ICP-OES Manual
ICP-OES Manual
ICP-OES Manual
Operating manual
Service: Analytik Jena AG
Customer Service
Konrad-Zuse-Str. 1
07745 Jena
Germany
Contents
1 Basic information 7
1.1 User manual notes .................................................................................................. 7
1.2 Intended use ........................................................................................................... 7
1.3 Warranty and liability ............................................................................................... 8
2 Safety instructions 9
2.1 General notes.......................................................................................................... 9
2.2 Symbols and signal words used ............................................................................. 9
2.3 Safety markings on the PlasmaQuant PQ 9000 ..................................................... 9
2.4 Requirements for the operating personnel ........................................................... 10
2.5 Safety instructions, transport and commissioning ................................................ 11
2.6 Safety instructions - operation .............................................................................. 11
2.6.1 General ................................................................................................................. 11
2.6.2 Safety instructions relating to ambient conditions................................................. 11
2.6.3 Safety instructions - electrical equipment ............................................................. 11
2.6.4 Hazards caused by plasma operation .................................................................. 12
2.6.5 Behavior in case of ring plasmas .......................................................................... 13
2.6.6 Safety instructions relating to the formation of ozone and toxic vapors ............... 13
2.6.7 Safety instructions relating to compressed gas containers and systems ............. 13
2.6.8 Handling of samples, auxiliary and operating materials ....................................... 14
2.6.9 Safety instructions relating to cleaning and decontamination measures in
case of biological contamination ........................................................................... 14
2.6.10 Safety instructions - maintenance and repair ....................................................... 15
2.7 Behavior during emergencies ............................................................................... 15
3 Specification 16
3.1 Technical data ....................................................................................................... 16
3.1.1 PlasmaQuant PQ 9000 data ................................................................................. 16
3.1.2 Control computer data .......................................................................................... 18
3.1.3 Cooling system data ............................................................................................. 18
3.1.4 Automatic sampler data ........................................................................................ 18
3.2 Guidelines and standards ..................................................................................... 19
4 Installation conditions 20
4.1 Environmental conditions ...................................................................................... 20
4.2 Energy supply ....................................................................................................... 20
4.3 Gas supply ............................................................................................................ 21
4.4 Exhaust unit .......................................................................................................... 22
4.5 Recirculating chiller ............................................................................................... 22
4.6 Device layout and space requirements ................................................................. 23
9 Fault removal 63
9.1 Fault removal ........................................................................................................ 63
9.2 Equipment faults and analytical problems ............................................................ 66
10 Transport and storage 70
10.1 Preparing the PlasmaQuant PQ 9000 for transport .............................................. 70
10.2 Ambient conditions for transport and storage ....................................................... 71
10.3 Recommissioning after transport or storage ......................................................... 71
10.4 Installing the recirculating chiller ........................................................................... 72
11 Index 73
Figures
Figure 1 Dimensions of the PlasmaQuant PQ 9000 - front view..................................... 24
Figure 2 Dimensions of the PlasmaQuant PQ 9000 - top view ....................................... 24
Figure 3 Sampling compartment and plasma compartment in the
PlasmaQuant PQ 9000 ...................................................................................... 26
Figure 4 Concentric nebulizer and spray chamber ......................................................... 27
Figure 5 Schematic structure of the torch with gas flows .............................................. 27
Figure 6 Demountable torch ........................................................................................... 28
Figure 7 One-piece torch................................................................................................. 28
Figure 8 Automatic sampler ............................................................................................ 29
Figure 9 Overview of connections on the left side of the device.................................... 30
Figure 10 Interfaces and fuses on the PlasmaQuant PQ 9000 .......................................... 31
Figure 11 Connections for cooling water and gases ......................................................... 31
Figure 12 Plug-in connectors for gas connections ............................................................ 31
Figure 13 Ventilation openings and air filter on the rear of the PlasmaQuant PQ 9000 .. 32
Figure 14 Data on the type plate ...................................................................................... 32
Figure 15 Serial number of the device in the plasma compartment ................................ 32
Figure 16 Plasma compartment ........................................................................................ 33
Figure 17 Sampling compartment with torch holder, spray chamber, nebulizer and
hose pump......................................................................................................... 33
Figure 18 Automatic sampler - overview .......................................................................... 37
Figure 19 Connections on the right side of the automatic sampler ................................. 37
Figure 20 Nebulizer cleaning tool with installed nebulizer ............................................... 52
Figure 21 Plug-in connectors for gas connections ............................................................ 56
Figure 22 Gas distribution during pure argon operation .................................................. 57
Figure 23 Automatic sampler cannula and sample hose dismantled ............................... 59
Figure24 Automatic sampler pump.................................................................................. 60
Summaries
Summary 1 Environmental conditions for operation ........................................................... 20
Summary 2 Power supply ..................................................................................................... 21
Summary 3 Gas supply ......................................................................................................... 21
Summary 4 Exhaust unit requirements ................................................................................ 22
Summary 5 Cooling circuit requirements ............................................................................. 22
1 Basic information
1.1 User manual notes
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 components 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.
Conventions
Instructions for actions which occur in chronological order are numbered and combined in
action units.
Lists which are not in chronological order are shown as itemized lists, sub-listings as bullet
points.
Safety notes are indicated by pictogaphs 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).
2 Safety instructions
2.1 General notes
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 accident 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.
CAUTION
Indicates a potentially hazardous situation which might cause light or minor injuries.
ATTENTION
Indicates a potentially hazardous situation which might cause damage to property.
IMPORTANT
Indicates application hints and other especially useful information without any resulting
hazardous or damaging situations.
The following notice sign is attached to the rear of the PlasmaQuant PQ 9000:
The user manual must be accessible to the operating and service personnel at all times!
2.6.1 General
Work on the electrical components of the PlasmaQuant PQ 9000 may only be performed by a
qualified electrical technician according to applicable electro-technical regulations. 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 whose 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.20).
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 electronics
(behind the device enclosure) may only be carried out by the service engineers of Analytik
Jena AG and specially authorized technicians.
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 radiation 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 injuries.
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 malfunction.
The safety circuits must not be bridged.
Before opening the plasma compartment door, extinguish the plasma in the ASpect PQ
The manual plasma deactivation switch is located on the left-hand 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
inside of the coil.
− Torch parts begin to glow.
2.6.6 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 oxides.
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.
3 Specification
3.1 Technical data
Optical system
Monochromator Echelle grating double-monochromator with a focal length of F=380 mm and variable
gap; pre-monochromator with quartz prism, wavelength selection via additional
reflected neon radiator
Wavelength range 160 – 900 nm
Wavelength accuracy < 0.4 pm
Spectral resolution 0.002 nm at 2 nm
Grating Mechanically ruled grating, 79 grooves/mm, blaze angle of 74°r
Optical bank Optics in modular construction on compact cast base plate for stability and
encapsulation endurance;
photometer protection against moisture, exhaust fumes and chemical environmental impacts
Detector Two-dimensional FFT backside illuminated CCD with high quantum efficiency and
increased UV sensitivity
Display modes
Signal evaluation
Power supply
Instrument fuses
Safety circuits
Gas supply
Environmental conditions
According to DIN ISO 9022-2:2003/01
Corrosion protection The device is corrosion-proof against the samples used in the analysis
Operating temperature +15°C to +35°C, at best +20°C to +25°C
as constant as possible during measuring
Humidity 20 to 90% at 20°C
Storage Temperature: -40°C to +70°C
Use desiccant
Mass 170 kg
Dimensions (WxDxH) 987 mm x 853 mm x 937 mm
Analytic data
Device safety
The PlasmaQuant PQ 9000 conforms to the safety standards
DIN EN 61010-1 (VDE 0411T.1; IEC 61010-1)
DIN EN 61010-2-061 (IEC 61010-2-061)
EMC compatibility
The PlasmaQuant PQ 9000 has been tested for radio interference elimination and interference
immunity and fulfills the requirements stipulated by
DIN EN 61326
Environmental compatibility
The PlasmaQuant PQ 9000 has been tested for environmental compatibility and fulfills the
requirements stipulated by
DIN ISO 9022-3:2000
DIN ISO 9022-32-03-0
DIN ISO 9022-2:2003/01
EC directives
The PlasmaQuant PQ 9000 is built and tested according to standards that fulfill the
requirements stipulated by the EC directives 2006/95/EC and 2004/108/EC. Each device leaves
the manufacturer in a pristine and technically safe state. To maintain this condition and to
ensure safe operation, the operator must strictly observe the safety and operating instructions
contained in this manual. For accessories which have also been supplied, and system
components from other manufacturers, their operating instructions should be referred to.
4 Installation conditions
4.1 Environmental conditions
The PlasmaQuant PQ 9000 may only be operated in closed rooms. The location must have the
character of a chemical laboratory. The location must meet the following conditions:
It must be free of dust, drafts, vibrations and caustic fumes.
Do not place the PlasmaQuant PQ 9000 near sources of electromagnetic interference.
Avoid direct sunlight and heater radiation on the PlasmaQuant PQ 9000. Air conditioning is
recommended at the location. The cool air emanating from the air conditioning unit should
not be directed at the device.
A separate room is recommended for sample preparation and storing liquid chemicals.
The following requirements are placed on the climatic conditions in the operating room of the
PlasmaQuant PQ 9000:
Switching-on conditions
The following gases are used in conjunction with the PlasmaQuant PQ 9000
Argon as the gas for the torch (plasma gas, additive gas, nebulizer gas)
Argon as the purge gas for the spectrometer and as the cone gas
Oxygen as the additive gas (oxygen can be optionally used as the additive to the nebulizer
gas for selected applications (some organic solvents))
The standard hose length is 5 m. If other hose lengths are preferred, please contact the service
department at Analytik Jena AG.
Correct exhaustion requires the connection of an extraction hose to the PlasmaQuant PQ 9000
smokestack.
The exhaust unit is meant to remove hazardous gases generated during plasma operation,
such as ozone or nitrous gases. Use an exhaust unit made of heat and corrosion-resistant
material. The first 6 m of the exhaust unit should be made of metal.
Parameters Properties
Material Heat and corrosion resistant (recommended: V2A steel)
External pipe diameter ∅ 125 mm
Extraction output Min. 3.5 m3/min, max. 5.5 m3/min (at best 4.5 to 5 m3/min)
Adapter using flexible aluminum pipe Internal pipe diameter ∅ 125 mm
Length: approx. 1000 mm
Parameters Properties
Length of water tubing 2.0 m
Length of mains cable 2.7 m
Water rate 1.0 – 1.8 L/s
Cooling water temperature range at device cooling 17 – 24°C
water inlet
Cooler target temperature 18°C
Cooling performance 3 000 W
Pressure setting 3.7 bar (53 Psi)
HF generator
The PlasmaQuant PQ 9000 uses a free-running 40 MHz HF generator (High-Frequency
Generator). The HF generator transfers power ranging from 700 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 conducting
spring located in the vicinity of the induction coil through the high-frequency field in the torch.
Torch
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 insulates 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 induction 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 melting due to the high plasma
temperatures.
The auxiliary gas flows in the intermediate space between the inner tube and the injector. 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 measurement
solution is transported by the nebulizer gas from the spray chamber through the injector into the
plasma.
subsequent assembly unnecessary. On the other hand, this torch has to be completely replaced
when worn.
The PlasmaQuant PQ 9000 includes a special V Shuttle Torch design. The up-right
arrangement of the torch reduces clogging and soot formation.
The torch is mounted with the holder (shuttle) onto the rail guide. Doing so automatically
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 adjusted operating
position.
Optical system
In the PlasmaQuant PQ 9000, 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.
The selectivity of analysis is implemented by the high-resolution double monochromator on the
basis of a prism and an echelle grating monochromator (High-Resolution Optics). This achieves
a very compact design and a high spectral resolution which corresponds to a spectral resolution
of < 2 pm per pixel at 200 nm. The monochromator is wavelength-stabilized by the use of an
integrated neon source. Wavelength reproducibility is achieved by the internal Ne-line
calibration 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 analysis 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.
The automatic sampler 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:
The purging vessel is installed at the automatic sampler. A hose pump at the automatic sampler
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 flows into the waste container during
purging. The wash liquid between the measuring breaks or for purging steps within a measuring
routine is also taken from the wash cup.
A mains connection supplies operating voltage to the automatic sampler.
1 "USB/B"
2 "PC"
3 "RS 232"
4 "Autosampler"
5 "Hydride System"
6 "I/O"
7 Fuse S3 25 A
8 Fuse S2 6 A
9 Fuse S1 10 A
In the PlasmaQuant PQ 9000, argon is used as a gas for the torch, the nebulizer and for
purging the spectrometer. The purge gas is then directed via the cone for axial observation as a
counter gas to avoid a heavy load being placed on the cone and plasma window by the plasma
torch. Oxygen can be optionally connected as an additive gas.
Plug-in connectors are used for the gas connections of the PlasmaQuant PQ 9000. Hoses are
pushed into the connector as far as possible and are thus securely fastened. To release the
connection, you have to push the blue ring inwards and pull the hose out at the same time.
The hoses for cooling water are also equipped with quick couplings. When connecting the
hoses, the connecting pieces on the hoses are pushed into the sockets all the way until they
engage with a click. When releasing the connection, you have to push the ring on the socket
back and pull the hose out of the connection. The valves in the quick couplings prevent the
cooling water from flowing out.
1 Air filter
2 Exhaust vent
3 Fan
Figure 13 Ventilation openings and air filter on the rear of the PlasmaQuant PQ 9000
The electrical connection data can be found on the type plate on the terminal strip.
1 Device type
2 Voltage
3 Frequency
4 Typical average power consumption
5 Serial number of the device
6 Disposal instructions (Do not dispose of as domestic
waste!)
7 CE marking
6 Manufacturer
The serial number is also printed behind the door in the plasma compartment.
Figure 17 Sampling compartment with torch holder, spray chamber, nebulizer and hose pump
6.4.1 Installation of the torch, nebulizer with spray chamber and sample supply
13. Connect the sample pump hose to the hose of the automatic sampler (for automatic
operation) or a hose leading directly into the sample (manual operation).
14. At the waste pump hose, connect the waste hose to the waste container.
Attention!
The waste hose must not dip into the liquid! This prevents waste material from being
pumped into the nebulizer system in case of faulty pump hose connection.
Note
DIP switch 5 is set to "ON".
For the use of the automatic sampler on the PlasmaQuant PQ 9000, only the connections
described in Figure 19 are required. All other connections and displays are for service purposes
or not in use.
ATTENTION!
The automatic sampler must not be connected to the mains during installation.
12. Connect the hose to the sample hose of the PlasmaQuant PQ 9000.
13. Connect the PlasmaQuant PQ 9000 and the automatic sampler to the interface cable
("Autosampler" on the PlasmaQuant PQ 9000 and "Host" on the automatic sampler.
14. Connect the mains cable first with the mains connector of the automatic sampler and
then with the mains socket.
15. Set the pump speed on the automatic sampler so that the liquid level remains constant
and not too much wash liquid overflows.
7 Operation
Click on to open the PLASMA / CONTROL window and click on [IGNITE PLASMA].
After a cooling phase of the detector the plasma will be ignited.
16. Verify that the plasma forms correctly, i.e., the plasma extends in a cone shape beyond the
induction coil and tapers upwards.
If a ring plasma forms (plasma is formed only inside the induction coil) or a rattling sound
can be heard, press the red plasma deactivation switch on the left side of the device.
Before the next ignition attempt, verify that the sample hose is immersed in the wash
solution and that the gas supply and the recirculating chiller are working properly.
The plasma ignites and the hose pump starts. The PlasmaQuant PQ 9000 is ready
for measurement after a brief plasma warm-up period.
ATTENTION!
Before plasma ignition, the following conditions are checked via internal safety circuits:
− Gas flow, cooling and exhaustion are switched on and comply with the specified
connection conditions.
− The torch is in working position.
− The plasma compartment door is closed.
If a fault is detected in one of the components the plasma will fail to ignite.
ATTENTION! Wait for the PlasmaQuant PQ 9000 to cool down before switching it
off!
After extinguishing the plasma, wait for at least 2 min. before switching off the device at the
power switch.
Alternatively, use to open the PLASMA window and click on [PLASMA OFF].
3. Select the FILE EXIT menu item and end the ASpect PQ program.
4. Confirm the query about switching off the purge gas for the detector with [YES] if the purge
gas should be switched off.
If work is only interrupted for a short period (up to 30 min.), do not switch off the purge gas.
This will save time during the ignition process until the detector is sufficiently purged.
5. Wait for the message stating that the device and the cooling can be switched off to appear.
6. Switch off the PlasmaQuant PQ 9000 and, if applicable, the automatic sampler at the
respective power switch.
7. Release the pump hoses at the PlasmaQuant PQ 9000.
− Release the pressure levers to ensure that the hose guide no longer exerts pressure
on the hoses.
− Pull the hose stoppers on the left-hand side of the pump from their lock.
8. In case the automatic sampler is used, release the pump hose in the same way as with the
hose pump on the PlasmaQuant PQ 9000.
9. Close the gas supply after switching off the devices.
After you select the file name, the measurement routine will start according to the
settings made in the method and the sequence.
6. If you use an automatic sampler, the measurement runs automatically. In the case of
manual sample feed without an automatic sampler, follow the instructions for the provision
of samples displayed on the screen.
This chapter contains all the instructions for care and maintenance which users can and must
perform themselves. All maintenance work and repairs beyond this scope must only be
performed by service engineers from Analytik Jena AG or persons authorized by Analytik Jena
AG. To guarantee perfect functioning, the PlasmaQuant PQ 9000 should be inspected on an
annual basis by service engineers from Analytik Jena AG. Only use replacement parts from
Analytik Jena AG. Laboratory parts required for routine operation can be ordered from Analytik
Jena AG.
CAUTION! Risk of eye and skin injuries due to UV and electromagnetic radiation!
Plasma emits UV radiation and high-frequency electromagnetic radiation which can cause
serious eye and skin injuries as well as other health problems. Therefore, the plasma
compartment door must be closed before igniting and operating the plasma. Safety circuits must
not be bridged by the user during maintenance work!
Recirculating chiller
Coolant tank Check coolant level at the After replacement, otherwise monthly
tank level indicator and Replenish on reaching the minimum
replenish level
Air filter Clean Check monthly for soiling,
cleaned if soiled
Foam sieve in the Check for deposits and Monthly
tank clean
Coolant Replace Annually
The torch must be cleaned in case of visible soiling (deposits or scaling). Depending on the
sample matrix, this may have to be performed on a daily basis or in much longer intervals
(monthly).
4. Pull first the outer and then the inner tube from
the holder.
Caution! Breakage of glass!
The quartz tubes are very fragile and are firmly
mounted in the ground glass connector of the
holder. Put on glass handling gloves to
dismantle the torch.
12. Insert the outer tube into the torch body. Make
sure that the ground joint seal is tight.
13. Install the torch and bonnet according to the section "Installation of the torch, nebulizer
with spray chamber and sample supply" p. 34.
The torch body of the demountable torch only needs to be replaced if it is cracked. It does not
need to be cleaned together with the other glass components of the torch.
1. Dismantle the torch as described in the section "Cleaning the demountable torch" p. 46.
Attention!
The connections are of different lengths and
must not be swapped. The torch body may
otherwise break when the connections are
screwed in!
8. Screw in the longer gas connection into
opening 1 (bottom) and the shorter gas
connection into opening 2 (top).
Tighten the connections alternately.
The connections must also be flush with the
upper edge of the holder. Do not screw in any
further under any circumstances!
1. Pull out the spring bolt at the height adjustment and allow the carriage with the torch on
the adjusting rail to slide carefully down.
2. Remove the fork clamp and take off the spray chamber.
Carefully place the spray chamber to one side.
3. Unscrew the torch from the carriage (see the section "Cleaning the demountable torch"
p. 46).
15. Install the torch and bonnet according to the section "Installation of the torch, nebulizer
with spray chamber and sample supply" p. 34.
The nebulizer must be cleaned if particles or high concentrations of salt in the samples have
clogged it up. An indicator that the nebulizer has clogged up is increased carrier gas pressure:
1. Unscrew the nebulizer holder from the syringe and fill the syringe with methanol. Pull the
plunger out to the first red O-ring.
2. Screw the nebulizer holder on the syringe.
3. Push the nebulizer with the tip first into the holder until the lateral carrier gas connection
comes to rest in the holder groove.
4. Hold the nebulizer cleaning tool over a receptacle and push the plunger into the syringe.
The methanol should flow out of both connection pieces.
To remove stuck particles from the nebulizer cannula, you can increase the pressure by
closing the carrier gas connector with a finger. Use the same method to increase the
pressure by closing the sample inlet to remove particles from the carrier gas connector.
5. Gently shake the nebulizer cleaning tool to remove the methanol from the nebulizer.
6. Remove the nebulizer from the holder. Shake any remaining methanol from the nebulizer
cleaning tool.
7. Place the nebulizer once again in the holder and move the plunger three times quickly in
and out to remove the methanol also from the nebulizer.
8. Remove the nebulizer from the holder. Connect the nebulizer to the spray chamber. Let
argon flow through the nebulizer for at least three minutes before using it for the next
analysis.
Clean the sampling compartment and the plasma compartment daily with a damp (not dripping!)
cloth. To remove stubborn contamination a commercial surfactant may be used.
Spots, drops or larger spillages should be removed and cleaned using an absorbent material
such as cotton wool, laboratory wipes or cellulose.
Check the pump hoses daily before starting work and replace any hoses if they are discolored,
no longer flexible or even porous (see the section "Installation of the torch, nebulizer with spray
chamber and sample supply" p. 34).
The windows situated in the plasma compartment in front of the transfer optics must be
replaced if their transmission has greatly deteriorated, especially in the UV range. Cleaning the
windows does not usually completely restore UV permeability; the cleaning effect varies with the
wavelength. Average losses of around 30% have to be expected in the UV vacuum. In the
visible range, transparency can generally be fully restored.
Checking permeability
To check permeability, use a method that you routinely use.
1. Select 3 lines, one line each in the low UV range, in the medium and in the high
wavelength range.
2. For a QC sample, determine the intensities at these 3 wavelengths and record the results
in a QC card or a table.
3. If the intensity has fallen to such an extent that the required detection limits can no longer
be reached, clean or replace the windows.
IMPORTANT
The quartz windows are sensitive. Use clean gloves when installing the new windows and avoid
touching the new quartz windows with your hand. Wipe away any fingerprints with pure alcohol
and dry the windows.
If the window has not been unscrewed with the cone, but remains in the window opening, it
must be pushed down from above. This requires the deflection mirror to be dismantled.
Check for leak tightness in the scope of the weekly safety check or before placing the
PlasmaQuant PQ 9000 into operation if the device has been previously disconnected from the
gas supply system.
For this purpose, close the shut-off valve of the gas supply system and check the pressure at
the downstream manometer. If the pressure drops sharply, search for leaks in the gas supply:
1. Open the shut-off valve.
2. Brush connections with a heavily foaming liquid (e.g., soap solution). If foam bubbles form
at the gas connections when starting up, disconnect the gas supply.
3. Unscrew the gas connections and check for correct fitting. If there are sealing rings, check
them. Replace worn out sealing rings.
4. Tighten the gas connections, observing the correct positioning and check again for gas
leaks.
A red lamp lights at the fuse holder if a fuse is damaged. Use only fuses of the following type:
The fuse holders are located on the terminal strip on the left-hand side of the device.
In case of repeated fuse failure, inform the service department at Analytik Jena AG.
The air inlet filter of the PlasmaQuant PQ 9000 is located at the rear of the device. Replace the
filter if it is very dirty.
The cannula and sample hose can be ordered ready for use. However, it is also possible to
replace both separately.
1. Switch off the automatic sampler at the power switch.
2. Disconnect the connection between the sample hoses of the automatic sampler and the
PlasmaQuant PQ 9000.
3. Carefully pull the sample hose from the hose guides on the automatic sampler.
4. Unscrew the cannula from the holder on the automatic sampler.
5. Unscrew the banjo bolt at the cannula and the sample hose from the connecting piece.
6. Only use a straight-cut, round and unpinched hose end for the connection when replacing
the sample hose. First push the banjo bolts and then one sealing cone with the conical side
onto the hose and the cannula. The sealing cone and the hose or cannula end must be
flush (see the figure below).
7. Screw the banjo bolts into the connecting piece hand-tight.
8. Install the cannula in the automatic sampler holder and thread the sample hose through the
hose guides at the automatic sampler (also see the section "Installing the automatic
sampler" p. 37).
1 Cannula
2, 6 Banjo bolt
3, 5 Sealing cone
4 Connecting piece
7 Sample hose
7. Place the hose guide over the hose and fix it with the clamping arm.
1 Hose guide
2 Clamping arm
3 Speed controller
4 Pump hose
5 Mixing cup
6 Connection to suction hose for
wash solution
7 Connection to pump hose wash
cup
8 Block for clamping the hoses
9 Pump rolls
If the wash cup has overflowed during an analysis run, immediately interrupt the workflow and
clean the device.
1. Stop the workflow immediately.
2. Take up the liquid with cellulose wadding or a cloth. Wipe the surface dry.
3. Ensure that the outlet can be drained, i.e., remove any sharp bends in the draining hose or
make sure that the draining hose does not dip into the liquid in the waste bottle.
The stainless steel air filter behind the front panel must be checked monthly and cleaned if
necessary.
1. Pull out the filter to the side.
2. Remove fluff and dust.
3. Clean the filter with water. A mild commercial surfactant may be added to the water. Then
rinse the filter with clean water.
4. Dry the filter carefully.
5. Slide the dried filter back behind the panel.
The stainless steel foam sieve is located in the filler neck. Clean the foam sieve once a month.
1. Unscrew the sealing cap on the filler opening and remove the foam sieve.
2. Rinse off all foam thoroughly from the sieve with distilled/deionized water.
3. Fit the foam sieve into the filler opening and close the sealing cap by screwing hand-tight.
CAUTION! Biocide!
Observe the safety data sheet of the biocide used.
Required equipment:
− 10 L of distilled/deionized water
− Biocide / corrosion protection set for recirculating chiller (order no. 418-13-5850-015-
14)
− A suitable appropriately sized vessel made of glass, plastic or stainless steel for mixing
the coolant
− A bucket to catch the drained coolant
− Pour the prepared coolant into the tank until the MAX level mark is reached.
− Switch on the recirculating chiller and observe the level indicator. The level drops when
the pump is operating.
− Continue to slowly fill the tank with the coolant until the level stabilizes slightly below
the MAX mark.
− Remove the funnel and seal the filling opening with the screw cap.
− Confirm the closing step in the wizard.
3. Wait for the message in the wizard indicating that the coolant has been changed. Exit the
wizard.
9 Fault removal
9.1 Fault removal
The following chapter describes a number of possible problems that the user can partially
remedy independently. If such problems occur frequently, the service department of Analytik
Jena AG must always be informed.
System monitoring takes place as soon as the PlasmaQuant PQ 9000 is switched on. Any
errors that occur are displayed in a window after start-up.
The user must acknowledge the error messages by clicking on the [OK] button.
3811 No factory data found in instrument storage (FINFO)! Please restart instrument and
software. If the problem persists, contact service!
Cause Remedy
− There is no production data for line − Contact service for line offsets
offset present in the device memory − Inform service
− The RAM memory is incorrect
3870 No purge gas available!
Cause Remedy
− No Ar gas pressure is present − Check the Ar gas pressure
3871 No cooling water available (detector cooling)!
Cause Remedy
− The recirculating chiller is not switched − Switch on the recirculating chiller
on − Check the cooling water flow for
− The cooling water flow is too low > 0.85 L/min
3872 CCD cooling is inactive!
Cause Remedy
− A termination occurred during plasma − If the plasma is burning, in the
ignition SPECTROMETER window, activate the
CCD COOLING option and then click on
[SET].
5208 Status: CCD cooling error! Please check purge gas flow!
Cause Remedy
− No Ar gas flow is present − If the plasma is burning, in the
SPECTROMETER window, activate the
CCD COOLING option and then click on
[SET].
3874 Spectrometer purging is still active!
Cause Remedy
− The Ar purging of the spectrometer is − Wait until the error message disappears
not yet complete and purging is complete
4003 Plasma shut-down because emergency switch has been activated!
Cause Remedy
− The red plasma deactivation switch on − Reignite the plasma
the left side of the device has been
operated
4004 Plasma shut-down by plasma sensor!
Cause Remedy
− Air is present during the ignition of the − Before ignition, close the cartridge of the
plasma in the spraying chamber pump hoses, dip the hoses in water,
− The plasma is flickering and unstable purge the spraying chamber with Ar via
due to the sample matrix nebulizer gas
− Dilute the sample matrix
− Adjust the plasma conditions
No signal
Cause Remedy
− The pump does not deliver any − Check the hose / hose pump
sample
− The nebulizer is clogged; the If necessary, check with Na solution (1 g/L) – if no plasma coloring
mass-flow rate is very high (in (orange) is observed:
the PLASMA REPORT window) − Check the nebulizer nozzles for obstructions and clean them
(see "Cleaning the nebulizer" p. 50)
− If the sample nozzle is clogged filter the solutions
− If the argon nozzle is clogged dilute the measurement
solutions or use an argon humidifier
− The injector is clogged Check with Na solution (1 g/L) – if no plasma coloring (orange) is
observed:
− Check the injector tip for deposits and clean it
− Increase the distance between the injector and plasma
(move the torch down on the height adjustment or increase
auxiliary gas flow)
− The nebulizer gas is set too low − Optimize the carrier gas flow
− Adjustment on the analyte − Adjust the x/y offset for the method parameter in the PLASMA /
channel ADJUST PLASMA VIEW window (see the online help or the
ASpect PQ operating instructions)
− There is a leak in the sample − Check the sample and pump hoses and their plug connectors
introduction system (sample and
pump hoses)
− The windows in the plasma − Replace the windows
compartment are dirty
− The transparency in the UV − Check the duration of the purge gas flow; wait until the purge
vacuum is missing gas has completely purged the spectrometer compartment
The sensitivity is too low
Cause Remedy
− The cause and remedy are the
same as for the error indication
No signal
The measured value is too low
Cause Remedy
− Calibration is incorrect − Check the calibration solutions
− Low solubility substances lead − Optimize sample preparation
to low concentrations
− Low solubility substances are
not completely digested
− Volatile substances escape − Optimize sample preparation
during sample preparation
− There is a spectral interference − Use another analytical line
in the calibration standard
− Error in the background − Select background correction points that are not spectrally
correction disturbed
− Better adjustment of a curved background by a non-linear
correction function
− When using an internal standard − Wrong dosage
− The internal standard is not in the linear range select a
lower concentration for the internal standard
− The adjustment of the response to changes in the plasma
temperature is inadequate
1. Adjust the matrix
2. Find a better adjustment between the behavior of the
analysis line and the internal standard
− Contamination/carry-over in the − Remedy the cause of carry-over/contamination
cal/zero solution
− The sample solution is viscous / − 1. Adjust the matrix (add to calibration solutions or dilute)
has a higher density than the − 2. Use one/several internal standards
calibration solution
− The pump hose is new − Wait until hose delivery is stable
− The spray chamber is filled − Empty the spray chamber
− Check the pump hose for drainage; if necessary, select a
larger cross-section
Drift
Cause Remedy
− Change in the temperature in − A change of 1°C causes a drift of approx. 1%
the spray chamber − Thermostatically control the spray chamber or ensure air
conditioning in the laboratory
− The transparency in the UV − Check whether the argon purging of the spectrometer is
vacuum is not sufficient complete (activate the purge gas flow long enough)
ATTENTION!
Use suitable transport packaging!
Unsuitable packaging material and cooling water residues may cause damage to the device!
Only transport the PlasmaQuant PQ 9000 in its original packaging! Ensure that the device is
completely empty!
Equipment: 4 handles
CAUTION!
Risk of injury if the device falls!
Handles which are screwed in loosely may result in damage during transport. Screw in the
handles up to the end stop!
ATTENTION!
Risk of damage to the device due to the cooling water freezing!
The ambient temperature may fall below freezing when transporting the device. Therefore,
make sure the cooling water is completely drained before transport.
Observe the safety instructions in the section "Safety instructions, transport and commissioning"
p. 11. Transport the PlasmaQuant PQ 9000 and its components very carefully to prevent
damage from impact or vibration. The device should be transported in such a way that major
temperature fluctuations are avoided and the formation of condensate is thus prevented.
The following requirements are placed on the climatic conditions during transport of the
PlasmaQuant PQ 9000:
Temperature range: -40°C to +70°C
If the PlasmaQuant PQ 9000 and add-on devices are not installed immediately after delivery or
are not required for a prolonged period of time, they should best be stored in their original
packaging. A suitable desiccant should be added to the packaging to prevent damage from
moisture.
ATTENTION!
Check that all requirements are met at the installation location (see the section "Installation
conditions" p. 20).
Observe the safety instructions in the section "Safety instructions" p. 9.
CAUTION
Observe the operating manual of the recirculating chiller!
1. Connect the PlasmaQuant PQ 9000 and the recirculating chiller with the cooling water
hoses:
Mobile cooling unit "Outlet" PlasmaQuant PQ 9000 "In"
Mobile cooling unit "Inlet" PlasmaQuant PQ 9000 "Out"
Note:
For better allocation of the connections, one of the hoses is marked with hose clips at both
ends.
2. Electrically connect the recirculating chiller and switch it on.
3. Prepare the cooling water (see the section "Changing the cooling water" p. 61).
4. Start ASpect PQ and open the wizard for changing the cooling water.
5. Switch on the PlasmaQuant PQ 9000.
6. Fill cooling water with the assistance of the wizard. Skip item (2) "Draining the cooling
water" in the wizard.
7. Set the following parameters at the recirculating chiller:
Temperature: 18°C
Pressure: 53 psi
11 Index
Maintain 56
Guidelines 18
A
Air filter 31 H
Recirculating chiller 60
Replace 57 High-Frequency Generator 25
ASpect PQ error message 62 High-Resolution Optics 27
Automatic sampler Hydrofluoric acid 5
Fuse 59
Replace cannula 58
Replace pump hose 58
I
Setup 28 ICP-OES
Auxiliary gas 26 Physical principle 24
Induction coil 25
C Injector 26
Installation
Compressed gas container 12 Automatic sampler 36
Conducting spring 25 Torch 33
Cooling system 21 Installation site 19
Cooling water Interfaces 30
Change 60
Prepare 60
Cooling water connection 30
L
Liability 7
D Liquid gas systems 12
Detector 27
Device layout 22
M
Device safety 18 Mains connection 19
DualView PLUS 27 Maintenance intervals 44
Maintenance tasks 44
E Measurement 41
Monochromator 27
EMC compatibility 18
Environmental compatibility 18
Equipment fault 65
N
Exhaust unit 21 Nebulizer 25
Clean 51
F Nebulizer cleaning tool 51
Nebulizer gas 25
Foam sieve 60
Function
Bonnet 26
O
Generator 25 Operating gas 24
Induction coil 25 Operating temperature 19
Injector 26 Ozone 12
Nebulizer 25
Pump 25
Spray chamber 25
P
Torch 26 Personnel 9
Transfer optics 27 Plasma
Fuse Extinguish 40
Change 56 Faults 41
Ignite 39
G Plasma compartment 24
Clean 52
Gas connection 30 Clean windows 52
Gas flows 26 Connections 32
Gas supply 20 Replace windows 52
Gas system Plasma gas 26
Problems T
Analytical 65
Protection class 18 Technical data
Protection type 18 Automatic sampler 17
Pump 25 Computer 17
Pump hose 35 Cooling system 17
Environmental conditions 16
Exhaust unit 21
R Fuses 16
Recirculating chiller Gas supply 16
Maintain 60 Optical system 15
Wizard 60 Power supply 15
Repair 14 Temperature
Ring plasma 12 Operation 19
Torch 26
Clean 45
S Clean one-piece torch 49
Safety circuits 11, 16 Demountable 26
Safety instructions One-piece torch 26
Exhaust unit 12 Replace torch body 47
Gas supply 12 Transfer optics 27
Ring plasma 12 Type plate 31
Transport 10
Sample racks 28 U
Sampling compartment 24
Clean 52 Use 5
Connections 33 User manual conventions 5
Serial number 31 UV permeability 52
Space requirement 22
Spray chamber 25 V
Symbols
Device 8 V Shuttle Torch 27
Manual 8
W
Warranty 7