Hardware Maintenance Manual: Agilent 7800/7850/7900 ICP-MS
Hardware Maintenance Manual: Agilent 7800/7850/7900 ICP-MS
1 Overview 7
Site Preparation Requirements 8
Configurations and Components 9
Configurations 9
Instrument Components 11
Part Names 13
Safety Symbols/Symboles de sécurité 18
Principle and Function 20
Brief Overview 20
Function of Components 21
2 Precautions 27
General Precautions 28
Precautions for Use 31
Protective Earth 31
Closing the Instrument Panels and Covers 31
Wearing Safety Glasses 31
Checking the Exhaust System 32
Handling Solvents Correctly 34
Checking the Drain Vessel 35
Compressed Gas Tanks 36
Storing Argon Safely 37
Cell Gas 38
Other Gas 39
Allowing the Hot Instrument to Cool 39
Torch Box Cover 39
Peristaltic Pump 40
Foreline Pump 40
Air Intake 40
Cautions for Toxic Materials 41
Moving the Agilent ICP-MS 44
3 Maintenance 49
Scheduling Maintenance 50
Managing the Maintenance 53
Maintenance Clocks 53
Maintenance Log 55
Preparation before Maintenance 57
Peristaltic Pump Area 58
Sample Uptake Tubing 59
Sample Line Connector Block 63
Internal Standard Tubing Kit 66
Nebulizer and Spray Chamber 69
Nebulizer 70
Spray Chamber 72
Torch Area 76
Torch 77
RF Coil 82
Testing Plasma Ignition 85
Interface 86
Sampling Cone and Skimmer Cone 87
Extraction Lens-Omega Lens Assembly 97
Maintaining the Other Parts 104
Foreline Pump (MS40+) for 7800/7850/7900 104
Foreline Pump (NeoDry36E) for 7900 112
Water Strainer 114
4 Appendix 115
Appendix A. Technical Information 117
Peristaltic Pump and Tubing 117
Spray Chamber 119
ICP Torch 120
Interface 120
ORS 121
Quadrupole 122
Electron Multiplier (EM) 124
APG remote interface 126
Appendix B. Troubleshooting 128
Items to Be Checked in Case of Low Sensitivity 128
Items to Be Checked in Case of Plasma does not Ignite 129
Appendix C. ICP-MS Web Utility 130
Appendix D. Purging the Cell Gas Line 131
Appendix E. Organic Solvent Kit 133
General 133
Replacing the torch 134
Warning Label 136
Appendix F.Inert Sample Introduction Kit Installation Instructions 137
General 137
Mounting 137
Appendix G.Maintaining the Collision/Reaction Cell 141
Opening/Closing the Vacuum Chamber 142
ORS Cell Assembly, Deflect Lens and Plate Bias Lens 145
Appendix H. Hydrogen Safety Guide 165
Hydrogen (H2) Gas 165
Dangers During the ICP-MS Operation 165
Dangers in the ICP-MS Shutdown or Power Failure 166
Necessary Precautions 166
The Agilent 7800/7850/7900 ICP-MS with H2 line, and ORS upgrade with H2 line
are licensed under U.S. Patents 5,767,512; 6,259,091 and associated
counterparts.
Prior to receiving your instrument you will have been provided with an Agilent
7800/7850/7900 ICP-MS Site Preparation Checklist, which describes the
environmental and operating requirements of the ICP-MS system. You must
prepare your laboratory according to these instructions before the ICP-MS can be
installed. You should keep the Site Preparation Checklist for future reference, for
example if you plan to move your instrument.
Configurations
Nebulizer MicroMist
HMI Yes
Interface Nickel
Lens x-lens
Nebulizer MicroMist
HMI Yes
Interface Nickel
Lens x-lens
Instrument Components
The general system consists of the following components. The Autosampler and
the water chiller are optional.
Part Names
The names of the parts of the Agilent 7800/7850/7900 are described in this
section.
Front View
Maintenance Switch
Sample Tray
Serial Number
Cover (Small) This cover is used to cover the ICP area and interface area during operation.
Cover (Large) This cover is used to cover the ion lens system, the mass filter and the detector areas.
Protective Tinted Window enables plasma to be observed.
Window
Status Indicator The status indicator shows the instrument's status by flashing a sequence of colors.
Shutdown to Standby: Long orange, short pause (and continue to repeat this
sequence)
Standby to Analysis: Short orange, long green (and continue to repeat this
sequence)
Analysis to Standby: Short green, long orange (and continue to repeat this
sequence)
Standby to Shutdown: Short orange, long pause (and continue to repeat this
sequence)
It is generally not necessary to turn off the instrument, but if you wish to power
NOTE off the instrument for an extended period of time (more than 1 day) it is
recommended that you turn off the Main Power Breaker Switch, instead of the
front power switch. If main breaker is not turned off, a small current (standby
power) still goes through the power supply unit.
The tubing must have a vertical drop to assist gravity drain. Connect the tubing
NOTE from the overflow port to the chemical waste container and avoid any restriction
of flow.
When the plasma is lit, do not open the top covers. Under normal operation, for
WAR N ING safety reasons, the plasma turns off automatically when either of the top
covers are opened.
Do not remove the front or side covers of the instrument. High voltage and
radio frequency radiation from the RF power supply is present and may be very
dangerous.
Rear View
LAN Interface
Remote Port
On the bottom side of the instrument, there are handles that can be used when
NOTE carrying the instrument.
0004-i2
These symbols, which have these meanings, may be marked on this instrument.
Ces symboles, dont les significations sont indiquées ci-dessous, peuvent être
apposés sur cet instrument.
: Hot Surface
Surface chaude
: Explosion hazard
Risque d'explosion
: Toxic material
Matières toxiques
: Corrosive liquid
Liquide corrosive
Brief Overview
The following steps provide a brief overview of how the ICP-MS analyzes a
sample. More details are provided in later sections.
1 The sample solution is pumped into the inlet system where it is nebulized,
forming a fine sample aerosol.
2 A portion of the sample aerosol is carried by an Ar gas stream to the plasma
(ICP), where elements in the sample are ionized.
3 The sample ions are extracted from the plasma into a vacuum system
containing a quadrupole mass filter. The ions are transported by an ion optic
system to the analyzer where they are separated by their mass-to-charge ratio
(m/z).
4 The ions of a specific mass-to-charge ratio, that is, the ions of an element
selected by the analyzer, are counted by an electron multiplier detector.
5 The count rate obtained for the ions of the particular element is compared
with a calibration plot to give the concentration for that element in the sample
(for quantitative analysis).
Function of Components
Sample Introduction This creates a sample solution mist, and carries it into the ICP torch.
ICP Ion Source This ionizes the elements in the sample using plasma.
Interface/Vacuum This samples the generated ions in a vacuum.
System
Ion Lenses/ORS The ion lenses focus the ions and carry them into the ORS (Octopole Reaction
System). The ORS removes interference resulting from plasma and the sample
matrix.
Quadrupole This filters by the measured mass number of the ions.
Detector This detects the ion signals after they have passed through the quadrupole.
Vacuum System This system evens out the lower vacuum pressure of the interface chamber, the
ion lens chamber, and the analyzer chamber to transmit the ions.
RF Generator This system supplies RF power to the work coil to generate the plasma.
Interface
Interface Chamber Ion Lens Chamber
Skimmer Cone
Sampling Cone Ion Lenses ORS Quadrupole
RF Cell Gas Analyzer Chamber
ICP Ion Source Generator
Detector
EM (Electron
Gas Multiplier)
Controller Turbomolecular
Pump
Ar Gas Vacuum
Sample
Sample Foreline
Introduction Pump
7900_0419
Sample Introduction
The Agilent 7800/7850/7900 ICP-MS features an on-board peristaltic pump that
controls the flow of sample solution into and waste (drain) out of the instrument.
The peristaltic pump continuously pumps the sample solution into the sample
introduction system. The solution passes into a nebulizer that disperses the
sample using a stream of argon gas referred to as nebulizer gas (also referred to
as carrier gas).
To Torch
Makeup Gas
Dilution Gas
Nebulizer
Sample
Spray Chamber
Nebulizer Gas
Drain
0001-i
A sample solution mist forms and passes through a double-pass spray chamber
where the larger sample droplets are removed by collision with the spray
chamber wall. To prevent the spray chamber from filling up with liquid, the
peristaltic pump drain channel constantly removes excess sample solution.
The Peltier cooler, a thermoelectric device, cools the spray chamber. This cooler
allows the temperature inside the chamber to be precisely controlled, which gives
the ICP-MS a very stable ion signal.
In addition, it also reduces the oxide ion generation, decreasing the load of water
vapor on the plasma, which in turn reduces the interference on certain analytes.
The makeup gas line is used to add argon gas to the nebulizer gas in the spray
chamber to analyze certain samples.
The dilution gas line is used to add argon gas to the nebulizer gas downstream of
the spray chamber to reduce the amount of sample aerosol delivered to the ICP
so that high matrix samples can be introduced to the mass analyzer.
RF Field
Auxiliary Gas
Nebulizer Gas
RF Field
Ar Plasma Gas
RF Coil (Cooled) 7900_0420
The end of the torch is situated inside the 3.5 turn induction coil (or, work coil),
through which a radio frequency (RF) current is passed. After seeding the plasma
with electrons, collisions of Ar atoms in the intense RF field generates and
sustains an argon plasma. The electrically grounded cylindrical metal plate is
inserted between the induction coil and the torch to minimize the capacitive
coupling between the coil and the plasma, that is, to establish “pure” inductively
coupled plasma.
In the center of the plasma, gas kinetic temperatures range from 4500 to 6500K,
depending on the nebulizer gas flow rate, the position relative to the coil, and the
RF power supplied to the plasma. The sample aerosol is instantaneously
desolvated and ionized. The argon plasma is a good source of singly charged
positive ions allowing most of the elements of interest to be ionized with an
efficiency of greater than 90 percent.
The plasma gas and auxiliary gas, which are the outer and intermediate gas
streams respectively, form the major part of the plasma. These two gases also
protect the outer tube and the injector tip of the torch from melting.
All the Argon gas supplies are gas controller controlled. This contributes to very
good signal stability.
An optional gas mass flow controller (if installed) allows for the addition of mixed
nebulizer gases to the plasma. This can be useful for certain applications.
Interface/Vacuum System
After the analyte ions are formed, they are extracted into the first vacuum stage
through a hole in the front plate of the vacuum chamber referred to as the
sampling cone. Ions pass through the sampling cone together with Ar gas into
the interface, which is an expansion region evacuated by a foreline pump. The
ions then pass through a second orifice of the skimmer cone, which acts as a
differential aperture between the interface and intermediate vacuum stage. Ions
are extracted from the interface stage by two extraction lenses and focused onto
ORS by the ion lenses. The intermediate stage contains the ion lenses and ORS,
and is evacuated by a turbomolecular pump.
Ion Lenses
To achieve high signal sensitivity, the ion beam must be focused before entering
the ORS and then the quadrupole mass analyzer. The ion lenses perform the dual
role of focusing the ion beam and preventing photons and neutral species
(arising from the plasma) from reaching the detector, giving the ICP-MS very low
random background.
ORS
The ORS is an octopole ion guide contained within a metal vessel and
pressurized with a gas, most often He or H2. The ORS is positioned between the
ion lens assembly and the quadrupole mass filter. As ions from the sample enter
this cell, they interact with the gas, resulting in the reduction of spectral
interferences.
Quadrupole
The quadrupole mass analyzer consists of four long metal rods with a hyperbolic
cross section which are arranged parallel to each other, and have RF and DC
voltages applied to them. The rods act as a mass filter allowing only ions of a
specific mass-to-charge ratio to pass through the center of the quadrupole at a
certain combination of applied voltages. The ions of all other mass-to-charge
ratios are unstable and collide with the rods. These voltages are ramped very
rapidly, for example from 2 to 260amu within 10ms, so spectra of mass versus
intensity can be obtained for all elements virtually simultaneously.
Detector
After passing through the quadrupole, ion signals are measured by the electron
multiplier detector.
The electron multiplier (EM) has many dynodes. When an ion enters the EM, the
ion hits the first dynode and a shower of electrons is generated. The electrons
then hit the next dynode generating more electrons. After going through a series
of dynodes, the multiplied electrons are detected as an electrical signal.
Both the quadrupole and detector are located in the analyzer stage, which is
evacuated by a turbo-molecular pump.
+ HV
Pulse
Ion
M+ e-
e-
- HV
Electron
Analog
Vacuum System
The sample is ionized in the plasma and the ions go through the interface, the ion
lens, and the mass filter to the detector. A lower vacuum pressure in the vacuum
chamber is required to transmit the ions. The ICP-MS has a 3-stage vacuum
system which consists of the interface chamber, the ion lens chamber, and the
analyzer chamber.
Interface Chamber
The interface chamber is located between the sampling cone and the skimmer
cone. The foreline pump evacuates the interface chamber.
RF Generator
This system supplies RF power to the work coil to generate plasma.
General Precautions
The Agilent ICP-MS is a very safe instrument with many built-in protective
C AU T I O N features:
• A safety interlock shuts off the plasma if either of the top covers is opened
during operation.
• A plasma viewing window provides eye protection.
• Sensors monitor the water and argon flow rate and pressure. If the water
flow is too low to sufficiently cool the ICP-MS, or if the argon supply is
insufficient, the plasma is turned off automatically.
• There are fans to help ensure that the instrument's internal temperature
stays within the preset limits. The plasma is turned off automatically if any
of these fans, except the QP fan, fail.
• Temperature sensors on the exhaust vent, instrument inside, and intake
water line stop the plasma if overheating occurs.
• A manual switch shuts down the instrument immediately, even if the
MassHunter Workstation is inoperable.
In case of uncertainty about a specific fluid, that fluid should not be used until
C AU T I O N confirmation by the manufacturer that it will not present a Hazard.
The bundled power supply cable and foreline pump power supply cable are for
C AU T I O N use exclusively with the ICP-MS. Do not use them for other devices or
instruments.
To shut down the instrument quickly, turn OFF the main switch located on the
NOTE lower center of the front panel. To switch the instrument to Standby mode and/or
Shutdown mode without using MassHunter Workstation, a “Vacuum ON/OFF
Switch” is available on the front panel inside. For positioning of the Vacuum
ON/OFF Switch, refer to Figure 1 on page 13.
• A sensor monitors the radio frequency (RF) generator and shuts it down if it
C AU T I O N is improperly matched to the RF coil.
• A fiber-optic sensor shuts off the RF high voltage power whenever the
plasma is not present or is turned off manually.
The ICP-MS MassHunter Workstation displays warning messages when the
sensors first detect a problem, enabling you to stop work before the
shutdown limits are reached.
• The parameters displayed in the instrument control window change from
green to yellow/red as the shutdown limits are approached/reached.
In addition to the above safety features, the following precautions should
always be taken during operation or maintenance:
• Check acid concentration. Continuous aspiration of a highly concentrated
acid might attack the inside of the instrument.
• Close the instrument covers and panels before operation.
• Check the exhaust system for a positive extraction at the exhaust duct.
• Handle solvents correctly.
• Check the drain vessel frequently.
• Check the condition of the pipes, replace as needed.
Pay close attention to the cautions and warnings within this manual and the
MassHunter Workstation online Help.
Protective Earth
Close the instrument top covers before starting the plasma. Because the
instrument can be optimized entirely via MassHunter Workstation, there is no
need to open the front and side panels or cover after the plasma is ignited. In
addition, a safety interlock shuts off the plasma if the cover is lifted.
The external covers of the instrument protect the operator from internal
WAR N ING hazards while the instrument is in operation. Exposure to high voltage and
radio frequency radiation from the RF power supply is present and can be very
dangerous.
Eye Hazard
WAR N ING
Always wear appropriate safety glasses when handling sample solutions and
other chemicals, or when the plasma is on, in order to minimize the risk of eye
damage by hazardous liquids and exposure to ultraviolet rays.
Asphyxiation Hazard
WAR N ING
Laboratory must be equipped with ventilation system to supply continuous and
sufficient fresh air from outside to prevent user from asphyxiation.
Health Hazard
WAR N ING
If the exhaust system stops for any reason, immediately shut off all gas
supplies at the source.
• Do not turn off the exhaust system while gas supplies are on.
• Do not cover the holes for air intake on the ICP-MS.
• If the exhaust fan is inoperable or there is insufficient air flow, do not start
the ICP-MS until the appropriate maintenance personnel have repaired the
problem.
The exhaust system must remain on at all times while the ICP-MS is on: in
NOTE Analysis mode, Standby mode and Shutdown mode.
Noxious Gases
WAR N ING
If the exhaust system stops for any reason while the vacuum pump or ICP-MS
are still running, immediately turn on the exhaust system or turn off the pump
and instrument. If inadequate ventilation occurs, vaporized pump fluid, ozone,
and other toxic combustion products will accumulate in the laboratory.
Hydrofluoric acid (HF) fumes, if inhaled, cause extensive burning of lung
tissue.
Explosion Hazard
WAR N ING
The laboratory exhaust system must always be operational and connected to
the instrument exhaust vent. Potential health hazards and the risk of
explosions may occur if exhaust gases are incorrectly ventilated.
Toxic Gases
WAR N ING
Immediately turn off the gas supplies at the source in the event the exhaust
system is stopped for any reason. Refer to “Appendix H. Hydrogen Safety
Guide” on page 165 and “Appendix I. Ammonia Safety Guide” on page 167.
These, and other gases which may be used with the ICP-MS present a variety
of risks.
Condensation
C AU T I O N
Ensure that the exhaust system is working correctly at all times. Instrument
damage from condensation may occur due to reverse flow through the exhaust
system.
Exhaust venting must comply with all local environmental and safety codes.
IMPORTANT Contact your Environmental Health & Safety (EHS) specialist.
When using Organic solvents, extra caution should be observed. If the spray
WAR N ING chamber drain is not pumped properly, the excess flammable solvents in the
spray chamber may ignite and/or become explosive. If the torch injector clogs,
the increased pressure in the spray chamber may cause the end cap to blow off
exposing the solvent to ignition.
The drain vessel contains the spray chamber effluent, which can be toxic.
WAR N ING Improper handling of the vessel can result in a serious explosion or fire if
incompatible substances accumulate. Corrosion of the vessel and connecting
tube can result in leaks that may damage the instrument or cause bodily harm.
If the effluent collected in the drain vessel contains toxic materials or solvents,
follow approved laboratory procedures to safely dispose of this hazardous
waste.
Ensure that the drain bottle is adequately ventilated (by the lab ventilation
system, the same as for the ICP-MS mainframe) to deal with vapors from the
bottle.
Clean the drain vessel every time you empty it by thoroughly flushing it with
water. If it contained organic solvents, wash the drain vessel in acetone and
allow it to dry.
Follow the procedures below to avoid exposure to the contents of the drain
vessel:
• When using organic solvent, please use a suitably sized waste container of
appropriately resistant material for the collection of organic solvent.
• Place the drain vessel on the instrument table, where it is easy to check the
liquid level.
• Tightly connect the drainage tubing from the spray chamber around the
peristaltic pump to the drain vessel. Do not crimp the tubing.
• Check the drain vessel frequently. Empty it before you ignite the plasma.
• Be aware of the nature of the vessel contents. If the contents are toxic,
dispose of them as hazardous waste. Also, always empty the vessel when
switching from aqueous to organic sample solutions.
• Check the tubing and vessel for deterioration. If the tubing becomes brittle
or cracked, replace it. Organic solvents generally cause more rapid
deterioration than aqueous solutions.
Do not set the cell gas supply pressure higher than the specification of the
WAR N ING ICP-MS instrument.
Compressed gas tanks must be handled with care. The contents of the
WAR N ING cylinders also may be hazardous, depending on the gases you choose to use.
All compressed gases (other than air) can create a hazard if they leak into the
atmosphere. Even small leaks in gas supply systems can be dangerous. Any
leak can create an explosion hazard, a fire hazard, or can result in an
oxygen-deficient atmosphere. Such hazards can cause death, serious injury,
asphyxiation, anesthetic effects, and serious damage to equipment and
property.
Consult the cylinder, regulator and/or gas supplier for additional safety
WAR N ING measures and ensure all staff are fully familiarized with all safety precautions.
Cell Gas
Health Hazard
WAR N ING
The exhaust gas tubing from foreline pump must be always connected to the
rear port of the ICP-MS instrument to ensure that the cell gas evacuated by the
foreline pump is exhausted via the external duct. Health hazards include the
possibility of flammable, toxic or asphyxiating gas entering the room air.
Health Hazard
WAR N ING
Close all gas supply valves to the ICP-MS instrument before turning off the
vacuum system. Health hazards include the possibility of flammable, toxic or
asphyxiating gas accumulating in the vacuum chamber or instrument
enclosure.
Individual stop valves must be installed for all gas lines for each individual
ICP-MS instrument.
Fully and strictly adhere to all local and national regulations and guidelines for
WAR N ING the proper storage, handling and transport of all gases.
Other Gas
The torch and interface remain hot after the plasma is turned OFF. Do not
WAR N ING touch the torch box or interface cones for 10 minutes after turning off the
plasma to let them cool.
Always re-attach the torch box cover after maintenance. This cover reduces
C AU T I O N the emission noise from the plasma.
Peristaltic Pump
Take care when you open and close the clamp of the peristaltic pump.
WAR N ING Otherwise, you could get your finger caught between the stator and the rotator,
or between the stator and the stopper.
Foreline Pump
The pump oil may be very hot. Direct skin contact may cause burns.
WAR N ING
If foreline pump oil is accidentally spilled on skin, in mouth, or eyes; wash
immediately and thoroughly and seek expert medical attention.
The surface of the Foreline Pump may be HOT, do not touch the pump until it
WAR N ING has cooled.
Air Intake
The ICP-MS is heavy (about 100 kg), so if you need to lift the instrument, it
WAR N ING should be lifted by at least 4 people or with a mechanical lifter.
If the exhaust fan is inoperable or there is insufficient air flow, do not start the
WAR N ING plasma until the appropriate maintenance personnel have rectified the
problem.
Do not cover the holes for air intake on the ICP-MS.
Environmental Conditions
“Pollution level” describes the degree to which a solid, liquid, or gas which
NOTE deteriorates dielectric strength is adhering. “2” applies to a normal indoor
atmosphere.
“Installation category” implies the regulation for impulse withstand voltage. It is
also called the “Over voltage category”. “II” applies to electrical equipment
This equipment requires the following space for ventilation, maintenance access,
and easy access to the Main Power Breaker Switch. There must be a clear space
of at least 60 cm (24 in) on all sides of the equipment. The bench in your
laboratory must be able to support the entire ICP-MS system and other
laboratory equipment.
Electromagnetic Compatibility
EN55011/CISPR11
Group 1 ISM equipment: group 1 contains all ISM equipment in which there is
intentionally generated and/or used conductively coupled radio-frequency energy
which is necessary for the internal functioning of the equipment itself.
Class A equipment is equipment suitable for use in all establishments other than
domestic and those directly connected to a low voltage power supply network
which supplies buildings used for domestic purposes.
ICES/NMB-001
This ISM device complies with Canadian ICES-001.
Cet appareil ISM est conforme à la norme NMB-001 du Canada.
Sound pressure
Sound pressure Lp < 70 dB(A) according to DIN EN ISO 7779.
Schalldruckpegel
Schalldruckpegel LP < 70 dB(A) nach DIN EN ISO 7779.
Cooling Water
Inlet Temperature: 15 to 40 °C
Inlet Pressure: 230 to 400 kPa
Minimum Flow Rate: 5.0 L/min
Exhaust Duct
Extraction Flow Rate: 5 to 7 m3/min
Foreline Pump
Current Rating: 5 A
Do not use any foreline pump except those specified by Agilent for use with the
C AU T I O N Agilent ICP-MS.
The rated current of foreline pumps (for use other than with the Agilent ICP-MS):
NOTE 6.0 A for MS40+; 6.8 A for DS402; 7.0 A for Dry pump (NeoDry36E), but the above
listed rating of 5 A is applicable for use with the Agilent ICP-MS.
Torch Area 76
Torch 77
RF Coil 82
Testing Plasma Ignition 85
Interface 86
Sampling Cone and Skimmer Cone 87
Scheduling Maintenance
Routine maintenance extends the operating life of the components, and lets the
Agilent 7800/7850/7900 ICP-MS perform at optimum level.
The following table shows the maintenance items/frequency for the ICP-MS.
Table 6. Maintenance Schedule
Weekly Sampling cone, Skimmer cone Check orifice for foreign Clean when necessary
matter, deformation and
enlargement
Annually Foreline Pump oil mist filter Check / replace mist filter
4 Years Foreline Pump (NeoDry36E) Maintenance free for 4 years Replace the pump as
needed*2
*1 Generally the cooling fluid requires replacement annually, however, if the cooling fluid shows noticeable
deterioration it may be necessary to replace sooner.
*2Contact your Agilent representative for the pump replacement after 4 years use.
*3 Contact your Agilent representative to arrange engineer visit if replacement needed. Note: The time for EM
replacement can be judged by the EM voltage (Analog HV and Pulse HV). The EM can be used until the
Analog HV reaches 3500 V or the Pulse HV reaches 2000 V, after adjusting the EM voltage. However, it is
recommended to replace EM well in advance.
Refer to the following sections on Maintenance for further guidance about when
NOTE maintenance may be needed.
Depending on the samples introduced, the foreline pump oil may degrade
C AU T I O N sooner than normal and turn black in color. Change the oil before the six-month
period if this occurs. Continued use with degraded oil may result in damage to
the foreline pump. Be aware that coverage does not extend to maintenance
neglect.
Maintenance Clocks
Figure 8.
You can also open the Instrument Status pane by clicking Status Viewer from
NOTE the Layout group on the View tab and then clicking EMF in the Status Viewer
dialog box.
2 Click EMF button in the Instrument Status pane, and the elapsed time
indication screen appears. Click the Setting icon.
Figure 9.
Maintenance Log
Figure 11.
You can also open the Maintenance table by clicking Settings from the Settings
NOTE group on the Tools tab and then clicking Hardware > Mainframe > Maintenance
Log in the Settings dialog box.
Figure 12.
Pure water used for cleaning is indicated as water that has been generated using
NOTE the ion-exchange method and a membrane filter, and has an electrical resistance
of at least 18 MΩ cm.
When the peristaltic pump (peripump) no longer pumps the sample with an even
flow, wash or replace the pump tubing or readjust the pump clamps.
Change the sample uptake tubing in the following cases.
• When signal is unstable due to the pulsation.
• When the tubing is cracked or damaged.
• When the tubing becomes too loose to uptake a solution.
• When the inside of the tubing is damaged and dregs are released.
• When it is impossible to remove sample memory.
This is especially important if you keep using old tubing. The inside tends to
come off and cause the nebulizer to become clogged. It is recommended to
replace the sample uptake tubing frequently.
There are three kinds of sample uptake tubing: (the colors of the tube stoppers
are indicated in parentheses)
• Sample tube: white-white, 1.02 mm i.d.
• Internal standard tube: orange-blue, 0.25 mm i.d.
* Set the maximum number of pump revolutions for the internal standard
tube at 0.3 rps.
• Drain the tube: yellow-blue, 1.52 mm i.d.
Some chemicals attack the sample uptake tubing. This might cause leakage in
C AU T I O N the sample introduction and drain line, and cause corrosion of the sample
introduction system.
Cleaning
The sample uptake tubing has to be washed prior to use. The common way is to
soak it in a 5 % Nitric Acid (v/v) solution for two or three days. If HCl is used, Sn is
eluted from the tubing. In this block, 3 % HCl (v/v) should be pumped at 0.1 rps
for an hour or less through the new sample uptake tube.
Installation
To Nebulizer
To Drain Vessel
Knob to Adjust the Clamp Tension
Levers
Clamps
Rollers
Sample Uptake Tubing
for Drain
Sample Uptake Tubing Direction of Rotation
for Sample
The term "Carrier Gas" has been changed to "Nebulizer Gas" in MassHunter 4.4.
NOTE
In Analysis mode, check that the pure water is reaching the nebulizer and that
excess water is draining from the spray chamber. Liquid and gas should be
discharged alternately from the spray chamber.
Flow Direction
3 To adjust the clamp tension, first loosen the clamp tension until a water flow
stops. Then slowly tighten the knob until the pump draws up the water again.
Finally tighten the sample knob an additional 1 to 2 turns, and the drain knob 2
to 3 more turns.
The sample line connector block grounds the sample introduction tubing,
eliminating any build up of electrostatic charging, that could lead to signal
instability.
We will now demonstrate how to assemble the sample line connector block.
The connector block may be left in place when the block is bypassed.
NOTE For on-line addition of the internal standard solution, see the “Internal Standard
Tubing Kit” section.
Installation
1 Cut the ends of the PTFE tubing at a 90 degree angle to avoid leaking or
clogging.
2 Slide the PTFE nut, back ferrule and front ferrule onto the PTFE tubing. The
PTFE tubing should protrude between 0.5 and 1.0 mm beyond the front
ferrule.
0.5 - 1.0mm
7700_0074
3 Fully insert the end of the PTFE tubing into the connector block.
To reduce the amount of dead volume, keep the PTFE tubing pushed in as far
as possible while tightening the nut.
4 Follow the same procedure to connect the tube from the nebulizer. Screw the
supplied white plug into the connector block.
Connect the sample uptake tube to the opposite end of the supplied sample
tube.
(White Plug)
PTFE Tubing PTFE Tubing from Nebulizer
0.5 - 1.0mm
To Drain Vessel
To Nebulizer
Allow the sample to flow for about 1 minute then check each connection for
leaks.
Further tighten the PTFE nuts, if you discover a leak.
If the leak persists, check the ends of the tubing and re-trim any rough ends
before refitting.
This kit is for the on-line addition of an internal standard solution. It also grounds
the sample line.
Sample Tube
PTFE Screw
Back Ferrule
Internal Standard Solution
Front Ferrule When Not Automatically
Added
Installation
1 Cut the ends of the PTFE tubing at a 90 degree angle to avoid leaking or
clogging.
2 Slide the PTFE nut, back ferrule and front ferrule onto the PTFE tubing. The
PTFE tubing should protrude between 0.5 and 1.0 mm beyond the front
ferrule.
0.5 - 1.0mm
7700_0074
3 Fully insert the end of the PTFE tubing into the connector block.
To reduce the amount of dead volume, keep the PTFE tubing pushed in as far
as possible while tightening the nut.
4 Follow the same procedure to install both the tube from the nebulizer and the
supplied sample tube to the connector block.
0.5 - 1.0mm
7700_0078
To Nebulizer
Sample Uptake Tubing for Drain
Sample Uptake Tubing for Sample Sample Uptake Tubing for Drain
PTFE Tubing for Sample
Allow the sample to flow for about 1 minute then check each connection for
leaks.
Further tighten the PTFE nuts if you discover a leak.
If the leak persists, check the ends of the tubing, and re-trim any rough ends
before refitting.
The nebulizer and spray chamber need to be cleaned if memory effects are
observed after running high matrix samples, or when ultimate detection limits
(ppt) are necessary.
The nebulizer and spray chamber are located in the open area of the sample
introduction part on the left of the instrument. The spray chamber is tilted to
facilitate drainage. This section contains steps to maintain the MicroMist and
PFA Concentric nebulizers, as well as the standard and inert spray chambers.
In this section, the following two kinds of nebulizers are described. The required
argon gas pressure is 500 to 700 kPa.
• MicroMist nebulizer
• PFA Concentric nebulizer
There are two kinds of materials for the spray chamber, quartz and PFA.
To maintain the nebulizer, you will need the following tools and supplies:
• Safety glasses
• Protective laboratory gloves
• 5 % Nitric Acid bath
• Pure water in a rinse container
Pure water used for cleaning is indicated as water that has been generated using
NOTE the ion-exchange method and a membrane filter, and has an electrical resistance
of at least 18 MΩ cm.
Nebulizer
Removal
Do not touch the nebulizer tip. Touching the tip may affect your results due to
C AU T I O N contamination.
MicroMist Nebulizer
1 Disconnect the sample tube.
2 Lift the yellow portion of the nebulizer gas line, and disconnect the quick
connect fitting.
3 Loosen the nebulizer holder nut, and slowly withdraw the nebulizer, taking
care not to strike the nebulizer tip against the end cap.
Nebulizer
7900_0072
PFA Nebulizer
1 Disconnect the sample line, and loosen the union connector to disconnect the
nebulizer gas tube.
When removing the nebulizer, do not disconnect the tubes from the nebulizer
connections.
2 Loosen the nebulizer holder nut, and slowly withdraw the nebulizer, taking
care not to strike the nebulizer tip against the end cap.
Cleaning
For normal cleaning, soak in 5 % Nitric acid until clean. Leave a MicroMist
nebulizer about 10 minutes, and a PFA nebulizer for few hours, or until the
monitored signal goes down to the required level. If the nebulizer is clogged, then
follow these steps.
Remove the nebulizer, and check for damage. Replace the nebulizer if necessary.
1 Reverse the sample uptake tubing for sample, on the peristaltic pump, and
place the nebulizer tip in pure water.
2 Run the peristaltic pump in high speed, and flush pure water from the
nebulizer tip toward the sample uptake for a few minutes.
3 If the steps above do not clear the clogging, use Nebulizer cleaner (P/N
G3266-80020) to back flush the sample line with pure water. This cleaner can
only be used with a MicroMist Nebulizer.
Do not use a wire or similar material to clear a clogged nebulizer, as this will
C AU T I O N cause irreparable damage to the nebulizer.
Take care not to damage the microstructure of the nebulizer tip.
Using ultrasonic cleaning can damage a nebulizer. Do not clean a nebulizer in
an ultrasonic bath.
Installation
MicroMist Nebulizer
1 Fully insert the nebulizer into the end cap, taking care not to damage the tip.
Position the nebulizer gas tube fitting onto the nebulizer in the same upward
direction as the makeup gas fitting.
2 Tighten the nebulizer holder nut.
3 Connect the nebulizer gas and sample tubes.
PFA Nebulizer
1 Fully insert the nebulizer into the end cap, taking care not to damage the tip.
Position the nebulizer gas tube fitting on the nebulizer in the same upward
direction as the makeup gas fitting.
2 Tighten the nebulizer holder nut.
3 Connect the nebulizer gas tube from the nebulizer and nebulizer gas tube
from the instrument with the union connectors.
Spray Chamber
Removal
Organic solvents, HF, and other types of acid remaining in the spray chamber
WAR N ING can be hazardous or flammable if they come into contact with skin or are
spilled on the tray. Before you remove the spray chamber from the spray
chamber chiller, follow the steps below:
1 Wash the spray chamber by aspirating pure water at a high speed and
flowing the nebulizer gas.
2 Stop the nebulizer gas. Aspirate air through the peristaltic pump for 1 to 2
minutes and confirm that all of the solution from the spray chamber has
drained.
Top Cover
Screw Connector Tube
Ball Joint Clamp
Retainer
End Cap
Spray Chamber
Drain Tube
7700_0071
Connector Tube
Top Cover
Screw Ball Joint Clamp
Dilution Connector
End Cap
Spray Chamber
Drain Tube
7900_0071
Do not touch the tip of the dilution nozzle, and do not disassemble the right
C AU T I O N angle connector and nozzle.
Do not use chemicals such as Hydrofluoric Acid (HF), which erodes quartz, to
C AU T I O N clean the spray chamber.
Installation
1 Fully insert the spray chamber into the end cap.
2 Securely connect the drain fitting on the spray chamber to the drain connector
to avoid drain leakage. Insert the spray chamber inside the chiller.
Make sure the spray chamber makes a good seal with the drain, especially
WAR N ING when using organic solvents. Organic solvent leaks can be a fire hazard.
If there is a crevice between the upper block and the lower block, the spray
C AU T I O N chamber cannot maintain a uniform inside temperature. This may cause poor
system performance.
Torch Area
Check the torch, shield plate, and bonnet according to the following criteria and
perform maintenance as necessary.
Torch
• Cracked, chipped, or deformed by high temperatures
• When performing analysis requiring ultra-sensitivity (ppt)
• Deposits have formed in the central torch tube
Shield Plate
• Extensive corrosion or high temperature deformation
Bonnet
• Fractured, cracked, or chipped
Slight deformation of the torch may not cause any problems. However, if the
C AU T I O N torch is badly distorted problems such as “no sensitivity” or “difficulty in
igniting plasma” may occur during use.
The torch is exposed to very high temperatures. Wait at least 10 minutes for
WAR N ING cooling before you start any torch maintenance.
Pure water used for cleaning is indicated as water that has been generated using
NOTE the ion-exchange method and a membrane filter, and has an electrical resistance
of at least 18MΩ cm.
An explanation is also given on the method for checking the position of the RF
coil.
Torch
Removal
1 Open the cover on the left of the instrument. Unlatch the torch box catch clip
and remove the cover.
2 Remove the torch-side clamp.
Loosen the spray chamber block thumbscrew, and slide the spray chamber
block to the left.
3 Loosen the plasma and auxiliary gas tube clamps, and disconnect the tubes
from the torch.
4 Unlock the torch stand clip. With the bonnet and shield plate still connected,
lift the torch out of the torch stand groove, and ease the torch away from the
RF coil.
Hold the bonnet in place when removing the torch to prevent it from dropping.
Torch Stand
Torch Stand Groove
RF Coil
Torch Projection
(for Torch Stand)
Bonnet
Torch
7900_0080
Shield Plate
Projection for
Torch Stand
Bonnet
Hole
Torch
7700_0081
If the torch is still wet when it's installed, it will break or may cause difficulty
C AU T I O N igniting the plasma.
Installation
1 Insert the shield plate and bonnet into the torch.
Slide the shield plate with the hole aligned with the torch projection.
Next, slip the bonnet over the shield plate, and slide it until it rests against the
projection of the torch.
Shield Plate
Projection for
Torch Stand
Bonnet
Hole
Torch
7700_0081
Ensure that the bonnet direction is correct. The brim of bonnet is set on left
C AU T I O N side.
2 Once the shield plate and bonnet have been connected to the torch, carefully
insert the torch inside the RF coil, and position it inside the torch stand groove
against the other torch projector.
Take care of the position of the shield plate, and not to drop the bonnet when
installing the torch.
Torch Stand
Torch Stand Groove
RF Coil
Torch Projection
(for Torch Stand)
Bonnet
Torch
7900_0080
Do not over-tighten the nuts on the quick-connect clamps. If you apply too
C AU T I O N much pressure, the torch will break.
5 Slide the spray chamber back to the right side, to connect the torch and
connector tube. Install the clamp.
6 Install the torch box cover and secure the torch box catch clip. Close the
instrument cover.
RF Coil
Tool Handle
Keep this edge in contact
with inside surface of torch box
Use the alignment tool only to gauge the coil span and spacing, do not force
C AU T I O N the tool. If adjustments are required to the coil, use a flat-bladed driver (do not
use the alignment tool to attempt to adjust the coil).
• The spaces between the 4 turns of the coil on top should be equal.
• The span of the 4 turns of the coil on top should fit within the tool as
shown.
Alignment Tool
Coil
7700_0423
• The spaces between the 3 turns of the coil on bottom should be equal.
Alignment Tool
Coil
7700_0424
The adjustment tool must be tilted slightly to fit the angle of the coils.
NOTE
Coil
7700_0425
• The span of the 3 turns of the coil on bottom should fit within the tool as
shown.
Alignment Tool
7700_0426
4 If the turns of the coils top and bottom, or the span of the coil top and bottom,
do not fit in the tool as shown, use a flat-bladed driver to carefully and gently
adjust the coil.
Confirm that the plasma ignites correctly after performing torch maintenance.
Ignite the plasma.
If the plasma ignites and the instrument transitions to Analysis mode, the
instrument is operating normally.
• In this case, you will be able to see the plasma through the viewing window.
• If the plasma does not ignite, check the connections on the clamp and the
position of the torch installation. Also check the gas connections for leaks.
Interface
Clean the cones when there are deposits on the orifice or the orifice is discolored
(due to heat). Because of its proximity to the torch, the sampling cone needs
cleaning more frequently than the skimmer cone.
The MassHunter Workstation software can also indicate that maintenance is
needed, if you observe high background memory, sensitivity loss, distorted peak
shapes, or an interface vacuum reading higher than 400Pa.
If the memory cannot be reduced, clean the sampling cone or skimmer cone, or
replace them with a new sampling cone or skimmer cone.
If opening the vacuum chamber such as when washing the ion lens, do so after
C AU T I O N turning the main switch of the ICP-MS OFF.
Pure water used for cleaning is indicated as water that has been generated using
NOTE the ion-exchange method and a membrane filter, and has an electrical resistance
of at least 18 MΩ cm.
Removal
The platinum skimmer cone should only be used with the brass skimmer base.
C AU T I O N This allows the cone to operate at a lower temperature than with the standard
stainless steel skimmer base, extending the life of the cone. When fitting the
brass skimmer base, transfer the extraction lenses from the stainless steel
base. For removing and refitting the skimmer base and the extraction lens,
refer to the “Removal” and the “Installation” in the section entitled “Ion Lens”.
The nickel skimmer cone works better at higher temperatures and should
always be used with the stainless steel base. The nickel skimmer should also
be conditioned before use. Refer to “Conditioning the Nickel Skimmer” on
page 92.
Torch Box
Maintenance Switch
7900_0083
The torch box moves to/back from the maintenance position each time the
NOTE maintenance switch is pressed.
Do not touch the sampling cone orifice. Even slight pressure can damage the
C AU T I O N orifice.
Loosen the sampling cone by holding it firmly.
4 Hold the outer edge of the sampling cone, and slowly pull it out along its axis.
It is not necessary to remove the graphite gasket.
Take care not to bang the sampling cone against the skimmer cone during
C AU T I O N removal. Do not touch the tip of the sampling cone. Even slight pressure will
damage the tip.
Be sure to set the sampling cone down with the orifice facing up. Also take
care not to damage the back surface of the cone as this is the sealing surface.
6 Insert the skimmer cone removal tool into the interface opening. Make sure
that you have aligned the tool’s tabs with the skimmer cone exterior holes.
When aligned, rotate the skimmer cone removal tool counterclockwise to
remove the skimmer cone. Be sure to hold the tool upright when removing the
cone to avoid dropping it.
Do not touch the skimmer cone orifice. Even slight pressure can damage the
C AU T I O N orifice.
7700_0042
7 Hold the perimeter of the skimmer cone, and remove it from the skimmer
cone removal tool.
Take care not to drop the skimmer cone or touch the tip.
Set the skimmer cone down with the orifice facing up.
Wear laboratory gloves; handle with care; avoid damaging the skimmer.
C AU T I O N
Conditioning Procedure
Prepare the following conditioning solution:
• 1 % Nitric acid blank
• 50 ppm Calcium in 1 % nitric acid
1 Use the interface wrench to install the new skimmer cone in the instrument.
2 Install the sampling cone.
3 Turn on the Plasma.
4 Aspirate 50 ppm Calcium solution for 10 minutes.
5 Change to the 1 % Nitric acid blank solution and aspirate for 10 minutes.
• Do not clean the cones too vigorously as this may shorten their operating
C AU T I O N life.
• When setting the sampling and skimmer cones down, place them with the
orifices pointing up. Even the slightest pressure can deform the orifice.
• Usually, do not use organic solvents like acetone for cleaning the sampling
cone and the skimmer cone. In extreme cases such as oily contamination of
the cones, you may use acetone, but be careful to rinse all trace of the
acetone off the cones before drying. Do not use acetone to dry the cones as
residue will remain.
The cones must not be stored in pure water for more than 30 minutes or they will
NOTE become damaged by corrosion.
• The tip part has great influence on analytical results. Handle with care and
C AU T I O N do not deform the tip.
• The tips of the sampling cone and the skimmer cone are easily deformed.
Be careful when handling them.
Installation
The platinum skimmer cone should only be used with the brass skimmer base.
NOTE This allows the cone to operate at a lower temperature than with the standard
stainless steel skimmer base, extending the life of the cone. When fitting the
brass skimmer base, transfer the extraction lenses from the stainless steel base.
For removing and refitting the skimmer base and the extraction lens, refer to
“Extraction Lens-Omega Lens Assembly” in the this section.
The nickel skimmer cone works better at higher temperatures and should
always be used with the stainless steel base.
Check the stamp on the skimmer cone to confirm that it is exclusively for use
C AU T I O N with this product.
Firmly install the sampling cone and the skimmer on the base. If the sampling
C AU T I O N cone and the skimmer are not tightly installed on the base, the sampling cone
and skimmer are not cooled enough and may cause bad effect on the analytical
performance, or the vacuum does not reach the standard value and it cannot
change to Standby mode.
3 Hold down the maintenance switch until the torch box returns to its original
position, and then close the instrument cover.
This procedure explains the removal, disassembly, and cleaning method for
individual lenses, and the reassembly of the ion lens (Extraction Lens-Omega
Lens Assembly) used in the Agilent ICP-MS.
The lenses should be cleaned if any of the following symptoms are observed:
• The signal is unstable. For example, more than 10 % signal drift in an hour.
This may also be caused by other parts such as sample introduction.
• The lens voltage is changed in the MassHunter software, and the resulting
signal changes very slowly. For example, if you change the parameters
drastically step by step, it will take more than 1 second for the signal to
stabilize.
• When changing the parameters during tuning, the response speed of the
signal is different when changing the value from the plus direction and
changing it from the minus direction.
• It is necessary to clean the Octopole if there is a signal drift, or a longer than
normal period of time is required for the signal to stabilize when switching
from hydrogen to standard mode.
You will need the following equipment when maintaining the ion lenses:
• Safety glasses
• Laboratory gloves
• Pure water
• Ethanol or acetone (EL grade) for cleaning the tools
• Polishing paper (#400, #1200 grit)
• Allen wrench (included in the tool kit)
• TORX driver (T8, T10)
• Ultrasonic bath
• Circuit tester
• Laboratory tissue
• Alumina abrasive powder
• Glass beaker (large/small)
• Tweezers
• Cotton swabs
• Plastic tray
Pure water used for cleaning is indicated as water that has been generated using
NOTE the ion-exchange method and a membrane filter, and has an electrical resistance
of at least 18 MΩ cm.
This procedure assumes that the ICP-MS is in Standby mode and the Sampling
NOTE and Skimmer Cones have been removed. For information on removing the
Sampling and Skimmer Cones, refer to “Interface” in the previous section.
When removing the Extraction Lens-Omega Lens assembly, it is not necessary to
open the vacuum chamber.
Removal
1 Loosen the 3 screws from the skimmer base using an Allen wrench (3 mm.)
2 Carefully remove the extraction lens-omega lens assembly from the
instrument.
Place the extraction lens-omega lens assembly on a clean surface.
Disassembly
Use the skimmer wrench to disassemble the Extraction lens-omega lens
assembly. Wipe the skimmer wrench with ethanol and laboratory wipes before
proceeding.
Carefully place the lens assembly on the wrench.
Expanded View of the Extraction Lens-Omega Lens Assembly (7800/7850 and 7900
x-lens configuration)
Through Hole
Skimmer Base
Spacer (lipped)
Spacer
Spacer
Spacer
Extraction Lens 1 Omega Bias-x
Spacer
Extraction Lens 2 Lens Screws (2)
Omega Lens-x
7900_0087
Figure 41. Expanded View of the Extraction Lens-Omega Lens Assembly (7800/7850 and 7900 x-lens
configuration)
Through Hole
Skimmer Base
Spacer (lipped)
Spacer
Spacer
Omega Lens-s
Spacer
Spacer
Extraction Lens 1
Extraction Lens 2
Omega Bias-s
Figure 42. Expanded View of the Extraction Lens-Omega Lens Assembly (7900 s-lens configuration)
Cleaning
It is possible to clean the Extraction Lens, Omega Lens-x (-s), and Omega Bias-x
(-s) separately, but it is more efficient to clean them together.
There is normally no need to clean the spacers and screws. Be careful not to
touch the spacers and screws with your bare hands.
1 Using the blue (#400) polishing paper, thoroughly clean the interior of the
lenses.
Shape the polishing paper to fit the lens.
Clean the interior, exterior and orifices of each extraction and omega lens, to
remove any discoloration.
Polishing Paper
Omega Lens-s
7700_0089
2 Repeat the cleaning procedure using the yellow (#1200) polishing paper.
3 Use a cotton swab with alumina paste mixed from alumina powder and pure
water to polish the interior and intricate parts of the lenses.
Pay particular attention to cleaning the orifices.
4 Rinse with pure water.
5 Ultrasonic clean in pure water for 5 minutes.
6 Dry on a clean surface.
Allow the lenses to air dry, do not wipe.
Do not clean plastic components (spacers) with acetone. The plastic will be
C AU T I O N damaged or deformed if it comes in contact with acetone.
Completely dry all components. If components are connected to the vacuum
chamber before they have completely dried, it will take an extraordinarily long
time for the chamber to pump down to Standby mode. Also, if the Extraction
Lens and Omega Lens are assembled before they are completely dried it can
have a potentially critical impact on the components when the plasma is
ignited. Do not use any solvents such as acetone or methanol to dry the lens
components. Organic solvents leave a thin layer on the surface of the lens and
create severe sensitivity problems.
Assembly
When assembling the Extraction and Omega Lenses to the Skimmer Base, refer
to the figure (7900: Figure 41, when using s lens configuration: Figure 42) for the
correct location and orientation of the components. After completing the
re-assembly, securely tighten the 2 lens screws.
Check the insulation between each of the extraction lenses and omega lenses.
Check that there is no electrical continuity between the extraction lenses and the
extraction lens or skimmer base.
Installation
Install the extraction lens-omega lens assembly with the skimmer cone
attachment facing outward.
1 Install the extraction lens-omega lens assembly by passing the through hole
on the skimmer base over the interface guide pin, and push the assembly to
contact the interface.
2 Use an Allen wrench (3mm) to lightly tighten the three screws.
3 Firmly, but evenly tighten the screws, turning all screws in succession 2 to 3
times.
4 Install the Skimmer Cone and Sampling Cone.
For details on installing the Skimmer Cone and Sampling Cone, see
“Interface” on page 86.
Check the color and oil level of the pump on a weekly basis. The oil level needs to
be between Minimum and Maximum on the level gauge during pump operation.
If the oil is too low, add more oil. If it is above the Maximum, drain some oil from
the pump. Check the color of the oil. If the color is bad, change it. The average oil
change interval is every six months, although this depends on the daily sample
throughput, the type of sample, the concentration of the sample, etc.
The surface of the Foreline Pump may be HOT, do not touch the pump until it
WAR N ING has cooled.
Make sure to open the exhaust tube and line for safety.
Vacuum Hose
Exhaust Port
Exhaust Tubing
Vacuum Port
Power Cord
Oil Inlet
Oil Level Gauge
Tilt Stand Oil Outlet
Oil Tray
(Part Number: G8400-60315)
Oil Drain Kit
• Make sure to connect the inlet and outlet of the foreline pump correctly.
C AU T I O N
• Connect the exhaust hose from the foreline pump tightly with a hose clamp.
• When you install the foreline pump, make sure the coolant hose does not
touch the surface of the foreline pump. Heat will damage the hose and may
result in water leaks.
• When you turn off the foreline pump, wait at least 15 seconds before
restarting it.
Since the oil level changes depending on where the vane stops inside the pump,
NOTE make sure you check the oil level during pump operation. Run the pump for at
least 30 minutes and then check the oil level while the pump is still running.
It is important that the oil level stays within the range that is indicated by the level
gauge on the side of the pump.
To maintain the correct level, you need to add or drain oil as necessary.
Only use the pump oil appropriate for your pump. Using a different oil can
C AU T I O N substantially reduce pump life and invalidates the pump warranty.
You can replace the oil in the pump manually, as described in “Replacing the Oil
Manually” on page 106.
Be sure that the horizontal bar of the tilt stand sits flat on the floor when
C AU T I O N locking the wheels in the tilt position.
Lock
Horizontal Bar
As the pump is heavy, keep feet clear of the pump while it is elevated.
WAR N ING
If tray is not available raise the pump so that it is higher than the container being
NOTE used to collect the oil. Place something beneath the pump that is capable of
withstanding its weight and will not tip over.
6 Place a container under the hose end of the oil drain kit (see Figure 47).
7 Remove the fill plug from the oil inlet using the Hex key (see Figure 47).
8 Remove the cap of the check valve attached to the oil outlet, and then attach
the metal fitting of the oil drain kit (see Figure 47) to the check valve on the
outlet. Connecting the oil drain kit opens the check valve on the outlet to allow
the fluid to drain.
Take care when lowering the pump from the tilted position.
C AU T I O N
11 Using the supplied Nozzle cap pour in about 1 liter of the oil (see Figure 48).
Nozzle Cap
Venting Port
Oil Bottle
If the oil is particularly dirty or contaminated, it may be necessary to flush the oil
NOTE reservoir. To flush the oil reservoir:
• Refit the oil drain plug and pour clean oil into the pump.
• Restart the pump and operate it for 5 to 10 minutes.
• Follow the above steps again to drain the oil.
• Repeat until the oil reservoir is clean.
Figure 49.
Once the operation time has been reset, it is impossible to restore its original
NOTE value. Reset with care.
Routine Maintenance
Check the condition of the pump such as the power supply, ultimate pressure
and back pressure etc. regularly and check that the pump is used under normal
operating conditions.
Check that the exhaust hose from the foreline pump is not damaged or clogged,
and that it is securely connected.
Check that the ballast valve is in the open position if the pump has the ballast
valve. The ballast valve should be open at all times. The ballast valve may not be
present, depending on the model.
Filter
Open
Ballast Valve
NEODRY002
During operation, the level may be lower than the lower limit, this is normal and
does not indicate an error. Stop the pump and wait until the level stabilizes, and
then check the actual level.
A service call may be necessary if the oil level is below the lower limit on the level
gauge. Contact Agilent Technologies.
This pump can not repair at on site. It is recommended to replace the pump every
NOTE 4 years.
Water Strainer
A strainer is attached to the fitting connector in order for the cooling water chiller
to provide clean cooling water. Prolonged strainer use results in clogging and
water stains. Remove and inspect the strainer annually, cleaning when
necessary.
To maintaining the water strainer you need the following supplies:
• Drip pan and sponge
Cleaning
1 Turn OFF the cold water source.
Turn OFF the cooling water chiller and close the valve, if present.
2 Remove the water strainer cap.
Place the vessel under the working area as cooling water will spill out.
3 Open the strainer cap and remove the mesh filter.
4 Check the condition of the strainer and clean if necessary.
The strainer is metallic. Clean with tap water or 2% Citranox solution. Replace
the strainer if it is corroded.
5 Refit the strainer.
6 Be sure that the gasket is correctly positioned, before closing the cap.
7 Check for leaks.
Open the valve, if present. Turn the cooling water chiller power switch ON.
The standard peristaltic pump of the Agilent 7800/7850/7900 has three channels
to set tubing for the sample solution, internal standard solution, and the spray
chamber drain.
There are three types of sample uptake tubing:
• Tubing for sample uptake (white/white, 1.02 mm i.d.)
• Tubing (PharMed® ismaprene) for the drain (yellow/blue, 1.52 mm i.d.)
• Tubing for the internal standard (orange-blue, 0.25 mm i.d.)
The colors refer to the peristaltic pump head-stops bonded to the tubing.
These tubing are standard issue. The tubing for sample uptake and internal
standard can be used for almost all reagents including HF. However, there is a
minor contamination problem with Sn; about 100 ppt Sn was measured when
1 % HNO3 was analyzed after being pumped through new tubing. Sn elution can
be reduced to a negligible level by washing with HNO3 or HCl before use.
The lifetime of the tubing for sample uptake and internal standard is about two to
three weeks when 1 % (v/v) HNO3 is pumped; it depends on the acid
concentration analyzed and on the shoe pressure of the peristaltic pump. When
higher concentrations of acid are introduced, the tubing swells and becomes
white in color. However, this change of color does not cause any contamination
or affect the analysis.
PharMed® ismaprene is a good material for use with almost all reagents and has
a lifetime about 10 times longer than silicone. However, there are many
impurities in it, therefore it cannot be used for sample introduction, only for the
spray chamber drain.
Some chemicals attack the sample uptake tube. This might cause leakage in
C AU T I O N the sample introduction and drain lines and corrosion of the sample
introduction system.
The sample uptake rate at 0.1 rps peristaltic pump speed is about 0.4 mL/min
with 1.02 mm i.d. tubing. The sample uptake rate linearly increases as a function
of the peristaltic pump speed up to 0.5 rps; 2.0 mL/min is the maximum sample
uptake rate. 0.1 rps is recommended as the standard peristaltic pump speed, and
0.5 rps for faster sample exchange and wash out.
When the SPS 4 Autosampler is used, it takes about 25 seconds for the sample
exchange and 15 - 30 seconds for stabilizing the signal. Use 30 seconds on fast
pump followed by 20 - 40 seconds stabilization time when the SPS 4 is used.
The inner diameter of the sample transfer tube (PTFE) is 0.5 mm. A tube smaller
than 0.5 mm i.d. can cause the generation of bubbles in samples. This problem
may occur due to highly pressurized tap water that contains gases (drinking
water samples). It degasses when depressurized. In this case, the sample has to
be degassed prior to introduction.
The orange/blue tubing (0.25 mm i.d.) is used for the internal standard solution.
The sample uptake rate at 0.1 rps is about 40 µL/min. When the internal standard
solution is added to the sample by the peristaltic pump, the concentration of the
internal standard is diluted about 10 times. Therefore, a 1 ppm internal standard
solution in 5 % (v/v) HNO3 is recommended.
The orange/blue tube (0.25 mm i.d.) is very soft and easily stretched. This
NOTE sometimes causes an instability of the sample uptake rate when the peristaltic
pump speed is varied drastically: the tube stretches at higher peristaltic pump
speeds and does not recover to its original length immediately when the
peristaltic pump speed is reduced to 0.1 rps. If the higher pump speed is not
used, it takes about 2 minutes for the sample exchange at 0.1 rps.
When the internal standard is added to a sample by means of the peristaltic
pump, the maximum peristaltic pump speed should be 0.3 rps. When this fast
pump speed is applied in order to reduce sample exchange time, a longer
stabilization time is required. Use 0.3 rps fast pump for 50 sec and 50 sec
stabilization time.
When orange/blue tubing (0.25 mm i.d.) is used, some adsorption can occur on
the walls of the tubing. Some elements such as Au, Ag, Pd and Pt are adsorbed
onto the tubing and it takes a long time to get stable signals. Alkali, alkali-earth,
and transition metals are not adsorbed. This adsorption may occur with the
white/white (1.02 mm i.d.) tubing as well, but the sample uptake rate is much
larger than with the orange/red tubing making the adsorption negligible. In order
to minimize this problem, HNO3 has to be added to the samples and standard
solutions; a concentration of at least 1 % (v/v) HNO3 is required and preferably
5 % (v/v) HNO3.
Spray Chamber
There are several types of spray chambers for ICP-MS. The Agilent
7800/7850/7900 uses the Scott-type double-pass spray chamber. The Agilent
ICP-MS spray chamber is available in the following materials:
• Quartz (QZ)
• PFA
The spray chamber is mounted in an aluminum block and cooled by a Peltier
thermoelectric module. The standard spray chamber temperature is maintained
at 2 °C for aqueous samples, and can go down to -5 °C for organic solvents or
higher vapor pressure samples. When the spray chamber temperature is
unstable, water loading to the plasma is affected, causing signal instability.
Higher spray chamber temperatures increase the oxide ion level as well. A drain
tube is connected to the spray chamber by means of a special cap that allows
easy attachment and detachment.
Quartz
The quartz is made of pure silica and it can be used for acids and organic
solvents, but not for HF or strong alkaline solutions. To reduce memory effects,
soak the quartz spray chamber in a 5 % NH4OH (v/v) solution for 2 hours prior to
use, followed by washing with pure water.
PFA
This PFA spray chamber is the standard spray chamber for the inert sample
introduction kit, and is used when aspirating hydrofluoric acid.
ICP Torch
The Agilent ICP-MS employs a Fassel type torch. There are three Ar gas lines:
plasma gas, auxiliary gas, and nebulizer gas. The plasma gas flow is tangentially
introduced into the outer sheath of the torch at about 15 L/min. Its role is to cool
the torch itself and to sustain the plasma. The auxiliary gas is also tangentially
introduced into the middle sheath of the torch at about 1 L/min. Its role is to push
the plasma forward in order to avoid melting the sample injector tip. The
nebulizer gas is introduced into the center of the torch through the injector.
In the case of the Agilent ICP-MS, the standard torch is a one-piece design and is
made of quartz. The inner diameter of the injector is 2.5 mm. For HF solutions, a
platinum (or sapphire) injector is used as the inert introduction system. The
injector is removable and a demountable torch is used.
The optimal nebulizer and makeup gas flows depend on the diameter of the
injector. It is about 1.2 L/min for the φ2.5 mm injector.
Interface
Ions in the plasma are extracted into the vacuum chamber through a sampling
cone and a skimmer cone. The orifice size of the sampling cone is φ1.0 mm and
that of the skimmer cone is φ0.4 mm on 7800/7850 (φ0.45 mm on 7900). There
are two types of material used, nickel (Ni) and platinum (Pt).
The base material of the sampling cone is Cu and the tip of the cone is Ni or Pt.
The skimmer cone is all Ni. Pt has to be used for HF solutions and higher
concentration of acids. The base material is Cu or Ni and the tip of the cones is Pt
for the sampling and skimmer cone.
There are two types of skimmer base: stainless steel and brass. The brass base
can be used for both the Ni and Pt skimmer cones. The stainless steel base is
only used and recommended for the Ni skimmer cone.
When H2SO4 and H3PO4 are analyzed, the Pt interfaces should be used.
When 10% H2SO4 or 1% H3PO4 are analyzed continually, a sampling cone with a
NOTE larger diameter (18 mm) Pt insert (available from Spectron) is recommended.
Each interface normally lasts more than one year, although it depends on the
type of samples analyzed and the plasma conditions. If the interface is removed
and cleaned more often, for example when switching between clean and dirty
matrices, the interface lifetime will be reduced due to physical wear.
ORS
The ORS is an octopole ion guide contained within a metal vessel and
pressurized with a gas, most often H2 or He. The ORS is positioned between the
ion lens assembly and the quadrupole mass filter. As ions from the sample enter
this cell, they interact with the gas, resulting in the reduction of spectral
interferences.
place. However, this does not necessarily mean that all types of reaction or
interaction between H2 and the analyte ions is negligible. When the H2 flow rate is
increased, Cu+ and As+ signals begin to decrease, however the loss of those ions
is relatively small compared with the loss caused by other more reactive gases. If
the background level is so high as to need a high flow rate of H2, the use of less
reactive gas such as He can be more effective. For example, He efficiently
dissociates NaAr because of its low bonding energy, while it does not cause a
severe loss of Cu ion.
A2+ + H2 → Ar2H+ + H k=1x10-9cm3/s
Se+ + H2 → Se+ + H2 no reaction
+ +
NaAr + He → Na + Ar + He dissociation
Cu+ + He → Cu+ + He no reaction
Quadrupole
The quadrupole of the Agilent ICP-MS consists of a pre-filter and a main filter.
The inner surface of the quadrupole rods is hyperbolic giving an ideal electrical
field inside the quadrupole.
Only RF voltage is supplied to the pre-filter, while RF and DC voltage is supplied to
the main filter. The purpose of the pre-filter is to direct ions from the ORS along
the right path into the main filter. RF voltage (V) and DC voltage (U) are supplied
to the main filter (Figure 52). When the highest mass 260 is analyzed, typically
maximum 559 V of DC voltage and maximum 3,338 V of RF voltage are supplied.
In addition, the DC bias voltage (referred to as PB in Figure 52) is supplied to the
quadrupole. This quadrupole bias controls the averaged DC potential in the
central area of the quadrupole where ions travel thereby controlling ion velocity in
the axial direction. Therefore, the pole bias can be used to implement kinetic
energy discrimination by which low energy ions are blocked by the quadrupole
potential while high energy ions are allowed to pass through the quadrupole. This
is the technique used with ORS to remove spectral interferences. Only an Agilent
Technologies engineer should perform quadrupole maintenance.
average voltage
PB - U - V cos w t Ground
U
238U
max.
513 V
Li
max. 3056 V V
Figure 53. Scan Line of Quadrupole Mass Filter
The scan line of a quadrupole is represented in Figure 53. The mass of ions that
are allowed to pass through the quadrupole to the detector is approximately
proportional to U and V, both of which are ramped rapidly along this scan line to
detect ions of multiple masses virtually simultaneously.
The EM used in the Agilent ICP-MS is a discrete dynode type, operated in both
pulse count and analog modes. A brief description of the principle of operation is
described below.
Pulse mode: When an ion enters the EM, the ion hits the first dynode and a
shower of electrons is generated. The electrons hit the next dynode generating
more electrons. This small signal is amplified and a higher pulse signal is
obtained: electrons are multiplied about 106 times. Finally, the pulse generated is
detected by the collector. The pulse width is about 20 nsec. At this moment, the
output signal from the multiplier contains electrical noise and the pulse signal.
After the signal is amplified, a discriminator circuit eliminates the electrical noise.
Then, pulse signals higher than the discriminator voltage are converted to an
ideal pulse shape. This pulse is measured as one ion count (Figure 54).
Analog mode: When the concentration of an element is high, the ions of that
element will not be measured as individual pulses because the interval of ions
entering the EM is often too short to separately measure them. In general, this
phenomenon becomes more critical when the average number of ions entering
the EM per second is greater than several millions. At count rates higher than 1.3
million counts/s (cps) for the 7900 (0.9 Mcps for the 7800/7850), the electrical
current at the collector connected to an intermediate dynode is measured by the
analog mode. The current is converted to log- voltage by the log amp. Then it is
sampled by the A/D converter, and is accumulated by the accumulator. The
accumulated value is then converted to ion counts by the P/A factor (Figure 54).
The EM operates in dual mode, that is, either in pulse or analog mode for each
element (mass) in each sample.
For adjustment of the dual mode, a P/A factor must be set.
+ HV
Electron Multipiler (EM)
Ions
- HV
Discrimi-
nator
Counter MassHunter Workstation
Pre-amp
Anti-log Accumu-
Logic lator MassHunter Workstation
Log-amp
7700_0109
When data acquisition starts, the CPU board automatically selects the pulse or
analog mode for each mass (element) to be analyzed. The threshold level
between the two modes is about 1.3 Mcps for the 7900 (0.9 Mcps for the
7800/7850).
When the EM mode is set to AUTO in method and the signal exceeds the
threshold, the signal is measured by analog mode only. If the count rate of a
certain mass exceeds 10 Gcps for the 7900 (4 Gcps for the 7800/7850), which
cannot be measured even by analog mode, the detection of this mass will be
skipped automatically to protect the EM. After finishing data acquisition, the data
is transferred to the MassHunter Workstation for data analysis.
The time for EM replacement can be judged by the EM voltage (Analog HV and
Pulse HV). The EM can be used until the Analog HV reaches 3500 V or the Pulse
HV reaches 2000 V, after adjusting the EM voltage. However, it is recommended
to replace EM well in advance.
1 Digital ground
2 N/A
3 Start Low
4 Shutdown Low
5 N/A
6 N/A
7 N/A
8 N/A
9 N/A
Appendix B. Troubleshooting
The ICP-MS Web Utility is an application that allows you to perform configuration
operations such as setting and restoring the IP address for the ICP-MS. To open
the ICP-MS Web Utility:
• Place the ICP-MS in SHUTDOWN mode (if using the Utility to change IP
address).
• Type the current ICP-MS IP address into the browser address bar on a
computer that is on the same LAN segment as the ICP-MS. Preferred browser
is Internet Explorer 8/9/11.
• Refer to the Help pages within the Web Utility for further explanations on use
of the utility.
3rd Cell Gas is available when the optional gas line is installed.
NOTE
If an H2 gas line is not connected, H2-gas-related items are grayed out and
cannot be selected.
Excessive amounts of cell gas raises the pressure in the vacuum chamber and
C AU T I O N the instrument safety feature will put the instrument in to shutdown mode.
When introducing the cell gas, increase the gas flow rate gradually maintaining
a good operating vacuum pressure.
To open the Cell Gas Line Maintenance table, complete the following steps:
1 Click the Collision/Reaction Cell illustration in the Dashboard pane, and then
click Maintenance.
The following information is displayed in the Cell Gas Line Maintenance table.
• Output (Column): Sets each cell gas flow rate.
• Open Bypass Valve (Icon button): Click icon, and opens valve. When close the
valve, click icon again.
• H2 Gas Flow Rate: H2 gas flow rate setting. Enter the flow rate value in the text
box.
• He Gas Flow Rate: He gas flow rate setting. Enter the flow rate value in the
text box.
• 3rd Cell Gas Flow Rate: 3rd gas flow rate setting. Enter the flow rate value (%)
in the text box.
• Input (Column): Current value.
The maximum flow rate of each gas is as follows:
• H2 gas: 10 (mL/min)
• He gas: 12 (mL/min)
• 3rd cell gas: 100 (%) [= 10 mL/min]
General
When analyzing organic solvents, Oxygen must be added in to the nebulizer gas
line to burn the carbon in the organic solvent. This will avoid depositing the
carbon on to the interface (Sampling cone / Skimmer cone). If the deposition is
allowed to build up the interface cones can clog.
A 1.5 mm (or 1 mm) I.D. torch is used for organic solvent samples to maintain
good plasma conditions. The drain volume when introducing the organic solvent
is smaller than when introducing aqueous solutions and most of the organic
solvent sample is introduced into the torch and it may extinguish the plasma
easily. So, it is necessary to use 1.5 mm I.D. torch to reduce the sample loading
on the plasma.
Be sure to wear solvent resistant gloves and protective glasses when handling
WAR N ING organic solvents.
Make sure that none of the drain lines are leaking (e.g. the Spray Chamber
WAR N ING outlet).
If there is a leak, there is a greater risk of explosion.
Drain Tubing
Flow Direction
(Drain Vessel) (Peristaltic Pump)
• When no flow is observed in the drain line, readjust the clamp tension for
drain tubing or replace the drain tubing.
• There is normally liquid and air as shown above. When there is only liquid,
tighten the clamp an additional turn or reduce sample uptake volume by
decreasing the nebulizer gas flow.
Make sure that the drainage is flowing. Check that the tube from the drain
WAR N ING peristaltic pump to the drain bottle is properly connected. You should see a
regular pattern of liquid and air as shown above.
When the spray chamber drain is not pumped properly, excess flammable
WAR N ING solvents in the spray chamber may ignite and explode. Make sure that the
spray chamber drain is being pumped properly during analysis.
If you introduce a sample that has a tendency to solidify, such as photoresist,
make sure that the spray chamber drain is being pumped properly and that the
torch injector is not becoming clogged.
Perform a daily inspection to make sure the drain tubing is not damaged.
WAR N ING Otherwise the risk of explosion increases.
Pump out the solvent in the drain line after analysis. The lifetime of the tubing
WAR N ING is drastically reduced if organic solvent remains in the drain tubing.
When pulling out the drain connector, remove it slowly so that the solvent left
WAR N ING inside the tubing does not scatter.
Pump out the solvent in the sample introduction lines, spray chamber, and
drain line after you finish an analysis. The lifetime of the tubing is drastically
reduced if organic solvent remains in the tubing.
Warning Label
Put the warning label in the kit on the left side of the body enclosure.
Table 8. Organic solvents having confirmed methods for the Agilent ICP-MS (Nebulizer; Concentric)
*
Organic solvent Dilution factor Sample tubing id Torch injector id Oxygen % in total
(mm) (mm) nebulizer & makeup
gas
General
Item Q’ty
Connector Tube 1
Torch 1
The surface of the PFA is slippery. Use the latex laboratory gloves when
C AU T I O N installating or removing of the PFA component,.
Mounting
1 First, switch the instrument to Standby mode and then remove the following
parts from the instrument.
• Connector tube clips and connector tube
• Torch
• Spray chamber and the connected tubes
• Spray chamber chiller (upper and lower parts) and connector
There is a plastic screw-in locking bolt on the underside of the spray chamber
NOTE chiller which fixes the spray chamber chiller (lower part) to the bracket. Loosen
this locking bolt to move the spray chamber chiller. If the bracket on the Agilent
7900 is fixed on the lower position, the bracket needs to be moved to the upper
position.
Bracket
7700_0219
Figure 59.
2 Assemble the parts as shown in the following figures. Please fit the parts
together with care, but firmly.
Injector
Bonnet, Torch Shield
Spray Chamber Plate (Reuse existing)
Torch
Connector Tube
Drain Tube
End Cap
7700_0217
Figure 60.
3 When the torch, injector and connector tube are assembled, install in the
instrument.
7700_0218
Figure 61.
On installing the spray chamber, connect to the injector while gently but firmly
C AU T I O N holding the connector tube against the connector tube guide. Be careful as any
pressure applied on the torch could cause breakage.
Figure 62.
5 Connect the chilled water hose and tighten the plastic locking bolt.
6 Connect the plasma gas and auxiliary gas tubing to the torch.
When the DILUTION / OPTION GAS is not used, remove the tubing from the
NOTE instrument.
7 Install the upper part of the spray chamber chiller and connect the makeup
gas tubing and drain tubing. Install the nebulizer and connect the sample
tubing and nebulizer gas tubing.
8 Installation is now complete. Please note the following:
For removal of the inert kit, please simply follow the reverse procedure. PFA parts
NOTE only (not torch parts) can be washed in a solution of 5% nitric acid and 5%
hydrofluoric acid by soaking for 8 hours.
This procedure explains the removal, disassembly, and cleaning method for
individual lenses, and the reassembly of the ORS cell used in the Agilent ICP-MS.
It is necessary to open the vacuum chamber to clean the ORS cell. Refer to the
procedure “Opening/Closing the Vacuum Chamber” on page 142 for an
explanation of the correct method for this procedure.
To minimize maintenance time, clean the ORS cell first. While cleaning the cell,
replace the chamber cover and start the pumps. After cleaning, reassemble and
install the ORS cell assembly, clean the Extraction Lens-Omega Lens assembly.
Before opening the vacuum chamber to clean the ORS cell or for other
C AU T I O N purposes, always switch OFF the power to the ICP-MS.
Pure water used for cleaning is indicated as water that has been generated using
NOTE the ion-exchange method and a membrane filter, and has an electrical resistance
of at least 18 MΩ cm.
Do not allow the parts in the vacuum chamber to become stained in any way.
C AU T I O N Always use clean laboratory gloves and handle the components in a
contamination free place.
Avoid contaminating or damaging the O-ring and flange surfaces.
Contaminants and damage may cause the vacuum to leak.
It is necessary to open the vacuum chamber when removing the ORS cell. It is
NOTE not necessary to open the vacuum chamber when you are removing the
Extraction Lens-Omega Lens assembly.
Vent Valve
7700_0086
3 When the vacuum chamber has equalized, use an Allen wrench (4mm) to
loosen the bolts. Remove the vacuum chamber lid.
Place the vacuum chamber lid down with the inner surface facing upward to
avoid contamination.
4 Be sure to close the vent valve after removing the vacuum chamber lid.
To avoid leaving the valve open, when pumping down the system afterwards.
When not performing any maintenance inside the vacuum chamber, cover the
NOTE chamber with the lid to prevent contamination.
During longer maintenance periods such as when cleaning the ion lens, close the
lid on the vacuum chamber and pump down the ICP-MS to Standby mode.
Do not grease the O-ring of the vacuum chamber cover. If you accidentally get
C AU T I O N grease on your gloves while you are working, you can potentially contaminate
the lens and other components.
2 After confirming that all components are positioned correctly inside the
vacuum chamber, place the lid on the vacuum chamber.
3 Check that the lid is placed correctly, and use an Allen wrench (4 mm) to
tighten the bolts temporarily.
4 Confirm that the vent valve on the vacuum chamber is closed.
5 Pump down by turning ON the main switch, waiting until the red light of status
indicator turns off and carrying out one of the following methods.
• Press the vacuum ON/OFF switch until the status indicator begins to blink.
• Re-start MassHunter.
Click the Mainframe illustration in the Dashboard pane, and then click
Vacuum On. After a short delay the pump will being operating and the
pump down will start. (Changing from Shutdown mode to Standby mode)
6 When the status indicator has changed to orange, check the MassHunter
screen to confirm that, the instrument has transitioned to Standby mode.
When the upper cover is opened for a long period of time, or the humidity is high,
NOTE it can take longer for the ICP-MS to reach Standby mode if any components have
been replaced or cleaned.
If the ICP-MS does not reach Standby mode within 5 hours an error will be
generated. After acknowledging the error, change the ICP-MS to Standby mode
again.
7 Use an Allen wrench (4 mm), to further tighten the screws of the vacuum
chamber lid.
Turn OFF the power to the instrument before you remove the ORS Cell
WAR N ING assembly from the vacuum chamber. Otherwise, you could expose yourself to
the extreme danger of contact with high voltage electricity.
1 Loosen the vent valve to equalize the pressure in the vacuum chamber and
remove the chamber lid.
Refer to the “Opening/Closing the Vacuum Chamber” on page 142 in this
chapter.
2 Disconnect the cell gas tube.
3 Disconnect the connectors and remove the cell gas tubing.
Disconnect the ORS Cell Connectors (two) from the ORS cell assembly. And
remove the cell gas tube from the vacuum chamber.
4 Disconnect the plate bias wire and deflect lens wire.
ORS Cell
Mounting Screw
7700_0091
Plate Bias
Deflect Lens
Screws (2)
7700_0428
Figure 66. Location of the Deflect Lens and Plate Bias Lens (with the ORS Cell Assembly Removed)
It is necessary to remove the ORS cell assembly before removing the Plate Bias
Lens.
1 Remove the Deflect Lens and Plate Bias Lens.
Loosen the 2 screws securing the Deflect Lens and Plate Bias Lens and
remove the Cell Exit Guide, Deflect Lens, Spacer and Plate Bias Lens.
Plate Bias
Spacer
Deflect Lens
Cell Exit
Connector Hole
Screws (2)
7700_0429
Disassemble the ORS cell assembly in an area free of contamination and while
C AU T I O N wearing clean laboratory gloves and use only clean tools.
When cleaning the ORS cell assembly, layout the dismantled components in the
NOTE order of their original configuration.
1 Loosen the Cell Entrance and Exit Lens assembly screws a quarter turn.
To avoid damage to the Octopole from force applied while dismantling the
Octopole in the next procedure, loosen the Cell Exit Lens assembly screws
and the Cell Entrance Lens assembly screws a quarter turn prior to
disassembly.
Only loosen the Cell Entrance and Exit Lens assembly screw a quarter turn.
NOTE Loosening the screws more than that could cause the components to come
apart and make the task more difficult.
2 Remove the 4 screws on the lower block of the ORS cell assembly.
3 Place the ORS cell assembly on a clean surface.
Remove the upper block, and then place the removed block on a clean
surface.
Octopole Shaft 1
Cell Exit Lens
Cell Entrance Lens
Octopole Shaft 2
Cell Focus, Spacer
Groove
7700_0093
Do not directly touch the rods of the Octopole. You may accidentally mis-align
C AU T I O N the Octopole.
The Cell Focus, Cell Entrance Lens, Cell Exit Lens and spacer are located on
either side of the Octopole. When removing the Cell Entrance Lens or Cell Exit
Lens, only remove one at a time, leaving the other Lens or Octopole plate
assembled. This will prevent you from potentially mis-assembling the lenses to
the wrong side.
The Cell Focus, Cell Entrance Lens, Cell Exit Lens, and spacer are shaped and
NOTE structured differently.
Spacer
Cell Focus
Octopole
Octopole Plate
Octopole
7700_0096
Octopole Plate
Spacer
Cell Focus
7700_0097
Figure 73. The Octopole with the Cell Entrance Lens and Cell Exit Lens Removed
Use a large beaker to prevent the rods of the Octopole are contact with the wall of
NOTE the beaker. The Octopole may become misaligned.
1 Using the blue (#400) polishing paper, thoroughly clean the interior and
exterior of the lenses.
Be sure to thoroughly clean the orifices through which the ion beam passes.
Take care not to deform the orifices when polishing the lenses. Any damage
may affect instrument performance.
2 Repeat the cleaning procedure using the yellow (#1200) polishing paper.
3 Use a cotton swab with alumina paste mixed from alumina powder and pure
water to polish the interior and intricate parts of the lenses.
Primarily polish the lens orifices.
4 Rinse with pure water.
5 Ultrasonic the lenses in pure water for 5 minutes.
6 Dry on a clean surface.
Allow the lenses to air dry, do not wipe.
Do not clean plastic components (spacers) with organic solvents. The plastic
C AU T I O N will be damaged or deformed if it comes in contact with organic solvents.
Completely dry all components. If components are connected to the vacuum
chamber before they have completely dried, it will take an extraordinarily long
time to pump down to Standby mode.
If the printed circuit board has been removed from the Cell’s upper block, pay
attention to the direction when re-attaching it. If it is incorrectly installed, the
bottom connector of the printed circuit board will hit the Cell’s upper block and
cannot be attached properly.
It is not normally necessary to clean the Cell’s upper and lower blocks.
NOTE
However, if these have been touched by bare hands or have oil on them, wipe
clean with alcohol (IPA or ethanol).
Remove the heater, temperature sensor and printed circuit board from the Cell’s
upper block and allow it to dry thoroughly.
The Cell Focus, Cell Entrance Lens, and Cell Exit Lens are different.
NOTE
The cell entrance lens should be refitted on the longer extruding side of the
octopole. The cell exit lens should be refitted on the shorter side. Take care to
refit the lenses onto the correct sides.
2 Remove the Octopole plate from the cell exit lens side. Refit the cell exit lens.
Lightly tighten the cell exit lens screws.
Octopole
7700_0096
3 Remove the octopole plate from the cell entrance lens side. Refit the cell
entrance lens, spacer and cell focus. Lightly tighten the cell entrance lens
screws.
Spacer
Cell Focus
The two shafts on the Octopole are of different diameters to prevent the Cell
C AU T I O N Entrance Lens and Cell Exit Lens from being mis-assembled. Pay careful
attention to the direction of the lenses when assembling.
Always remove only one Octopole support plate (located on both sides of the
Octopole assembly) at a time, leaving the other support plate assembled to the
other Cell Entrance Lens / Cell Exit Lens. Removing both at the same time can
lead to confusion when it comes time to refit the instrument.
Do not directly contact the rods of the Octopole. The Octopole may become
misaligned.
5 Fasten the cell block screws on the bottom of the ORS cell assembly. Tighten
the screws evenly.
Octopole Assembly
7700_0100
6 Now securely fasten the screws on the cell entrance lens and cell exit lens
that were only lightly tightened before.
Cell Focus
Figure 77. Checking the continuity (Cell Lower Block and Connector Electrodes)
• Also check that the pin terminals are insulated from each other.
Ohmmeter
7700_0102
Cell Focus
2 Tighten the mounting screw, securing the ORS cell assembly to the vacuum
chamber.
3 Connect the wires.
Insert the wire leading to the plate bias lens and the wire leading to the Deflect
lens into the terminal installation section.
4 Connect the wire connectors.
Connect the heater/sensor and ORS cell connectors to the ORS cell assembly.
5 Connect the tube.
Connect the cell gas tube to the ORS cell assembly.
Before installing the vacuum chamber lid, check the heater cable and
NOTE temperature sensor cable are connected to the terminals on the cell.
ORS Cell
Mounting Screw
Some models of the Agilent ICP-MS use Hydrogen (H2) gas. While the Agilent
WAR N ING ICP-MS is designed for safe operation under normal usage, Hydrogen gas has
the following characteristics and extreme care must be taken to safely control
its use.
• Hydrogen is flammable over a wide range of concentrations. At atmospheric
pressure, Hydrogen is combustible at concentrations from 4% to 75%.
• Hydrogen has the highest burning velocity of any gas.
• Hydrogen has a very low ignition energy.
• Hydrogen temperature increases as the gas expands.
• Hydrogen that is allowed to expand rapidly from high pressure can actually
self-ignite.
• Hydrogen burns with a nonluminous flame that is often invisible under
bright light.
Use deliberate and careful judgment when shutting down the ICP-MS. The
WAR N ING ICP-MS can also be shut down accidentally by an internal or external failure.
Even though the ICP-MS is shut down, Hydrogen still remains in the vacuum
system. As a result, Hydrogen may slowly accumulate in the vacuum pump line
and possibly vent through the foreline pump oil mist filter to the exhaust duct
of the ICP-MS. Make sure the exhaust duct is always operating.
Necessary Precautions
Some models of the Agilent ICP-MS use Ammonia (NH3) gas. While the Agilent
WAR N ING ICP-MS is designed for safe operation under normal usage, Ammonia gas has
the following characteristics and extreme care must be taken to safely control
its use.
• Flammable in the presence of open flames and sparks.
• Explosive (explosion limit 15-28 vol% in the air).
• Contact with chemicals such as mercury, halogen, silver oxide or
hypochlorites can form explosive compounds.
• Irritant and corrosive to skin, eye, respiratory tract and mucous membranes.
Use deliberate and careful judgment when shutting down the ICP-MS. The
WAR N ING ICP-MS can also be shut down accidentally by an internal or external failure.
Even though the ICP-MS is shut down, Ammonia still remains in the vacuum
system. As a result, Ammonia may slowly accumulate in the vacuum pump line
and possibly vent through the foreline pump oil mist filter to the exhaust duct
of the ICP-MS. Make sure the exhaust duct is always operating.
Necessary Precautions
The following are general precautions that should be taken to prevent dangers
WAR N ING and effects of Ammonia gas. Other precautions may be necessary depending
on the setting and configuration in which you use the system. Pay careful
attention to safety management when using this system.
• Store in cool, well-ventilated area with containers tightly closed.
• Make sure the Ammonia gas line is without leaks.
• Periodically check equipment for Ammonia leaks using the appropriate
devices (leak detector, pressure test, etc.).
• Eliminate from your laboratory as many ignition sources as possible (open
flames, devices that can spark, sources of static electricity, etc.).
• Always turn off the Ammonia gas at its source whenever you turn off the
ICP-MS.
• Always turn off the Ammonia gas at its source before opening the vent valve
or introducing ambient air into the ICP-MS.
• Turn off the Ammonia gas at its source as soon as a power failure occurs.
Do not resume operation of the ICP-MS before inspecting it for damage or
irregularities.
• The exhaust duct should always be operating. Ammonia gas released while
the exhaust duct is not operating can result in accumulation of the gas in the
ICP-MS and/or the exhaust duct.
• The safety for external gas line is the customer's responsibility.
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© Agilent Technologies, Inc. 2022
*G8400-90015*
Part Number: G8400-90015
Printed in USA
August 2022 Document Revision: A.00