Thermo Scientific iCAP 6000 Series User manual

iCAP 6000 Series
ICP-OES Spectrometer
User Guide

© September 2009 Thermo Fisher Corporation Registration No. 441506 SOL R House, 19 Mercers Row,
Cambridge, CB5 8BZ, United Kingdom.
Telephone [phone], Fax [phone],
www.thermo.com
849940090011

Thermo Fisher Scientific iCAP User Guide iii
Contents
Introduction to the iCAP 6000 Series...........................................1-5
Overview........................................................................................1-5
User Documentation......................................................................1-6
Pre-Installation Manual...............................................................1-6
Hardware Manual .......................................................................1-6
iTEV Software Manual.............................................................1-6
iTEV Help ...............................................................................1-6
Instrument Set-up ..........................................................................2-7
Pre-Installation Manual...............................................................2-7
Standard Sample Introduction Glassware ssembly .......................2-8
ssembling the Torch .................................................................2-8
Inserting the Torch and Centre Tube into the instrument. .......2-10
Connecting the Spray Chamber and Nebuliser .........................2-11
Connecting up the sample and drain pump tubing ...................2-13
Torch lignment ......................................................................2-15
uto Peak djust ......................................................................2-15
Sample Introduction System Set-up .............................................2-17
Peristaltic Pump Tubing Options..............................................2-17
Internal Standards.....................................................................2-17
pplication-Specific Hardware..................................................2-18
Databases ........................................................................................3-1
Local Database Creation ................................................................3-1
Creating a Database Connection.................................................3-3
Using the iCAP ...............................................................................4-1
Preparing the System for Use .........................................................4-1
Instrument Shut-down...................................................................4-1
nalytical Operation ......................................................................4-2
Method Optimisation ....................................................................4-2
Running the iC P .........................................................................4-2
Sequence of operation .................................................................4-3
How to Run an nalysis.................................................................4-5
Creating a Method......................................................................4-5
Running the nalysis ..................................................................4-6
Spectrometer Optimise ...............................................................4-7
Calibration..................................................................................4-7
nalysing Unknowns ..................................................................4-7
Shutting Down the System ............................................................4-8
Chapter 1
Chapter 2
Chapter 3
Chapter 4

Contents
iv iCAP User Guide Thermo Fisher Scientific
Maintenance ...................................................................................5-1
Instrument Cleaning ...................................................................5-1
Sample Introduction System Cleaning and Decontamination .....5-1
Torch Cleaning...........................................................................5-2
Spray Chamber Cleaning ............................................................5-2
Nebuliser Cleaning......................................................................5-2
Purged Optical Path Window Cleaning ......................................5-3
Preventive Maintenance .................................................................5-3
Water Chiller ..............................................................................5-3
Gas Filters...................................................................................5-3
Safety...............................................................................................6-4
iC P 6000 Safety...........................................................................6-4
Introduction................................................................................6-4
Safety Precautions .......................................................................6-5
Electrical Safety...........................................................................6-6
Equipment Cleaning and Decontamination................................6-6
Impaired Safety Protection..........................................................6-6
WEEE Compliance.....................................................................6-6
Regulatory Notices......................................................................6-6
iC P 6000 Sicherheit.....................................................................6-8
Elnfúhrung..................................................................................6-8
llgemeine richtlinien zur sicheren handhabung des Gerätes.......6-8
Elektrische Sicherheit ..................................................................6-9
Reinigung und Dekontamination der Geräte ..............................6-9
Beeinträchtigung der Sicherheitseintichtungen............................6-9
WEEE Konformität ..................................................................6-10
Übereinstimmung mit Regularien .............................................6-10
Sécurité pour iC P 6000 .............................................................6-11
Introduction..............................................................................6-11
Précautions de Sécurité..............................................................6-11
Sécurité Electrique ....................................................................6-12
Nettoyage et Décontamination de l’Equipement.......................6-12
ltération des Protections de Sécurité........................................6-12
Conformité DEEE ....................................................................6-12
Conformitè Normative..............................................................6-13
EC Declaration of Conformity......................................................7-1
EC Declaration of Conformity.......................................................7-2
SOFTWARE LICENSING AGREEMENT................................7-2
Chapter 5
Chapter 6
Chapter 7

Thermo Fisher Scientific iCAP User Guide 1-5
Chapter 1
Introduction to the iCAP 6000
Series
The iC P 6000 Series is a range of Inductively Coupled rgon Plasma
Optical Emission Spectrometers (ICP-OES) which use an Echelle
optical design and a Charge Injection Device (CID) solid-state detector
to provide elemental analysis.
Most samples are liquids that are pumped through a nebuliser to
produce a fine spray. The large droplets are removed by a spray
chamber and the small droplets then pass through to the plasma. The
solvent is evaporated and the residual sample decomposes to atoms and
ions that become excited and emit characteristic light which is measured
and corresponds to the concentration of each element type in the
original sample.
Control of the spectrometer is provided by PC-based iTEV software.
To avoid loss of analytical performance and compromising safety only
Thermo Scientific specified parts should be used.
The iC P 6000 spectrometer consists of several major components:
plasma torch and sample introduction parts
radio frequency power generator
optical system
CID detector with thermoelectric cooling
Warning: Before operating your iC
Before operating your iCBefore operating your iC
Before operating your iC P ensure you read a
P ensure you read aP ensure you read a
P ensure you read and
nd nd
nd
understand all the safety in
understand all the safety inunderstand all the safety in
understand all the safety information at the end of this manual.
formation at the end of this manual.formation at the end of this manual.
formation at the end of this manual. ▲
Overview

Introduction to the iCAP 6000 Series
User Documentation
1-6 iCAP User Guide Thermo Fisher Scientific
This user guide includes basic information required to get you started
with operating your iC P 6000. More advanced operating instructions
can be found in the Hardware Manual, the Software Manual and
directly from the iTEV software’s built-in Help. In addition, the Pre-
Installation Manual details all the lab requirements for your instrument.
These manuals are described below.
The Pre-Installation Manual provides the details of the services and
environment that must be available before an iC P 6000 can be
installed.
The Hardware Manual details the operation and maintenance of your
instrument hardware. It also includes full information about the safety
hazards involved in working with the spectrometer and its accessories,
and the means by which such hazards can be minimised. This manual is
supplied in dobe PDF format on the Supplementary Information CD
supplied with this User Guide.
Note: ensure you have read and understood all the safety instructions
contained in the Hardware Manual before operating your iC P.
The iTEV Software Manual describes the functions and features of
the Data Station software. This manual is supplied in dobe PDF
format on the Supplementary Information CD.
The iTEV Software has its own active Help system that describes
features and functions of the software. This can be accessed by clicking
on Help T
Help THelp T
Help Topics
opicsopics
opics from the Help
HelpHelp
Help dropdown menu (shown below)
Relevant help topics for particular areas of the software can also be
found by pressing the F1
F1F1
F1 key at any time.
Figure 1–1. Help Topics in iTEVA
User
Documentation
Pre-
Installation
Manual
Hardware Manual
iTEVA Software
Manual
iTEVA Help

Instrument Set-up
User Documentation
Thermo Fisher Scientific iCAP User Guide 2-7
Chapter 2
Instrument Set-up
To comply with safety and warranty requirements, the iC P 6000,
accessories and associated equipment must be installed by a Thermo
Scientific trained and certified engineer.
Specific site requirements are required for the iC P 6000. Please see the
separate Pre-Installation Manual section.
Pre-
Installation
Manual

Instrument Set-up
Standard Sample Introduction Glassware Assembly
2-8 iCAP User Guide Thermo Fisher Scientific
Warning: ppropriate care and safety procedures should be
: ppropriate care and safety procedures should be : ppropriate care and safety procedures should be
: ppropriate care and safety procedures should be
followed to avoid breaking any glassware and causing injury to the
followed to avoid breaking any glassware and causing injury to the followed to avoid breaking any glassware and causing injury to the
followed to avoid breaking any glassware and causing injury to the
operato
operatooperato
operator. Broken glassware should be handled with appropriate
r. Broken glassware should be handled with appropriate r. Broken glassware should be handled with appropriate
r. Broken glassware should be handled with appropriate
care.
care. care.
care. ▲
Figure 2–2. Glassware assembly
The sample introduction systems for an iC P Duo instrument and a
Radial instrument are put together in a similar way. The key differences
are the length of the torch and the spray chamber adapter.
Insert the torch into the torch holder by pushing it gently but firmly.
Note: Ensure that it is fully inserted and orientated in the correct way,
as shown in the figure below.
Figure 2–3. Torch assembly - torch body
Insert the centre tube as far as it will go into the plastic centre tube
holder.
Standard Sample
Introduction
Glassware
Assembly
Assembling the
Torch
Correct Incorrect

Instrument Set-up
Standard Sample Introduction Glassware Assembly
Thermo Fisher Scientific iCAP User Guide 2-9
Figure 2–4. Torch assembly - centre tube
Note:
::
: The tip of the centre tube holder will discolour with use as
shown in the figure above. This discoloration is normal and will not
affect the performance of the torch holder assembly.
Once the centre tube is in the centre tube holder, carefully insert the
centre tube assembly into the metal torch holder. Screw the centre tube
holder assembly in a clockwise direction into the metal torch holder
until the O-ring is compressed. Do not over tighten as this will reduce
the lifetime of the O-ring seal.
Figure 2–5. Insertion of centre tube into torch assembly

Instrument Set-up
Standard Sample Introduction Glassware Assembly
2-10 iCAP User Guide Thermo Fisher Scientific
Insert the torch holder into the torch box and turn the metal torch
holder anticlockwise until the red orientation lock self locates in the
torch box casting. Be sure to make sure you don’t loosen the centre tube
holder whilst doing this.
Figure 2–6. Insertion of the torch assembly into the box
Figure 2–7. Relative coil and torch position on a Duo (left) and a
Radial instrument
Ensure that the torch is centred in the coil, and on a Duo instrument
that the radial view window is positioned close up against the torch.
Inserting the Torch
and Centre Tube
into the
instrument.

Instrument Set-up
Standard Sample Introduction Glassware Assembly
Thermo Fisher Scientific iCAP User Guide 2-11
Insert the white plastic tubing connector with wide bore tubing (0.79
mm internal diameter) into the spray chamber drain tube.
Liquid should be delivered to the nebuliser using an identical plastic
tubing connector but with narrow bore tubing (0.50 mm internal
diameter) relative to the spray chamber drain tubing. Push the white
plastic tubing connector with the attached narrow bore sample tubing
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.
Two white plastic collars come with the nebuliser which can be used to
aid to set a consistent insertion depth and aid reproducibility of results.
To achieve best results the insertion depth of the nebuliser will need to
be optimised by experimentation.
Note: The sample inlet connector has a red
redred
red ring on it and the drain
outlet connector has a black
blackblack
black ring on it.
Figure 2–8. Spray chamber/adapter assembly
ttach the spray chamber adaptor to the spray chamber with the fitting
clamp provided. The adaptor provided with the instrument is specially
designed to prevent UV radiation from escaping from the torch box.
Note: Duo configuration is shown in the above figure. Radial
instrument will be similar except for a straight spray chamber adapter.
Connecting the
Spray Chamber
and Nebuliser
d
rain
out
sample in
nebuliser
gas in
t
o torch
red
black

Instrument Set-up
Standard Sample Introduction Glassware Assembly
2-12 iCAP User Guide Thermo Fisher Scientific
Figure 2–9. Spray chamber fitted to a Duo and a Radial iCAP
Insert spray chamber adaptor fitting into torch assembly as far as it will
go and connect the Nebuliser gas supply to the push-fit fitting on the
nebuliser.
fter 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 torch is fully rotated and locked in place.Make sure the torch is fully rotated and locked in place.
Make sure the torch is fully rotated and locked in place.
Make sure the centre tube holder is fully rotated and
Make sure the centre tube holder is fully rotated and Make sure the centre tube holder is fully rotated and
Make sure the centre tube holder is fully rotated and screwed
screwedscrewed
screwed
into the
into theinto the
into the torch
torchtorch
torch holder
holderholder
holder.
..
.
Make sure the spray chamber adaptor is
Make sure the spray chamber adaptor is Make sure the spray chamber adaptor is
Make sure the spray chamber adaptor is fully pushed into the
fully pushed into the fully pushed into the
fully pushed into the
torch assembly
torch assemblytorch assembly
torch assembly.
..
.
Make sure the spray chamber is tightly clamped to the spray
Make sure the spray chamber is tightly clamped to the spray Make sure the spray chamber is tightly clamped to the spray
Make sure the spray chamber is tightly clamped to the spray
chamber
chamberchamber
chamber adaptor.
adaptor.adaptor.
adaptor.
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.
WARNING: It is extremely important that the correct Thermo
It is extremely important that the correct Thermo It is extremely important that the correct Thermo
It is extremely important that the correct Thermo
Scientific part is used for the spray chamber adaptor. In addition,
Scientific part is used for the spray chamber adaptor. In addition, Scientific part is used for the spray chamber adaptor. In addition,
Scientific part is used for the spray chamber adaptor. In addition,
systems interlocks on the torch holder and elsewhere are there for
systems interlocks on the torch holder and elsewhere are there forsystems interlocks on the torch holder and elsewhere are there for
systems interlocks on the torch holder and elsewhere are there for
safety reasons and must not be bypassed. Operators could be
safety reasons and must not be bypassed. Operators could be safety reasons and must not be bypassed. Operators could be
safety reasons and must not be bypassed. Operators could be
exposed to dangerous UV
exposed to dangerous UV exposed to dangerous UV
exposed to dangerous UV radiation
radiation radiation
radiation and radio frequency radiation
and radio frequency radiation and radio frequency radiation
and radio frequency radiation
if alternate parts are used for the spray chamber adaptor.
if alternate parts are used for the spray chamber adaptor. if alternate parts are used for the spray chamber adaptor.
if alternate parts are used for the spray chamber adaptor. ▲
Duo Instrument
Radial
Instrument

Instrument Set-up
Standard Sample Introduction Glassware Assembly
Thermo Fisher Scientific iCAP User Guide 2-13
Ensure there are no twists or bends in the nebuliser and drain tubing
that may prevent flow of the sample.
Feed the sample capillary tubing from the rear of the nebuliser through
the upper hole, as shown below, and towards the pump.
Figure 2–10. Sample and drain capillary tubing
Pass the drain capillary tubing through the lower hole and towards the
pump. The lower hole contains a drain sensor that detects bubbles
produced when the spray chamber is draining normally. The plasma
and the pump will be switched off after two minutes if no bubbles are
detected.
Insert the sample and drain tubing into their respective peristaltic pump
tubes. Cut the capillary tubing at an angle with a sharp knife and insert
as shown in the figure below.
Figure 2–11. Pump tubing connection
Note: The drain tubing should be connected correctly to the peristaltic
pump to account for the anticlockwise flow. The direction of the
rotation of the pump is shown in the figure below.
Connecting up the
sample and drain
pump tubing
Drain
Sample

Instrument Set-up
Standard Sample Introduction Glassware Assembly
2-14 iCAP User Guide Thermo Fisher Scientific
Figure 2–12. Pump tubing connected. Rotational direction of pump
shown
Release the pump tubing clamps and locate the sample and drain pump
tubing over the pump rollers, hooking the plastic bridges on the pump
tubing into the left and right slots.
Connect both pump tubes to the capillary tubing as outlined above.
Pump tubing should be inspected before each analysis and should be
replaced if there are indications of wear.
Figure 2–13. Pump tension adjustment
With a concentric nebuliser, the pump tension can be adjusted with the
plasma running and the pump stopped. Lock the sample pump tubing

Instrument Set-up
Standard Sample Introduction Glassware Assembly
Thermo Fisher Scientific iCAP User Guide 2-15
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.
Set the drain pump tubing tension to obtain an even and steady flow
out of the spray chamber.
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.
For maximum sensitivity and optimum results the alignment of the
plasma image is critical. Whenever a torch has been removed or
replaced in the instrument, or if the torch body or centre tube have
been replaced, a torch alignment procedure should be carried out.
When the plasma is on and stabilised click on the Instrument
InstrumentInstrument
Instrument menu
and select Torch lignment
Torch lignmentTorch lignment
Torch lignment. The window below will be shown. Select
queous
queousqueous
queous or Organic
OrganicOrganic
Organic according to the matrix you are using and click on
the Run
RunRun
Run button to start the routine. You will be prompted to aspirate a
solution of 2 ppm zinc and this should be made up with either an
aqueous or an organic matrix as required.
Figure 2–14. Torch alignment window
For optimum performance it is important that the analyte wavelengths
are correctly aligned in the centre of the subarray measurement window.
The iC P 6000 Series Spectrometer will automatically check a
reference line each time the plasma is ignited to maintain wavelength
accuracy.
uto
utouto
uto P
P P
Peak
eakeak
eak only
only only
only needs to be run whenever a new wavelength is used
needs to be run whenever a new wavelength is used needs to be run whenever a new wavelength is used
needs to be run whenever a new wavelength is used
for analysis.
for analysis.for analysis.
for analysis. The auto peak may also need to be run if the instrument
has been switched off for an extended period of time.
Torch Alignment
Auto Peak Adjust

Instrument Set-up
Standard Sample Introduction Glassware Assembly
2-16 iCAP User Guide Thermo Fisher Scientific
To carry out an uto Peak, allow the plasma to stabilise for 10 minutes
and in iTEV nalyst select Perform uto Peak…
Perform uto Peak…Perform uto Peak…
Perform uto Peak… from the
Instrument
InstrumentInstrument
Instrument menu.
Figure 2–15. Auto Peak window
Select HighStd
HighStdHighStd
HighStd and aspirate this standard. Ensure you leave enough
time for the sample to enter the plasma and then click Run
RunRun
Run. This
procedure will set the default position for this line until the next uto
Peak takes place. If all elements are not in the same solution then
multiple standards may be used.
Select Close
CloseClose
Close when the test is successfully completed. If there is an error
message associated with the test highlight the element and select
Reason
ReasonReason
Reason to ascertain the cause of the failure. This is normally due to the
solution not being aspirated for long enough before the test began, or a
problem with the solution.
warning may be given if the analyte peak is not within the expected
region. In this case check the alignment in the subarray display. If
necessary move the central examination position, click “update
method” and then repeat the routine.

Instrument Set-up
Sample Introduction System Set-up
Thermo Fisher Scientific iCAP User Guide 2-17
When a sample is aspirated and a proportion of the aerosol generated by
the nebuliser is passed to plasma through the torch assembly, it
generates a load on the plasma. The RF generator, the plasma
conditions and the sample introduction system should be optimised for
the particular sample and solvent type being introduced.
The iC P 6000 requires pump tubing with two clamping points (two
bridges). Your instrument will be supplied with Tygon® tubing suitable
for the aqueous installation tests.
range of different tubing is available for different sample and matrix
types. For full details of these, refer to the Hardware Manual on the
Supplementary Information CD.
n internal standard is a reference element that can be used to correct
for changes in signal intensity caused external factors. By definition it
should not occur naturally in the sample, but is added to compensate
for sampling differences. It must behave the same as other elements
requiring analysis in the sample.
Figure 2–16. Internal Standards Mixing Kit
The use of internal standards is not required for all types of analysis but
is typically employed where fluctuations in sample loading of the
plasma occur. This is often caused by differing sample physical
properties, for example viscosity, dissolved solids, surface tension or
volatility.
Rather than adding an internal standard manually to all the solutions to
be analysed it is possible to add it automatically on-line using the
Internal Standards Mixing Kit.
To minimise sample dilution, the tubing for the internal standard
solution has a smaller bore than that of the sample solution.
Sample
Introduction
System Set-up
Peristaltic
Pump
Tubing Options
Internal Standards

Instrument Set-up
Sample Introduction System Set-up
2-18 iCAP User Guide Thermo Fisher Scientific
To ensure a thorough mixing of the internal standard with the sample,
a mixing loop is provided after the Y-piece prior to connecting to the
nebuliser.
Pump tubing for the Internal Standard Mixing Kit should be installed
in a similar manner to the sample pump tube as previously described.
Your iC P 6000 Series instrument will be installed and tested with
aqueous solutions. For applications involving organic solvents, high
dissolved solid and HF samples, and hydride generation a slightly
different configuration of sample introduction may be required. For
example different spray chambers, centre tubes and nebulisers are
available. dditional hardware accessories may also be required.
Full details of these can be found in the Hardware Manual on your
supplementary CD.
Application-
Specific Hardware

Thermo Fisher Scientific iCAP User Guide 3-1
Chapter 3
Databases
To store results from your iC P you must create a databases, or
databases, which can be held either locally or on a network. Local
database management is done through iTEV using the pplications
Database options as shown below.
The steps outlined in this chapter explain how to create a new local
database. For details on backing-up and managing your databases, and
on remote database management, refer to the Software Manual
Software ManualSoftware Manual
Software Manual.
For iTEV Security please refer to the separate iTEV Security
manuals.
To create a local database click on T
TT
Tools
oolsools
ools/O
/O/O
/Options
ptionsptions
ptions on iTEV control
panel.
Click on pplication Database
pplication Databasepplication Database
pplication Database Tab.
Local Database
Creation

Databases
Local Database Creation
3-2 iCAP User Guide Thermo Fisher Scientific
Click on Run database wizard
Run database wizardRun database wizard
Run database wizard box.
Type .\
\\
\iTEV
iTEViTEV
iTEV in Server Name box
Type sa
sasa
sa in User Name box
Type teva
tevateva
teva in Password box
Click on Test connection
Test connectionTest connection
Test connection box
This should fill in the Server type and Server version boxes.
Click on Create
CreateCreate
Create box