the column tubing completely from the injector
and column nut.
88
Maintenance
3. Using a ¼-inch open-end wrench, loosen the 1/16-inch column nut on the
transfer line. Slide the column tubing completely from the transfer line and
column nut. Remove the column from the GC oven.
Remove Column
Injector
Remove Column
4. Open the Clarus 600 MS access door, loosen and remove the two black
thumbscrews, hold the source by the handle, and pull it out.
89
Clarus 600 MS Hardware Guide
5. Place the source on a clean surface. Preferably place the handle end on a flat
surface so that the source stands in an upright position.
Access
Door
Inner Source
Black
Thumbscrews Handle
90
Maintenance
20 cm
Column
91
Clarus 600 MS Hardware Guide
2. Insert a septum, 1/16-inch column nut (part number 09903392), and 1/16-inch
graphite ferrule (0.8-mm i.d. Part Number 0992-0141, or 0.5-mm i.d. Part
Number 0990-3700) over one end of the column as shown in Figure 13 .
1/16-inch
Graphite/Vespel
Ferrule
Column
1/16-inch Column Nut
Septum
Column
NOTE: Verify that the tapered end of the ferrule is facing towards the nut as shown above.
3. Cut about 1 cm (3/8 inch) from the column end using a wafer scribe
(part number N930-1376, pkg. of 10 scribes). Break off the tubing at the score
mark so that the break is clean and square. Examine the cut with a magnifying
glass and compare it to the examples shown in Figure 14.
Good Cut
Bad Cuts
92
Maintenance
1/8-inch Capillary
Injector Fitting
93
Clarus 600 MS Hardware Guide
2. Slide the septum, 1/16-inch column nut and 1/16-inch graphite/Vespel ferrule
over the end of the column.
Column
1/16-inch Column
Graphite/Vespel
Ferrule Septum
1/16-inch Column Nut
Figure 17 Inserting a septum, column nut and ferrule on a column
3. Slide the septum, column nut, and ferrule along the column to the position
shown below. Score and break 1.0 cm off the end of the column. Wipe the
column with a methanol dampened lab tissue (for example, a Kimwipe).
94
Maintenance
Use glove.
1. Slide the septum, column nut,
and ferrule to this position.
1 cm
Column
4. Carefully insert the end of the column through the transfer line and into the
mass spectrometer source until it is positioned midway between the hole and
the wall on the right side of the source. See Figure 19.
5. Hold the column in this position as you slide the column nut and ferrule to the
transfer line and tighten the nut fingertight. Slide the septum until it is flush
against the rear of the column nut. See Figure 20.
This marks the position of the column end in the source.
NOTE: Finger tight means just tight enough to hold the column in place so that you are still
able to move the column slightly if necessary to reposition it.
95
Clarus 600 MS Hardware Guide
Clarus 600
Mass Spectrometer
Clarus 600
Gas Chromatograph
Transfer Line
2 mm or midway
between the hole
and the wall
Hole
Column End
Wall
96
Maintenance
Septum
6. Pull the column back until the distance between the back of the nut and septum
is about 10 cm.
To prevent breaking the end off the column, you need to pull the column
CAUTION back to reinstall the source in the mass spectrometer.
97
Clarus 600 MS Hardware Guide
10 20 30 40 50 60 70 8
metric
7. Position the inner source so it aligns with the guide pin, gently insert the source
into the mass spectrometer, and secure it in place with the two black
thumbscrews. Tighten the black thumbscrews until they are fingertight.
Do not overtighten.
Access Ma ssClarus 60
Spec 0
tro me
ter
Door
Inner Source
Black
Thumbscrews Handle
98
Maintenance
8. Carefully slide the column into the transfer line until the septum is flush to the
back of the column nut. To make a leak-free seal, use a ¼-inch wrench to
tighten the column nut ¼ turn past fingertight.
Injector
Slide Column
2. Start the vacuum by selecting Pump from the Options menu on the Tune
window. Monitor the vacuum and search for leaks if necessary.
Refer to the vacuum leak-checking procedure described in Leak Checking on
page 79.
3. Once you have verified that no leaks exist, set the transfer line temperature to
its original value and close the GC oven door to heat the column.
99
Clarus 600 MS Hardware Guide
NOTE: You should check liquid level in the reference gas vial any time you need to remove
the mass spectrometer cover and vent the instrument. Using a tool such as a dental
mirror will help you observe the liquid level in the Reference Gas Vial.
Items Required
• Lint-free, powder-free PVC or polypropylene gloves (Part No. N621-2495).
• Pasteur Pipette or 50 µL syringe.
• Heptacosa (FC43) (Part No. N621-2407).
Make sure to vent the instrument and turn the power off.
WARNING
100
Maintenance
2. With the power off, unplug the source connector for more room to work. Use a
5/32 inch Allen wrench to remove the two allen nuts from the handle. See
following photo.
Source Connector
Allen Nuts
3. With the handle off remove the reference gas vial assembly and bracket out.
See the following figure.
101
Clarus 600 MS Hardware Guide
Figure 24 Removing the reference gas vial from the mass spectrometer
WARNING
4. Loosen the knurled fitting behind the gas vial by ½ turn, and pull out the vial.
A black O-ring may remain in the fitting.
102
Maintenance
Gas Tight
Syringe
Reference
Gas Vial
8. Return the bracket to the proper position and use a 5/32 inch Allen wrench to
retighten the two Allen nuts to the bracket.
9. Replace the top cover and pump the system down to the proper vacuum.
10. From the Gas Menu select the Reference Gas Option from the drop down menu.
Leave the Reference Gas Valve open for 60 minutes with Operate off to pump to
pump out the gas from the bulb before tuning the mass spectrometer.
NOTE: On the Tune Page the Gas drop down the Pump Out Reference Gas choice no
longer works. If you try to have both the Reference Gas On and the Pump Out
Reference Gas options selected you will get an error message. To avoid an error
message make sure to only check Reference Gas On.
103
Clarus 600 MS Hardware Guide
104
Maintenance
Transfer Line
Remove
Column
1/4-inch Nut
Figure 26 Pulling back the transfer line
105
Clarus 600 MS Hardware Guide
5. Loosen the two thumbscrews on the inner source, grab it by its handle, pull it
out of the mass spectrometer and set it on a clean surface.
Access
Door
Inner Source
Black
Thumbscrews Handle
NOTE: For this procedure use the Inner Source Rebuild Kit Part No. E640-0043.
106
Maintenance
Disassembling
1. Prepare a clean, uncluttered work area and place a square of aluminum foil
with the shiny side up. Obtain some clean, small containers (for example, small
beakers) to store the screws and small parts as you remove them.
2. Using a small flat-blade screwdriver, loosen the screw that secures the old
filament assembly to the source. Use tweezers to remove the screw and washer.
Pull out the filament assembly.
Defective
Filament
Assembly
Screw
(P/N E531-4043)
Washer
(P/N E533-1031)
107
Clarus 600 MS Hardware Guide
3. Using a small flat-blade screwdriver, loosen and remove the four screws on the
ion chamber cover plate and remove the cover plate.
4. Using a 2 mm open-end wrench, loosen and remove the nut and washer that
secure the repeller. Then remove the repeller.
5. Using a 2 mm open-end wrench, loosen and remove the nut and washer that
secure the ion trap. Then remove the ion trap.
Clean this
area.
Trap
(P/N E640-1220)
Screw (4)
2 mmSpacer
(P/N E640-1222)
12 mm Spacer
(P/N E640-1221) Clean underside
of Ion Exit Plate. Clean this
(P/N E640-1213) area.
Repeller
(P/N E640-1219)
Clean these
areas.
2 mm Spacer
(P/N E640-1222)
12 mm Spacer
(P/N E640-1221)
6 mm Ceramic Spacer
(P/N E640-1224)
Trap Contact
(P/N E640-1217) 6 mm Ceramic Spacer
(P/N E640-1224)
Washer
Insulator
Nut (P/N E640-1218)
Viton O-Ring
(P/N E571-1061) Repeller Contact
(P/N E640-1216)
Washer
Nut
108
Maintenance
Cleaning
NOTE: You can do the following cleaning method of aluminum oxide paste or use the 6000
or 8000 grade micro mesh to polish the flat surfaces of the parts. For either
cleaning method, the final step you must sonicate the parts in an ultrasonic bath of
methanol for at least five minutes. Dry off the parts using lint-free tissue and/or
clean compressed Nitrogen gas to prevent solvents from drying on these parts and
leaving a residue
1. Mix together aluminum oxide and de-ionized water and a few drops of
methanol to make a watery paste.
2. Dip a wooden-stick cotton swab in the solution and clean the darkened areas on
the source. Work quickly to prevent the mixture from drying on the surface.
Place the cleaned components in de-ionized water prior to rinsing to prevent
drying.
Rinsing
1. Add 50 mL of acetone to a 100 mL beaker, insert the source assembly, repeller,
ion trap, ion chamber plate, and sonicate in an ultrasonic bath for ten minutes.
Do not allow the acetone and methanol to touch the O-ring on the
CAUTION source.
109
Clarus 600 MS Hardware Guide
Source Assembly
50 mL sonocation solution
in 100 mL Beaker
Figure 30 Rinsing the aluminum oxide from the source
5. Dry off the repeller, ion trap, source assembly and ion chamber plate using lint-
free tissue and/or clean compressed Nitrogen gas to prevent solvents from
drying on these parts and leaving a residue.
6. Take the parts amd wrap them in a clean, lint-free cloth and bake them in the
GC oven at about 80 ºC for about fifteen minutes.
Reassembling
1. Insert the ion trap and repeller through the spacer and insulator. Then insert it
into the source.
110
Maintenance
2 mm Spacer 2 mm Spacer
(P/N E640-1222) (P/N E640-1222)
12 mm Spacer 12 mm Spacer
(P/N E640-1221) (P/N E640-1221)
Figure 31 Inserting the ion trap and repeller into the inner source
2. Invert the source and insert a crumpled laboratory wipe into the repeller and
ion trap.
3. Using tweezers, install the remaining ceramic pieces, spacers and nut first on
the ion trap and then on the repeller.
4. Tighten each nut with a 2 mm open-end wrench.
111
Clarus 600 MS Hardware Guide
Nut
(P/N E532-1018)
Washer
(P/N E533-1013)
Nut
(P/N E532-1018)
Trap Contact Washer
(P/N E640-1217) (P/N E533-1013)
Locator
and Clarus 560 D (P/N E640-1218)
6 mm Ceramic Spacer
(P/N E640-1224)
Figure 32 Installing the ceramics, contacts, washers and nuts on the repeller
and ion trap
112
Maintenance
Rhenium
Filament Assembly
(P/N N6470012)
Screw
Washer
Contacts
Figure 33 Replacing the filament assembly
To gain access to the parts on the CI inner source that need cleaning, follow this
procedure.
113
Clarus 600 MS Hardware Guide
Disassembling
1. Prepare a clean, uncluttered work area and place a square of aluminum foil
with the shiny side up. Obtain some small containers (for example, small
beakers) to store the screws and small parts as you remove them.
2. Using a small flat-blade screwdriver, loosen the screw that secures the old
filament assembly to the source. Use tweezers to remove the screw and washer.
Pull out the filament assembly.
Defective
Filament
Assembly
Screw
(P/N E531-4043)
Washer
(P/N E533-1031)
3. Using a small flat-blade screwdriver, loosen and remove the four screws on the
ion chamber cover plate and ion aperture plate, then remove the plates.
114
Maintenance
Screw (1 of 4)
Clean these
areas.
Figure 35 Removing the ion chamber and aperture plates and cleaning the
areas shown
Cleaning
NOTE: You can do the following cleaning method of aluminum oxide paste or use the 6000
or 8000 grade micro mesh to polish the flat surfaces of the parts. For either
cleaning method, the final step you must sonicate the parts in an ultrasonic bath of
methanol for at least five minutes. Dry off the parts using lint-free tissue and/or
clean compressed Nitrogen gas to prevent solvents from drying on these parts and
leaving a residue
115
Clarus 600 MS Hardware Guide
1. Mix together aluminum oxide and de-ionized water and a few drops of
methanol to make a watery paste.
2. Dip a wooden-stick cotton swab in the solution and scrub the darkened areas on
the source. Work quickly to prevent the mixture from drying on the surface.
50 mL sonocation solution
in 100 mL Beaker
Figure 36 Rinsing the aluminum oxide from the source
116
Maintenance
5. Dry off source assembly and plates using lint-free tissue and/or clean
compressed Nitrogen gas to prevent solvents from drying on these parts and
leaving a residue.
6. Take the parts amd wrap them in a clean, lint-free cloth and bake them in the
GC oven at about 80 ºC for about fifteen minutes.
7. Reassemble the ion aperture plate and ion chamber plate on the source.
Screw (1 of 4)
Clean these
areas.
117
Clarus 600 MS Hardware Guide
Rhenium
Filament Assembly
(P/N N6470012)
Screw
Washer
Contacts
Figure 38 Replacing the filament assembly
118
Maintenance
Access
Door
Inner Source
Black
Thumbscrews Handle
2. Insert the inner transfer line tube back in the outer transfer line.
119
Clarus 600 MS Hardware Guide
Transfer Line
Replace
Column
1/4-inch Transfer
Line Nut
1. Start the carrier gas flowing and leak-check the fittings for leaks.
3. Once you have verified that no leaks exist, set the transfer line temperature to
its original value, and close the GC oven door to heat the column.
120
Maintenance
Replacing a Filament
Make sure you are wearing powder-free PVC gloves (Part No. N621-
CAUTION 2495), and that you wipe each part with a methanol dampened
Kimwipe.
1. Prepare a clean, uncluttered work area and place a square of aluminum foil with
the shiny side up.
2. Remove the EI source by following the procedure Removing the Inner Source as
described on page 105.
121
Clarus 600 MS Hardware Guide
Defective
Filament
Assembly
Screw
(P/N E531-4043)
Washer
(P/N E533-1031)
5. Using a 0.8 mm hex wrench, loosen the two screws that secure the contacts to
the filament assembly leads. Remove the two contacts.
122
Maintenance
0.8 mm
Hex Wrench
Contacts
Defective Filiment
Assembly
6. Position the new filament assembly with the filament side up.
7. Insert the contacts on the new filament assembly leads so that they are flush with
the white ceramic and positioned with the hex screw side facing up.
8. Secure the contacts to the filament assembly by tightening the hex screws with a
0.8 mm hex wrench. Tighten firmly but do not overtighten.
123
Clarus 600 MS Hardware Guide
1. Insert Contacts
Contacts (2)
(P/N E640-1215)
2. Secure Contacts
0.8 mm
Hex Wrench
9. Position the new filament assembly so that it faces the source and the white
ceramic rests on the tab.
10. Ensure that the filament coil is aligned with the entrance hole on the inner source
assembly.
124
Maintenance
11. Using a small flat-blade screwdriver, secure the filament assembly in place with
the screw and washer that you previously removed.
Ensure that the filament coil
aligns with the entrance hole.
Filament Coil
New Filament
Tab Assembly
Screw
Washer
Contacts
12. Install the source assembly back into the mass spectrometer by following the
procedure described in Reinstalling the Source on page 119.
125
Clarus 600 MS Hardware Guide
To replace the Photomultiplier head amplifier (Part Number E649-9032), follow this
procedure and refer to Figure 45:
4. Remove the four screws securing the rear panel and remove the rear panel.
5. Remove the two screws on the left side of the top panel and remove the top
panel.
8. Pull off head amplifier board, removing the screw with the ground wire on it.
9. Install a new board, making sure that you do not over-tighten the screw with
the ground wire.
10. Replace the photomultiplier head amplifier board cover, cable connector,
replace the panels, turn on the mass spectrometer, and pump-down the system
to the proper vacuum.
126
Maintenance
Detail of Photomultiplier
Tube Pin Connections
Cover
Ground Cable
Nut
Lock
Washer
127
Clarus 600 MS Hardware Guide
128
Maintenance
Cleaning Materials
When cleaning internal components it is important to maintain the quality of the
surface finish. Deep scratches or pits can cause loss of performance. Where no
specific cleaning procedure is provided, you should use fine abrasives to remove dirt
from metal components. Recommended abrasives are:
• 6000 Grade Micro Mesh (Part No. N930-3420).
• 8000 Grade Micro Mesh (Part No. N930-3421).
• 600 grit aluminum oxide in DI Water with a few drops of methanol to make a
paste
After the components are reassembled, they should be blown with oil-free nitrogen
to remove dust particles.
2. Open the GC oven door and locate the mass spectrometer transfer line.
3. Using a 9/16-inch wrench, loosen the ¼-inch nut on the transfer line.
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Clarus 600 MS Hardware Guide
WARNING
Transfer Line
Remove
Column
1/4-inch Nut
5. Loosen the two thumbscrews on the inner source, grab it by its handle, gently
pull it out of the mass spectrometer, and set it on a clean surface.
130
Maintenance
Access
Door
Inner Source
Black
Thumbscrews Handle
131
Clarus 600 MS Hardware Guide
5. Remove the two screws on the left side of the top panel and remove the top panel.
NOTE:
The rear panel vent fan should NOT be removed
from the instrument. It is removed in this illustration
only to clearly show how to access the PMT Access
Panel. ONLY remove the PMT Access Panel.
Screws (4)
132
Maintenance
2. Using a long flat-blade screwdriver, loosen the two captured screws securing
the photomultiplier tube (PMT) amplifier cover, and remove the cover.
PMT Amp
Cover
Lock
Screw
NOTE:
The rear panel vent fan should NOT be removed
from the instrument. It is removed in this illustration
only to clearly show how to access the PMT Access
Panel. ONLY remove the PMT Access Panel.
3. Using a 4 mm hex wrench, remove the screw securing the PMT amplifier
board-grounding strap.
4. Carefully remove the amplifier board from the PMT by pulling it straight back.
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Clarus 600 MS Hardware Guide
5. Using a 4 mm hex wrench, remove the screws securing the PMT flange to the
vacuum chamber.
7. Carefully remove the PMT. Cover it with a laboratory wipe and place it in a
safe, dark place.
8. Insert a crumpled laboratory wipe into the PMT hole in the vacuum chamber to
prevent particulates from entering the vacuum chamber.
Cover
Ground Cable
Nut
Lock
NOTE: Washer
The rear panel vent fan should NOT be removed
from the instrument. It is removed in this illustration
only to clearly show how to access the PMT Access
Panel. ONLY remove the PMT Access Panel.
134
Maintenance
Make sure to vent the instrument and turn the power off and
unplug the mass spectrometer from the AC power source.
WARNING
1. Disconnect the cables connected to the ion optics assembly and place them to
the side so they will not interfere with the removal of the ion optics assembly.
See the following figure.
2. Disconnect the Reference and CI gas lines from the top of the ion optics
assembly. See the following figure.
REAR VIEW
Reference Gas
CI Gas
RF Generator
Location of Reference Cable
Gas Vial Assembly
Figure 51 Disconnecting cables and tubing from the ion optics assembly
135
Clarus 600 MS Hardware Guide
3. With the power off , unplug the source connector for more room to work. Use a
5/32 inch Allen wrench to remove the two allen nuts from the handle. See
following photo.
Source Connector
Allen Nuts
4. With the handle off remove the reference gas vial assembly and bracket out and
move it out to the side of the instrument. See the following photo.
136
Maintenance
5. Remove the four hex head bolts loosely holding the ion optics assembly to the
vacuum chamber. See the following figure.
6. Grabbing the ion optics assembly by the two handles, carefully lift the ion
optics assembly straight up and away. See the following figure.
Hexagon
Fan Plug Head Bolt (4)
Handle
Handle
Guide Pins
Figure 52 Lifting the ion optics assembly from the vacuum manifold
137
Clarus 600 MS Hardware Guide
7. Place the ion optics assembly on a clean work surface, with the RF box down
and the mass analyzer facing up (see Figure 3).
8. Cover the open vacuum chamber with aluminum foil to prevent particulates
from contaminating the chamber.
Outer Source Prequads
Assembly
of Ion Optics
Assembly
Analytical Quads
138
Maintenance
To replace the thermocouple, follow this procedure and refer to the following figure:
1. Using a small flat-blade screwdriver, remove the screw and the thermocouple.
2. Loosen and remove the nut.
3. Remove all wires from the contact pins.
4. Pull all the wires down through the feed connector
5. Thread the new wires up through the feed connector and connect all the wires
on the contact pins. Tighten the nuts.
6. Secure the new thermocouple with the screw.
139
Clarus 600 MS Hardware Guide
1.
Remove the
screw securing
thermocouple (1)
(P/N E640-0213)
2.
Loosen and
Remove Nut
Feed
Connector
3.
Remove all wires
from contact pins
(10)
4.
Pull all wires down
through feed connector
5.
Thread all new wires
up through feed connector and
connect wires on contact pins
6.
Tighten
Nut
7.
Secure the
replacement
thermocouple
with the screw.
140
Maintenance
Screw (1 of 2)
(one each side)
Figure 55 Removing the outer source from the ion optics assembly
141
Clarus 600 MS Hardware Guide
The four ceramic rods (Part Number E640-1319) are very fragile. Use
CAUTION extreme care when removing the support plate and lens.
3. Carefully lift the clamp plate (Part Number E640-1322) straight up and put it
aside.
4. Carefully lift and remove the contact support plate from the four ceramic rods.
5. Remove the pillar.
6. Unplug the outer source heaters from the quadrupole heater.
7. Using a flat-blade screwdriver, loosen the outer source heater setscrews.
8. Slide the old heaters out of the outer source block and insert the new heaters
(Part Number E640-0202).
9. Tighten the setscrews 1/8 turn past fingertight.
Do not overtighten the setscrews.
10. Connect the heater wires together and plug the quadrupole heater wire into the
remaining connector.
11. Reassemble the outer source.
142
Maintenance
Screw (1 of 3)
(P/N E531-4016)
Clamp Plate
(P/N E640-1322)
Pillar
(P/N E640-1320)
Heater
Locking
Screws
Source Heaters
(P/N E640-0265)
143
Clarus 600 MS Hardware Guide
1. Unplug the quadrupole heater wire from the outer source heater wires.
2. Loosen the setscrew that secures the quadrupole heater to the standoff.
3. Slide the heater out, discard it, and slide the new heater into the standoff.
4. Secure the heater in place by tightening the setscrew 1/8 turn past fingertight.
Do not overtighten the setscrew.
5. Plug the quadrupole heater wire into the outer source heater wire connector.
144
Maintenance
To outer source
Quadrupole cartridge heater (other side)
Cartridge Heater
(P/N E640-0266)
Purple wire
To outer source
cartridge heater (this side)
Quadrupole Cartridge
Heater Connections
145
Clarus 600 MS Hardware Guide
146
Maintenance
Cleaning
1. Mix together aluminum oxide and methanol to make a watery paste.
2. Dip a wooden-stick cotton swab in the solution and clean the darkened areas on
the source. Work quickly to prevent the mixture from drying on the surface.
3. Remove the residual aluminum oxide by sonication in a beaker of methanol for
ten minutes.
4. Blow dry with helium or dry nitrogen.
5. Reassemble the outer source.
147
Clarus 600 MS Hardware Guide
3 x 10 Screw (1)
(P/N E531-4017)
3 x 6 Screw (1 of 2)
(P/N E531-4016)
Support Plate
(P/N E640-1321)
Figure 58 Removing the lenses from the outer source for cleaning
148
Maintenance
Wavy Washer
(1 of 8)
(P/N E533-5005)
Typical Contact Attachment
2mm Ceramic Spacer
(1 of 4) Stainless Steel Spring Contact Screw (1 of 7)
(P/N E640-1222) (P/N E640-1389) (P/N E531-4044)
Copper Spring Contact
Ceramic Rod (P/N E640-1230)
(1 of 4) Stainless Steel Spring Contact
(P/N E640-1319) Contact Terminal
(1 of 3) (P/N E640-1390) (1 of 3)
Copper Spring Contact (P/N E640-1328)
(1 of 3) (P/N E640-1231)
Pillar (1 of 3) Copper Spring
(P/N E640-1320) Contact
(P/N E640-1232)
12mm Metal Spacer
(1 of 4) Contact Support Plate Stainless Steel Spring
(P/N E640-1324) (P/N E640-1229) Contact
(P/N E640-1391)
Outer Ion Block
(without magnet) Magnet
(P/N E640-1233) 4mm Ceramic
(P/N E640-1227) Insulating Spacer
Magnet Cap (P/N E640-1317)
7.7mm Metal Spacer (P/N E640-1226)
(1 of 4)
(P/N E640-1323)
Lens 1 Focus Plate 2mm Ceramic
2mm Ceramic Spacer (P/N E640-1307) Insulating Spacer
(1 of 4) (P/N E640-1222)
(P/N E640-1222)
Washer
5mm Ceramic Spacer Lens 2 Focus Plate (P/N E533-1013)
(1 of 4) (P/N E640-1235)
(P/N E640-1325)
Nut
(P/N E532-1018)
3 x 6 Screw (1 of 2 bottom)
(P/N E531-4016)
3 x 10 Screw (1)
(P/N E531-4017)
Earth Plate
(P/N E640-1326)
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Clarus 600 MS Hardware Guide
1. Place the assembled outer source on the ion optics assembly and secure it in
place with the two screws.
2. Reattach the tubing to the outer source.
Screws (2)
(one each side)
150
Maintenance
4. Reconnect the wires to the outer source as shown in the following illustration.
Outer Source Assembly
of Ion Optics
Assembly
Ground
(green/yellow wire)
Purple wire
To outer source
cartridge heater (this side)
Lens 2 Focus Plate Orange wire Lens 1 Focus Plate
(green wire) (gray wire)
Wiring Connections
to the Contact Trap (yellow wire)
Support Plate
(View from Front)
Contact Ring
Part No.
N6470055
Repeller
(white wire)
Filament
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Clarus 600 MS Hardware Guide
2. Hold the ion optics assembly by its handles and align the guide pins with the
holes in the vacuum manifold.
3. Gently lower the ion optics assembly until it is seated on the vacuum manifold.
5. Remove the laboratory wipe from the PMT hole and reinstall the PMT
assembly. Observe the orientation of the PMT tube as shown in the detail.
6. Insert the end of the head amplifier ground wire through one of the screws for
the PMT assembly. Insert this screw into the hole in the 2 o’clock position and
insert the other screw in the other hole. Tighten both screws fingertight. Using
a 4 mm hex wrench, tighten both screws ¼ turn past fingertight.
7. Plug the head amplifier board onto the pins on the PMT.
152
Maintenance
Detail of Photomultiplier
Tube Pin Connections
Cover
Ground Cable
Nut
Lock
Washer
153
Clarus 600 MS Hardware Guide
Complete pump instructions are in the instruction manual supplied with the pump.
154
Maintenance
Voltage Selection
Switch Under Cover
Handle
TurboMass
Connection Port
Exhaust Port
Max
On/Off Min
Switch
Gas Ballast
Switch
Mode Selection
Switch Drain Plug
Oil Level
Indicator
Figure 63 Location of the forepump oil viewing window
2. Determine if the oil level is between the Max Oil Level and Min Oil Level
marks next to the window.
• If the oil level is closer to the Min Oil Level mark, add oil. Use Edwards 45 oil
(Part No. 0992-3492, 1 liter).
• If it is near the scheduled six-month service, drain and refill the pump with
clean oil.
• If the oil is contaminated (indicated by a darkened color), try gas ballasting and
if that does not help, drain and refill the pump with clean oil.
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Clarus 600 MS Hardware Guide
Vent the mass spectrometer before opening the plug to add oil.
CAUTION
1. Unscrew and remove one of the filler plugs on the top of the pump.
2. Locate the bottle of pump oil supplied with the pump and add oil until it
reaches the MAX mark on the top of the sight glass. Do not overfill.
3. Replace the oil filler plug by tightening it until it is fingertight. Do not
overtighten the oil filler plug.
4. After restarting the pump and allowing it to run for a few minutes, recheck the
oil level. If the oil level is below the MAX mark, repeat the above procedure by
adding more oil until it reaches the MAX mark.
156
Maintenance
Filler Plug
Drain Plug
2 Liter
Drain Container
157
Clarus 600 MS Hardware Guide
4. Place the pump on a table. Place a drain container under the drain plug. Raise
the end of the pump opposite the drain plug by putting a block under it.
WARNING
5. Remove the drain plug and allow the oil to drain into the container.
If the pump oil was contaminated, pour clean oil into the filler hole and allow it
to drain until the oil appears clear.
6. Replace the drain plug, remove the block and reconnect the vacuum system.
7. Add oil until it reaches the MAX mark on the top of the sight glass.
Do not overfill.
9. After restarting the pump and allowing it to run for a few minutes, recheck the
oil level. If the oil level is below the MAX mark, repeat the above procedure by
adding more oil until it reaches the MAX mark.
158
Maintenance
The inline gas purifier lets you change the trap without introducing contaminants
into your system. This eliminates the need to flush the system. The trap contains
oxygen, moisture and hydrogen adsorbents and is packed and purged under helium.
Color changes in the glass indicating trap will indicated when filter needs to be
replaced.
The click on connector fitting has a spring loaded needle valve, which seals when
the trap is removed and only opens when the new trap is connected and locked into
position. When the click on connectors are installed into the gas line here is no need
to loosen or tighten any fittings, the new trap will just click in.
Replacement Traps
Click On Connectors
Refer to the installation instructions that accompany your new in line gas purifier
trap for detailed installation and operating instructions.
159
Clarus 600 MS Hardware Guide
• Leak-checking.
• Setting-up CI.
Hazardous gas vapors. When using ammonia gas when running in the
chemical ionization (CI) mode, it is necessary to vent the mass
spectrometer effluent from the forepump exhaust into a fume hood or
outside the building.
WARNING
160
Maintenance
Recommended Gases
Reagent gases used in chemical ionization (CI) are methane with a minimum purity
of 99.999%, isobutene with a minimum purity of 99.98% and ammonia with a
minimum purity of 99.998%. Carrier gas tubing should be ultra-clean.
Methane and isobutene require a gas delivery pressure of 15 psi (104 kPa) to the
bulkhead fitting on the back of the mass spectrometer. A two-stage stainless steel
diaphragm, high purity regulator is. A single-stage stainless steel diaphragm, high
purity, rated for corrosive service is required for ammonia. Clean tubing must be
used. It must be solvent-washed and nitrogen-dried. The bulkhead connector at the
rear of the instrument is a 1/8 inch Swagelok fitting.
NOTE: Make sure to purge the CI line before you attach it to the rear of the mass
spectrometer.
1. Obtain the CI gas cylinder for your analysis.
2. Connect the gas line to the CI Gas connector on the rear of the mass
spectrometer.
3. Ensure that the mass spectrometer is at the proper vacuum level.
4. Turn on the CI gas and set the delivery pressure to 15 psi (104 kPa).
5. Leak-check all connections.
161
Clarus 600 MS Hardware Guide
ROTARY PUMP
Rotary
Warning Pump
Power
POWER IN
NH 3
CH4
C 4H 10 N2 WATER WATER Power In
CI GAS VENT IN OUT
15 psi
(103 kPa)
5 psi
(35 kPa)
50 psi
(345 kPa) Warning
MAX MAX MAX Labels
Vacuum
Line
Changing to CI
To change from the EI to the CI mode:
162
Maintenance
5. In the Vacuum Pressure Gauges area of the window, observe the Pirani gauge
time line and the Penning gauge time line. Wait about 5 minutes until the
vacuum gauge achieves about 2.5 x 10-5.
Leak Checking
Before running in the CI mode, confirm that the column is properly installed and the
system is leak-free. The best way to check this is by running CI without the reagent
gas.
163
Clarus 600 MS Hardware Guide
164
Maintenance
If mass 28 is larger than mass 18, you have a leak. Determine the source of the leak
and correct it. For example, leak-check all fittings and connections.
Setting-Up CI
After verifying that no leaks exist, you can proceed to set up the CI mode for an
analysis.
165
Clarus 600 MS Hardware Guide
If using methane reagent gas, the reagent ions at m/z 17 (CH5+) and 29 (C2H5+)
should be of approximately equal intensity. Maximize the m/z 29 intensity. With
m/z 29 maximized, the ion at m/z 16 should be about 1% of the m/z 17 peak height.
(Higher indicates a leak at the transfer line/inner source connection.) Operate
slightly to the low-pressure side of the maximum to minimize gas load on the MS.
(The vacuum gauge pressure will be 1.5x10-4 to 5x10-4 Torr.)
If using ammonia reagent gas, reagent ions at m/z 18 (NH4+) and 35 [(NH3)2H+]
should be present and the ions at m/z 35 should be optimized.
If using isobutane reagent gas, the reagent ions at m/z 43 (C3H7+) and 57 (C4H9+)
should be tuned in the approximate ratio of 1:2.
NOTE: The CI gas adjustment knob controls a delicate needle valve. To avoid damaging the
needle valve, do not overtighten it. Always use the CI gas button on the screen to
turn off the CI gas.
167
Clarus 600 MS Hardware Guide
Access Door
Inner Source
1. Carefully turn the delicate CI Gas adjustment knob fully clockwise until you
feel it stop.
2. Select CI Gas On from the Gas menu. A check mark appears next to the
option.
NOTE: Always turn on the CI gas before Operate to avoid a pressure surge hitting the
filament.
168
Maintenance
3. Click Press for Operate and monitor the Penning gauge as you adjust the CI
gas. Observe that mass 16 initially grows larger. As pressure increases in the
ion chamber of CI source, the mass 29 peak will begin to grow. Keep the
pressure below 5 e-4 Torr.
169
Clarus 600 MS Hardware Guide
6. Turn the knob to maximize the intensity of mass 29. Also verify that mass 16 is
small (< 1.0% of the height of the peak at mass 17).
If mass 16 does not appear as a small peak, STOP. You probably have a gas
leak at the transfer line/inner source connection. Locate and correct the leak.
7. After you have maximized the peak, slightly decrease the reagent gas by
turning the knob clockwise 1/8 turn.
170
Maintenance
8. Tuning may be optimized on the m/z 69, 219, 414, and 652 ions of the
heptacosa reference gas.
9. Click Press for Standby to turn off Operate, followed by the CI gas.
171
Clarus 600 MS Hardware Guide
1. Open the CI gas inlet by selecting CI Gas from the Gas menu. Wait at least 10
seconds before clicking Press for Operate.
2. Optimize the amount of reagent gas flowing into the source by using two
heptacosa ions, m/z 452 and 633, which usually produce relative intensities of
65 – 85% and 95% respectively.
Heptacosa can be used to calibrate the m/z range for negative ion CI analyses.
172
Maintenance
3. Maximize the peak intensities, then slightly decrease the reagent gas by turning
the knob clockwise 1/8 turn.
4. Save the Tune page parameters by selecting Save As…from the File menu.
Make sure the “Use Air Refs” check box is not selected.
CAUTION
173
Clarus 600 MS Hardware Guide
174
Troubleshooting 5
Clarus 600 MS Hardware Guide
176
Overview
The following sources of problems can occur in gas chromatography and mass
spectrometry:
• The column: The column is most often the major factor contributing to poor
analyses. The more a column is used, the greater the possibility of
contamination, loss of substrate, etc. Columns do not last forever and should be
changed when results become suspect.
• The gas flow system: Gas leaks are a major concern in gas chromatography
and can lead to many problems.
• The vacuum system: Vacuum leaks are a major concern in mass spectrometry
and can lead to many problems.
• Ion Optics: Over time, the ion optics can become contaminated. This results in
reduced sensitivity and difficult or impossible tuning.
Spare Components
The following list contains items you should have on hand to help solve problems.
• New syringes: a syringe can break, become plugged or begin leaking. Always
have spare syringes available.
• Duplicate columns: a column does not last forever; always have a duplicate
column on hand in the event that your separation begins to degrade. Also,
capillary columns can be damaged if oxygen is introduced at high
temperatures. A duplicate column will allow you to determine if the column is
the cause of the problem.
• Septa: this is the one area of the gas chromatograph that requires routine
maintenance. Always have spare septa available.
• Leak detector: the gas flow system can be a problem as fittings wear with age
and can begin to leak. You should have a thermal conductivity leak detector to
help find and fix leaks.
• Injector liners: are made of glass or fused silica and can be easily broken when
removed. You should keep a supply of spare liners on hand. Please remember
that you cannot run satisfactory analyses without an injector liner.
178
Change only one parameter at a time and check for its effect. If you change
three items at once and your problem goes away, you may not know which of
the three moves or combination of moves corrected the problem. This way, if
the problem happens again, you will know exactly what corrective action to
take.
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Clarus 600 MS Hardware Guide
Troubleshooting Chart
Mass Spectrometer will AC line cord not plugged into Plug the Mass
not turn on (no indication an AC outlet. Spectrometer AC line cord
of power to the into an AC outlet.
instrument).
Mass Spectrometer is on Forepump is not plugged into Plug the forepump line
but the forepump is not the AC outlet on the rear of cord into the mass
running. the mass spectrometer. spectrometer.
180
Problem Probable Cause Solution
The ultimate pressure is Is the cooling inadequate? Check the cooling-air flow and
poor. correct if possible.
The pump is very noisy or Is the noise irregular and If so, a bearing may be
there is excessive vibration getting progressively defective. Contact your
or both. worse? PerkinElmer service
representative.
181
Clarus 600 MS Hardware Guide
182
Problem Probable Cause Solution
No spectra, not even noise at Loose electrometer cable. Reset the cable.
a high PMT voltage.
183
Clarus 600 MS Hardware Guide
184
Problem Probable Cause Solution
Loss of high end compounds. Temperature setting too Increase the injector, column
low on the injector, oven or transfer line
column oven or transfer temperature to allow the less
line. volatile compounds of the
sample to reach the mass
spectrometer.
Peaks at masses 14 and 16 are Leaks or improper tuning. Tighten the fittings and
larger than the peak at mass 28. connection points to the high
vacuum system.
Set the injector split flow to
50:1.
Run AutoTune.
185
Clarus 600 MS Hardware Guide
Skewed spectra. Improper scan speed (too Increase the scan speed.
slow for the narrow peaks
produced by capillary
columns).
186
Problem Probable Cause Solution
Unusually high emission Ion volume dirty. Clean the inner source.
setting.
187
Clarus 600 MS Hardware Guide
No ion beam but the filament Large air leak. See procedure for leak-
status OK. checking.
188
Problem Probable Cause Solution
189
Clarus 600 MS Hardware Guide
190
Chromatography Related
Tailing peaks (sloping on Improperly installed column. Check the column and
RHS). reinstall if necessary.
191
Clarus 600 MS Hardware Guide
192
Problem Probable Cause Solution
Slowly falling baseline Split valve left closed during Open the split valve.
(from a high initial value). acquisition.
193
Clarus 600 MS Hardware Guide
Column flow rate too high. Reset the column flow rate.
194
Spectral Related
Spectrum distortion. Scanning too fast or slow. Reset the scan rate.
195
Clarus 600 MS Hardware Guide
Molecular Ion too Source temperature too high. Reduce the source
weak. temperature.
196
Communications Related
Will not boot MS. PC (computer) to MS cable Check and reset the cable.
has a loose connection.
Will not control GC. RS 232 communications Check and restart the mass
cable loose connections. spectrometer.
Power failure/transient
surge to GC or
autosampler.
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Clarus 600 MS Hardware Guide
Forepump Related
Pump does not start. Forepump switched off. Switch on the pump.
198
Problem Probable Cause Solution
199
Clarus 600 MS Hardware Guide
External oil leak. Outer shaft seal worn or Call a PerkinElmer service
damaged. engineer.
200
Message Dialogs
When operating the instrument message dialog boxes will sometimes appear. The
following table is the Icon Key followed by tables that show the Message Title, icon,
dialog message and recommended action.
Icon Key
Icon Meaning
201
Clarus 600 MS Hardware Guide
202
Message Icon Message Action
Title
Vacuum The backing pump could not reach the Press OK to close the
Leak necessary vacuum level to start the message.
Detected diffusion pump. There could be a
problem with a vacuum leak, the Check the system for any leaks
backing pump or the vacuum gauge. and correct. If the problem
The backing pump will be turned off. continues contact your
Make sure that the vent valve is closed PerkinElmer service
before restarting the backing pump. representatives.
203
Clarus 600 MS Hardware Guide
204
Message Title Icon Message Action
Vacuum Gauge The vacuum system is off and the Press OK to close the
Failure-Safe to system can now be vented. The message.
Vent carrier gas should be turned off.
To replace the vacuum
There is a problem with the gauge contact your
vacuum gauge. Please look in the PerkinElmer service
Hardware Guide for additional representatives.
instruction.
205
Clarus 600 MS Hardware Guide
Backing Pump is
The system is not in an operating If the transfer line or the
on
state. A diffusion pump failure, a source temperatures are
vacuum leak or a vacuum gauge above 100C, please wait
failure could have occurred. until they have cooled
before pressing OK.
If the transfer line or the source
Pressing the OK button
temperatures are above 100C, please
will turn off the backing
wait until they have cooled before
pump.
pressing OK.
Pressing the OK button will turn off
the backing pump.
The backing pump could not reach
Problem with Press OK to close the
the necessary vacuum level to start
Vacuum message.
the diffusion pump.
There could be a problem with a
vacuum leak, the backing pump or
the vacuum gauge.
The backing pump will be turned off.
Make sure that the vent valve is
closed before restarting the backing
pump.
206
Replacement Parts
To place an order for supplies and many replacement parts, request a free catalog, or
ask for information:
Telephone:
• U.S. only: Call toll free 1-888-PE-CHROM, 8 a.m. to 8 p.m. EST. Your order
will be shipped promptly, usually within 24 hours.
Internet: http://www.perkinelmer.com
e-mail: [email protected]
207
Clarus 600 MS Hardware Guide
208
Index
Index
Index
C F
Caution, 9, 86 Filament
Changing a column, 88 replacing, 121
Checklist
pre-installation, 39 G
pre-operational, 71
Chemicals Gases, 36
definitions of warnings, 26
hazardous, 24
CI
H
leak checking, 163 Hardware
setting parameter values, 166 maintenance, 85
setting up, 165 Heated surfaces, warnings, 23
CI Inner Source, 113 Heaters
disassembling, 114 quad, replacing, 144
maintenance, 113 source, replacing, 142
rinsing and reassembling, 116
Cleaning the Instrument, 21
Column, 70 I
leak checking, 99 Inline Gas Purifiers, 159
selection, 70 Inner Source, 104
Compressed gases, safety practices, 22 maintenance, 104
Computer requirements, 37 removing, 105
Introduction to TurboMass, 49
D Ion optics assembly
removing, 129, 135
Diffusion Pump, 61 Ion source, 57
pumping down, 64
L
E
Labels
EI Inner Source, 106 WEEE Instructions, 30
cleaning, 109, 115 Leak checking, 79
disassembling, 107 CI, 163
reassembling, 110
rinsing, 109
211
Clarus 600 MS Hardware Guide
M Power requirements, 33
Pre-installation checklist, 39
Maintenance, 75 Pre-operational checklist, 71
cable removal, 135
cleaning the prequads, 138
EI inner source, 106
R
inner source, 104 Reference Gas Inlet, 54
leak-checking, 79 Refilling the reference gas vial, 100
mass analyzer, 128 Removing a column, 88
outer source Removing the photomultiplier tube, 133
wire connections, 151
outer source, cleaning, 146
outer source, detail view, 149 S
overview, 75 Safety practices
PMT tube removal, 133 ammonia gas, 24
preparing for, 85 compressed gases, 22
reassembling TurboMass, 152 electricity, 20
removing the cover panels, 131 environmental requirements, 32
replacing an outer source themocouple, 139 general laboratory safety, 29
replacing the quadrupole heater, 144 generic warnings, 18
schedule, 77 heated zones, 23
source heaters, 142 hydrogen, methane, isobutane, 24
tuning, 82 overview, 18
vacuum system, 154 pollution degree, 27
oil, 154 requirements, 35
venting the system, 87 space, 31
Mass analyzer storage, 28
maintenance, 128 ventilation, 23
Software, 68
O top level screen, 68
Tune page, 69
Operating conditions, 27 Source, 119
Outer source reinstalling, 119
cleaning, 146 Space requirements, 31
detail view, 149 Spare components, 178
Overview Storage, 28
Clarus 600/560D GC, 51 Supplies, accessories, replacement parts, 45
ion source, 57 system requirements, 37
maintenance, 75
reference gas inlet, 54
troubleshooting, 177 T
Transfer line
P cooling, 86
Traps
Photomultiplier Tube (PMT) click on connectors, 159
removing, 133 replacement, 159
Pollution degree, 27
212
Index
213