iCAP 7000 Series ICP-OES User Guide PDF
iCAP 7000 Series ICP-OES User Guide PDF
iCAP 7000 Series ICP-OES User Guide PDF
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ICP-OES
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Users Guide
Version 1.0 May 2013
The contents of this document are subject to change without notice. All technical information in this document is for
reference purposes only. System configurations and specifications in this document supersede all previous information
received by the purchaser.
Thermo Fisher Scientific Inc. makes no representations that this document is complete, accurate or error-free
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Thermo Fisher Scientific.
No. : DEC0002
Manufacturer or
Authorised Representative:
Representative Thermo Electron Manufacturing Ltd
Address : SOLAAR House, 19 Mercers Row, Cambridge
CB5 8BZ, UK
Product Identification
dentification : iCAP 7000
000 Series Inductively Coupled Plasma
Spectrometer
Reference No Title
2006/95/EC Low Voltage Directive
2004/108/EC EMC Directive
Last two digits of the year in which the CE marking was affixed : 13
Signature :
No. : DEC0002
- harmonized standards :
EMC:
Conducted & Radiated Emissions
EN61000-3-3:2008 Flicker Emissions Pass
EN61000-3-2:2006 Harmonic Emissions Pass
EN61326-1:2006 Electrical Equipment for Measurement, Control and Laboratory Use. Pass (class B)
EMC Requirements. General Requirements.
Methods:
CISPR11 Conducted Emissions Pass
CISPR11 Radiated Emissions Pass
Immunity
EN61326-1:2006 Electrical Equipment for Measurement, Control and Laboratory Use. Pass
EMC Requirements. General Requirements.
Methods:
IEC61000-4-3 Radiated Field Immunity Pass
IEC61000-4-6 Conducted RF Immunity Pass
IEC61000-4-4 Electrical Fast Transients Pass
IEC61000-4-2 Electrostatic Discharge Pass
IEC61000-4-5 Surges Pass
IEC61000-4-11 Voltage Dips & Interruptions Pass
- other technical solutions, the details of which are included in the technical
documentation or the technical construction file :
Notices:
1. About the System: Use only with Thermo Fisher Scientific approved computer and
accessories
2. About Shielded Cables: Use only shielded cables supplied by Thermo Fisher Scientific when
connecting this instrument to the computer and other accessories
3. About System Installation: Installation of the system to be performed in accordance with
instructions contained in the appropriate Thermo Fisher Scientific User Guide.
Compliance with the above notices is necessary to ensure that the appropriate radio frequency
emissions will be maintained within the limits of the specifications referred to in this declaration.
This product is required to comply with the European Union’s Waste Electrical & Electronic Equipment (WEEE)
Directive 2002/96/EC. It is marked with the following symbol:
Thermo Fisher Scientific has contracted with one or more recycling or disposal companies in each European Union
(EU) Member State, and these companies should dispose of or recycle this product.
See www.thermo.com/WEEERoHS for further information on Thermo Fisher Scientific’s compliance with these Di-
rectives and the recyclers in your country.
WEEE Konformität
Dieses Produkt muss die EU Waste Electrical & Electronic Equipment (WEEE) Richtlinie 2002/96/EC erfüllen. Das
Produkt ist durch folgendes Symbol gekennzeichnet:
Conformité DEEE
Ce produit doit être conforme à la directive européenne (2002/96/EC) des Déchets d’Equipements Electriques et
Electroniques (DEEE). Il est marqué par le symbole suivant:
Thermo Fisher Scientific s’est associé avec une ou plusieurs compagnies de recyclage dans chaque état membre de
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duits Thermo Fisher Scientific qui peuvent aider la détection des substances sujettes à la directive RoHS sont disponi-
bles sur www.thermo.com/WEEERoHS.
Unless specified otherwise in the ‘technical specifications’ part of this manual, all iCAP 7000 Series
ICP-OES systems comply to the following European norms:
• BS EN 61010-1:2001 + IEC 61010-2-061:2003 + EN 61010-2-081:2002/A1:2003
• EN61000-3-3:2008 + EN61000-3-2:2006
• EN61000-3-3:2008 + EN61000-3-2:2006
• Emission: Class B
• Immunity: Industrial
NOTE: Please note that the serial number mentioned on the certificate does not match that of
your system. CE testing procedures are very demanding on the tested system itself. Systems
that have been tested are for this reason not sold but dismantled or kept as reference system in
our Research & Development labs.
The iCAP 7000 Series ICP-OES also complies with the ASTM D4839, ASTM G 144, IS08245, EPA
415 and EN 1484 methods.
WEEE Compliance
This product is built in compliance with the European Union’s Waste Electrical & Electronic
Equipment (WEEE) Directive 2002/96/EC.
CONTENTS
Introduction to the iCAP 7000 Series ICP-OES......................................................................................1
User Documentation (this manual)...........................................................................4
Quick Start Guide....................................................................................................4
Technical Specification............................................................................................................................5
Optical System..........................................................................................................7
Detector .............................................................................................................7
Detector Modes........................................................................................................7
Plasma Viewing.........................................................................................................8
Plasma Source...........................................................................................................8
Sample Introduction.................................................................................................8
Safety ................................................................................................................................................11
Spectrometer Installation.......................................................................................................................13
Pre-Installation Manual...........................................................................................15
Standard Sample Introduction Glassware Assembly................................................15
Duo Torch Assembly...............................................................................................15
Radial Torch Assembly............................................................................................21
Torch Alignment.....................................................................................................26
Auto Peak Adjust....................................................................................................26
Autosampler Use......................................................................................................................................39
Autosampler Installation.........................................................................................41
Autosampler Set-up................................................................................................41
Hydride Generation..................................................................................................................................43
On-line Hydride Generation Kit.............................................................................45
Set Up ...........................................................................................................45
Integrated Hydride Generation Kit.........................................................................46
Set-up ...........................................................................................................46
Gas Liquid Separator (GLS)....................................................................................47
Pump Tubing..........................................................................................................48
Drain ...........................................................................................................48
Sample Uptake........................................................................................................48
Reductant ...........................................................................................................48
Acid ...........................................................................................................48
To fit the pump tubing:..........................................................................................49
Gas Supply ...........................................................................................................49
Optimization..........................................................................................................49
Ultrasonic Nebulizer................................................................................................................................51
Ultrasonic Nebulizer Installation.............................................................................53
Ultrasonic Nebulizer Set-up....................................................................................53
System Operation.....................................................................................................................................55
Preparing the System for Use..................................................................................57
Instrument Shut-down............................................................................................57
Instrument Optimization..........................................................................................................................59
Method Optimization.............................................................................................61
Example Standard Operating Procedures................................................................61
Preparing the System...............................................................................................61
Lighting the Plasma................................................................................................61
Setting up Analyses.................................................................................................62
Running the Analysis..............................................................................................65
Shutting Down the System.....................................................................................65
Advanced Hardware................................................................................................................................67
Additional Gas Accessory........................................................................................69
Sprint valve ...........................................................................................................69
Safety Notices.........................................................................................................69
A Description of the Timings..................................................................................73
A Description of the Manual Control Features........................................................74
Manual sampling....................................................................................................74
Tables
Table 1. System Configuration.....................................................................................................3
Table 2. Operating parameters for on-line hydride generation....................................................45
Table 3. Colour coded connectors on a Gas Liquid Separator unit..............................................48
Table 4. Operating parameters for integrated hydride generation................................................49
Introduction to the
iCAP 7000 Series ICP-OES
The Thermo Scientific™ iCAP™ 7000 Series ICP-OES is a range of inductively coupled argon
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.
Contents
•• System Configuration
•• User Documentation
Model Description
iCAP 7200 ICP-OES Duo standard gas box, axial and radial plasma view
optics
iCAP 7400 ICP-OES Radial pressure controlled plasma gases, mass flow
controlled nebulizer gas and radial view
optics
iCAP 7600 ICP-OES Radial full mass flow control gas box, radial view
optics and enhanced software
iCAP 7400 ICP-OES Duo pressure controlled plasma gases, mass flow
controlled nebulizer gas and axial and radial
plasma view optics
iCAP 7600 Duo ICP-OES full mass flow control gas box, axial and radial
optics and enhanced software
User Documentation This manual includes detailed information about the use and maintenance of
your iCAP 7000 Series ICP-OES hardware and accessories. It describes the
(this manual)
safety hazards involved in working with the spectrometer and its accessories,
and the means by which such hazards can be minimized.
Quick Start Guide The Quick Start Guide includes basic information required to get you started
with operating your iCAP 7000 Series ICP-OES. This will be supplied with
your instrument and an electronic copy is also provided.
Reference Guide The manual is included with the User Manual, it provides the details of the
(incorporating Pre-Installation Manual) services and environment that must be available before an iCAP 7000 Series
ICP-OES can be installed. This will be supplied with your instrument and an
electronic copy is also provided.
Qtegra Help system The Qtegra Help topics describe features and functions of the software,
covering how to use your instrument. It can be accessed through the
Dashboard page in Qtegra ISDS.
Technical Specification
Utilizing the latest design techniques and innovative new technologies, the iCAP 7000 Series
ICP-OES is not only ideal for routine use but also able to expand its capabilities as
circumstances dictate.
Contents
•• Optical System
•• Detector
•• Detector Modes
•• Plasma Viewing
•• Plasma Source
•• Sample Intrduction
Optical System Type: High energy echelle cross dispersion optical system with “side by side”
optical arrangement of prism and grating. Unique, all spherical mirror design
for very high image quality, improved optical resolution and very low stray light
performance.
Imaging: 1:1
Spectrometer Optical Path: The entire spectrometer and fore optics are purged
with either argon or nitrogen. A normal running flow of 2 L/min is used with a
boost of 2 L/min for optimum performance at wavelengths <200 nm. A purged
environment is maintained with a standby flow of 1 L/min when the plasma is
extinguished.
Cross dispersion: 9.5 degree prism. Ultra pure ultraviolet fused silica.
Detector Type: RACID86 Charge Injection Device (CID). High performance solid state
CID camera system. The Thermo Scientific CID is an enhanced charge transfer
device delivering high contrast/low noise imaging and quantification of all
wavelengths in the analytical range without blooming.
Pixel Size: 27 x 27 µm
Detector Modes Random Access Integration (RAI): User selected analytical wavelengths are
simultaneously integrated in a manner whereby the signal to noise ratio is
optimized while the photogenerated charge level is maintained in the linear
range of the CID. This is accomplished by utilizing the unique nondestructive
readout (NDRO) capability only available with a CID detector. NDRO allows
for the measurement of the signal level on any pixel at any point in the exposure.
In this manner the readout frequency is varied from pixel to pixel based on the
real time observation of the emission intensity.
The major advantage of the CID’s pixel to pixel based real time observation is
that optimum signal to noise is achieved for any wavelength anywhere on the
detector while maintaining wide dynamic range for all signals.
Plasma Viewing Dedicated Radial Plasma: The plasma is viewed directly in a radial mode
using high efficiency magnesium fluoride coated mirrors. The entrance optics
are housed in a purged enclosure for corrosion resistance and to provide
enhanced performance in the UV region of the spectrum.
Duo View Plasma: The plasma may be viewed axially for applications
requiring the lowest detection limits or radially to minimize matrix effects.
Radial signals are measured via an auxiliary optical path that collects light
from an aperture in the side of the torch and images it on the entrance optics.
The orientation of the plasma view can be set in the method and is completely
automatic. Available viewing options are all axial, all radial, Autoview, or on a
line by line basis selected by the operator.
Plasma Source Type: Inductively Coupled Argon Plasma using the internationally approved
ISM (Industrial Scientific and Medical) radio frequency bands. Solid state RF
generator with power efficiency >78 %.
Sample Introduction Nebulizer: Glass concentric fitted as standard; optional: Aerosalt (high solids
concentric), V-groove, Miramist (HF resistant), Ultrasonic nebulizer.
Spray Chamber: Glass cyclonic type with separate radial or axial connection
adaptor fitted as standard; optional: IsoMist temperature controlled, Jacketed
cyclonic with internal baffle, HF resistant cyclonic.
The iCAP 7400 ICP-OES and iCAP 7600 ICP-OES - high precision 4
channel mini pump with speed adjustable from 0 - 125 rpm. Standby mode
prevents damage to pump tubing when the plasma is shutdown. Pump tubing
is available for both aqueous and samples containing organic solvents.
Torch: Demountable quartz torch fitted with either a 1.5 mm centre tube
(Radial instruments) or 2 mm centre tube (Duo instruments).
The torch design includes a quick release, prealigned mounting block which
doesn’t require tools for removal. The mount incorporates automatic torch gas
connections making removal and replacement a very simple operation.
Optional: 1.0, 1.5 and 2.0 mm quartz centre tubes; 2.0 mm HF resistant centre
tube.
Gas control: The iCAP 7200 ICP-OES – The nebulizer gas flow is manually
controlled from 0 to 0.4 MPa. The auxiliary gas is controlled with precision
restrictors with flows of 0, 0.5, 1.0 and 1.5 L/min. The coolant flow is fixed at
12 L/min.
The iCAP 7400 ICP-OES A mass flow controller (MFC) with flows of 0-1.5L/
min in 0.1L/min increments controls the nebulizer gas. The auxiliary gas is
controlled with precision restrictors with flows of 0, 0.5, 1.0 and 1.5 L/min. The
coolant flow is fixed at 12 L/min.
Safety
WARNING: Before operating your iCAP 7000 Series ICP-OES ensure you read and
understand all the safety information in the iCAP 7000 Series ICP-OES
Reference Guide Pack.
The safety standards contained therein comply with the requirements of the Health and Safety at
Work Act 1974 as published by the Health & Safety Executive (HSE).
To comply with safety and warranty requirements, the instrument and accessories described
in this manual are designed to be used by properly trained personnel only. Any installation,
adjustment and repair of this equipment must only be carried out by Field Service Engineers
who have been trained and certified by Thermo Scientific and are aware of the
hazards involved.
Spectrometer Installation
To comply with safety and warranty requirements the iCAP 7000 Series ICP-OES, accessories and
associated equipment must be installed by a Thermo Scientific trained and certified engineer.
Contents
•• Standard Sample Introduction Glassware Assembly
•• Duo Torch Assembly
•• Radial Torch Assembly
•• Torch Alignment
•• Auto Peak Adjust
Pre-Installation Specific site requirements are required for the iCAP 7000 Series ICP-OES.
Please see the Pre-Installation section in the separate iCAP Series ICP-OES
Manual Reference Guide.
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
circle on the quartz torch should be aligned with the notch on the torch holder
assembly and the associated line marking on the torch should be aligned with
the edge of the torch holder assembly.
NOTE: The tip of the centre tube holder will discolour with use. This
discoloration is normal and will not affect the performance of the
torch holder assembly.
The O-rings in the spray chamber should be inspected and replaced if any wear,
or damage, is visible. Using a twisting motion, insert the nebulizer into the spray
chamber so that the collar is a tight fit. The collar will set the insertion depth
and aid reproducibility of results.
Ensure there are no twists or bends in the nebulizer and drain PTFE tubing that
may prevent flow of the sample.
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.
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 nebulizer 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.
Radial Torch
Assembly
Figure 14. Radial torch - metal torch mount
The O-rings in the metal torch mount (3 internal and 2 external) should be
inspected and replaced if any wear, or damage, is visible.
After assembly of the sample introduction system and prior to ignition of the
plasma a check should be made to ensure 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 clamped to the spray
chamber 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.
Pass the drain capillary tubing through the lower holder in the cover and
towards the pump. This holder contains a drain 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.
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 be replaced if
there are indications of wear.
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 nebulizer to free aspirate. Tighten the tension
adjustment until the flow just stops then tighten by one turn. Turn on the pump
and, if necessary, increase 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.
Torch Alignment For maximum sensitivity and optimum results it is advisable to check the
alignment of the torch whenever it has been removed and replaced in the
instrument or if the torch body or centre tube has been replaced.
Auto Peak Adjust For optimum performance it is important that the analyte wavelengths are
correctly aligned in the centre of the sub array measurement window. The
iCAP 7000 Series ICP-OES will automatically check a reference line each
time the plasma is ignited to maintain wavelength accuracy.
Auto Peak only needs to be run whenever a new wavelength is used for
analysis. The autopeak may also need to be run if the instrument has been
switched off for an extended period of time.
To carry out an Auto Peak, allow the plasma to stabilize for 10 minutes and in
the “Acquisition Parameters” of the “Methods Parameters” of your “LabBook
Qtegra” select “Perform Auto Peak”.
The result of the test is displayed in the bottom (right side) of the page. If the
test is unsuccessful or partially successfully there is a message in the log view tab
stating the reason 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.
When a sample is aspirated and a proportion of the aerosol generated by the nebulizer 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 optimized for the particular sample and
solvent type being introduced.
Contents
•• Centre Tube Options
•• Internal Standards
•• Organic Solvent Analysis
•• High Dissolved Solid Samples
•• Installation of the Argon Humidifier Accessory
•• Maintenance of the Argon Humidifier Accessory
•• HF Samples
Centre Tube Options One of the options to alter the characteristics of the sample reaching the plasma
is to use a different centre tube in the torch. The options are:
• 1.5mm quartz for aqueous solutions (single red ring, standard on
Radial configurations)
• 1.0mm quartz for organic solutions (double red ring)
• 2.0mm quartz for high dissolved solids solutions (single blue ring,
standard on Duo configurations)
• 2.0mm Ceramic for HF solutions
Nebulizer Options There are a variety of nebulizer options for the iCAP 7000 Series ICP-OES. The
use of each type is application and method specific, this is discussed below.
Control of the nebulizer pressure, or flow, is either through the control software
or via a manual adjustment. The control is specific to the model of the iCAP
7000 Series ICP-OES.
Pumping Pump Tubing The iCAP 7000 Series ICP-OES requires pump tubing with two clamping
points (two bridges). Three types of tubing are available:
Options
Tygon® for aqueous samples, strong acids and highly polar solvents (methanol
and ethanol).
Once the appropriate peristaltic pump tubing has been selected and configured,
it will be necessary optimize the speed of the pump to ensure optimum sample
delivery to the nebulizer and drainage of the spray chamber during instrument
operation.
The use of a reduced peristaltic pump speed will reduce sample loading in the
plasma and may therefore contribute to improved plasma processing
efficiency, long term stability and resultant analytical performance. Caution is
however advised when operating the peristaltic pump at low speeds (typically
below 35 rpm) as this may lead to pulsing of the analytical signal and may
compromise the associated internal precision of the measurements.
Internal Standards An 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.
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 may
vary. This is often caused by differing sample physical properties, for example
viscosity, dissolved solids, surface tension or volatility.
To minimize sample dilution, the tubing for the internal standard solution has
a smaller bore than that of the sample solution.
Pump tubing for the internal standard kit should be installed in a similar
manner to the sample tube - as previously described.
Organic Solvent When an organic, rather than aqueous, solvent is used, the lower boiling point
of the solvent leads to more sample and matrix loading of the plasma. This may
Analysis impair the analysis, or even extinguish the plasma.
It is important to note that this design of nebulizer will not free aspirate. Flow
rates must be carefully controlled by adjusting the pump speed as previously
described.
High Dissolved Solid A standard nebulizer may be used in a wide range of applications. However,
samples containing levels of dissolved solids greater than 2-3% m/v may cause
Samples the standard nebulizer to block. Cleaning a nebulizer is very difficult and
should be done with great care.
To help prevent nebulizer from blocking, a variety of sample introduction
accessories are available. These include: an Argon Humidifier; an AeroSalt
Nebulizer; and a V-groove nebulizer.
Argon Humidifier The argon supply to the nebulizer is first passed through a humidifier, where
the nebulizer gas is bubbled through a small water reservoir (as below).
Humidified argon will permit the use of a standard nebulizer for samples with
a dissolved solid content of up to approximately 5% m/v.
Installation of your Follow the steps shown below to ensure safe and consistent operation of your
argon humidifier.
Argon Humidifier 1. Ensure the main Argon gas pressure to your ICP instrument is set in
Accessory accordance with the manufacturers requirements for installation and
operation.
2. Check the condition of the glass vessel for surface damage.
3. Fill the glass vessel with deionized water to a level between the minimum
and maximum graduations. Once filled, ensure that the Plastic Lid is
screwed in place until hand tight.
4. Remove the Shield Lid and insert the Glass Vessel into the Plastic
Containment Shield.
5. Re-fit the Shield Lid by aligning the slots on the lid. Twist clockwise to
lock in place.
6. Connect the Blue gas tubing to the gas ‘OUT’ connection on the Plastic
Lid of the Glass Vessel.
7. Connect the Green gas tubing to the gas ‘IN’ connection on the Plastic
Lid of the Glass Vessel.
8. Connect the Yellow gas tubing to the gas connector on the nebulizer of
the ICP-OES.
9. Connect the nebulizer gas supply from the ICP-OES (using the existing
tube on instrument) to the open end of the gas tube adaptor.
Daily Operation of Follow the steps shown below to operate the Argon Humidifier accessory with
your Argon Humidifier your ICP-OES.
WARNING: If the nebulizer gas pressure exceeds 0.4 MPa the over
pressure relief valve will operate and release gas to atmosphere.
The nebulizer pressure should be maintained below this level.
7. When the required sample analysis has been completed, leave the
two way switch in the ‘ON-LINE’ position before switching off
the plasma.
8. Before re-igniting the plasma, switch the two way switch to
‘BYPASS’.
9. When required, re-light the plasma and repeat steps 4 to 6 as
described above prior to commencing sample analysis.
NOTE: If the plasma has been switched off for a long period it may be
necessary to purge the Argon Humidifier to remove air. This is achieved
by following steps 1 to 3 in this section.
Maintenance of your Follow the steps described below when cleaning or re-filling the Argon
Humidifier with deionized water.
Argon Humidifier
1. Ensure that the plasma and the nebulizer gas flow from the
Accessory ICP-OES instrument are switched off.
2. Switch the two way switch to ‘ON-LINE’ and wait for 1 minute
to allow depressurization of the glass vessel.
AeroSalt Nebulizer Samples containing dissolved solids above approximately 5% m/v will require
the use of an AeroSalt Nebulizer. A high solids centre tube and argon humidifier
should also be used.
V-Groove Nebulizer Above 15% m/v dissolved solids in a sample will require the use of a V-groove
nebulizer. A high solids centre tube and argon humidifier should also be used.
HF Samples
The components that must be exchanged are: Ceramic centre tube, HF resistant
nebulizer and HF resistant spray chamber with spray chamber adaptor.
Autosampler Use
Autosampler To comply with safety and warranty requirements the iCAP 7000 Series
ICP-OES, accessories and associated equipment must be installed by a Thermo
Installation Scientific trained and certified engineer.
Autosampler Set-up
Hydride Generation
Contents
•• On-line Hydride Generation Kit
•• Integrated Hydride Generation Kit
•• Gas Liquid Separator
•• Pump Tubing
On-line Hydride The on-line hydride generation kit is used with the iCAP 7200 ICP-OES. It
consists of two pump tubes linked to a Y-piece and mixing loop. Acidified
Generation Kit sample solution and sodium borohydride solution are mixed in the loop to
generate the hydride gases. The mixture is passed to the spray chamber where
separation of liquid and hydride gases takes place.
Set Up 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 nebulizer. Pump
tubing for the internal standard kit should be installed in a similar manor to the
sample tube and the correct tension set.
All standard and sample solutions must be acidified with 2-5% hydrochloric
acid prior to analysis. A solution of 0.5% sodium borohydride prepared in
0.05% sodium hydroxide solution is used as the reducing agent.
Place the orange/blue pump tubing in the sodium borohydride solution, the
orange/white pump tubing is used for the sample and standard solutions.
Ignite the plasma and set the following operating parameters using the plasma
control dialogue:
Parameter Setting
RF power 1150 W
Auxiliary gas 0.5 L/min
Nebulizer gas typical operating range 0.19 – 0.29 MPa
Pump speed 45 rpm
Aspirate a solution of 50 µg/l arsenic solution and check the signal in the
subarray window. Compare the net signal intensity to the intensity of the
background signal.
Vary the nebulizer pressure over the range 0.15-0.20 MPa checking the signal
to background ratio until a maximum is found. This will give a good
compromise set of operating conditions.
Integrated Hydride The integrated hydride generation accessory requires the use of a four channel
sample pump and may only be used with iCAP 7400 ICP-OES or the iCAP
Generation Kit 7600 ICP-OES. It consists of an integrated acrylic reaction cell and gas/ liquid
separator for generation and separation of the hydride gases and is connected
directly to the plasma torch following removal of the spray chamber.
Gas Liquid Separator When assembled, the Reaction Zone of the GLS contains 4 mm glass beads,
which minimize the dead volume of the zone and ensure proper mixing of the
(GLS) carrier gas and liquid reagents. It also contains a semi permeable Teflon
membrane to prevent moisture and salts from being carried over into the tube
leading to the ICP torch. These parts are supplied with the unit, and must be
fitted before the accessory is used.
1. Refer to the figure below, and unscrew the cap of the GLS.
2. Add a sufficient quantity of the 4 mm glass beads supplied
to fill the Reaction Zone. There should be no beads on the
floor of the Expansion Volume (at the top of the reaction zone
column).
3. Take care to prevent the glass beads from falling into the Drain,
where they may cause blockage.
4. Take one of the 47 mm Teflon membranes supplied. Orientate
it so that the Teflon covered face is on the underside, and place
it in position.
5. Carefully re-fit the ‘O’ Ring seal and cap, ensuring that the
position of the membrane is not disturbed.
Pump Tubing The unit is supplied with four types of pump tubing which fit onto the
ICP-OES four channel peristaltic pump. The colours of the pump tubing
bridges correspond to the colour coded connectors on the Gas Liquid
Separator unit, as follows:
Place the GLS to the left of the pump, in the kitchen area.
All of the pump tubing (with the exception of the drain) will attach with the
inlet on the right hand side of the pump i.e. from the sample/reductant/acid
blank solutions across the pump and into the GLS.
The drain is the only tubing that needs to be connected in the opposite
direction, i.e. the tubing is passed under the pump so that the drain outlet is
on the left hand side.
Drain The BLACK (Drain) channel must be fitted to pump tubing with BLACK/
WHITE bridges i.e. a single piece of pump tubing will have a black bridge
fitted at one end, and white bridge fitted at the other end. This tubing has an
ID of 3.17 mm and an OD of 4.85 mm. It runs from the black connector of
the GLS, across the peristaltic pump and to a drain. Connect a suitable length
of the 1.6 mm OD tubing, using the barbed connector supplied, from the end
of the black/white pump tubing (at the peristaltic pump) to a suitable low
level drain or wide necked plastic container. Please note that the drain tubing
is connected anti-clockwise to the unit, to allow draining from the GLS.
Sample Uptake The GREEN/YELLOW (sample) channel must be fitted to pump tubing with
two GREEN bridges. This tubing has an ID of 1.85 mm and an OD of 3.53
mm. This pump tubing goes from the sample, across the pump to the Gas
Liquid Separator.
Reductant The RED (Reductant) channel must be fitted to pump tubing with two
BLACK bridges. This tubing has an ID of 0.76 mm and an OD of= 2.43 mm.
This pump tubing goes from the reductant, across the pump to the Gas Liquid
Separator. The PEEK barb is fitted with an additional piece of 1.6 mm ID
Tygon tubing, for easy connection to the peristaltic pump tubing.
Acid The BLUE (Acid) channel must be fitted to pump tubing with YELLOW/
ORANGE bridges. This tubing has an ID of 0.5 mm and an OD of 2.33 mm.
This pump tubing goes from the acid, across the pump to the Gas Liquid
Separator. The PEEK barb is fitted with an additional piece of 1.6 mm ID
Tygon tubing, for easy connection to the peristaltic pump tubing.
To fit the pump tubing: 1. Release the plungers to free the pump platens.
2. Take the pump tubing, and feed it around the pump rollers.
3. Stretch the pump tubing slightly, and fit the bridges under the
bridge retaining pillars.
4. Push the ends of the tubing over the appropriate push on
connectors on the Gas Liquid Separator connection panel.
5. Move the platen arm back over the rollers, and confirm that the
tubing is properly located beneath it.
6. Return the plunger to the normal position, and adjust the pressure
screw to release the pressure on the tubing.
Gas Supply Connect a supply of argon (normally from the nebulizer supply on the front of
the sample introduction area of the ICP-OES), with the supplied 4 mm o.d.
rigid black tubing. The flow should be regulated between 0.4 – 0.6 L/min, to
the gas inlet at the rear of the Gas Liquid Separator.
Optimization Ignite the plasma and set the following operating parameters using the plasma
control dialogue.
Table 4. Operating parameters for integrated hydride generation
Parameter Settings
RF power 1100 W
Coolant gas 14 L/min
Auxiliary gas 0.5 L/min
Nebulizer gas 0.5 L/min
Pump speed 45 rpm
Aspirate a solution of 50 µg/l arsenic solution and check the signal in the
subarray window. Compare the net signal intensity to the intensity of the
background signal.
Vary the nebulizer flow over the range 0.4-0.6 L/min checking the signal to
background ratio until a maximum is found. This will give a good compromise
set of operating conditions. If better sensitivity is required for a particular
element then that element should be used for optimization.
For each hydride group element, there is an optimum nebulizer gas flow rate
that will give the maximum sensitivity for that element. For mercury, the
analytical sensitivity increases as the Nebulizer gas rate decreases. Low Nebulizer
gas rates require longer flush times (to allow the hydride to travel to the plasma),
and, except for mercury, offer no benefits. Higher nebulizer gas flows allow the
use of shorter flush times, at the expense of some analytical sensitivity, and can
be used if you want to complete your analysis as quickly as possible.
The sample pump speed will also have an influence on the sensitivity. As the
pump speed is increased, the analytical sensitivity increases, but so does the
consumption of samples and reagents. The flush time required will be decreased
at higher pump speeds. Reducing the pump speed reduces the reagent
consumption at the expense of the analytical sensitivity and increased flush
time. The default pump speed is 30 rpm, and good results can be obtained with
pump speeds up to 45 rpm.
Ultrasonic Nebulizer
Ultrasonic Nebulizer To comply with safety and warranty requirements the iCAP 7000 Series
ICP-OES, accessories and associated equipment must be installed by a Thermo
Installation Scientific trained and certified engineer.
Ultrasonic Nebulizer Locate the Ultrasonic nebulizer accessory on the bench to the right of the iCAP
7000 Series ICP-OES. Remove the cyclone spray chamber, concentric
Set-up
nebulizer and associated pump tubing if fitted. (Refer to earlier section on
sample introduction removal.) Connect the sample pump tubing to the sample
capillary tubing of the ultrasonic nebulizer.
Use the 4 mm argon tubing supplied with the accessory to connect the nebulizer
outlet of the iCAP 7000 Series ICP-OES with the inlet on the rear panel of the
ultrasonic nebulizer.
Using the adaptor provided with the accessory connect the sample outlet from
the ultrasonic nebulizer to the plasma torch. Push the adapter firmly into the
base of the torch until it “bottoms out” to prevent leaks.
Place the three drain tubes from the outlet of the pump on the rear panel in to a
suitable waste container.
System Operation
The iCAP 7000 Series ICP-OES is designed to be constantly powered up and the optical system
continuously purged.
Contents
•• Preparing the System for Use
•• Instrument Shut-down
The instrument is powered via an on/off switch at the rear of the left side.
Preparing the System The instrument is powered via an on/off switch at the rear of the left side.
for Use If the instrument power is switched off, allow at least two hours after restoring
power to thermally stabilize the instrument.
If the gas supplies have been switched off, the optical components should be
purged for at least two hours before turning on the water chiller and running
samples. Even then, if the purge gas has been off for sometime signals in the low
wavelength range may only be acceptable after several hours.
WARNING: Do not turn on the water chiller until the instrument has
been purging with gas for at least two hours. Doing so can seriously
damage the CID detector.
Deionized water should be aspirated for twenty minutes to allow the instrument
to fully stabilize before analysis.
Instrument Shut-down After an analysis is finished a blank sample should be aspirated for five minutes
to ensure the sample introduction components have been rinsed of sample. To
remove the blank sample, deionized or distilled water should be aspirated for a
further minute.
When organic solvent based samples are being analyzed the final rinse should be
the pure solvent. Air should be aspirated for one minute to remove organic
solvent from the sample lines and to remove organic vapors.
After completing the above the plasma should be turned off. The optical
components will move to a parked position after about thirty seconds.
After switching off the plasma, allow two minutes before switching off the water
chiller and gas supplies.
Allow five minutes after switching off the instrument, or accessories, before
disconnecting the electrical power or other supplies.
Instrument Optimization
The iCAP 7000 Series ICP-OES will require optimization that is dependent on the sample being
analyzed 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 Scientific Sales Office; contact details are
available on http://www.Thermoscientific.com.
Contents
•• Method Optimization
•• Lighting the Plasma
•• Setting up Analyses
•• Running the Analysis
•• Shutting Down the System
Method Optimization The following parameters can all affect the data obtained and should be
optimized. Usually a default setting will give data that is satisfactory, but may
not be optimal for the analysis requirements:
•• Nebulizer 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 ionization and
solvent effects.
Example Standard This method setup procedure, which by no means covers all the possible
parameters used in Qtegra ISDS, should be enough for setting up a basic
Operating Procedures analysis. It is recommended that the user reads the Qtegra ISDS software
manual for more advanced use of the system.
Preparing the System 1. Turn Argon Gas on at Cylinder and set for 0.6 MPa (6 BAR)
pressure on gauge near instrument
NOTE: for normal use gas should be left purging constantly
2. Switch on power to iCAP 7000 Series ICP-OES Spectrometer.
NOTE: for normal use power should be left on constantly
3. Switch on Water Chiller
4. Push Platen on to rollers of pump by way of the 4 (3) pressure
screws
5. Make sure the drain tube is placed in an open neck vessel
6. Place sample tube in a blank solution
7. Switch on computer
8. Click on the “Qtegra” Icon on desktop
On the Dashboard Page, click on the “Get Ready” icon to open the window.
Running the Analysis In the toolbar of your LabBook click “Run” to schedule the LabBook for
execution. The LabBook is added to the scheduler. If the check box Automatic
has been selected for Start Queue in the options settings of the scheduler the
measurement is started immediately.
Shutting Down the Place the sample tube in Deionized water and let it pump through the system
for 3 to 5 minutes. When organic solvent based samples are being analyzed the
System final rinse should be the pure solvent. Air should be aspirated for one minute to
remove organic solvent from the sample lines and to remove organic vapors.
After switching off the plasma, allow two minutes before switching off the
water chiller. Follow manufacturer’s instructions for switching off the chiller.
If switching off power to the instrument, allow five minutes after the plasma
has been switched off.
Advanced Hardware
Contents
•• Additional Gas Accessory
•• Sprint Valvve
•• Safety Notices
•• Description of Timings
•• Manual Control Features
Additional Gas This accessory is fitted as standard iCAP 7600 ICP-OES. It provides an
additional gas that is added to the plasma to modify the conditions. For
Accessory example, the additional gas can be used to add air preventing the buildup of
carbon on the torch when running organic samples.
Sprint valve This manual describes the procedures for using the integrated sprint valve rapid
sample introduction system.
Safety Notices NOTE: If the equipment is used in a manner not specified by Thermo
Fisher Scientific, the protection provided the equipment may be
impaired.
Repair or service that this not covered in this manual should only be performed
by qualified personnel.
EXPLOSION HAZARD
Do not operate in an explosive atmosphere.
Explanation of Caution and Warning symbol marked on equipment. This symbol means
Warning Notices “Attention! Refer to the manual.”
Who Should Read This Book The primary audience for this manual consists of analytical chemists and lab
technicians. To use this manual effectively, you should have a basic knowledge
of chemistry, a basic knowledge of electronic sampling equipment, at least a
beginning level of computer experience, and working knowledge of the
analytical instrument used with the sample introduction system.
Supported Autosamplers The integrated sprint valve Rapid Sample Introduction System works with
many autosamplers including:
➣➣ CETAC ASX-520
➣➣ CETAC ASX-520HS
➣➣ CETAC ASX-520/520HS with XLR-8 extended rack
➣➣ CETAC ASX-1400
➣➣ CETAC ASX-1600
The 6-port injection valve is constructed of polyphenylene sulphide (PPS), an
inert and dimensionally stable material. The tubing is all inert PTFE (waste
tubing materials may vary by application). Components in the sample flow
path are inert, non metallic materials; they can withstand repeated exposure to
the following substances:
Caution
The plumbing connections should be made without using tools. In fact, using
tools such as screwdrivers or pliers to perform installation tasks may result in a
damaged or unusable instrument. Do not tighten fittings with anything other
than your fingers.
The sprint valve should be setup as per the installation guide, the plumbing
configuration is crucial to the proper operation of the sprint valve system and
must be followed.
The operational settings of the iCAP 7600 ICP-OES sprint valve are controlled
via a separate software package. This software package allows the user to upload
and save the sprint valve’s operating settings in the instruments inbuilt firmware.
Sprint Valve Configurator is not required to operate the valve on a day to day
basis but is used to setup and change the valve settings and to provide manual
control of the valve.
When the software loads it looks like this, with most of the options greyed out:
Once the required options are inserted, then you must click “Save
Configuration to Sprint Valve” in order to upload these settings into the valve
firmware, otherwise the new settings will not take effect.
A Description of the
Timings
Enables/disables the sprint valve control, allowing the auto
Enables/disables the sprint valve control, allowing the auto sampler
sampler to be usedtowithout
be usedthe valvethe valve
without
Rinse time
Time to let the sample using
‘settle’ the loop,
in the autosampler
beforerinse, during
the valve is analysis
switched
Time for autosampler peri pump to continue after rinse uptake, in
order to re-fill rinse station
A Description of
the Manual Control In order to access the manual control features, click the button, the
Rapidly switches the valve between load and inject mode several
times ‘homing the valve’.This needs to be done each time the
valve is removed and re-attached
Switches the iCAP 7600 ICP-OES vacuum pump on and off
Manual sampling In order to perform manual sampling, i.e. for the torch alignment or autopeak
features, then the bubbler should be removed from the white peri-pump
tubing and replaced with a standard sampling probe:
Index
E-O
Example Standard Operating Procedures................................ 61
Explanation of Caution and Warning Notices.......................... 70
Gas Liquid Separator (GLS)......................................................... 47
Gas Supply..................................................................................... 49
Heavy Organic Samples............................................................... 33
HF Samples.................................................................................... 37
High Dissolved Solid Samples..................................................... 34
Installation of your Argon Humidifier Accessory..................... 35
Instrument Optimization............................................................... 59
Instrument Shut-down................................................................. 57
Integrated Hydride Generation Kit............................................. 46
Internal Standards........................................................................ 32
Light Organic Samples................................................................. 33
Lighting the Plasma...................................................................... 61
Maintenance of your Argon Humidifier Accessory................ 36
Manual sampling.......................................................................... 74
Method Optimization.................................................................... 61
Nebulizer Options......................................................................... 31
On-line Hydride Generation Kit................................................... 45
Optical System................................................................................ 7
Optimization................................................................................... 49
Organic Solvent Analysis............................................................. 33
P-S
Plasma Source................................................................................ 8
Plasma Viewing............................................................................... 8
Pre-Installation Manual............................................................... 15
Preparing the System for Use..................................................... 57
Preparing the System................................................................... 61
Pump Tubing.................................................................................. 48
Pumping Pump Tubing Options................................................... 31
Radial Torch Assembly................................................................. 21
Reductant....................................................................................... 48
Running the Analysis.................................................................... 65
Safety Notices............................................................................... 69
Sample Introduction....................................................................... 8
Sample Uptake.............................................................................. 48
Set Up............................................................................................. 45