Agilent Technologies 4100 User manual

Agilent Microwave
Plasma Atomic
Emission
Spectrometers
For models 4100, 4200,
and 4210
User’s Guide

2 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
Notices
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2013, 2016, 2018
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Guide Part Number
G8000-90002
Edition
Fourth edition, July 2018
Agilent Technologies Australia [M] Pty
Ltd
679 Springvale Road, Mulgrave,
Victoria, Australia. 3170
www.agilent.com
Printed in Malaysia
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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 Microwave Plasma Atomic Emission Spectrometers User’s Guide 3
Contents
1. Safety Practices and Hazards 7
General 7
Verifying Safe State 8
Plasma 9
Heat, Vapors and Fumes 10
Compressed Gas Hazards 10
Dangerous Goods 11
Electrical Hazards 11
Other Precautions 12
Warning Symbols 12
Color Coding 14
CE Compliance 14
Electromagnetic Compatibility 15
EN55011/CISPR11 15
South Korean Class A EMC declaration 16
ICES/NMB-001 16
2. Introduction 17
Site Preparation Requirements 17
User Documentation 17
Conventions 18
Notes and tips 18

Contents
4 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
Specifications 18
Installation category 18
Pollution level 18
Environmental conditions 19
Electrical power supplies 19
Gas supplies 20
Exhaust system 21
MP-AES instrument cooling air supply 22
Drain vessel 22
Personal computer requirements 23
Weights and dimensions 23
3. Installation 25
Agilent MP-AES Instrument Overview 26
Installing the MP Expert Software 28
Hardware Components Replacement 29
Accessories 30
Organic solvents kit 30
External Gas Control Module (EGCM) 31
SPS 3 and SPS 4 Autosampler 31
Advanced Valve System (AVS) 4 31
SVS 1/1+ 32
SVS 2 32
Agilent 4107 Nitrogen Generator 32
Multimode sample introduction system (MSIS) 33
Monochromator air purge 34
4. Operation 35
Analysis Checklist 35

Contents
Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide 5
Turning On the MP-AES Instrument and Software 36
Preparing for Analysis 37
MP-AES Instrument Wavelength Calibration 38
Creating/Opening a Worksheet 39
Creating a new worksheet 39
Opening an existing worksheet 40
Creating a new worksheet from a template 40
Developing a Method 40
Running Samples 42
Printing a Report 43
Turning Off the MP-AES instrument 43
5. Maintenance, Spare Parts and Troubleshooting 47
Routine Maintenance 48
Cleaning the MP-AES Instrument 49
Cleaning the MP-AES Easy Fit Torch 49
Cleaning the Spray Chamber 50
Checking the Gas Supply Tubing for Leaks 51
Spare Parts 51
Technical Support 52
Troubleshooting 52

Contents
6 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
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Safety Practices and Hazards
Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide 7
1. Safety Practices and Hazards
General 7
Verifying Safe State 8
Plasma 9
Heat, Vapors and Fumes 10
Compressed Gas Hazards 10
Electrical Hazards 11
Other Precautions 12
Warning Symbols 12
Color Coding 14
CE Compliance 14
Electromagnetic Compatibility 15
ICES/NMB-001 16
General
Unless otherwise specified, statements in this manual apply to the
Agilent 4100, 4200, and 4210 MP-AES instruments.
Operation of an Agilent Microwave Plasma Atomic Emission
Spectrometer (MP-AES) involves the use of compressed gases, high
microwave energy and hazardous materials including corrosive fluids
and flammable liquids. Careless, improper or unskilled use of this
instrument can cause death or serious injury to personnel, and/or
severe damage to equipment and property. Only trained personnel
should use this equipment.

Safety Practices and Hazards
8 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
The MP-AES instrument incorporates interlocks and covers that are
designed to prevent inadvertent contact with any potential hazards.
If the MP-AES instrument is used in any manner not specified by
Agilent, this protection 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.
The safety practices described below are provided to help the user
operate the MP-AES instrument safely. Read each safety topic
thoroughly before attempting to operate the MP-AES instrument and
always operate the MP-AES instrument in accordance with these
safety practices.
If you are unsure of the effects of any liquid, gas or chemical on the
MP-AES instrument, consult your Agilent field service engineer or
approved representative before use.
If the MP-AES instrument is to be used in conjunction with other
non-Agilent equipment, the safety requirements of any system
incorporating the MP-AES instrument is the responsibility of the
assembler of the system.
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
before use. 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.

Safety Practices and Hazards
Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide 9
Plasma
The plasma is extremely hot (about 6,000 °C, 11,000 °F) and operates
using high levels of microwave energy. The plasma emits high
intensity light. Always wear appropriate eye protection if viewing the
plasma. Close contact with the operating plasma can result in severe
heat burns to the skin, and exposure to microwave radiation can
cause sub-surface skin burns.
Do not operate the plasma if:
the microwave excitation assembly appears to be damaged
foreign material is present in the viewing port (left end of the
microwave excitation assembly) or the torch aperture (vertical
space for the torch)
the space above the chimney is not clear of objects
the MP-AES instrument exhaust system is not connected or
turned on
The microwave excitation assembly is designed to reduce microwave
radiation to safe levels while still permitting easy installation of the
torch and viewing of the plasma. The MP-AES instrument has an
interlock system that is designed to extinguish the plasma if either
the pre-optics window holder is opened or the torch is unloaded
before the plasma has been extinguished. Do not attempt to bypass
the interlock system.
Before opening the pre-optics window holder or unloading the torch,
extinguish the plasma by:
pressing SHIFT and F5 on the keyboard
selecting the ‘Plasma off’ option from the ‘Plasma’ drop-down
arrow on the MP Expert software toolbar
pressing the Plasma Enable switch on the front of the MP-AES
instrument
The torch remains hot for up to five minutes after the plasma is
extinguished. Touching the torch before it has cooled sufficiently may
result in burns. Allow the torch to cool before removing it from the
loader.

Safety Practices and Hazards
10 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
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
MP-AES instrument may render the system inoperative and/or
hazardous. It may also invalidate the warranty on the MP-AES
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 MP-AES 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 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 fan must always be switched on
before igniting the plasma.
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) can result in an oxygen-
deficient atmosphere which can cause asphyxiation. The storage area
must be adequately ventilated and must comply with the rules and
regulations imposed by the local authorities responsible for such use
in the workplace.
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.
If gases are to be plumbed from a remote storage area to the
instrument site, ensure that the local outlets are fitted with stop
valves, pressure gauges and suitable regulators that are easily
accessible to the instrument operator. The gas outlets must be
provided within 1.5 meters (5 feet) of the MP-AES instrument.

Safety Practices and Hazards
Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide 11
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 cylinder before connecting it to the MP-AES instrument.
If using cryogenic (liquid) gases (for example, liquid nitrogen or
argon) prevent severe burns by wearing suitable protective clothing
and gloves.
Dangerous Goods
The Onboard Argon Bottle is considered dangerous goods when
shipped and must comply with the rules and regulations imposed by
the local and recipient’s authorities.
Electrical Hazards
The MP-AES instrument 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 that are
retained by screws on the MP-AES instrument and accessories may
be opened only by Agilenttrained, Agilent-qualified or
Agilentapproved field service engineers (unless specifically
instructed). Consult the documentation or product labels supplied
with your personal computer (PC), monitor and printer to determine
which parts are operator-accessible.
The power cord set shipped with the MP-AES instrument cannot be
used with other products.
If necessary, replace the power cord only with a cord equivalent to
the one specified in the site preparation guide.

Safety Practices and Hazards
12 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
Other Precautions
Use of the MP-AES instrument and accessories may involve
materials, solvents and solutions that are flammable, corrosive, toxic
or otherwise hazardous. Careless, improper or unskilled use of such
materials, solvents and solutions can create explosion hazards, fire
hazards, toxicity and other hazards that can result in death, serious
personal injury or damage to equipment.
Always ensure that laboratory safety practices governing the use,
handling and disposal of hazardous materials are strictly observed.
These safety practices should include wearing appropriate safety
clothing and safety glasses.
Air flow to the MP-AES instrument and accessories must be
unobstructed. Do not block the ventilation grill on the instrument.
Allow at least 50 mm (2 in.) of space on the sides, and 150 mm (6 in.)
at the rear of the system to permit free air circulation. Consult the
documentation supplied with your PC, monitor and printer 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
attaching plastic tubing to glass barbs, or removing and replacing
pieces of broken torch.
The MP-AES instrument weighs approximately 73 kg (161 lb). To
avoid injury or damage to the MP-AES instrument or property,
always use a forklift or other suitable mechanical lifting device to
move the MP-AES instrument.
Use only Agilent-supplied spares with your MP-AES instrument.
Warning Symbols
The following is a list of symbols that appear in conjunction with
warnings in this guide and on the MP-AES instrument. The hazard
they describe is also shown. The beginning of the warning text is
noted by a warning icon:
WARNING

Safety Practices and Hazards
Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide 13
A triangular symbol indicates a warning. The meanings of the
symbols that may appear alongside warnings in the documentation
or on the MP-AES instrument itself are as follows:
Corrosive liquids
Electrical shock
Extreme cold
Eye hazard Fire hazard
Heavy weight
(danger to feet)
Heavy weight
(danger to hands)
Hot surface
Moving parts
Non-ionizing radiation
Noxious gases
Sharp object
The following symbol may be used on warning labels attached to the
MP-AES instrument. When you see this symbol, refer to the relevant
operation or service documentation for the correct procedure
referred to by that warning label.

Safety Practices and Hazards
14 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
The following symbols appear on the MP-AES instrument.
I Mains power on
0 Mains power off
Single phase alternating current
Socket for Agilent accessory USB cable
Color Coding
The various indicator lights appearing on Agilent instruments and
associated accessories represent the status of the instrument or
accessory.
A green light indicates the instrument is in normal/standby
mode.
A flashing green light indicates that firmware is being uploaded
from the PC to the MP-AES instrument or that there is no USB
connection from the PC to the MP-AES instrument.
CE Compliance
Your MP-AES instrument has been designed to comply with the
requirements of the Electromagnetic Compatibility (EMC) Directive
and the Machinery Directive 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.
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.

Safety Practices and Hazards
Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide 15
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.
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.
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.

Safety Practices and Hazards
16 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
Changes or modifications not expressly approved by Agilent
Technologies could void the user’s authority to operate the
equipment.
South Korean Class A EMC declaration
This equipment is Class A suitable for professional use and is for use
in electromagnetic environments outside of the home.
A급 기기
(업무용 방송통신기자재)
이 기기는 업무용(A급) 전자파적합기기로서 판
매자 또는 사용자는 이 점을 주의하시기 바라
며, 가정외의 지역에서 사용하는 것을 목적으
로 합니다.
ICES/NMB-001
This ISM device complies with Canadian ICES- 001.
Cet appareil ISM est conforme à la norme NMB-001 du Canada.

Introduction
Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide 17
2. Introduction
Site Preparation Requirements 17
User Documentation 17
Specifications 18
Site Preparation Requirements
Prior to receiving your Agilent MP-AES instrument, you will have
been provided with an Agilent MP-AES Site Preparation Guide,
which describes the environmental and operating requirements and
specifications of the MP-AES instrument. You must prepare your
laboratory according to these instructions and specifications before
the instrument can be installed. You should keep the site preparation
guide for future reference. If you have misplaced your copy, you can
obtain a replacement from your local Agilent office.
User Documentation
You have been provided with the following documentation to help
you set up and operate your MP-AES instrument:
The Agilent MP-AES Site Preparation Guide, with information on
how to set up your laboratory in preparation for the MP-AES
instrument.
This User’s Guide, with safety practices and hazards information,
instructions for finding information about installing and
maintaining the components of the MP-AES instrument and a
brief operation overview.

Introduction
18 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
An extensive Help system containing context-sensitive Help, step-
by-step instructions for frequently performed operations and
instructions for using any accessories you ordered. Access the
Help by pressing F1 on your keyboard with the MP Expert
software open, by clicking the resources icon and then Help and
Documentation on the Start page, or by double-clicking the MP
Expert Help icon on the computer desktop.
Conventions
The following conventions have been used throughout the
documentation:
Menu items, menu options and field names (for example, click
Copy on the Edit menu) have been typed in bold. Bold is also
used to signify the pushbuttons appearing throughout the
software (for example, click OK).
ALL CAPITALS indicate keyboard and mouse commands (for
example, press the F2 key) and text you must type using the
keyboard (for example, 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 MP-AES instrument.
Specifications
Installation category
The installation category is based on IEC61010:II. The installation
category implies the regulation for impulse withstand voltage. It is
also called the ‘Over voltage category’. ‘II’ applies to electrical
equipment.
Pollution level
The pollution level is based on IEC61010:2. Pollution level describes
the degree to which a solid, liquid or gas that deteriorates dielectric
strength is adhering. ‘2’ applies to a normal indoor atmosphere.

Introduction
Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide 19
Environmental conditions
See the Agilent MP-AES Site Preparation Guide for specifications.
Laboratory conditions
The area selected for the operation of an MP-AES instrument:
must be free from drafts, corrosive atmospheres and vibration
should have sample preparation areas and materials storage
facilities located in a separate room
must be a dust-free, low humidity environment
should have air conditioning for control of the environment
Temperature control
Most of the heat generated by the MP-AES instrument into the
laboratory is extracted from the laboratory by the exhaust system.
When the plasma is operating, approximately 200 W of heat from the
MP-AES instrument electronics flows into the laboratory.
Electrical power supplies
All power supplies should be single phase AC, 3 wire system (active,
neutral, ground or two active and ground) and should be terminated
at an appropriate connection receptacle that is within reach of the
system power cable. Use of power boards or extension cables is not
recommended.
Electrical requirements
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).

Introduction
20 Agilent Microwave Plasma Atomic Emission Spectrometers User’s Guide
Other electrical connections
USB
NOTE Basic insulation is provided for single fault protection on the USB connector.
Gas supplies
The primary gas used by the MP-AES instrument is nitrogen, which is
the supply gas for the plasma. A small quantity of argon is used in
the plasma ignition cycle. Oil-free compressed air is used for the
pre-optics protection gas. Other gases may be required for future
options and accessories. Use only ‘instrument-grade’ nitrogen with
your MP-AES instrument.
The installation of compressed or liquid gas supplies must comply
with the rules and/or regulations imposed by the local authorities
responsible for such use in the workplace.
See the Agilent MP-AES Site Preparation Guide for gas pressure
requirements.
Liquid or gaseous argon and nitrogen may be used with the MP-AES
instrument. Agilent recommends the use of liquid gases, which are
more pure, more convenient and cheaper per unit volume.
The main gas supply requirements used with the MP-AES instrument
are:
Nitrogen — for the plasma and nebulizer gas supply
Air — for the pre-optics protection gas
Argon — only required during plasma ignition
Additional gas supply requirements used when the optional External
Gas Control Module (EGCM) or Monochromator Air Purge
accessories are installed are:
Purge gas: nitrogen — for optics purging when analyzing elements
below 185 nm, or air — for optics purging in corrosive
environments