Endress+Hauser Analytik Jena PlasmaQuant PQ 9000 User manual

Operating Manual
PlasmaQuant PQ 9000 (Elite)
High-Resolution Array ICP-OES

Analytik Jena AG
Konrad-Zuse-Str.1
07745 Jena Germany
Phone + 49 3641 77 70
Fax + 49 3641 77 9279
Email [e-mail]
Analytik Jena AG
Konrad-Zuse-Str. 1
07745 Jena Deutschland
Phone + 49 3641 77 7407
Fax + 49 3641 77 7449
Email [e-mail]
For safety and proper use follow these instructions.
Keep it for later use.
http://www.analytik-jena.com
13-5850-002-23
04.19
Analytik Jena AG
© Copyright 2019, Analytik Jena AG
Manufacturer
Service
General information
Documentation number
Issue
Implementation of the
Technical Documentation

Contents
3
Contents
1Basic information............................................................................................................. 7
1.1 User manual notes...................................................................................................................7
1.2 Intended use .............................................................................................................................8
2Safety ................................................................................................................................ 9
2.1 Safety markings on the PlasmaQuant PQ 9000 ..................................................................9
2.2 Requirements for the operating personnel........................................................................ 10
2.3 Safety instructions, transport and commissioning............................................................ 10
2.4 Safety instructions - operation ............................................................................................ 11
2.4.1 General safety instructions for operation........................................................................... 11
2.4.2 Safety instructions relating to ambient conditions ........................................................... 11
2.4.3 Safety instructions - electrical equipment.......................................................................... 11
2.4.4 Hazards caused by plasma operation ................................................................................. 12
2.4.5 Behavior in case of ring plasmas......................................................................................... 12
2.4.6 Safety instructions relating to the formation of ozone and toxic vapors ....................... 13
2.4.7 Safety instructions relating to compressed gas containers and systems........................ 13
2.4.8 Handling of samples, auxiliary and operating materials.................................................. 13
2.4.9 Safety instructions relating to cleaning and decontamination measures ...................... 14
2.5 Safety instructions - maintenance and repair ................................................................... 14
2.6 Behavior during emergencies.............................................................................................. 15
3Function and setup of the PlasmaQuant PQ 9000 ..................................................... 16
3.1 Physical functional principle of ICP-OES ............................................................................ 16
3.2 Function and setup of the PlasmaQuant PQ 9000........................................................... 16
3.3 Autosampler ASPQ 3300..................................................................................................... 20
4Installation and commissioning ................................................................................... 22
4.1 Installation conditions .......................................................................................................... 22
4.1.1 Environmental conditions.................................................................................................... 22
4.1.2 Energy supply ........................................................................................................................ 22
4.1.3 Gas supply.............................................................................................................................. 23
4.1.4 Exhaust unit........................................................................................................................... 24
4.1.5 Recirculating chiller .............................................................................................................. 24
4.1.6 Device layout and space requirements............................................................................... 25
4.2 Supply and control connections .......................................................................................... 27
4.3 Connections in the plasma compartment, sampling compartment and type plate ...... 31
4.4 Installing the PlasmaQuant PQ 9000................................................................................. 32
4.5 Connecting and comissioning the PlasmaQuant PQ 9000.............................................. 32
4.5.1 Installation of the torch, nebulizer with spray chamber and sample supply ................. 33
4.5.2 Initial operation of the autosampler ASPQ 3300 ............................................................. 36
4.6 Installing additional accessories.......................................................................................... 39
4.6.1 Installing Isomist................................................................................................................... 39
4.6.2 Installing the argon humidifier............................................................................................ 41
4.6.3 Installing the in-line filter .................................................................................................... 42
4.6.4 Installing the kit for internal standard (KIS)...................................................................... 44
4.6.5 Installing the Hg/hydride systems ...................................................................................... 44
5Operation........................................................................................................................ 46
5.1 Switching on the PlasmaQuant PQ 9000 and igniting the plasma ................................ 46
5.2 Switching off the PlasmaQuant PQ 9000.......................................................................... 47
5.3 Using the plasma deactivation switch in the event of faults ........................................... 48
5.4 Starting a measurement routine......................................................................................... 48
6Maintenance and care................................................................................................... 50
6.1 Maintenance intervals.......................................................................................................... 51
6.2 Base device maintenance..................................................................................................... 52
6.2.1 Cleaning the demountable torch......................................................................................... 52

Contents
4
6.2.2 Replacing the torch body ......................................................................................................54
6.2.3 Servicing the one-piece torch...............................................................................................57
6.2.4 Cleaning the nebulizer ..........................................................................................................59
6.2.5 Cleaning the sampling compartment and the plasma compartment..............................60
6.2.6 Replacing pump tubes...........................................................................................................60
6.2.7 Changing the plasma compartment windows....................................................................61
6.2.8 Checking the gas system for leaks .......................................................................................63
6.2.9 Changing fuses.......................................................................................................................63
6.2.10 Replacing the air filter of the PQ 9000...............................................................................64
6.2.11 Servicing the water filter.......................................................................................................64
6.2.12 Replacing the argon hose .....................................................................................................65
6.3 Maintenance of the autosampler ASPQ 3300...................................................................65
6.3.1 Replacing the cannula and the sample tube ......................................................................65
6.3.2 Replacing the pump tubing of the autosampler pump .....................................................66
6.3.3 Replacing the fuses ...............................................................................................................67
6.4 Maintenance of the recirculating chiller - Changing the cooling water..........................68
7Fault removal ................................................................................................................. 70
7.1 Device faults and error messages in the software.............................................................70
7.2 Equipment faults and analytical problems .........................................................................73
8Transport and storage ................................................................................................... 76
8.1 Preparing the PlasmaQuant PQ 9000 for transport .........................................................76
8.2 Ambient conditions for transport and storage...................................................................77
8.3 Recommissioning after transport or storage......................................................................77
8.4 Installing the recirculating chiller ........................................................................................78
9Disposal........................................................................................................................... 79
10 Specification ................................................................................................................... 80
10.1 Technical data........................................................................................................................80
10.1.1 PlasmaQuant PQ 9000 data ................................................................................................80
10.1.2 Control computer data..........................................................................................................82
10.1.3 Cooling system data ..............................................................................................................82
10.1.4 Autosampler data ..................................................................................................................83
10.2 Guidelines and standards .....................................................................................................84
11 Index................................................................................................................................ 85

Figures and Overviews
5
Figures
Figure 1 Sampling compartment and plasma compartment .......................................................... 17
Figure 2 Concentric nebulizer and spray chamber ........................................................................... 18
Figure 3 Schematic structure of the torch with gas flows ............................................................... 18
Figure 4 Demountable torch............................................................................................................... 19
Figure 5 One-piece torch..................................................................................................................... 19
Figure 6 Autosampler ASPQ 3300..................................................................................................... 20
Figure 7 Dimensions of the PlasmaQuant PQ 9000 - front view................................................... 26
Figure 8 Dimensions of the PlasmaQuant PQ 9000 - top view ..................................................... 27
Figure 9 Overview of connections on the left side of the device.................................................... 28
Figure 10 Interfaces and fuses .......................................................................................................... 29
Figure 11 Connections for cooling water and gases ....................................................................... 29
Figure 12 Plug-in connectors for gas connections.......................................................................... 30
Figure 13 Ventilation openings and air filter on the rear-side...................................................... 30
Figure 14 Plasma compartment........................................................................................................ 31
Figure 15 Data on the type plate ...................................................................................................... 31
Figure 16 Sampling compartment .................................................................................................... 32
Figure 17 ASPQ 3300- overview....................................................................................................... 36
Figure 18 Connections on the right side of the autosampler ........................................................ 36
Figure 19 Wash cup und pump at the ASPQ 3300......................................................................... 37
Figure 20 Isomist in the sampling compartment ............................................................................ 41
Figure 21Argon humidifier in the sampling compartment........................................................... 42
Figure 22 In-line filter in sampling compartment........................................................................... 43
Figure 23 Position of the ferrule in the banjo bolt.......................................................................... 43
Figure 24 KIS in sampling compartment.......................................................................................... 44
Figure 25 Nebulizer cleaning tool with installed nebulizer............................................................ 60
Figure 26 Plug-in connectors for gas connections.......................................................................... 63
Figure 27 Gas distribution.................................................................................................................. 63
Figure 28 ASPQ 3300 cannula and sample tube dismantled........................................................ 66
Figure 29 Autosampler pump............................................................................................................ 67
Figure 30 Replacing the fuses of the autosampler ......................................................................... 68
Overviews
Overview 1 Environmental conditions for operation .................................................................... 22
Overview 2 Power supply ................................................................................................................. 23
Overview 3 Gas supply...................................................................................................................... 23
Overview 4 Exhaust unit requirements .......................................................................................... 24
Overview 5 Cooling circuit requirements........................................................................................ 24

Figures and Overviews
6

PlasmaQuant PQ 9000 (Elite) Basic information
7
1Basic information
1.1 User manual notes
The user manual describes the following models of the PlasmaQuant series:
PlasmaQuant PQ 9000
PlasmaQuant PQ 9000 Elite
In the text below both devices are collectively called PlasmaQuant PQ 9000. Differences
are only stated when appropriate.
The PlasmaQuant PQ 9000 is intended for operation by qualified specialist personnel
observing this user manual.
The user manual informs about the design and function of the PlasmaQuant PQ 9000
and provides the necessary know-how for the safe handling of the device and its compo-
nents to personnel familiar with analysis. The user manual further includes notes on the
maintenance and service of the equipment and potential causes and remedies of any
faults.
Instructions for actions which occur in chronological order are numbered and combined
in action units.
Safety notes are indicated by pictographs and signal words. The type and source of the
danger are stated together with notes on preventing the danger. The meaning of the
pictographs and signal words used is explained in the chapter "Safety notes".
The elements of the control and analysis program are indicated as follows:
Program terms are identified with SMALL CAPS (e.g., Menu FILE).
Buttons are shown by square brackets (e.g., [OK] button)
Menu items are separated by arrows (e.g., FILE OPEN).
The user manual uses the following symbols and signal words to indicate hazards or in-
structions. The safety instructions are always placed before an action.
WARNING
Indicates a potentially hazardous situation which might cause fatal or very serious inju-
ries (deformities).
CAUTION
Indicates a potentially hazardous situation which might cause light or minor injuries.
Notice
Provides
indications of potential material and environmental damage.
Conventions
Symbols and signal words

Basic information PlasmaQuant PQ 9000 (Elite)
8
1.2 Intended use
The ICP Emission Spectrometer (ICP-OES) PlasmaQuant PQ 9000 is used in a chemical
analysis laboratory for the analysis of liquid - mainly aqueous - samples to determine
the concentrations of up to 75 elements up to the trace range.
The PlasmaQuant PQ 9000 may only be used for the analyses described in this user
manual. Any other use is not intended. The operator is solely liable for any damage re-
sulting therefrom. The safety of the user and the instrument can only be guaranteed if it
is used as intended.
The PlasmaQuant PQ is not suitable for solutions containing hydrofluoric acid if the neb-
ulizer or spray chamber are made of glass or quartz. Use hydrofluoric acid-resistant com-
ponents for this purpose. Special provisions must be made for operations involving or-
ganic solvents. In addition to apparatus-related and methodical aspects, fire and health
protection for the particular organic solvent must be observed here.

PlasmaQuant PQ 9000 (Elite) Safety
9
2Safety
For your own safety and to ensure error-free and safe operation of the PlasmaQuant PQ
9000, please read this chapter carefully before using the appliance.
Observe all safety notes listed in this user manual and all messages and notes displayed
by the control and analysis program on the monitor.
Besides the safety instructions in this user manual and the local safety regulations that
apply to the operation of the device, the general applicable regulations regarding acci-
dent prevention, occupational health and safety and environmental protection have to
be observed and complied with.
References to potential dangers do not replace the work protection regulations which
must be observed.
2.1 Safety markings on the PlasmaQuant PQ 9000
Warnings and notice symbols have been attached to the PlasmaQuant PQ 9000 which
must always be observed.
Damaged or missing warning and notice symbols can cause incorrect actions leading to
personal injury or material damage! The symbol labels must not be removed! Damaged
symbol labels must be replaced without delay!
Warning symbol Meaning Remark
Warning of a hazard location At the extractor device:
Warning of optical radiation. If no exhaust tube is con-
nected, it is possible to look indirectly (by mirror) into the
radiation of the plasma.
At the sampling compartment:
Warning of moving parts; warning of hot torch
At the plasma compartment:
Warning of hot surfaces.
At the power inlet:
Caution when connecting the media (gases, cooling wa-
ter and power)
Warning of a hot surface At the plasma compartment:
Warning of hot surfaces. Immediately after extinguishing
the plasma, the surface of the plasma compartment and
in particular the torch and the plasma chamber window
components and the induction coil are hot. There is a risk
of getting burnt!

Safety PlasmaQuant PQ 9000 (Elite)
10
Notice symbol Meaning Remark
Observe the operating manual At the power switch:
Before starting work, read the operating manual.
Before opening the device, al-
ways disconnect the mains plug
On the side wall at the power inlet:
Before opening the device cover, switch off the device
and disconnect the mains plug from the mains socket.
Only for
People's Republic of China
Das Gerät enthält reglementierte Substanzen. Analytik
Jena garantiert, dass die Stoffe bei bestimmungsgemäßer
Verwendung in den nächsten 25 Jahren nicht austreten.
The following notice sign is attached to the rear of the PlasmaQuant PQ 9000:
2.2 Requirements for the operating personnel
The PlasmaQuant PQ 9000 must only be operated by qualified specialist personnel in-
structed in the use of the device. The instruction must also include conveying the con-
tent of this user manual and the user manuals of other system components.
In addition to the safety at work instructions in this user manual, the generally applica-
ble safety and accident prevention regulations of the respective country of operation
must be observed and adhered to. The operator must ascertain the latest version of
these regulations.
The user manual must be accessible to the operating and service personnel at all times!
2.3 Safety instructions, transport and commissioning
Observe the following notes:
The PlasmaQuant PQ 9000 is always installed by the service engineers of Analytik
Jena AG or its authorized and trained specialist personnel. Independent assembly
and installation are not permitted. Incorrect installation can create serious hazards.
The device weighs 170 kg. Use a lift truck to transport the device.
Four people are required to move the device in the laboratory by holding the device
on four firmly screwed-in carrying handles.

PlasmaQuant PQ 9000 (Elite) Safety
11
2.4 Safety instructions - operation
2.4.1 General safety instructions for operation
Observe the following notes:
The operator of the PlasmaQuant PQ 9000 must make sure before each commis-
sioning that the condition of the device including its safety equipment is sound. This
applies in particular after each modification to or extension of the device or its repair.
Modifications, conversions and extensions to the device may only be carried out after
consultation with Analytik Jena. Unauthorized modifications will result in limitations
of warranty and liability in the event of damage. Unauthorized modifications may
limit the safety of the device during operation and lead to limitations in warranty and
access to customer service.
The device may only be operated if all protective equipment (e.g., covers and doors)
are in place, properly installed and fully operational. The sound condition of the pro-
tection and safety equipment must be checked regularly. Any defects must be cor-
rected as soon as they occur. Protective and safety equipment must never be re-
moved, modified or decommissioned during operation.
During operation, free access to the connections, the power switch and the manual
plasma deactivation switch on the left housing wall must always be ensured.
The ventilation equipment on the device must be in good working condition. Covered
vents or ventilation slits etc. may cause the device to break down or may cause dam-
age to it.
Caution when handing quartz glass and glass parts. Risk of broken glass and there-
fore risk of injury!
Prevent liquids from penetrating into the device. Liquids can cause a short circuit.
During operation there is a danger of crushing the hose pump. Long hair and loose
clothing can get caught in the pump and be drawn in. Wear suitable hair protection
and close-fitting clothing.
2.4.2 Safety instructions relating to ambient conditions
The PlasmaQuant PQ 9000 must not be operated in explosion-hazard areas. Smoking
or open flames in the operating room of the PlasmaQuant PQ 9000 are prohibited.
Keep all combustible materials away from the device.
2.4.3 Safety instructions - electrical equipment
Work on the electrical components of the PlasmaQuant PQ 9000 may only be per-
formed by a qualified electrical technician according to applicable electro-technical regu-
lations. Lethal voltages may occur in the device! Contact with live components may
cause death, serious injury or painful electrical shock.
Observe the following notes:
The mains plug must be connected to a proper CEE power socket to ensure that the
device meets protection class I (ground connector). It may only be connected to
power sources where the nominal voltage is the same as that on the type plate of the
equipment. The protective effect must not be invalidated by the use of an extension
line, which does not have a protective conductor (→section "Energy supply" p.22).
Explosion protection

Safety PlasmaQuant PQ 9000 (Elite)
12
The PlasmaQuant PQ 9000 and its system components must always be switched off
before being connected to the mains.
Before opening the device, it must be switched off at the device switch and the
mains connector must be disconnected from the mains outlet! Any work on the elec-
tronics (behind the device enclosure) may only be carried out by the service engi-
neers of Analytik Jena AG and specially authorized technicians.
2.4.4 Hazards caused by plasma operation
Plasma is extremely hot (up to 10,000 K) and it emits electromagnetic and UV radiation.
The induction coil is operated with 1500 V RMS and 40.68 MHz. High-frequency radia-
tion and UV radiation can cause serious injuries to skin and eyes. Contact with the torch
(plasma torch) shortly after operation will cause skin burns. An electrical discharge may
also occur across larger distances and cause fatal injuries, electrical shock and skin inju-
ries.
Observe the following notes:
To ensure safe torch operation, you must not ignite the plasma unless the following
conditions are met:
—The plasma compartment door is closed.
—The torch is in working position.
—Sufficient cooling is supplied.
—The extractor device is connected and switched on.
—Argon supply is ensured.
Note: The above mentioned components are backed up by hardware safety circuits.
Unless the reliable functioning of these components is guaranteed, the plasma will
not be ignited or it will be extinguished automatically if a component reports a mal-
function.
The safety circuits must not be bridged.
Before opening the plasma compartment door, extinguish the plasma in the AS-
pect PQ program. To do this, click on the button in the program toolbar.
Wait for the compartment to cool down for at least 5 min and avoid touching any
hot parts of the torch and its environment immediately after extinguishing the
plasma.
2.4.5 Behavior in case of ring plasmas
The manual plasma deactivation switch is located on the left side of the device (red).
In the following situations, press the deactivation switch without delay to prevent the
torch from melting:
The plasma produces loud noises (rattles).
The shape of the plasma changes considerably and a shining ring is visible on the in-
side of the coil.
Torch parts begin to glow.

PlasmaQuant PQ 9000 (Elite) Safety
13
2.4.6 Safety instructions relating to the formation of ozone and toxic vapors
The interaction between the UV radiation from the torch and the surrounding air results
in the formation of a high concentration of toxic gases such as ozone and nitrogen ox-
ides. Additionally, toxic byproducts may escape from the samples and during sample
processing.
Observe the following notes:
The PlasmaQuant PQ 9000 may only be operated with an active exhaust unit.
The exhaust unit must be switched on before igniting the plasma.
2.4.7 Safety instructions relating to compressed gas containers and systems
Observe the following notes:
Argon is taken from compressed gas containers or local liquid gas systems. The re-
quired purity of the gases must be ensured.
Work on compressed gas containers and systems must only be carried out by individ-
uals with specialist knowledge and experience in compressed gas systems.
For compressed gas container or gas plant operation, the safety instructions and
guidelines which are valid at the operating location must be strictly complied with.
High pressure tubes and pressure reducers may only be used for the assigned gases.
Pipes, hoses, screw connections and pressure reducers for oxygen must be kept free
from grease.
All pipes, tubes and screw connections must be checked weekly for leaks and exter-
nally visible damage. Possible pressure losses from closed systems and lines under
pressure must be determined. Leaks and damaged must be repaired without delay.
The gas supply must be closed prior to servicing and repairs!
After successful repair and servicing of the components of the compressed air con-
tainers or system, the device must be checked for sound operation prior to recom-
missioning!
Independent assembly and installation are not permitted!
2.4.8 Handling of samples, auxiliary and operating materials
Observe the following notes:
The operator is responsible for the selection of substances used in the process as well
as for their safe handling. This is particularly important for radioactive, infectious,
poisonous, corrosive, combustible, explosive and otherwise dangerous substances.
When handling dangerous substances, local safety codes and guidelines must be ob-
served.
Warnings on the labels must always be observed. Only use clearly marked containers
as well as protective goggles and rubber gloves. Use suitable body protection (coat,
safety glasses and rubber gloves) when handling samples. Ensure sufficient ventila-
tion.
Cleaning with hydrofluoric acid must be carried out in an exhaust chamber. When
handling hydrofluoric acid, rubber aprons, gloves and face masks must be worn.

Safety PlasmaQuant PQ 9000 (Elite)
14
Biological samples must be handled according to local guidelines regarding the han-
dling of infectious material.
When measuring material containing cyanide, you have to make sure that prussic
acid cannot be generated in the waste bottle, i.e., the waste solution must not be
acidic.
Ensure that all residue liquid from the nebulizer and the autosampler is directed into
the waste bottle supplied.
The operator is responsible for ensuring that waste materials such as drained cool-
ant and residue liquid from the waste bottle are disposed of in an environmentally
responsible manner and according to local regulations.
Methyl isobutyl ketone (MIBK) Flammable, highly volatile, noxious-smelling
Toluene Flammable, hazardous to health
Kerosene Flammable, hazardous to the aquatic environment, haz-
ardous to health
Methanol, ethanol, propanol Flammable, partly acutely toxic
Tetrahydrofuran (THF) Flammable, hazardous to health, extremely volatile, dis-
solves polyethylene and polystyrene
This list is in so far incomplete that other solvents could also come into consideration for
use in the PlasmaQuant PQ 9000. In cases of uncertainty about an unnamed fluid, this
may only be used when the manufacturer has confirmed that there is no danger to
safety.
2.4.9 Safety instructions relating to cleaning and decontamination measures
Observe the following instructions in case of biological and over contamination:
The operator is responsible for carrying out suitable decontamination should the de-
vice be contaminated externally or internally with dangerous substances.
Remove and clean splashes, drops or spilled substances with absorbent material such
as cotton wool, laboratory wipes or cellulose. In the case of contamination with bio-
logical samples, then wipe off the affected areas with Incidin Plus solution.
Before using a cleaning or decontamination procedure other than that prescribed by
the manufacturer, the user is required to check with the manufacturer that the in-
tended procedure will not damage the device. Safety labels attached to the Plasma-
Quant PQ 9000 must not be wetted by methanol.
2.5 Safety instructions - maintenance and repair
Observe the following notes:
The PlasmaQuant PQ 9000 is always serviced by the service engineers of Analytik
Jena AG or its authorized and trained specialist personnel. Independent servicing can
maladjust or damage the device. Therefore, the operator may only carry out the tasks
listed in the chapter "Maintenance and care" p. 50.
The exterior of the PlasmaQuant PQ 9000 may only be cleaned with a damp, not
dripping, cloth. Use only water and, if required, commercial surfactants.
Examples of
organic solvents

PlasmaQuant PQ 9000 (Elite) Safety
15
For cleaning the sampling compartment and transport channels (tube system) of the
PlasmaQuant PQ 9000 the operator is responsible for establishing appropriate
safety precautions – particularly in terms of contaminated and infectious materials.
Before returning the instrument to Analytik Jena AG, clean all parts of the instrument
from biologically hazardous, chemical or radioactive contamination. Fill in a decon-
tamination declaration and sign it.
To do this, copy the decontamination declaration enclosed with your product docu-
mentation. Alternatively, you can download the decontamination declaration as a
describable pdf document in German and English from the Analytik Jena AG website.
Attach the signed decontamination declaration to the outside of the consignment.
Only use original spare parts, wearing parts or consumables. These are tested and
ensure safe operation. Glass parts are wearing parts and are not subject to warranty.
2.6 Behavior during emergencies
Observe the following notes:
If there is no immediate danger of injury, you must extinguish the plasma immedi-
ately by using the deactivation switch in case of danger or accidents.
If possible, switch off the device at the power switch after allowing a cooling down
period of 30 s. Then disconnect the mains plugs of the device and the system com-
ponents from their power sockets!
Close the gas supply as soon as possible after switching off the devices.

Function and setup of the PlasmaQuant PQ 9000 PlasmaQuant PQ 9000 (Elite)
16
3Function and setup of the PlasmaQuant PQ 9000
3.1 Physical functional principle of ICP-OES
ICP Emission Spectrometry (ICP-OES) makes use of plasma with temperatures of up to
10 000 K. This high temperature is focused on a very small area of approx. 5 cm3. The
sample is introduced to this plasma in the form of aerosol (small droplets in a glass).
The droplets dry, melt, vaporize and atomize or ionize. During this process, the analysis
channel of the plasma through which the sample is flowing cools down to approx. 6 000
to 7 000 K.
Atoms and ions are excited to emit light at these high temperatures. The light is broken
down by the device optics into wavelengths ("colors") tube intensity is measured to indi-
cate concentrations. A detector is used to measure the intensity of the emission line and
its spectral environment. The net intensity of the measured signal is used as a measur-
and ("peak").
The inert gas argon is used as the operating gas. This gas flows inside a plasma torch
made up of three concentric pipes. The plasma gas (also called cooling gas) flows at a
rate of 10-18 L/min on the outside to cool the external torch pipe. The sample aerosol
is injected in the plasma in the inmost pipe, hence its name "injector". The sample aero-
sol is created shortly before with a nebulizer and a downstream spray chamber in which
larger droplets are separated.
The exhaust heat of the plasma is dissipated partly by the recirculating chiller and partly
by the exhaust unit.
3.2 Function and setup of the PlasmaQuant PQ 9000
Essentially the PlasmaQuant PQ 9000 consists of the following components
Components for plasma generation (HF generator, induction coil, torch)
Sample supply system with peristaltic pump, nebulizer and spray chamber
Optical system with transfer optics, spectral photometer and detector
Technologically, the difference between both models, PlasmaQuant PQ 9000 and Plas-
maQuant PQ 9000 Elite, is in their optics. The components for plasma generation and
the sample supply system are identical. For applications with severe spectral interfer-
ences (e.g. for rare earths, refractory metals) the higher resolving power of the Plasma-
Quant PQ 9000 Elite benefits high detectability, precision and ease of use. Despite the
lower spectral resolution, the PlasmaQuant PQ 9000 offers excellent detection limits in
standard applications.
The sample introduction system is freely accessible in the sampling compartment. The
torch and the induction coil, however, are located in the shielded plasma compartment
to protect the user from the high-frequency radiation and the UV radiation from the
plasma. The spatial separation between sample supply and plasma also prevents the
heat radiation from the plasma being transferred without obstruction to the spray
chamber and causing a drift there.
Sampling compartment
and plasma compartment

PlasmaQuant PQ 9000 (Elite) Function and setup of the PlasmaQuant PQ 9000
17
Figure 1 Sampling compartment and plasma compartment
The PlasmaQuant PQ 9000 uses a free-running 40 MHz HF generator (High-Frequency
Generator). The HF generator transfers power ranging from 800 to 1700 W into the
plasma assisted by the high-performance coil. Fully automated matching of the power
output to the actual sampling loads in the plasma enables ultimate consistency of
plasma conditions. This means the plasma is very robust and is able to master even
challenging sample matrices such as organic solutions or salt loads. The HF generator is
located immediately behind the plasma compartment and is shielded separately because
of the high intensity of high frequencies.
The power for maintaining the plasma is transferred by means of an induction coil with
four windings in the torch in the plasma compartment. The induction coil is water-
cooled.
During the initial plasma ignition period, a high voltage spark is passed from the elec-
tronic ignition unit to the conducting spring located in the vicinity of the induction coil
through the high-frequency field in the torch.
A peristaltic pump conveys the measurement solution at the same rate to the nebulizer.
The rotational speed of the pump and the diameter of the pump tubing used determine
the amount of sample delivered. By using the pump, sample introduction into the nebu-
lizer and thus also the sensitivity of the measurement signal is nearly independent of
the viscosity of the measurement solution.
The aerosol of the measurement solution required for atomization/ionization in the
plasma is generated by a pneumatic concentric nebulizer. An argon flow is directed past
the sample nozzle of the nebulizer as nebulizer gas. The gas flow continuously tears the
surface of the liquid at the nozzle and produces small sample droplets. The sample aero-
sol that is formed is transported with the nebulizer gas through the spray chamber to
the plasma. On the way through the spray chamber, large droplets in the spray chamber
are separated by the centrifugal force and flow out via the waste outlet. A cyclone cham-
ber is used as the spray chamber.
HF generator
Pump, nebulizer and
spray chamber

Function and setup of the PlasmaQuant PQ 9000 PlasmaQuant PQ 9000 (Elite)
18
Figure 2 Concentric nebulizer and spray chamber
The torch has a three-shell construction and comprises an outer tube, an inner tube and
the inner injector tube.
The outer tube, in conjunction with the bonnet inserted into the coil, electrically insu-
lates the plasma from the induction coil and shields the plasma from the ambient air.
The plasma gas flows between the outer and inner tube. This gas is ionized at the induc-
tion coil and converted to a plasma state. The tangential flow of the plasma gas into the
space between the outer and inner tube cools the outer tube and prevents it from melt-
ing due to the high plasma temperatures.
The auxiliary gas flows in the intermediate space between the inner tube and the injec-
tor. It pushes the aerosol of the sample solution away from the injector.
The injector has the task of injecting the sample aerosol into the plasma. The measure-
ment solution is transported by the nebulizer gas from the spray chamber through the
injector into the plasma.
Figure 3 Schematic structure of the torch with gas flows
The torch is fully demountable and thus offers the possibility of replacing worn individ-
ual parts, such as the outer tube, which is subjected to extreme thermal loads. During
assembly, however, care must be taken to ensure the individual parts are inserted gas-
tight into one another and especially to check that the injector is seated correctly. Be-
sides, the standard torch (made of quartz glass with an injector, 2 mm) is also available
as a one-piece torch.
Torch

PlasmaQuant PQ 9000 (Elite) Function and setup of the PlasmaQuant PQ 9000
19
The cost of purchasing a one-piece torch is slightly lower. It is cleaned as a whole, mak-
ing disassembly and subsequent assembly unnecessary. On the other hand, this torch
has to be completely replaced when worn.
Figure 4 Demountable torch
Figure 5 One-piece torch
The PlasmaQuant PQ 9000 includes a special V Shuttle Torch design. The up-right ar-
rangement of the torch reduces clogging and soot formation.
The torch is mounted with the holder (shuttle) onto the rail guide. Doing so automati-
cally connects the internal gas inlets for the plasma and auxiliary gas. The torch is then
moved by hand along the rail guide to the plasma compartment where it locks in the ad-
justed operating position.
Analytik Jena offers sample introduction kits optimized for special applications:
Kit Applications Components
Standard Kit standard applications: environmental, food,
pharmaceutical samples
PVC-tubing, nebulizer, spray chamber made of
borosilicate glass and torch (injector, 2 mm)
made of quartz glass
HF Kit fusion samples containing HF:
metal, ceramics, rare earth samples
PVC-tubing, PFA-nebulizer and PTFE-spray
chamber, HF-resistant ceramic torch
Organic Kit organic samples:
oils, petroleum products as kerosene, organic
solvents
PU-tubing, nebulizer and torch (quartz glass, in-
jector, 1mm) for low gas flows, spray chamber
with dip tube to reduce matrix loading
Salt Kit samples with high salt loads:
brine, caustic and sulphurous solutions, sea wa-
ter
PVC-tubing, nebulizer with self-washing tip,
spray chamber with dip tube to reduce desolva-
tion, torch (quartz glass, injector, 2mm)
The analyte emission in plasma is observed from two directions, axial and radial
(DualView PLUS). The emission radiation is selectively coupled via the transfer optics
from one of the two directions to the monochromator. The working range is increased
by attenuating both directions of observation.
A double monochromator comprising of a prism and an echelle grating is used for spec-
tral analysis. A grating with high blaze angle (76°) achieves the high spectral resolution
of 0.002 nm at 200 nm of the PlasmaQuant PQ 9000 Elite (High-Resolution Optics).
The PlasmaQuant PQ 9000 has a spectral resolution of 0.006 nm at 200 nm.
Optical system

Function and setup of the PlasmaQuant PQ 9000 PlasmaQuant PQ 9000 (Elite)
20
With both models, the monochromator is wavelength-stabilized by the use of an inte-
grated neon source. Wavelength reproducibility is achieved by the internal Ne-line cali-
bration of the monochromator when approaching a wavelength.
A low noise, UV-sensitive semiconductor detector (CCD line detector) is located at the
exit slit of the monochromator. This detector not only registers the intensity of the anal-
ysis line, but also its spectral neighborhood. In this way, a spectral range of up to 1 nm
in the vicinity of the analysis line is detected simultaneously and at a high resolution.
3.3 Autosampler ASPQ 3300
Figure 6 Autosampler ASPQ 3300
The autosampler ASPQ 3300 allows fully automated routine analysis. It can be equipped
with three sample racks and two racks each with 6 special samples, e.g., standards.
The following sample racks are available:
Rack/number of samples Cup volume (mL)
6 (special samples) 50
21 50
24 30
40 20
60 14
90 7
The purging vessel is installed at the autosampler. A peristaltic pump at the ASPQ 3300
delivers the wash liquid from the diluent bottle into the wash cup – this action cleans
the dipped cannula by washing it inside and out. Excess wash liquid is pumped into the