Icp 6000

iCAP 6000 Series ICP-OES Spectrometer
Diagnostics Manual
©
2010 Thermo Fisher Scientific Registration No. 441506 SOLAAR House, 19 Mercers Row, Cambridge CB5 8BZ,
United Kingdom. Telephone +44 (0) 1223 347400, Fax +44 (0) 1223 347402,
http://www.thermoscientific.com
ICAP 6000 Series ICP-OES Spectrometer Diagnostics Manual
Contents
1 Introduction......................................................................................................................... 3
1.1 iTEVA Journal............................................................................................................... 3
1.2 iTEVA Database ........................................................................................................... 3
2 Installation Problems .......................................................................................................... 4
2.1 Alignment...................................................................................................................... 4
2.2 Carbon Position check for iCAP 6300 and 6500.......................................................... 4
2.3 Carbon Position check for iCAP 6200 .......................................................................... 5
3 Sequence of Operations .................................................................................................... 6
4 Fault Finding Section ......................................................................................................... 9
4.1 LEDs on side of instrument .......................................................................................... 9
4.2 I/O Board Fuses ........................................................................................................... 9
5 Instrument Communication Problems .............................................................................. 10
6 Instrument Error Codes and Definitions ........................................................................... 12
6.1 CID Camera................................................................................................................ 12
6.2 RF and I/O Board Problems ....................................................................................... 14
7 RF Ignition Problems........................................................................................................ 15
7.1 RF Test Indicator ........................................................................................................ 16
8 Ignition Problems Hints and Tips ..................................................................................... 17
8.1.1 Check for Argon/Air leaks around Torch & Spray Chamber.............................. 17
8.1.2 Check and Clean Fibre Optic Cable .................................................................. 18
8.2 Cleaning the Plasma Torch ........................................................................................ 18
8.3 Cooling Water for the RF Load................................................................................... 18
8.4 Check or Replace Argon Supply ................................................................................ 19
8.4.1 Igniter Position ................................................................................................... 19
9 Mk2 RF Diagnostics ......................................................................................................... 20
9.1 Error messages .......................................................................................................... 20
9.2 Ignitor module failure .................................................................................................. 22
9.3 LEDs........................................................................................................................... 22
9.3.1 Control board LEDs ........................................................................................... 22
9.3.2 RF interface PCB board LEDs........................................................................... 22
9.3.3 Manufacturing software ..................................................................................... 23
10 Analytical Problems Hints and Tips............................................................................ 24
10.1 Poor Precision and Analytical Drift......................................................................... 24
10.1.1 Gas pressures ................................................................................................... 24
10.1.2 Spray chambers................................................................................................. 25
10.1.3 Nebulisers and centre tubes .............................................................................. 25
10.1.4 Teflon Capillary Tubing...................................................................................... 26
10.2 Poor Accuracy/Feedback ....................................................................................... 28
11 Poor Detection Limits ................................................................................................. 28
12 Suggested Maintenance in the Case of Poor Precision and Detection Limits ........... 29
12.1 Introduction ............................................................................................................ 29
12.2 Typical Maintenance Schedule .............................................................................. 29
12.3 Replacing Pump Windings ..................................................................................... 29
12.4 Preventing Blocking of the nebuliser...................................................................... 30
12.5 Removing the Concentric Glass nebuliser............................................................. 32
12.6 Removing Solids from the Nebuliser...................................................................... 32
12.6.1 To Rinse the Nebuliser ...................................................................................... 32
12.6.2 Particles ............................................................................................................. 32
12.6.3 Solid Deposit in Sample Capillary ..................................................................... 33
12.6.4 Organic Matter ................................................................................................... 33
12.6.5 Plugged Capillary (fusible solids e.g. waxes) .................................................... 34
Page 2 of 34 Version 5.2

1 Introduction
This section is written to help diagnose problems within the iCAP 6000 system.
It includes error codes from the iTEVA software and how to interpret them.
Flow charts to guide you through operational process, and hints and tips to resolve other
problems.
1.1 iTEVA Journal
A useful tool for diagnostic purposes is the Journal found in iTEVA. It lists all the daily
operations that happen when the instrument is used.
In conjunction with this chapter the journal enables decisions to be made on how to proceed
with the repair of the instrument. Engineers should familiarise themselves with its function.
The iTEVA Journal file can be loaded onto your laptop (as explained below) computer for
further investigation of possible problems.
To load the Journal file onto a laptop computer: Copy the file Cid_MS32.TJA found in the
iTEVA/SysData directory into the same directory on your Laptop.
1.2 iTEVA Database
In addition to the journal, it is sometimes necessary to send an iTEVA database to Technical

Support. This is useful when problems are being seen with results – perhaps saturation or
poor results.
Databases can be found in the AnData folder of the iTEVA directory on the hard drive of the
instrument control PC. To send the database, both the .ldf and the .mdf files must be sent
together.

2 Installation Problems
The section discusses problems that may occur when carrying out an Alignment check during
an installation. The process is checking for the position of the carbon line at 193 nm. This line
is theoretically positioned at 380, 220 on the camera.
2.1 Alignment
The installation procedure involves performing a Spectrometer Optimise. During this, the
software checks the carbon position. The x and y drift correction values are recorded in the
journal as shown below.
Note: this operation is carried out and recorded in the journal whenever the plasma is lit.
However, for an accurate measurement the instrument must be stabilised, so if an instrument
has just been installed it will take at least 3 hours for the polychromator to thermally stabilise.
If an instrument has been switched off for a long period of time, the polychromator
temperature read out may not be an accurate gauge of tank stability.
Once the instrument is stable, if these numbers are greater than ± 3, then some optical
alignment will need to be carried out.
The techniques for aligning the carbon position for 6200, 6300 and 6500 instruments are
shown below.
2.2 Carbon Position check for iCAP 6300 and 6500
Using iTEVA Analyst, take a Low Wavelength full frame image.
The carbon line 193.091nm (475) should be found at column 380, row 220 ±3.
The installation procedure If it is not within 3 pixels adjust the rear M3/M4 Yaw and Pitch
screws to correct the error as shown in Section 7.2 below.
Before any alignment record the carbon line centre position
Column =
Row =

2.3 Carbon Position check for iCAP 6200
Using the Manufacturing Software, take a Low Wavelength full frame image.
Using the diagnostics window, take a full frame image of the carbon line 193.091nm (475)
column 380, row 220 on the UV slit and make sure it is within 3 pixels, if not adjust the rear
M3/M4 Yaw and Pitch screws to correct the error as shown in Section 7.2 below.
Zoom in on the carbon position by dragging a box around the bright spot.
Position in this
case is
385 – 4 = 381
and
225 – 4 = 221
therefore C
position is OK.
4 pixels
4 pixels
Note: if the box you created to zoom is not exactly square, white lines will show the edge of
the box.
The row and column numbers at the corners of the box are shown on the screen. To check
the carbon position is within 3 pixels of 380,220, count across from the edge of the zoomed
box. If it is not within 3 pixels adjust the rear M3/M4 Yaw and Pitch screws to correct the error
as shown in Section 7.2 below.
If the alignment is significantly out and the carbon line cannot be positively identified, use the
Optical Alignment tools in the Manufacturing software.
Before any alignment record the carbon line centre position
Column =
Row =
3 Sequence of Operations
iCAP Instrument ON sequence
Turn gases on
OK
Turn water recirculator

Correct AC problems
on
No No
Check side panel
Switch power on No OK LED's are as shown
Check AC power
fans switch on in LED section
Switch on computer
and start up iTEVA
OK
See communication
iTEVA communicates No
section
with instrument
OK
Yes See I/O problems

I/O error messages
displayed
OK
Unit standby
OK
OK
No See iCAP ignition

Ignite plasma problems
See ignition sequence

iCAP Ignition Sequence

Analysis Sequence
Set flush pump speed
Apply flush pump delay
Set slit view (move fore-optic

Motors)
Set analytical pump speed
Set RF power
Set gas flows
Wait for source and pump to

stabalise
Yes Yes
Flash LED
Run pre-exposure
Open shutter
Close shutter
Flash LED
Run the exposure Open shutter
Close shutter
Are there more slit/views to run?
No
Send results for single repeat
to iTEVA
Are there more repeats to be run
No

4 Fault Finding Section

Check the LEDs at the rear of the right side before proceeding to diagnostics
4.1 LEDs on side of instrument

LED 1 FLASHING* RF processor has booted up properly
LED 2 ON TE Peltier supply on
LED 3 ON + 5 volt supply is on (camera and I/O board logic)
LED 4 ON + 24 volt supply is on (solenoids, MFCs, camera
shutter)
LED 5 ON + 15 volt supply is on (camera and I/O PCB analogue
supply, also required by both RS232 channels)
LED 6 ON - 15 volt supply is on (camera and I/O PCB analogue
supply, also required by both RS232 channels
LED 7 ON + 12 volt supply is on (used to hold solenoid valves in
on state) (not camera shutter)
LED 8 ON PIC watchdog (blinks on/off once a second when PIC is
running correctly)
LED 9 ON the boost purge switch is depressed
* LED 1 will be on permanently on instruments with a Mk1 RF generator fitted.
Note: the power supply LEDs only show that there is a supply, not that it is OK and
within tolerance. If they are glowing dimly it could mean the power supply has a problem.
Check voltages using a digital volt meter.
Note also, some solenoid valves are initially turned on with the 24 volt supply and then
held on with the 12 volt supply.
4.2 I/O Board Fuses

FS 200 5V and Heater Blanket 6.3 A
FS 300 +/- 15V 1A
FS 301 +/- 15V 1A
FS 600 Heater Blanket 6.3 A
Replacement fuses can be purchased locally or are available as spare parts:

6.3A (20x5mm), antisurge fuse, 250Vac – 2422 086 01136
1A (20x5mm), antisurge fuse, 250Vac – 2422 086 01021
See repair section of the manual for details of replacement.

5 Instrument Communication Problems
Before trying anything else, switch off the instrument and re-start iTEVA.
PROBLEM/SYMPTON THINGS TO CHECK

iTEVA will not Ensure the instrument has had enough time to initialise. Leave it
connect/initialise the at least five minutes to see if anything happens.
instrument, or there Has there been a change to the PC set up?
are intermittent Perhaps firewall updates or new software has been added that
communication errors may affect communications.
If possible try connecting to the instrument with a different PC or
laptop.
Does it cure the problem if you eliminate the RJ45 connector by
connecting the network lead from the PC directly into the
camera?
Is the PC configured as per the installation instructions, including
the firewall configuration and network settings, etc?
Ping the instrument from the Command Prompt by typing “ping
90.0.0.50”. Do you get a successful response? If YES it
confirms the network card is configured correctly, and the
connection to the instrument is okay.
Once you have confirmed the Ethernet port is set up correctly
confirm the problem still exists. If YES, open the network
connections property page and confirm the status is “connected”
and the packets sent and received values are occasionally
increasing. If the status is not displaying “connected” check the
connection between the instrument and the PC.
If this hasn’t yet resolved the problem the problem may be with the instrument so
please move onto the next section, to check for instrument communication
problems.
Ping the instrument from the Command Prompt by typing “ping
ICPOES_PCB”.
Does the instrument respond?
If 90.0.0.50 pings successfully but ICPOES_PCB doesn’t then
there is a problem with the Hosts file.
(The command prompt can be found via

Start\AllPrograms\Accessories)
If you see a different IP address it means the host file has been
set-up incorrectly. If the response is successful, it confirms the
host file is set-up correctly.
NO
YES
If iTEVA fails to initialise the instrument, move onto the next section to determine if
the instrument side of the communications are okay.
While using the Does the IO Controller board function normally as detailed
instrument, or during elsewhere in this manual? Pay special attention to the I/O
analysis the network Controller LEDs at the rear right of the instrument.
connection, and/or NO
communications YES
between iTEVA and
the instrument is lost.
The network
connection is then re-
established
automatically; however
the instrument may or

may not reconnect to
iTEVA.
Connection between Are the I/O Controller board power supply LEDs stable and not
iTEVA and the cycling, and is the Watchdog LED flashing at all times? You will
instrument keeps need to monitor these LEDs for at least 6 to 10 minutes checking
resetting every 3 to 5 for an infrequent or short loss of supply.
minutes. You will
notice one of both of Are all cables and connections between the camera and I/O
the following effects: controller board OK?
The instrument Try unplugging and re-plugging all connectors.

connection as shown
in the windows task Disable the TE cooler by disconnecting the smaller of the 2
bar will disconnect connectors on the front of the camera, is the camera still
then reconnect every rebooting?
3 to 5 minutes.
NOTE: The TE cooler should only be disconnected when the
The foreoptics motors instrument is powered off.
may reinitialise every 3
to 5 minutes.
Only when it has been confirmed IO Controller board is functioning correctly,

should the camera be replaced.
If the camera is working correctly, when you connect a spare flash up LED and turn the
power on, the LED should flash 4 times.

6 Instrument Error Codes and Definitions
6.1 CID Camera
Before trying anything else, switch off the instrument and re-start iTEVA.
PROBLEM/SYMPTON POSSIBLE CAUSE
MAKE SURE THE I/O CONTROLLER BOARD IS FUNCTIONING CORRECTLY (AS

DESCRIBED ELSEWHERE IN THIS MANUAL), BEFORE ADDRESSING ANY CAMERA
ERROR CODES. I/O CONTROLLER BOARD PROBLEMS, ESPECIALLY WITH THE
POWER SUPPLIES TO THE CAMERA CAN CAUSE SPURIOUS CAMERA ERRORS
Camera error 507 DMA There have been isolated cases where instruments turned
timeout off (i.e. powered off) for long periods of time display this error
after being first turned on.
Try restarting the instrument.

Check the I/O board is functioning correctly, as specified
elsewhere in this document, to ensure the power supplies
are not causing spurious camera problems.
Does this solve the problem?

Does this error occur only when the user is running a
particular sample or method?
If YES, please contact Technical Support, through your local

support organisation, describing the steps required to
reproduce the problem and also a copy of the Help -About
Dialog, iTEVA journal, any applicable data (in a new
database) and the firmware log file.
If the error is not related to a user action and the error
persists, change the Camera.
Camera error 509-FPGA There have been isolated cases where instruments turned
Programming error off (i.e. powered off) for long periods of time display this error
Does restarting the instrument clear the error?

Is the I/O board functioning correctly, as specified elsewhere
in this document, to ensure the power supplies are not
causing spurious camera problems?
Try unplugging and re-plugging all connectors.
Change the camera if error persists

Camera error 513- There have been isolated cases where instruments turned
Timeout polling FPGA off (i.e. powered off) for long periods of time display this error
Note: FPGA = Field Does restarting the instrument clear the error?
Programmed Gate Array
Check the IO Board is functioning correctly, as specified

elsewhere in this document, to ensure the power supplies
are not causing spurious camera problems.
Does this fix the problem?

Camera error 517 - Is the connection between the camera and polychromator
Autobias timeout, check flash-up (pre-exposure) LED (inside rear of polychromator)
LED. OK?
Is the LED is correctly inserted into the polychromator?
Is the LED is working correctly?
This can be tested by removing the LED and checking it
flashes using the LED flash command in the manufacturing
software.
NOTE: Removing the LED may cause purge problems,

therefore if you have a spare LED try plugging it in rather
then removing the LED from the tank.
If the LED is not flashing, replace the LED.
Is anything blocking the LED light path to the camera in the

polychromator?
Note: This is VERY unlikely especially if the customer was

previously running samples, etc; however worth checking.
Camera error 33207 - Does the manufacturing software show any problems?
Detector un-initialised
If YES
Record all the steps/actions to reproduce the problem and
contact Cambridge Technical Support providing a copy of the
Journal and version information (using a screenshot of the
Control Centre Help->About screen).
If NO
Try restarting the instrument and iCAP data station software.
There have been isolated cases where instruments turned
off (i.e. powered off) for long periods of time display this error
Is the IO Board functioning correctly, as specified elsewhere

in this document, to ensure the power supplies are not
causing spurious camera problems?
E33211 – The firmware Use the manufacturing software “Instrument Status” page to
recently rebooted due to a determine the reason for the error. Send a copy of the
non recoverable error. Instrument Status page, the firmware error log file, a copy of
The firmware Error log will the help->about dialog and the journal to Technical Support.
download.
Change camera only if instructed by technical support

6.2 RF and I/O Board Problems
Note: see Mk 2 RF Diagnostics section below for Mk2-specific problems.
PROBLEM/SYMPTON POSSIBLE CAUSE
Loss of I/O and/or RF Is the I/O controller board functioning correctly, as specified
communication while elsewhere in this document? I/O Controller board problems
instrument is idle. may cause spurious communications errors.
If YES
Use the manufacturing software to determine whether the
RF doesn’t spark after problem is with I/O Controller or RF power supply
several attempts communications. The following screen clearly shows an I/O
Communications problem.
Does the manufacturing software indicate an I/O

communications problem?
If YES
Then the problem is likely with the I/O Controller board.
Check the connections between the I/O Controller Board and
the camera.
If the connections are all ok,
Replace the I/O Controller board.
Does the manufacturing software indicate an RF

communications problem?
If YES
Then there could be a problem with either the RF power
supply or the I/O Controller board.
Are the connections between the RF Power Supply to I/O
Controller Board and I/O Controller board to Camera OK?
If YES
Note: The cause of the problem needs to be determined, as
it can be either the I/O Controller board or the RF Power
Supply
I/O communications error NOTE: If this error is displayed the communications between
displayed on start-up. the PC and the instrument are functioning correctly, therefore
the camera should not be changed!
E33212 - An I/O board
communications error has Does the RF spark during ignition attempt?
occurred. Ensure the Do nothing.
controller board is
powered and connected Note: Any generators with RF Power Supply software before
correctly, if the condition version 23 can exhibit this problem. To eradicate the
persists please contact problem, please change the RF power supply to a newer unit
customer support. with version 23 or greater of software.
Is the following error displayed on or before instrument
initialisation?
If YES
Go into the manufacturing software “Instrument status”
dialog and confirm the firmware has timed-out while waiting

for the I/O Controller and/or RF power supply to
communicate as shown
Are the connections between the RF Power Supply to I/O

Controller Board and I/O Controller board to Camera OK and
does the manufacturing software indicate whether the I/O
controller or RF communications are bad?
If YES
And if only the I/O Comms OK is bad, or both the I/O and
RF Comms OK are bad,
change the I/O control board.
If the RF Comms are bad and the IO Comms OK is

good:
change the RF power supply
E33213 Try lighting plasma. Does plasma light?
RF gets into a If YES

communication loop Turn the instrument off and on. Does this get it out of the
loop?
RF is too hot If NO
Is Chiller working correctly (temperature and pressure)?
7 RF Ignition Problems
Note: see Mk 2 RF Diagnostics section below for Mk2-specific problems.
Have there been interlock errors in the iTEVA Journal

history?
If YES
Investigate the interlock(s) indicated
The Plasma will not ignite, Is the Torch fitted correctly or damaged?
or ignites and goes out
before the end of the If NO:
instrument optimisation. Check correct parts have been used (correct size centre tube
for example)
NOTE: This is intended as Check for argon leaks from the torch to the argon gas
a guide only and is not a cylinder or liquid tank. An argon leak will result in
substitute for common entrainment of air.
sense. Is there poor quality argon?

If YES try a different batch.
You should ensure no Is the RF power supply producing RF? (check with the RF
other errors are displayed test indicator.)
before attempting to solve Is the Exhaust between 4.5 and 5.5ms-1 for a radial
ignition problems. instrument and 8.5 to 11 for a Duo?
If NO adjust the flow.
If you are getting other Note: measure this at the centre of the end of the 5inch
instrument errors before extraction tube using an anemometer.
ignition, this may be Is the igniter wire touching the body of the torch?
affecting ignition. If NO then adjust ignitor cable position.
Note: it maybe necessary to trim back the insulation at the

end of the cable to provide clean metal
Is the Argon pressure 6 bar (87psi)?
Does it remain at 6 bar during ignition?
If No adjust the pressure.
Is the RF power supply getting too hot?
If YES check the chiller is working correctly and the cooling
fluid does not have particles or crystals in it.
It may be necessary to flush out the whole system if the
cooling water is found to be contaminated.
Is there insufficient torch coolant gas to the torch?
If YES this maybe due to poor seal between o-rings on torch
body holder and torch box gas inlets, if so replace O-rings.
Does the torch base fit into the torchbox casting?
Does the Torch fit into the base correctly?
If not, replace the part.
Is the fibre optic in good condition?

If the plasma comes on and then goes off after about 0.5
seconds, the optical fibre may be defective.
If NO, replace the fibre optic cable, or trim the end to ensure
a good view of the plasma
DO NOT EXCHANGE AN RF GENERATOR UNLESS THE

CHECKS ABOVE HAVE BEEN COMPLETED
7.1 RF Test Indicator

 To Check if RF is present
at the Coil remove torch
from holder and fit injector
tube along with metal nut
as shown in diagram
opposite and secure with a
piece of tubing to hold the
nut in place.
Note: this will only work if all

other interlocks are OK

 Place assembly so that nut is

approximately 2 mm from coil as
shown opposite
 Run ignition sequence and
after it has finished remove torch
assembly and check to see if the
nut is hot which indicates RF is
present
 CAUTION: Nut may be
hot to the touch and may
cause severe burns if
mishandled.
8 Ignition Problems Hints and Tips

If the plasma always lights the second time then that may be inherent to the instrument
and not indicate a hardware problem.
8.1.1 Check for Argon/Air leaks around Torch & Spray Chamber
Air leaking into the torch is the primary cause of problems in the RF system. Air will
dilute or contaminate the argon in the torch and will prevent ignition. If the leak is small
enough, the torch may light but will then go out.
Note: such leaks could be anywhere in the system including the main regulator fitting.
 A typical symptom would be that the torch lights and goes out a few seconds
afterwards. This would be because prior to ignition, the nebuliser pressure is shut
off. This causes the torch to be exposed to argon coming only from the primary and
auxiliary gas lines.
 If the Plasma goes out within 0 to 0.5 seconds of striking, it is probably caused by
an interruption occurring within the system, or that the optical fibre is defective.
 Once the torch is lit and established,

the nebuliser turns ON. If there is a
problem in the spray chamber such
as a leak, excess air is immediately
"blown" up into the torch and
generally puts it out. A temporary way
to get the torch lit under these
conditions is to remove the spray
chamber from the ball and socket joint
and cover with tape. The primary
locations for air leaks are at the o-
rings, around the torch, centre tube,
end cap, drain etc. Other o-rings
should be simply inspected for flat
spots, swelling or shrinkage, nicks
and cuts etc.
 Contaminated Argon gas could also

cause poor ignition

8.1.2 Check and Clean Fibre

Optic Cable
 The fibre optic cable in the torch
compartment monitors the light from
the torch. If the torch light is not seen,
the instrument assumes that the torch
went out or never lit. If the torch
appears to be lighting but goes out
within 0.5 to 1 second of striking, it
could mean that the fibre optic is dirty
and may require replacement.
Fibre Optic Cable (MK1 RF only)
8.2 Cleaning the Plasma Torch

 Remove the quartz torch from its metal holder.
 To remove salt deposits, wash the torch for a few minutes using soapy water. To
remove metallic deposits from the tip, remove the torch from the holder; immerse
the tip of the torch into hot acid, either hydrochloric acid (HCl), nitric acid (HNO3) or
a mixture of the two acids.
 After cleaning, rinse the torch copiously with de-ionised water and place in a drying
oven at 95°C until it is dry. Sometimes rinsing the torch with methanol and blowing it
dry with compressed air reduces the drying time.
 To clean the torch of carbon deposits, place the torch in a muffle furnace and heat
to 400-500ºC. Open the door to admit air for a few seconds, then close the door and
allow the temperature to return to 400-500ºC. Repeat two or three times until the
carbon is burned off. Switch off the muffle furnace and allow it to cool down without
opening the door This will take several hours
 The furnace will cool sufficiently slowly to prevent stress in the quartz. It is
recommended that at least 2 torches be rotated, so that you do not have to stop
work while waiting for the torch to be cleaned.
8.3 Cooling Water for the RF

Load
 Contaminated RF load coil cooling
water can cause difficulty with plasma
ignition by acting like a shorted turn
across the coil.
 Check the instrument’s external water
re-circulator system.
 Use anti-corrosion agent as detailed
in the installation section

 Check all areas around the torch and

spray chamber where a leak could
exist. There are two o-rings in the
spray chamber: (for nebuliser), two for
the torch (Auxiliary and coolant flows),
one on the top of the sample injector
mount and two on the bottom were
the spray chamber inserts and three
inside the torch holder. Inspect each
for flexibility, cuts, abrasions or flat
spots.
(Pictures show tulip and parallel

torch holders)
8.4 Check or Replace Argon Supply

 Bad or contaminated argon is sometimes a difficult and aggravating problem to
solve. Quite often it is mistaken for an RF problem, which leads to disassembly and
numerous parts replacement. The argon pressure supplied to the instrument should
be 6 bar (87 psi)
 Argon will come in two forms: compressed and liquid. The compressed form will
generally have oxygen as a contaminant. The liquid form will generally have
nitrogen as a contaminant. The symptom for bad argon is that the torch will not
light. There could be sparking or sputtering in the torch compartment.
 The best way to test for problems in argon supply is to try and different batch or
supply of argon.
 Sometimes a supplier fills bottles with the wrong gas. If this is suspect be sure to
use a supply of argon from a totally different batch or supplier
8.4.1 Igniter Position
Radial Torch (just touching the torch) Dual Torch (just touching the torch)
The insulation surrounding the ignitor wire may need to be cut back by 5 to 10 mm to
ensure that the wire is touching the glass of the torch.

9 Mk2 RF Diagnostics
The big difference between diagnostics for a Mk1 and a Mk2 RF is that with a Mk 2 it is
necessary to diagnose which module is causing a problem and not just change the
whole unit as with a Mk1 RF.
The section below explains how to diagnose faults with Mk2 RF modules. The figure of
the Mk 2 RF Generator below indicates the different modules within it.
9.1 Error messages

Two general categories:
 Failure to ignite
 Failure when plasma is on
If the plasma goes out and the user sees any error messages, always try to re-light the
plasma. More error checks are done during ignition so a more useful error message may
be generated.
Note: iTEVA can crash if an interlock or other failure occurs during spectrometer
optimisation. You will need to re-start iTEVA to overcome this.
#2209: Plasma ignition failed; low ignition current. If the condition persists please contact
customer support with this error code.
#2206: Plasma ignition failed; RF interface board reported over-current failure. If the
condition persists please contact customer support with this error code.

 If this happens every time you try to light the plasma, suspect the RF Board
 Customer visit required with spare RF board. If all LEDs and Service software
status indicators look good change the board.
#2200: Plasma ignition failed; 3kW DC

power supply reported bad AC input. If the
condition persists please contact customer
support with this error code.
#9007: Plasma went out unexpectedly; RF

3kW DC power supply reported bad AC
input. If the condition persists please
contact customer support with this error
code.
#2202: Plasma ignition failed; 3kW DC

power supply output is bad. If the condition
persists please contact customer support
with this error code.
 Re-start the instrument and see if

it successfully initialises
 Check Service software status
indicators
 For DC output problems, change 3
kW power supply.
 For AC input problems, check
mains input is reaching the 3 kW
power supply. If mains is OK,
change 3 kW DC Power supply
#9000: Plasma ignition failed; reason unknown…
#2208: Plasma ignition failed; RF seems OK. Check your sample introduction system as
described in iTEVA Help. If the condition persists please contact customer support with
this error code.
 These messages are similar. To get this far the software has already checked
RF board and 3 kW power supply status so these should be OK.
 Customer can check sample introduction for leaks.
 Engineer can remove sample intro to check. (as shown in picture to the right)

9.2 Ignitor module failure

 Check lead plugged in to board and connector in ignitor.
 If you forget to connect it you will get error ‘E2209 Ignition Failed, RF Seems
OK, check sample introduction’. The second LED on the interface PCB will flash
for a second, and ‘Ignition power’ in the Service software will go red. You will not
hear the noise of the ignitor clicking.
9.3 LEDs
9.3.1 Control board LEDs

 With a Mk2 RF fitted, LED 1 now
flashes to indicate communication
with the RF generator.
(Will flash when bottom LED flashes on the
RF interface PCB.
9.3.2 RF interface PCB board

LEDs
 With a Mk2 RF fitted, LED 1 now
flashes to indicate communication
with the RF generator.

9.3.3 Manufacturing software

 The manufacturing and service software provides useful diagnostic information.
 For the Mk2 RF in particular use the Instrument Status tab in the diagnostics
window.
 For further explanation of using the manufacturing and service software look at
the Help topics in the software, as shown below.


10 Analytical Problems Hints and Tips
10.1 Poor Precision and Analytical Drift

 Before jumping to any conclusions, a quick test should be run to
determine if the poor analytical results are matrix related.
 iCAP test solution should be used.
 After standardisation, the standard should read back, on the iCAP
for example, with a precision of typically 0.2 to 0.5 percent (with a
10 second integration time). If the precision obtained is
substantially greater than this try torch alignment then go on to
trouble-shoot further if the problem remains.
 If the instrument meets these specifications then the sample matrix
itself may be the cause of the problem.
Poor precision generally relates to

problems in the sample
introduction system.
10.1.1 Gas pressures

 First check to ensure that the
nebuliser pressure or flow is set
correctly by aspirating a
1000ppm Yttrium solution
(Sodium will also work if no
Yttrium is available).
 Check to ensure that the centre
orange "bullet" is even with or
slightly above the top of the
Radial torch. If not, adjust the
nebuliser pressure up or down
until the "bullet" looks correct.
 At this point the pressure
should be approximately 0.15
MPa for aqueous solutions. If
the pressure is substantially
higher, the nebuliser orifice is
generally to blame and should
be cleaned. For the new k-type
nebulisers the pressures
should be 0.22MPa and
0.26MPa for Duo and Radial
respectively.

10.1.2 Spray chambers

 Pooling and dripping in the
spray chamber can also cause
many precision problems. You
may be able to see this visually
using the Y test described
above.
 If the Yttrium "bullet" is
bouncing up and down inside
the plasma, it is usually
indicative of dripping. In a glass
or Teflon chamber the chamber
should be wetted properly; that
is there should be no water
droplets building up on the
walls of the spray chamber.
 This is usually caused by an
oily film and can be easily
cured by soaking the spray
chamber in a mild detergent
solution.
10.1.3 Nebulisers and centre

tubes
 Other causes of poor precision
can be in the expendable parts
such as nebuliser and
torch/centre tube. Spares
should always be available and
these should be substituted
one by one to observe the
result. If the nebuliser is the
culprit, check the inside of the
orifice, by removing the gas
fitting, then with a magnifying
glass look for any small
obstruction. Also check the
capillary for obstructions.

 Less prone to clogging are the

high solids nebuliser designs,
such as the Babington or V-
Groove but orientation is critical
as the sample is gravity fed
across the argon orifice for
atomisation.
10.1.4 Teflon Capillary Tubing
Tubing should be free of kinks and

pinched ends, caused by scissors
for example. For best results, cut
at 45° with a sharp blade. Also
check the sample peristaltic pump
winding condition and platen
pressure for proper adjustment.
Replace the winding if it is used or
collapsed. Pump windings typically
last only a couple of days.
Introduce an air bubble into the
sample uptake tube and watch its
migration through the tubing, it
should be smooth and consistent.
Worn rollers, bent pump head shaft

or bad roller bearings can cause
inconsistent pump action and any
such damaged pumps should be
replaced.
10.1.4.1 Peristaltic Sample Pump

Note: When using a concentric, or free aspirating type nebuliser, the
pump platen pressure should be adjusted with the plasma torch ignited
and the pump stopped.
 To adjust the Platen Pressure

 Dip the uptake capillary (which
is normally connected to a
sipper probe) into deionised
water.
 With the nebuliser gas switched
on, and the pump switched off,
gradually increase the platen
pressure until the water just
stops aspirating through the
pump tubing, then add ½ turn
more pressure. You can briefly
remove the capillary or sipper

probe from the rinse for a short
period to introduce a small air
bubble to help show the flow.
 With pump turned on adjust the
drain pressure to allow small
bubbles to flow in the drain
tube.
 Finally, argon/air leaks can

cause many problems including
poor precision.
 Check the gas fittings on the
lines coming from the bulkhead
to the torch and nebuliser with
a suitable soapy liquid. Leaks
at these joints are usually
caused by rough tubing and
can be stopped by cutting off
about 20mm of tubing and
reinserting. Replace the tubing
with 6mm Teflon if the tubing
becomes too short.

10.1.4.2 Drift
 Check for analytical drift problems in the same way as for analytical
precision checks in an earlier section.
 Check for drafts from doorways, air conditioning and windows.
 Ensure that the laboratory is at a constant temperature and air
conditioning/heating is steady 24 hours a days, seven days a week.
 Check the optical tank heater is working – should be 38 °C
Note: High sample volatility can be confused with instrument drift.
10.2 Poor Accuracy/Feedback

First we should define accuracy as reproducing the standard value once
the instrument is standardised.
Proceed by making a standard as in the previous section (10ppm Cu, Mn,
Cd, Zn, Fe) and using this as the test solution. Remember we are not
defining accuracy for this test as the ability to read a 1 or 100ppm
standard after standardising on the 10ppm. Most of the time that problem
is operator-related. As far as we are concerned at this point we have only
one standard to test with. If this simple standard will not repeat back for
all elements, check the pump winding first. Replace it if it is used or
collapsed.
Note: Pump windings typically last only a couple of days.
 Check the method to see if a fast pump rate is used for the flush
period. If it is, then make the flush pump rate the same as the
analysis rate and try it again. Inaccuracy can sometimes be traced to
the inability of the pump tubing to recover its shape after being
stretched.
 Check the flush time for adequate rinse time. A 30-second rinse time
is adequate in most cases but not if a slow pump rate is being used or
if a very long piece of tubing is used (as with the autosampler probe).
11 Poor Detection Limits

 This problem can be also
related to the poor precision
problem discussed earlier and
is usually solved by
approaching it as such.
However, if the loss of
intensities is especially
pronounced at lower
wavelengths it may be due to
bad purge or a dirty window
mounted in the purged optical
path. UV burn or a dirty mirror
is characterised by a long term
decline (six months or longer)
of intensities.
 Contaminated blank can also
cause poor detection limits.
12 Suggested Maintenance in the Case of Poor Precision

and Detection Limits
12.1 Introduction
Maintenance refers to a series of periodic activities that should be performed on a
periodic basis to optimise the short term and long term performance of the system. In
this chapter we describe activities that should be performed by the typical user of the
instrument.
12.2 Typical Maintenance Schedule

 Replace Pump Tubing Weekly
 Clean the Nebuliser Weekly
 Clean the Plasma Torch Monthly
12.3 Replacing Pump Windings
Type Solvent Types
Aqueous solutions, strong acids

Tygon and highly polar organic solvents
(e.g. methanol and ethanol)
Solvents of low polarity (e.g.
Viton alkanes, aromatics and
halogenated hydrocarbons such as
gasoline, kerosene, Toluene,
xylene, chloroform and carbon
tetrachloride).
 Pump tubing in poor condition is characterised by either being
flattened hard or discoloured. Squashed tubing is usually caused by
overuse or leaving the platen pressure on the tubing when it is not
being used
 To minimise squashing of the tubing, release platen pressure when
the pump is not being used, even for short periods. Hardened and
discoloured tubing can be caused by chemical reactions with the
sample. While these phenomena cannot be avoided, they can be
minimised by frequently flushing it with deionised water.

12.4 Preventing Blocking of

the nebuliser
 The most common problem
with the nebuliser is the
blockage of the tip by the
deposition of particulate matter.
In this section we provide a
series of suggestions to
minimise blockage.
 In most instances blockage in
the nebuliser is caused by
either particulate matter (from
the sample) or chemical
deposits. It normally occurs in
the nozzle where the flow
passages are extremely small
and constriction is greatest in
the annular gas channel
between the tip of the capillary
and the taper of the nozzle.
o Tip: Filter the sample. The sample capillary is more tolerant of
particulate matter than the gas annulus. For high sample uptake
nebulisers, the capillary will frequently transport visibly turbid
suspensions. We suggest that you filter or centrifuge the sample if
the solids are not of analytical importance. Particulates and
colloids of a polar nature such as silica, peptides, polyvalent metal
hydroxides and others tend to build up on the (polar) glass and
impede the fluid flow. In some instances you can prevent
deposition by adjusting the pH of the suspension away from its
isoelectric point.

o Tip: Rinse the nebuliser. It is very important to rinse the nebuliser

at the end of the method. It is advisable to rinse the nebuliser
periodically throughout the sequence (depending on the chemistry
of your samples).
o Solids may be deposited in the nozzle as sample solvent
evaporates, further constricting the flow passages and reducing
the signal. Rinsing will minimise or eliminate these deposits.
o After the testing of any salt solution, promptly rinse the system with
a chemically compatible rinse consisting only of volatiles.
o A low-pH (acidic) sample should be followed by a low-pH rinse, a
high-pH sample by a high-pH rinse and an organic sample by an
appropriate solvent. The final rinse should use deionised water
and/or isopropyl alcohol.
o
Note: Allow the nebuliser to dry before turning off the gas and make
sure that the liquid feed is disconnected or arranged so that siphoning
into the nebuliser while the gas is off cannot occur.
DO NOT use ultrasonic cleaning to remove particulate matter as

sympathetic vibrations may be set up in the capillary causing it to
bounce against the inside of the nozzle and chip. This can cause
fatal failure of the nebuliser.

12.5 Removing the Concentric Glass nebuliser

 Remove the sample capillary by pulling the small white Teflon stopper
that attaches it to the back of the nebuliser.
 Remove the nebuliser carefully out of the spray chamber using a
rotation motion at the same time as pulling it out.
12.6 Removing Solids from the Nebuliser

 If solids inside the nebuliser are interfering with performance of the
system, the steps described below will generally remove them and
provide normal operation.
12.6.1 To Rinse the Nebuliser

 Introduce a rinsing agent into the shell, either from the gas input or
the nozzle (a squeeze bottle works well in both cases). Fill all areas
previously exposed to solutions.
 Attach pressurised gas to the side-arm to expel the liquid.
 Inject more rinse solution into the liquid input while the gas is flowing
and allow venture suction to draw it through the capillary.
 The final rinse should use isopropyl alcohol to speed the drying
process.
 Repeat the treatment if you think it is necessary.
 After the rinse is complete, dry the nebuliser completely.
12.6.2 Particles
These operations are ranked in order of increasing aggressiveness. We
recommend that you start with the gentlest procedure and continue with
more aggressive procedures as required.
 Tap the liquid input line of the nebuliser gently against a wooden
surface (or a surface of comparable hardness) to shake the particle
loose. This helps the particle to move in the direction of increasing
inner diameter. Repeat the tapping as necessary to work the particle
toward the appropriate exit orifice. Avoid extremely harsh tapping.
 Apply compressed gas (15-30psi) to the nozzle, forcing the gas
backwards through the annulus and the capillary (back flushing).
Note: Make sure you hold the nebuliser securely during this operation.

 Force isopropyl alcohol backwards through the nozzle in an attempt

to float the particle out through the larger gas and liquid input tubes.
Use a squeeze bottle or plastic dropper with a tip that will form a good
seal over the nebuliser nozzle. After the particle has been removed,
remove the alcohol through the input tubes using compressed gas, or
drain onto lint-free tissue. A variation of this procedure involves the
use of a solvent that is known to dissolve the particle (this variation
works best if you know which passage the particle is in and your
nebuliser is a type C or K with a recessed capillary. In this procedure,
inject a slug of 6mm to 12mm of solvent into the shell through the
nozzle or the gas input tube and close off the nozzle with a fingertip.
Apply pressurised gas to the passage that does not contain the
particle. Pressurised solvent will force its way out the other channel in
the direction of increasing diameter, hopefully carrying the particle
along with it).
 If the particle still remains and you believe that it might be a shred of
PTFE tape from the gas line, immerse the nebuliser nozzle in hot
water and apply gentle gas pressure to the side arm. The hot water
"relaxes" the polymer and allows it to be forced out of the nozzle.
12.6.3 Solid Deposit in Sample Capillary

Note: This step assumes that a passage still exists through the
contaminating material (i.e. the tip is not entirely clogged).
 Try to deduce the chemical nature of the deposit from the type of
samples that are being analysed and select the solvent most likely to
dissolve it. Inject the solvent into the nozzle with a plastic dropper or
squeeze bottle until the affected area is filled. Expel the solvent with
compressed gas. Refill and expel the solvent repeatedly. Examine the
nebuliser under magnification. If the material is gone, rinse the
nebuliser with isopropyl alcohol and dry thoroughly.
 Immerse the nozzle in a rinse solution. Warm the solution for
stubborn deposits. Follow with a rinse of pure solvent, then isopropyl
alcohol and dry thoroughly.
 If the deposit remains after prolonged soaking, apply pressurised gas
at the appropriate input(s) to help force the deposit away.
12.6.4 Organic Matter

 Immerse the nozzle of your nebuliser in a hot cleaning solution of
chromic and sulphuric acids at 100ºC.
Caution: This solution is corrosive, use suitable precautions
 Allow the solution to rinse into the passages of the nebuliser until the
affected area is filled. Expel and replace the solution at intervals until
the deposit is gone or until the chromium reduction (green colour)
ceases. Rinse the nebuliser thoroughly with water, then with isopropyl
alcohol and dry completely.

12.6.5 Plugged Capillary (fusible solids e.g. waxes)

Note: This procedure should be used when no passage remains through
the deposit.
 Carefully heat the nebuliser in the region of the capillary obstruction.
Simultaneously (or intermittently) apply gentle gas pressure at the
sample input tube.
Caution: Avoid overheating residues that may produce insoluble
pyrolysis products
 Stop treatment when you have opened a passage through the
blockage.

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iCAP 6000 Series ICP-OES Spectrometer

Page 2 of 34 Version 5.2

1.1 iTEVA Journal

1.2 iTEVA Database

In addition to the journal, it is sometimes necessary to send an iTEVA database to Technical

Page 3 of 34 Version 5.2

2.2 Carbon Position check for iCAP 6300 and 6500

Using iTEVA Analyst, take a Low Wavelength full frame image.

Before any alignment record the carbon line centre position

Page 4 of 34 Version 5.2

2.3 Carbon Position check for iCAP 6200

Before any alignment record the carbon line centre position

Turn water recirculator

Yes See I/O problems

No See iCAP ignition

See ignition sequence

Page 6 of 34 Version 5.2

iCAP Ignition Sequence

Page 7 of 34 Version 5.2

Set flush pump speed

Apply flush pump delay

Set slit view (move fore-optic

Set analytical pump speed

Set gas flows

Wait for source and pump to

Run the exposure Open shutter

Are there more repeats to be run

Page 8 of 34 Version 5.2

4 Fault Finding Section

4.1 LEDs on side of instrument

* LED 1 will be on permanently on instruments with a Mk1 RF generator fitted.

Check voltages using a digital volt meter.

4.2 I/O Board Fuses

Replacement fuses can be purchased locally or are available as spare parts:

Page 9 of 34 Version 5.2

5 Instrument Communication Problems

PROBLEM/SYMPTON THINGS TO CHECK

(The command prompt can be found via

the instrument may or

The instrument Try unplugging and re-plugging all connectors.

Only when it has been confirmed IO Controller board is functioning correctly,

Page 11 of 34 Version 5.2

6 Instrument Error Codes and Definitions

6.1 CID Camera

PROBLEM/SYMPTON POSSIBLE CAUSE

MAKE SURE THE I/O CONTROLLER BOARD IS FUNCTIONING CORRECTLY (AS

Try restarting the instrument.

Does this solve the problem?

If YES, please contact Technical Support, through your local

Does restarting the instrument clear the error?

Try unplugging and re-plugging all connectors.

Change the camera if error persists

Check the IO Board is functioning correctly, as specified

Change the camera if error persists

NOTE: Removing the LED may cause purge problems,

If the LED is not flashing, replace the LED.

Is anything blocking the LED light path to the camera in the

Note: This is VERY unlikely especially if the customer was

Is the IO Board functioning correctly, as specified elsewhere

Page 13 of 34 Version 5.2