Agilent Technologies 5100 ICP-OES User manual

Agilent 5100 and 5110
ICP-OES
User’s Guide

2 Agilent 5100 and 5110 ICP-OES User’s Guide
Notices
© Agilent Technologies, Inc. 2014,
2016, 2017, 2018
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Manual Part Number
G8010-90002
Edition
Sixth edition, July 2018
Printed in Malaysia
Agilent Technologies, Australia (M)
Pty Ltd
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Mulgrave, Victoria, 3170
Australia
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Safety Notices
A CAUTION notice denotes a hazard.
It calls attention to an operating
procedure, practice, or the like that, if
not correctly performed or adhered to,
could result in damage to the product
or loss of important data. Do not
proceed beyond a CAUTION notice
until the indicated conditions are fully
understood and met.
A WARNING notice denotes a
hazard. It calls attention to an
operating procedure, practice, or the
like that, if not correctly performed or
adhered to, could result in personal
injury or death. Do not proceed
beyond a WARNING notice until the
indicated conditions are fully
understood and met.
WARNING
CAUTION

Contents
Agilent 5100 and 5110 ICP-OES User’s Guide 3
Contents
1. Safety Practices and Hazards 7
General 7
Verifying Safe State 8
Plasma 8
Heat, Vapors and Fumes 9
Compressed Gas Hazards 10
Electrical Hazards 11
Other Precautions 11
Warning Symbols 13
CE Compliance 14
Electromagnetic Compatibility 15
EN55011/CISPR11 15
ICES/NMB-001 16
South Korean Class A EMC declaration 16
2. Introduction 17
Site Preparation Requirements 17
User Documentation 18
Conventions 18
Notes and tips 18
Specifications 19
Temperature control 19
Environmental conditions 19

Contents
4 Agilent 5100 and 5110 ICP-OES User’s Guide
Electrical Power Supplies 19
Circuit breaker 19
Other Connections 20
Personal Computer Requirements 20
Gas Supplies 20
Exhaust system 21
ICP-OES instrument cooling air supply 21
Water Chiller System 22
Drain Vessel 23
3. Installation 25
Agilent ICP-OES Instrument Overview 26
Instrument Status LED Color Coding 28
Front Power On/Off Button 28
ICP Expert Software 29
Connecting ICP Expert software to the ICP-OES 30
Performing a Detector and Instrument Calibration 30
Saving and viewing the calibration data 32
Hardware Components Replacement 32
ICP-OES torches 33
Torch Assembly and Disassembly 34
Torch assembly 35
Torch disassembly 37
Accessories 38
SPS 4 39

Contents
Agilent 5100 and 5110 ICP-OES User’s Guide 5
SPS 3 39
Advanced Valve System (AVS) — AVS 4, AVS 6 and AVS 7
39
SVS 2 and SVS 2+ 40
5-channel Peristaltic Pump 40
External Inlet Duct Adapter 41
Air inlet dust filter 41
Vapor Generation Accessory (VGA) 41
Multimode Sample Introduction System (MSIS) 41
Argon Humidifier 42
IsoMist Programmable Temperature Spray Chamber 42
4. Operation 43
Analysis Checklist 43
Turning On the Instrument and Software 44
Turning on the instrument for the first time (or from long
term shutdown) 44
Running the instrument from an idle state 45
Preparing for Analysis 46
Performing a Detector and Instrument Calibration 46
Creating/Opening a Worksheet 47
Creating a new worksheet 47
Opening an existing worksheet 47
Creating a new worksheet from a template 47
Developing a Method 47
Running Samples 49
Printing a Report 50

Contents
6 Agilent 5100 and 5110 ICP-OES User’s Guide
Instrument Idle State 50
Setting the instrument to idle 50
Turning off the instrument for long term shutdown 52
5. Maintenance and Troubleshooting 55
Routine 56
Cleaning 58
Torch Cleaning 58
Acid cleaning of the torch for aqueous or acid based
samples 59
Rinsing the torch 61
Drying the torch 62
Additional checks after cleaning 63
Troubleshooting 63
Spare Parts 63
Technical Support 64

Safety Practices and Hazards
Agilent 5100 and 5110 ICP-OES User’s Guide 7
1. Safety Practices and Hazards
General 7
Verifying Safe State 8
Plasma 8
Heat, Vapors and Fumes 9
Compressed Gas Hazards 10
Electrical Hazards 11
Other Precautions 11
Warning Symbols 13
CE Compliance 14
Electromagnetic Compatibility 15
General
Unless otherwise specified, statements in this manual apply to both
the Agilent 5100 and 5110 ICP-OES instruments.
Operation of an Agilent ICP-OES involves the use of compressed
gases, high voltage radio frequency energy and hazardous materials
including corrosive fluids and flammable liquids. Careless, improper
or unskilled use of this spectrometer or chemicals used with it can
cause death or serious injury to personnel, and/or severe damage to
equipment and property. Only trained personnel should use this
instrument.
The spectrometer incorporates interlocks and covers that are
designed to prevent inadvertent contact with any potential hazards.
If the instrument is used in any manner not specified by Agilent, this
protection provided by the equipment may be impaired. It is good
practice to develop safe working habits that do not depend upon the
correct operation of the interlocks for safe operation. It is essential
that no interlock or cover is bypassed, damaged or removed.

Safety Practices and Hazards
8 Agilent 5100 and 5110 ICP-OES User’s Guide
The safety practices described below are provided to help the user
operate the instrument safely. Read each safety topic thoroughly
before attempting to operate the instrument and always operate the
spectrometer in accordance with these safety practices.
Verifying Safe State
The following general safety precautions must be observed during all
phases of operation, maintenance and service of this instrument.
To ensure continued safety of the instrument after maintenance or
service procedures verify the instrument is returned to a safe state
for the user. This includes running performance checks to verify the
instruments safety systems are functioning correctly. Check the
general condition of the instrument during operation for wear or
signs of corrosion that are likely to inhibit function or safety.
Failure to comply with these precautions or with specific warnings
elsewhere in this manual violates safety standards of design,
manufacture, and intended use of the instrument. Agilent
Technologies assumes no liability for the customer’s failure to
comply with these requirements.
Plasma
The plasma is extremely hot (about 10,000 °C) and radiates
dangerous levels of radio frequency (RF) and ultraviolet (UV) energy.
The work coil operates at 1,500 V RMS and about 27 MHz. Exposure
to the RF and UV energy can cause severe skin damage and cataracts
of the eyes, while close contact with the operating plasma can result
in severe heat burns to the skin, and an electrical discharge that can
jump a considerable distance and may cause death, severe electric
shock or sub-surface skin burns.
The plasma must never be operated unless:
the plasma compartment door is closed, with the door handle
fully closed; and
the space above the chimney and air intake is clear of objects.

Safety Practices and Hazards
Agilent 5100 and 5110 ICP-OES User’s Guide 9
The shielding around the torch compartment is designed to reduce
UV, visible and RF radiation to safe levels while still permitting easy
access to, as well as installation and viewing of, the torch. The
spectrometer has an interlock system that is designed to extinguish
the plasma if the mains supply fails, the handle on the torch
compartment door is opened, or the torch loading handle is open. Do
not attempt to bypass the interlock system.
Before opening the torch compartment door, always extinguish the
plasma by pressing SHIFT + F5 on the keyboard or by clicking the
‘Plasma Off’ icon on the ICP Expert software toolbar.
The torch and its surroundings remain hot for up to five minutes
after the plasma is extinguished. Touching this area before it has
cooled sufficiently may result in burns. Allow the torch and torch
compartment to cool before carrying out any work in this area, or
wear heat-resistant gloves.
The plasma system has been carefully designed to operate safely and
effectively when using torches and related components that conform
to Agilent’s design criteria. Use of non-approved components in the
plasma compartment may render the system inoperative and/or
hazardous. It may also invalidate the warranty on the instrument.
Use only torches and related components supplied or authorized by
Agilent.
Heat, Vapors and Fumes
Heat, ozone, vapors and fumes generated by the plasma can be
hazardous, and must be extracted from the instrument by means of
an exhaust system. Ensure that an exhaust system of the appropriate
type is fitted (as specified in the Site Preparation Guide). The system
must be vented to the outside air in accordance with local regulations
and never within the building. Regularly check the exhaust system by
smoke test to ensure that the exhaust system is functioning correctly.
The exhaust system must always be switched on before igniting the
plasma.

Safety Practices and Hazards
10 Agilent 5100 and 5110 ICP-OES User’s Guide
Compressed Gas Hazards
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 (except that of air or oxygen) can result in an
oxygen-deficient atmosphere, which can cause asphyxiation. The
area in which cylinders are stored and the area surrounding the
instrument must be adequately ventilated to prevent such gas
accumulations.
Gas cylinders must be stored and handled strictly in accordance with
local safety codes and regulations. Cylinders must be used and stored
only in a vertical position and secured to an immovable structure or
a properly constructed cylinder stand. Move cylinders only by
securing them to a properly constructed trolley.
Use only approved regulator and hose connectors (refer to the gas
supplier’s instructions). Keep gas cylinders cool and properly
labeled. (All cylinders are fitted with a pressure relief device that will
rupture and empty the cylinder if the internal pressure is raised
above the safe limit by excessive temperatures.) Ensure that you have
the correct gas before connecting it to the instrument.
The primary gas used with the spectrometer is argon, which is the
conductive gas for the plasma. Argon or nitrogen can be used as the
polychromator purge gas. Other gases may be required for future
options and accessories. Use only ‘instrument grade’ gases with your
spectrometer.
If using cryogenic gases (for example, liquid argon), prevent severe
burns by wearing suitable protective clothing and gloves.

Safety Practices and Hazards
Agilent 5100 and 5110 ICP-OES User’s Guide 11
Electrical Hazards
The spectrometer system and some accessories contain electrical
circuits, devices and components operating at dangerous voltages.
Contact with these circuits, devices and components can cause death,
serious injury or painful electric shock. Panels or covers which are
retained by screws on the spectrometer and accessories may be
opened only by Agilenttrained, Agilent-qualified or Agilentapproved
field service engineers (unless specified otherwise). Consult the
manuals or product labels supplied with your personal computer
(PC), monitor, printer and water-cooling system to determine which
parts of those systems are operator-accessible.
Connecting the Agilent ICP-OES to a power source that is not
equipped with a protective earth contact creates a shock hazard for
the operator and can damage the instrument. Likewise, interrupting
the protective conductor inside or outside the Agilent ICP-OES or
defeating the power cord ground creates a shock hazard for the
operator and can damage the instrument.
Other Precautions
Use of the spectrometer system and accessories may involve
materials, solvents and solutions which are flammable, corrosive,
toxic or otherwise hazardous. Careless, improper or unskilled use of
such materials, solvents and solutions can create explosion hazards,
chemical burn hazards, fire hazards, toxicity and other hazards that
can result in death, serious personal injury or damage to equipment.
Apply all necessary precautions including use of lab coats, safety
goggles and other appropriate forms of personal protection. All
wastes should be disposed of in accordance with local regulatory
requirements.
Operation of an ICP-OES involves analysis of solutions that have
been prepared in or digested with acids, or in some cases, samples
that have been prepared in organic solvents.
In case of uncertainty about a specific fluid, that fluid should not be
used until confirmation by the manufacturer that it will not present a
hazard.

Safety Practices and Hazards
12 Agilent 5100 and 5110 ICP-OES User’s Guide
The acid concentration in the sample that is measured varies,
depending upon the digestion steps and acid types used. Instrument
users should be aware of the hazards associated with use of the acids
used for sample preparation and apply all necessary precautions
including use of lab coats, safety goggles and other appropriate forms
of personal protection. The acid wastes should be disposed of in
accordance with local regulatory requirements.
The type, volatility and concentration of the organic solvents used in
the sample that is measured varies, depending upon the selected
solvent and the sample preparation involved. Instrument users
should be aware of the hazards associated with use of the organic
solvents for sample preparation, and apply all necessary precautions
including ensuring adequate ventilation during use, and use of lab
coats, safety goggles, gloves and other appropriate forms of personal
protection. The organic wastes should be disposed of in accordance
with local regulatory requirements.
Air flow to the air intake port of the spectrometer and accessories
must be unobstructed. Do not block the ventilation grills on the
spectrometer and accessories. Consult the manuals supplied with
your PC, monitor, printer and water-cooling system for their specific
ventilation requirements.
Great care should be taken when working with glass or quartz parts
to prevent breakage and cuts. This is especially important when
inserting the nebulizer into the spray chamber, or removing and
replacing pieces of broken torch.
The spectrometer weighs approximately 106 kg (234 lb). To avoid
injury to personnel or damage to the instrument or property, always
use suitable mechanical lifting device to move the instrument.
Use only Agilent-supplied or approved spares with your instrument.
Only trained operators should use the instrument.

Safety Practices and Hazards
Agilent 5100 and 5110 ICP-OES User’s Guide 13
Warning Symbols
The following is a list of symbols that may appear in conjunction with
warnings in this manual or on the spectrometer. The hazard they
describe is also shown. The beginning of the warning text is noted by
a warning icon:
WARNING
A triangular symbol indicates a warning. The meanings of the
symbols that may appear alongside warnings in the documentation
or on the instrument itself are as follows:
Broken glass Chemical hazard Electrical shock
Extreme cold hazard
Eye hazard
Fire hazard
Heavy weight
(danger to feet)
Heavy weight
(danger to hands)
Hot surface
Noxious gases
RF radiation
The following symbol may be used on warning labels attached to the
instrument. When you see this symbol, refer to the relevant operation
or service manual for the correct procedure referred to by that
warning label.

Safety Practices and Hazards
14 Agilent 5100 and 5110 ICP-OES User’s Guide
The following symbols appear on the instrument for your
information.
I Mains power on
0 Mains power off
Single phase alternating current
Protective ground terminal.
Socket for Agilent accessory serial cable
Socket for Ethernet LAN cable
Socket for Agilent accessory USB cable
Indication of correct orientation of gas filter flow direction
CE Compliance
Your Agilent ICP-OES instrument has been designed to comply with
the requirements of the Electromagnetic Compatibility (EMC)
Directive and the Machinery Directive (MD) of the European Union.
Agilent has confirmed that each product complies with the relevant
Directives by testing a prototype against the prescribed EN
(European Norm) standards.

Safety Practices and Hazards
Agilent 5100 and 5110 ICP-OES User’s Guide 15
Proof that a product complies with these directives is indicated by:
the CE Marking appearing on the rear of the product, and
the documentation package that accompanies the product
containing a copy of the Declaration of Conformity. The
Declaration of Conformity is the legal declaration by Agilent that
the product complies with the directives listed above, and shows
the EN standards to which the product was tested to
demonstrate compliance.
Electromagnetic Compatibility
EN55011/CISPR11
Group 1 ISM equipment: group 1 contains all Industrial, Scientific
and Medical (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.
This device complies with the requirements of CISPR11, Group 1,
Class A as radiation professional equipment. Therefore, there may be
potential difficulties in ensuring electromagnetic compatibility in
other environments, due to conducted as well as radiated
disturbances.
Operation is subject to the following two conditions:
1This device may not cause harmful interference.
2This device must accept any interference received, including
interference that may cause undesired operation.

Safety Practices and Hazards
16 Agilent 5100 and 5110 ICP-OES User’s Guide
If this equipment does cause harmful interference to radio or
television reception, which can be determined by turning the
equipment off and on, the user is encouraged to try one or more of
the following measures:
1Relocate the radio or antenna.
2Move the device away from the radio or television.
3Plug the device into a different electrical outlet, so that the device
and the radio or television are on separate electrical circuits.
4Make sure that all peripheral devices are also certified.
5Make sure that appropriate cables are used to connect the device
to peripheral equipment.
6Consult your equipment dealer, Agilent Technologies, or an
experienced technician for assistance.
Changes or modifications not expressly approved by Agilent
Technologies could void the user’s authority to operate the
equipment.
ICES/NMB-001
This ISM device complies with Canadian ICES-001.
Cet appareil ISM est conforme à la norme NMB-001 du Canada.
South Korean Class A EMC declaration
A 급기기 ( 업무용 방송통신기자재 )
This equipment is Class A suitable for professional use and is for use
in electromagnetic environments outside of the home.
이 기기는 업무용 (A 급 ) 전자파적합기기로서 판 매자 또는 사용자는
이 점을 주
의하시기 바라 며 , 가정외의 지역에서 사용하는 것을 목적으 로
합니다 .

Introduction
Agilent 5100 and 5110 ICP-OES User’s Guide 17
2. Introduction
Site Preparation Requirements 17
User Documentation 18
Specifications 19
Electrical Power Supplies 19
Other Connections 20
Personal Computer Requirements 20
Gas Supplies 20
Exhaust system 21
ICP-OES instrument cooling air supply 21
Water Chiller System 22
Drain Vessel 23
Site Preparation Requirements
Prior to receiving your instrument, you will have been provided with
an Agilent 5100 and 5110 ICP-OES Site Preparation Guide, which
describes the environmental and operating requirements of the
ICP-OES system. You must prepare your laboratory according to
these instructions before the ICP-OES can be installed. You should
keep the Site Preparation Guide for future reference for example, if
you plan to move your instrument. If you have misplaced your copy,
you can obtain a free replacement from your local Agilent office.
Position the equipment for easy access to the disconnecting switch
on the left side of the instrument.

Introduction
18 Agilent 5100 and 5110 ICP-OES User’s Guide
User Documentation
You have been provided with the following documentation to help
you set up and operate your Agilent ICP-OES system:
This User’s Guide, with safety practices and hazards information,
instructions for finding information about installing and
maintaining the components of the ICP-OES and a brief
operation overview.
An extensive Help system containing context-sensitive Help, step-
by-step instructions for frequently performed operations and
instructions for using any accessories you ordered.
A Familiarization DVD that includes information on how to set
up methods and run instrument tests, some hardware basics and
maintenance videos.
Conventions
The following conventions have been used throughout the
documentation:
Menu items, menu options and field names (for example, click
Copy from the Edit menu) have been typed in bold. Bold is also
used to signify the buttons appearing throughout the software
(e.g., click OK).
ALL CAPITALS indicate keyboard commands (e.g., press the F2
key) and text you must type in from the keyboard (e.g., type
SETUP at the prompt).
Notes and tips
A Note is used to give advice or information.
A Tip is used to give practical hints to help you achieve the best
possible performance from your ICP-OES.

Introduction
Agilent 5100 and 5110 ICP-OES User’s Guide 19
Specifications
The Agilent ICP-OES instrument is suitable for indoor use only and is
classified suitable under Equipment class I category.
Temperature control
For optimum analytical performance, it is recommended that the
ambient temperature of the laboratory be between 20 and 25 °C (68
and 77 °F), and be held constant to within ±2 °C (±3.6 °F) throughout
the entire working day.
Environmental conditions
See the Agilent ICP-OES Site Preparation Guide for specifications.
Electrical Power Supplies
For electrical specifications, refer to your Agilent ICP-OES Site
Preparation Guide.
Use of power boards or extension cables is not recommended.
The installation of electrical power supplies must comply with the
rules and/or regulations imposed by the local authorities responsible
for the use of electrical energy in the workplace.
Avoid using power supplies from a source that may be subject to
electrical interference from other services (such as large electric
motors, elevators, welders and air conditioning units).
If necessary, replace the power cord only with a cord equivalent to
the one specified in the site preparation guide.
Circuit breaker
NOTE For safety reasons, any internal fuse or circuit breaker is not operator accessible,
and should only be replaced by Agilent-authorized personnel.

Introduction
20 Agilent 5100 and 5110 ICP-OES User’s Guide
The mains power switch contains a 20 A circuit breaker, which is
reset when the power switch is cycled.
Other Connections
IEEE 802.3, Ethernet LAN cable
Personal Computer Requirements
The recommended and minimum PC specifications can be found in
the Agilent ICP-OES Site Preparation Guide.
Locate the PC keyboard and mouse for ergonomically correct access.
Gas Supplies
Liquid or gaseous argon and nitrogen may be used with Agilent
ICP-OES spectrometer systems. Agilent recommends the use of liquid
gases, which are purer, more convenient and cheaper per unit
volume.
Table 1. Gas supply requirements
Component Gas
Plasma, nebulizer, optics interface purge Argon
Polychromator assembly Argon or Nitrogen (supplied through
optional nitrogen purge kit)
Gas supply regulator pressure setting may need to be adjusted to
ensure the pressure is in the permissible pressure range when
delivering the gas flow demanded during operation.
Table 2. Gas requirements
Permissible pressure range* 500-600 kPa (73 to 88 psi) gauge
Recommended pressure* 550 kPa (80 psi) gauge regulated
*when supplying required gas flows