Thermo Scientific iCAP 6000 Series User manual

iCAP Customer Training Manual
iCAP 6000 Series ICP-OES Spectrometer
Customer Training and Maintenance Manual
Version 1 - March 2009
© © 2009Thermo Electron Corporation Registration No. 441506
Stafford House, Boundary Way, Hemel Hempstead, HP2 7GE
United Kingdom. Telephone [phone] , http://www.thermo.com

iCAP Customer Training Manual
Contents
1Introduction........................................................................................................................3
1.1 Check Led indicators ....................................................................................................3
1.2 Preparing the System for Use.......................................................................................4
1.3 Instrument Shut-down...................................................................................................4
2Sample Introduction Glassware Assembly........................................................................5
2.1 Torch Assembly ............................................................................................................5
Spray Chamber assembly ....................................................................................................10
2.2 Final assembly ............................................................................................................11
2.3 Attaching sample and drain tubing .............................................................................13
3Autosampler Use.............................................................................................................15
3.1 Introduction .................................................................................................................15
3.2 Autosampler Installation..............................................................................................15
3.3 Autosampler Set-up ....................................................................................................15
4iTEVA Familiarisation......................................................................................................16
4.1 Introduction .................................................................................................................16
4.2 Method Optimisation ...................................................................................................16
4.3 Example Standard Operating Procedures ..................................................................16
5Maintenance....................................................................................................................28
5.1 Introduction .................................................................................................................28
5.2 User Maintenance.......................................................................................................28
5.3 Purged Optical Path Window Cleaning.......................................................................29
5.4 Preventative Maintenance ..........................................................................................29
6Analytical Problems Hints and Tips.................................................................................30
6.1 Poor Precision.............................................................................................................30
6.2 Poor accuracy/feedback .............................................................................................34
7Poor detection limits ........................................................................................................34
8Suggested maintenance in the case of poor precision and detection limits ...................35
8.1 Introduction .................................................................................................................35
8.2 Typical Maintenance Schedule ...................................................................................35
8.3 Replacing pump windings ...........................................................................................35
8.4 Preventing blocking of the nebuliser...........................................................................36
8.5 Removing the concentric glass nebuliser ...................................................................38
8.6 Removing solids from the nebuliser............................................................................38
8.7 Cleaning the glass mixing chamber............................................................................40
9Notes ...............................................................................................................................41

iCAP Customer Training Manual
1 Introduction
The iCAP 6000 is designed to be constantly powered up and the optical system
continuously purged.
The instrument is powered via an on/off switch at the rear of the left side.
Figure 1 – iCAP 6000 Power On/Off
1.1 Check Led indicators
On the rear right hand side of instrument there are row of Led’s which indicate, when
power on and the status of the instrument.
Once the chiller has been turned on and reached it set temperature led’s 1-7 should be
on and led 8 should be flashing
Led 9 is for engineer fast purge for gas to optical tank and should only be on if fast purge
is required and turned off when analysing samples.

iCAP Customer Training Manual
1.2 Preparing the System for Use
If the gas supplies have been switched off, the optical components should be
purged for at least one hour before powering the instrument.
If the instrument is switched off, allow at least two hours after restoring power to
thermally stabilise the instrument before the chiller is turned on.
A blank sample should be aspirated for ten minutes to allow the instrument to fully
stabilise before analysis.
1.3 Instrument Shut-down
After an analysis is finished a blank sample should be aspirated for five minutes to insure
the sample introduction part have been rinsed of sample. To remove the blank sample
deionised or distilled water should be aspirated for a further minute.
When organic solvent based samples are being analysed the final rinse should be the
pure solvent. Air should be aspirated for two minutes to remove organic vapours.
After completing the above the plasma should be turned off. The optical components will
move to a parked position after about thirty seconds.
Allow five minutes after switching off the instrument, or accessories, before disconnecting
the electrical power or other supplies.

iCAP Customer Training Manual
2 Sample Introduction Glassware Assembly
Warning: Appropriate care and safety procedures should be followed to
avoid breaking any glassware and causing injury to the operator. Broken
glassware should be handled with appropriate care.
2.1Torch Assembly
Figure 1 Duo Torch Assembly – Metal Torch Mount
Figure 2 Radial Torch Assembly – Metal Torch Mount
Figure 3 Torch Assembly – torch body
The quartz body of the torch should be pushed fully into the metal torch mount.
The O-rings in the metal torch mount (internally and externally) should be inspected and
replaced if any wear, or damage, is visible.
The quartz body of the torch should be pushed into the metal torch mount. Ensure the
torch body is pushed fully into the metal torch mount. The marked symbol on the quartz
torch is used to locate the radial view hole correctly and should touch the metal body.

iCAP Customer Training Manual
Correct Incorrect
Figure 4 Torch Assembly – torch body
Figure 5 Torch Assembly – centre tube
Insert the centre tube (ground glass joint) fully into the centre tube holder.
Figure 6 Torch Assembly – centre tube insertion
Insert the centre tube assembly into the metal holder.

iCAP Customer Training Manual
Figure 7 Torch Assembly – centre tube insertion
Screw the centre tube assembly into the metal holder.
Figure 8 Torch Assembly –spray chamber adaptor
Insert the spray chamber adaptor (ground glass joint) into the rear of the centre tube
holder

iCAP Customer Training Manual
Figure 9 Torch assembly holder
Make sure metal holder is turned and locked in position.

iCAP Customer Training Manual
Figure 10 – Torch Holder
Push the torch assembly up into the holder and twist to lock.

iCAP Customer Training Manual
Spray Chamber assembly
Start by connecting the drain tubing as figured below
Figure 11 – Spray chamber drain
Insert drain tube connector until it meets the main chamber.
Figure 12 – Nebuliser to Spray Chamber
The O-rings in the spray chamber should be inspected and replaced if any wear, or
damage, is visible. Push the Teflon insert with the attached sample tubing (supplied with
the nebuliser) into the rear of the nebuliser as far as possible without exerting undue
pressure.
Using a twisting motion insert the nebuliser into the spray chamber so that the collar is a
tight fit. The collar will set the insertion depth and aid reproducibility of results.

iCAP Customer Training Manual
2.2 Final assembly
Duo Spray chamber
Figure 13 – Duo Spray chamber assembly
Attach the swan neck fitting to the Spray chamber with the fitting clamp provided. The
swan neck provided with the instrument is specially designed to prevent UV radiation from
escaping from the torch box.
Figure 14 – Duo Spray Chamber fitted
Insert swan neck fitting into torch assembly holder as far as it will go, and connect
up the Nebuliser gas supply to the push-fit fitting.
Warning: It is extremely important that the correct Thermo part is used for the
swan neck. In addition, systems interlocks on the torch holder and elsewhere are
there for safety reasons and must not be bypassed. Operators could be exposed to
dangerous UV and radio frequency radiation if alternate parts are used for the
swan neck.

iCAP Customer Training Manual
For Radial
Connect spray chamber and nebuliser assembly to the torch assembly as figure below
Figure 15 – Radial Sample Introduction setup
The torch compartment door must be closed before use.

iCAP Customer Training Manual
After assembly of the sample introduction system and prior to ignition of the plasma a
check should be made for correct assembly :-
Make sure the torch is fully rotated and locked in place.
Make sure the centre tube holder is fully rotated and locked into the torch.
Make sure the spray chamber connector is fully pushed into the torch body.
Make sure the spray chamber is tightly connected to ball the joint.
Problems in any of these areas may cause air leaks or disruption of the gas flows making
the plasma difficult to ignite and may cause damage to the torch.
2.3 Attaching sample and drain tubing
Figure 13 – Sample Capillary Tubing
Feed the sample capillary tubing from the rear of the nebuliser through the upper holder in
the cover and towards the pump.
Ensure there are no twists or bends in the nebuliser and drain PTFE tubing that may
prevent flow of the sample. Insert the sample and drain PTFE tubing into their respective
Tygon pump tubing, making sure that the drain tubing is threaded through the lower hole in
the case (see Figure 14 below) for the drain sensor to work correctly.
Please note: the drain tubing should be connected correctly to account for the counter-
clockwise flow.
Figure 14 – Sample Capillary Tubing

iCAP Customer Training Manual
Pass the drain capillary tubing through the lower holder in the cover and towards the pump.
This holder contains a sensor detecting bubbles produced when the spray chamber is
draining normally.
The plasma and the pump will be switched off after 2 minutes if no bubbles are
detected.
Figure 15 – Pump Tubing
Release the pump tubing clamps and locate the sample and drain pump tubing over the
pump rollers, locking the lugs on the pump tubing into the left and right clamps.
Connect the sample pump tubing to the sample capillary tubing and the drain pump tubing to
the drain capillary tubing; remember to allow for the direction of flow.
Pump tubing should be inspected before each analysis and should be replaced if there are
indications of wear.
Additional lengths of capillary tubing should be used to allow connection to the input of the
sample pump tubing to the sample and the output of the drain pump tubing to a waste
container.
Figure 16 – Pump Tension Adjustment
The pump tension can be adjusted with the plasma running and the pump stopped. Lock the
sample pump tubing and clamp into position. Release the tension adjustment and allow the
nebuliser to free aspirate. Tighten the tension adjustment until the flow just stops then tighten
by one turn. Turn on the pump and, if necessary, tighten the tension until a smooth flow is
produced. Do not over-tighten the pump clamps as it will result in excessive wear and tear of
the pump tubing and require replacement tubing at more frequent intervals.

iCAP Customer Training Manual
3 Autosampler Use
3.1 Introduction
The autosampler can be configured to suit an application, or several applications.
The volume, number and type of sample will all influence the set-up of the autosampler.
3.2 Autosampler Installation
To comply with safety and warranty requirements the iCAP 6000, accessories and associated
equipment must be installed by a Thermo Fisher trained and certified engineer.
3.3 Autosampler Set-up
Figure 37 Autosampler Tubing Set-up
For analysis with an autosampler the capillary tubing attached to the end of the autosampler
probe should be attached to the end of the sample pump tubing on the iCAP 6000. To minimise
the sample volume required the length of the capillary tubing should be minimised, but should
allow free movement over the whole sample area of the autosampler.
.
.

iCAP Customer Training Manual
4 iTEVA Familiarisation
4.1 Introduction
The iCAP 6000 will require optimisation that is dependent on the sample being analysed and the
method requirements.
It is important that the method development verifies the data produced by the method.
It is also important that a suitable quality control regime is established that verifies the continuing
validity of data.
Training courses are available through a local Thermo Fisher Sales Office; contact details are
available on http://www.Thermo.com.
4.2 Method Optimisation
The following parameters can all affect the data obtained and should be optimised. Usually a
default setting will give data that is satisfactory, but may not be optimal for the analysis
requirements:
Nebuliser Gas flow
Plasma viewing height
RF Power
Pump speed
Auxiliary gas flow
Coolant gas
All these instrument parameters are separate to the development of the chemical requirements of
the method, for example variation in sample ionisation and solvent effects.
4.3 Example Standard Operating Procedures
This method setup procedure, which by no means covers all the possible parameters used in
iTEVA, should be enough for setting up a basic Analysis. It is recommended that the user reads
the iCAP software manual and/or Help files for more advanced use of the system.
4.3.1 Preparing the system
Turn Argon Gas on at Cylinder and set for 90psi or 6 Bar pressure on gauge near
instrument
Note: for normal use gas should be left purging constantly
Switch on power to iCAP Spectrometer.
Note: for normal use power should be left on constantly or you must wait until the
optics temperature reaches 38 degrees C and Stabilizes which can take 2 hours.
Switch on Water Chiller
Push Platen on to rollers of pump by way of the 4 (3) pressure screws
Make sure the drain tube is placed in an open neck vessel
Place sample tube in a blank solution
Switch on computer
Click on the iTEVA Icon on desktop

iCAP Customer Training Manual
Type admin in user name field and click on OK or press enter
4.3.2 Striking the Plasma
Click on the Plasma Icon and then make sure the
interlock indicators all show green, click on Plasma
On. After the plasma strikes, wait until the
Spectrometer Optimization is completed and then
click on the close box
Note: To allow the plasma to stabilise leave Plasma
on with blank solution running for about 10 minutes
before carrying out an analysis.
4.3.3 Setting up Analyses
Click on the Analyst icon
Either select one of the stored methods or create a
New method. To create a new method click on
Cancel
Click on the Method drop down
menu
Click on New and select the
Elements required from the Periodic
table.
To select suitable lines from the list
displayed click OK and OK again

iCAP Customer Training Manual
Click on Method tab as shown
Click on Analysis Preferences
Set Parameters as required (see
iTEVA software manual for fuller
explanation of the various
parameters that can be selected)
Note: The parameters shown will be
a good starting point for an Analysis
Click on Automated Output and fill in the relevant
boxes
Note: Make sure you tick save results to database
if you require a record of your results
Click on Source Settings
Note: the source settings will
depend on the particular analysis
that is to be performed but for test
purposes the defaults should give
reasonable results for an aqueous
solution.
Clicking on Standards allow you to edit the
concentration of the standards in the box.
Note: by clicking on Add you can add more
standards if required.

iCAP Customer Training Manual
4.3.4 Running the Analysis
Put the sample uptake tube in the blank solution.
Click on the Analysis tab and then click on the
Calibration Icon, click on Run in the Calibration box
this will then analyze the blank solution
Display of Blank solution results
showing the Elements selected in
the method setup.
Put the sample uptake tube into the High standard
solution
The HighStd is now highlighted so click on Run
Display of High Std results showing
elements selected in the method
setup.
Click on Unknown sample Icon then fill in Run
Unknown box as required Place the sample tube in
unknown and Click on Run

iCAP Customer Training Manual
Display of the Results page
Save the Method if required by clicking on Method
drop down menu and Save As, filling in the
appropriate name.
4.3.5 Shutting down the system
Place the sample tube in Deionised water and let it
pump through the system for 3 to 5 minutes.
Click on the Plasma Icon
and then click on Plasma Off.
Release the tension on the sample pump Platen.
Switch off water circulator.