G8000-90002 MP-AES Users Guide
G8000-90002 MP-AES Users Guide
Plasma Atomic
Emission
Spectrometers
User’s Guide
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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
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
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.
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.
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.
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 Agilenttrained, Agilent-qualified or
Agilentapproved 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.
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
I Mains power on
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.
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:
1 This device may not cause harmful interference.
2 This 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:
1 Relocate the radio or antenna.
2 Move the device away from the radio or television.
3 Plug the device into a different electrical outlet, so that the device
and the radio or television are on separate electrical circuits.
4 Make sure that all peripheral devices are also certified.
5 Make sure that appropriate cables are used to connect the device
to peripheral equipment.
6 Consult your equipment dealer, Agilent Technologies, or an
experienced technician for assistance.
ICES/NMB-001
This ISM device complies with Canadian ICES- 001.
Cet appareil ISM est conforme à la norme NMB-001 du Canada.
2. Introduction
Site Preparation Requirements 17
User Documentation 17
Specifications 18
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.
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).
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.
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 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).
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
CAUTION Use only the tubing supplied with the instrument (or equivalent quality) to deliver
argon to the instrument. Inferior plastic or rubber tubing may cause ignition
problems due to contamination of the argon by atmospheric gases.
Exhaust system
The plasma operates at extremely high temperatures. The MP-AES
instrument exhaust fumes can be noxious or corrosive.
The MP-AES instrument exhaust must be directly connected to an
exhaust system. The exhaust system must include an exhaust fan, be
ducted to an external vent and provide a minimum flow of 3 m3/min
(106 ft3/min).
The exhaust system installation must comply with any rules and/or
regulations that may be imposed by the local authorities responsible
for control of facilities and fixtures in the workplace.
The exhaust fan should be located at least 2 meters (6 ft, 6 in) away
from the top of the MP-AES instrument chimney. The fan control
switch and running indicator lamp should be located in a position
where the instrument operator can view the indicator and access the
control switch.
Drain vessel
The MP-AES instrument needs a drain vessel for disposal of excess
fluids and vapors from the spray chamber. Suitable tubing is
supplied with the MP-AES instrument for use with inorganic
solvents. When using organic solvents, different drain tubing that is
suitable for the solvent in use will be required.
3. Installation
Agilent MP-AES Instrument Overview 26
Installing the MP Expert Software 28
Hardware Components Replacement 29
Accessories 30
1 7
2
3 9
10
4 11
5 12
2. Plasma Enable button/ 6. Pre-optics window 10. Torch clamp for spray
status LED access door chamber and torch
NOTE If the Plasma Enable button is used to extinguish the plasma, you will need to
reset the Plasma Enable button to the ‘Enable’ (pushed in) position before the
plasma can be re-ignited.
4
1
5
6
2 7
3
Figure 2. Input and output connections on the side of the MP-AES instrument
Item Description
1 Accessory port DA-15 receptacle
For connection of Agilent-specified accessories only
2 Sampler port DE-9 plug. RS-232 port for connection of the Agilent SPS 3
autosampler
3 Power switch Combination power switch and main circuit breaker (12 A) for
the MP-AES instrument
4 Power inlet IEC-C14 mains power inlet receptacle
Accepts IEC-C13 mains lead
5 USB port USB type B receptacle. Supports USB 2.0 Full Speed
Length of USB cable to PC is to be a maximum of 3 m (10 ft)
6 Gas inlets Connect required gas supplies
7 Onboard argon Onboard argon bottle location
bottle receptacle
NOTE Install the MP Expert Software first, and then plug the USB cable into the
computer.
TIP To familiarize yourself with the MP Expert software, after installation, double-
click the MP Expert icon on your computer desktop. When the MP Expert Help
appears, click the How to link to view step-by-step instructions on how to use
the MP-AES instrument.
1 If you have turned off the auto-start capability of your CD-ROM drive, you will need to run the MPExpertSetup.exe file on
the disk.
NOTE Torches used with Agilent 4100 MP-AES instruments are different from the
torches used with the Agilent 4200 and 4210 MP-AES instruments and are not
interchangeable. Torches for the 4100 MP-AES have a grey base (Figure 3).
Torches for the 4200 and 4210 MP-AES have a blue base (Figure 4).
Figure 3. 4100 MP-AES EasyFit torch Figure 4. 4200 and 4210 MP-AES EasyFit
torch
Accessories
The following accessories may be available for use with your MP-AES
instrument:
Organic solvents kit
External Gas Control Module (EGCM)
SPS 3 and SPS 4 Autosamplers
Advanced Valve System (AVS) 4
SVS 1/1+ Switching Valve System
SVS 2 Switching Valve System
Agilent 4107 Nitrogen Generator
Multimode sample introduction system (MSIS)
Monochromator air purge
For installation information, please see the accessory documentation
provided with the accessory or the MP Expert Help.
NOTE You must turn off the MP-AES instrument when accessories are plugged into or
unplugged from the Accessory Port.
SVS 1/1+
For safety information and to prepare the SVS 1 or SVS 1+ for
installation, please see the instructions that came with the accessory.
The SVS 1/1+ is a 4-port switching valve positioned between the
spray chamber and the peristaltic pump of the spectrometer. During
the rinse time, when the instrument is usually idle, the autosampler
cleans the probe and presents the next sample for measurement,
increasing productivity. Excess sample is diverted away from the
spray chamber immediately after measurement, reducing sample
carry-over.
SVS 2
For safety information and to prepare the SVS 2 for installation,
please see the instructions that came with the accessory.
The SVS 2 increases sample throughput and decreases turnaround
time and operating costs. The SVS 2 features triple-stacked, 4-port
switching valve positioned between the spray chamber and the
peristaltic pump of the spectrometer. Samples are quickly loaded
into the SVS 2 sample loop, ready for immediate analysis by the
MP-AES, greatly reducing sample uptake delays. Pre-emptive rinsing
of the sample line means analysis times are reduced. The SVS 2 also
features an internal T-piece within the valve, reducing dead volume
and providing online addition of internal standard and ionization
buffer solutions. A bubble injector automatically injects bubbles after
the sample is loaded into the loop, isolating the sample from the rinse
solution. This reduces the volume of sample required for
measurement as tailing (or dilution) effects are minimized.
NOTE Separate nitrogen generator units must be used to supply the nitrogen to the
MP-AES instrument and the ECGM.
4. Operation
Analysis Checklist 35
Turning On the MP-AES Instrument and Software 36
Preparing for Analysis 37
MP-AES Instrument Wavelength Calibration 38
Creating/Opening a Worksheet 39
Developing a Method 40
Running Samples 42
Printing a Report 43
Turning Off the MP-AES instrument 43
This chapter provides a quick guide to getting the Agilent MP-AES
instrument set up and running samples.
You will find step-by-step instructions for common operations in the
MP Expert Help. To access this information:
1 Double-click the MP Expert Help icon on the computer desktop.
2 When the MP Expert Help appears, click How to to view the
available step-by-step instructions.
Analysis Checklist
You need to complete the following steps in turn to measure a
solution. You will find information on each step in this chapter.
Turn on the MP-AES instrument and open the software
Prepare for analysis
Perform a wavelength calibration of the MP-AES instrument
Create/open a worksheet
Develop a method
Run samples
Print a report
NOTE See the MP Expert Help for instructions on how to adjust the peristaltic pump
pressure bars.
NOTE For optimum performance and stability, for the MP-AES instrument a warm up
time of 30 minutes is recommended, from standby.
NOTE When using the nitrogen generator, a purge time of up to 20 minutes is required
from power on, depending on the prior usage history, to allow the nitrogen
generator to achieve required nitrogen purity.
NOTE The plasma will take between 10–15 seconds to ignite. If it fails to ignite, refer to
the Troubleshooting section in the Help for further information. In addition, the
plasma can be run dry (no solution) without damaging the torch.
CAUTION The plasma cannot be run without the spray chamber and nebulizer gas supply
connected. Doing so will damage the torch.
NOTE You must install the correct peristaltic pump tubing for the wavelength
calibration:
Pump Drain
4100 MP-AES White/white Blue/blue
4200 and 4210 MP-AES Orange/green Blue/blue
Creating/Opening a Worksheet
NOTE If you attempt to open a worksheet that is setup for use with a model other than
the one currently connected, you will be prompted as to whether or not you
would like the worksheet to be converted or that it will be opened as a Read-
only file. Converting the worksheet will ensure that all settings are compatible
with the connected instrument. Any changes that have been made will be
visible in the Operation Log of the worksheet.
Developing a Method
To develop a method:
1 Open a new worksheet or one from a template.
2 On the ‘Elements’ page, select the element(s) from the ‘Element’
drop-down box or type the element name or symbol and then
perform one of the following:
a Click to add the primary wavelength for the selected
element.
NOTE Alternatively, press CTRL and the element from the periodic table to add the
primary wavelength for the selected element to your method.
The element will appear in the table with the selected wavelength
and default settings selected.
3 Check that there are no interferents or other analytical lines
close to the selected analytical line. Their relative intensity will
govern how close the lines can be to each other. For example, if
your matrix contains an element that is not of analytical interest,
but is a potential interferent and has a line close to one of your
analytical lines, the concentration of that element in your matrix
will determine whether you need to choose another analytical
line.
4 Make any required adjustments to each element including
selecting a different wavelength, entering additional information
into the ‘Label’ column, selecting the type of sample (choose from
analyte, internal standard or interferent) and the type of
background correction is to be used.
5 Enable QC and/or IEC in the Configuration tab if these features
are going to be used. (Available only on the full version of the MP
Expert software.)
6 Click Conditions to modify both common settings for the run and
settings for each element. Nebulizer gas settings and viewing
positions can now be optimized.
NOTE The software can automatically determine and set the optimal operating
conditions for each element. For detailed information on how to select the
conditions, see the MP Expert Help > Software > Worksheet Page > Conditions.
NOTE See the MP Expert Help for a more detailed description of setting up a method.
Running Samples
To run samples:
1 Click the Analysis tab and do the following:
a Ensure your samples are selected. This will be indicated by a
check next to the Rack:Tube column. To select all solutions,
select the checkbox next to the Rack:Tube title.
b Click the Run icon in the toolbar (or press the SHIFT+F8
keys) to begin the analysis, and follow the subsequent
prompts.
NOTE For further information about running an analysis, refer to the MP Expert Help.
Printing a Report
To print a report:
1 Click Report on the toolbar or File > Report.
2 Choose whether you want to print or preview the report or save
the report as a PDF file.
TIP Previewing the report allows you to ensure that you have included all of the
data you require.
NOTE When running organic samples it is recommended that the spray chamber be
cleaned and dried thoroughly between analyses.
NOTE The green Plasma enable button, located on the front of the MP-AES
instrument, is intended to be used only in an emergency. It is not intended to be
used every time you want to extinguish the plasma. If it is used to extinguish
the plasma, you will need to reset the Plasma enable button to the ‘on’ position
before the plasma can be re-ignited.
3
2
NOTE If the MP-AES instrument is not going to be in use for a period of time the torch
should be cleaned of any deposits, dirt or residue. For further information about
cleaning the torch see Page 49.
NOTE This section refers to maintenance procedures for the MP-AES instrument. You
should refer to your PC and printer documentation for their maintenance
procedures, and to the MP Expert Help for the maintenance procedures for any
accessories you ordered.
Routine Maintenance
The following parts of the MP-AES instrument require routine
maintenance.
Daily
Check and, if necessary, empty the drain vessel.
Inspect the torch condition and cleanliness. Clean as necessary.
See Page 49.
Clean the surface of your MP-AES instrument (spills should be
cleaned up immediately).
Inspect the pump tubing and replace if it has lost its elasticity.
Unclip the pump tubes when the pump is not in use.
Weekly
Inspect the spray chamber for cleanliness. Clean as necessary.
See Page 50.
Clean the nebulizer.
Inspect the pre-optics window for cleanliness. Clean or replace
as necessary.
Monthly
Clean the air inlet filter on top of your MP-AES instrument.
Perform an MP-AES instrument calibration.
Inspect the external gas supply system for leaks including the
tubing connected to the MP-AES instrument. Replace any
damaged, leaking or worn components.
To find instructions on how to perform maintenance procedures
double-click the MP Expert Help desktop icon or, with the MP Expert
software open, press F1 on your keyboard. Expand the ‘Maintenance’
section and then select the appropriate topic.
CAUTION The torch is fragile. To prevent damage to the torch, always take care when
handling or storing it.
Spare Parts
For details on spare parts and consumables ordering information,
refer to the Agilent Technologies website:
www.agilent.com
To replace the items listed below, you must use Agilent-
manufactured parts, which can be ordered online from the Agilent
website or through your local sales representative.
The following is a list of recommended spares to keep on hand to
minimize downtime during maintenance and repairs:
Torch
Air inlet filter
Pre-optics windows
Spray chamber
Nebulizer
Peristaltic pump tubing
Drain tubing
Technical Support
For technical support contact information, refer to the Agilent
Technologies website for details:
www.agilent.com
Troubleshooting
For troubleshooting information, please see the Help provided with
the MP Expert software.
To access it, double-click the MP Expert Help on the computer
desktop and then click Troubleshooting.
In This Guide
The guide describes the following:
Safety Practices and Hazards
Introduction
Installation
Operation
Maintenance, Spare Parts and
Troubleshooting