Thermo Scientific iCAP 7000 Series User manual

iCAP 7000 Series ICP-OES Spectrometer
Customer Familiarisation and Maintenance Manual
© March 2013 Thermo Fisher Scientific Inc.
www.thermoscientific.com
http://www.thermofisher.com

iCAP Customer Familiarisation Manual
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1 Contents
iCAP 7000 Series ICP-OES Spectrometer...................................................................................... 1
Customer Familiarisation and Maintenance Manual....................................................................... 1
1 Contents .................................................................................................................................. 2
2 Instrument Overview................................................................................................................ 4
2.1 General............................................................................................................................ 4
2.2 Optical system and light path .......................................................................................... 4
3 Further information .................................................................................................................. 6
3.1 Qtegra ISDS Help............................................................................................................ 6
3.2 Quick Start Guide ............................................................................................................ 6
3.3 User Manual .................................................................................................................... 6
3.4 Online Assistance............................................................................................................ 6
4 Instrument Hardware............................................................................................................... 7
4.1 LED indicators ................................................................................................................. 7
4.2 Preparing the System for Use ......................................................................................... 7
4.3 Instrument Shut-down...................................................................................................... 8
5 Standard Sample Introduction Glassware Assembly.............................................................. 9
5.1 Duo and Radial Torch Assembly..................................................................................... 9
5.2 Center Tube Options ..................................................................................................... 10
5.3 Centre tube holder......................................................................................................... 10
5.4 Centre tube insertion into torch holder .......................................................................... 11
5.5 Torch holder insertion into the torch box....................................................................... 11
5.6 Positioning of the spray chamber drain......................................................................... 11
5.7 Position of the nebulizer in the spray chamber ............................................................. 12
5.8 Connection of spray chamber adaptor to torch assembly............................................. 13
5.9 Connection of pump tubing............................................................................................ 14
5.10 Radial view window on a Duo instrument...................................................................... 16
5.11 iCAP Sprint Valve installation guide (iCAP 7600 only).................................................. 17
6 Autosampler Use ................................................................................................................... 21
6.1 Introduction.................................................................................................................... 21
6.2 Autosampler Installation ................................................................................................ 21
6.3 Autosampler Set-up....................................................................................................... 21
7 Instrument Optimization......................................................................................................... 22
7.1 Instrumental method optimization.................................................................................. 22
7.2 Example Standard Operating Procedures..................................................................... 23
7.3 Preparing the System.................................................................................................... 23
7.4 Striking the Plasma........................................................................................................ 23
7.5 Setting up Analyses....................................................................................................... 25
7.6 Running the Analysis..................................................................................................... 35
7.7 Auto Peak Adjust........................................................................................................... 37
7.8 Setting the pump tension............................................................................................... 38
7.9 Torch Alignment............................................................................................................. 39
7.10 Reporting results............................................................................................................ 39
7.11 Exporting Labbooks....................................................................................................... 46
7.12 Shutting Down the System ............................................................................................ 47
8 Maintenance .......................................................................................................................... 49
8.1 Instrument Cleaning....................................................................................................... 49
8.2 Preventive Maintenance................................................................................................ 50
9 Analytical Problems Hints and Tips....................................................................................... 61
9.1 Poor Precision ............................................................................................................... 61
9.2 Poor accuracy/feedback................................................................................................ 64
9.3 Poor detection limits ...................................................................................................... 64

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10
Suggested maintenance in the case of poor precision and detection limits...................... 65
10.1 Introduction.................................................................................................................... 65
10.2 Typical Maintenance Schedule...................................................................................... 65
10.3 Replacing pump windings.............................................................................................. 65
10.4 Preventing blocking of the nebuliser.............................................................................. 66
10.5 Removing solids from the nebuliser .............................................................................. 67
10.6 Cleaning the glass mixing chamber............................................................................... 69
11 Sample Introduction Spares & Consumables.................................................................... 70

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2 Instrument Overview
2.1 General
The iCAP 7000 Series 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 measure trace elemental concentrations in a wide range of samples.
Liquid samples are pumped through a nebuliser to produce a fine spray. Large droplets are
removed by a spray chamber, small droplets then pass through the center tube in the torch to the
plasma. Solvent is evaporated and the residual sample decomposes to atoms and ions that are
excited by the electrical Radio Frequency (RF) generated Plasma to 9000K that will emit a unique
set of wavelengths of light for each element as they decay to a lower energy state. The intensity
of this light is measured and this corresponds to the concentration of element type in the original
sample.
The iCAP 7000 spectrometer consists of several major components:
•Plasma torch and sample introduction parts
•Radio frequency power generator
•Echelle polychromator optical system
•CID detector
•Data station
2.2 Optical system and light path

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The dispersive elements in the optic system are the Echelle grating and the prism. The
orientation of the prism is such that the light is dispersed at right angles to the direction of light
dispersal by the grating. This combined dispersal generates a two dimensional spectrum
(“echellogram”) consisting of a wavelength and order separation.
The CID detector is cooled to -45ºC to increase sensitivity and dynamic range.
Warning: Before operating your iCAP ensure you read and understand all the safety
information in the iCAP 7000 reference guide.

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This document is part numbered 849940090071
3 Further
information
3.1
Qtegra ISDS Help
Help with running your instrument, including comprehensive software user guides can be found in
the Qtegra Help page.
The Quick Start Guide includes basic information required to get you started with operating your
iCAP 7000 Series ICP-
OES.
3.3 User Manual
The User Manual details the operation and maintenance of your instrument hardware. It also
includes full information abo
ut 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 Adobe PDF format on
the DVD
3.4 Online
Assistance
For informa
tion about Thermo Scientific and your iCAP 7000 Series ICP
including application notes and other material visit the Thermo Scientific website
iCAP 7000:
www.thermoscientific.com
3.2 Quick Start
Guide
iCAP Customer Familiarisation Manual
This document is part numbered 849940090071
information
Qtegra ISDS Help
Help with running your instrument, including comprehensive software user guides can be found in
The Quick Start Guide includes basic information required to get you started with operating your
OES.
The User Manual details the operation and maintenance of your instrument hardware. It also
ut 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
the DVD
supplied with your instrument.
Assistance
tion about Thermo Scientific and your iCAP 7000 Series ICP
-
OES Spectrometer,
including application notes and other material visit the Thermo Scientific website
www.thermoscientific.com
Guide
Version 1.02
Help with running your instrument, including comprehensive software user guides can be found in
The Quick Start Guide includes basic information required to get you started with operating your
The User Manual details the operation and maintenance of your instrument hardware. It also
ut 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
OES Spectrometer,
including application notes and other material visit the Thermo Scientific website
and search for

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4 Instrument Hardware
The iCAP 7000 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.
4.1 LED indicators
On the rear right hand side of instrument there are row of LED’s which
indicate the status of the instrument.
Once the chiller has been turned on and has reached its set temperature
LED’s 2-7 should be on and led 1 and 8 should be flashing.
LED 9 indicates engineer fast purge has been selected and should be
turned off when analysing samples.
4.2 Preparing the System for Use
If the gas supplies have been switched off, the optical components should be purged and
for at least one hour before powering on the instrument. This is to stop ice damage to the
camera which is cooled to -45ºC. It will take at least 4-8 hours of normal purge for the iCAP
7400, or iCAP 7600 instruments, to measure aluminium at 167nm with the specified
stability and sensitivity.
Ideally the system should be purged constantly, under trickle purge this is a very small
gas flow.
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.
With the plasma aspirated a blank sample for 15 minutes to allow the instrument to fully stabilise
before analysis. Warm up time can be set up in the get ready page of Qtegra.

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4.3 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.
After plasma has been turned off for at least 30 seconds turn off the chiller, following the
manufacturer’s instructions (turning off the chiller by removing the power can often cause
breakages!)
Allow five minutes after switching off the plasma before disconnecting the electrical power or
other supplies to the instrument, or accessories.
The tension on the pump platens should be released to preserve the life of the pump tubing.
NOTE: For the iCAP 7600 the valve and tubing should be rinsed and then purged of solutions. To
purge the 7600 Sprint Valve - open the Sprint Valve Configurator. Verify both Sample and Rinse
probes are in air, confirm (or set) Load, turn On the Vacuum Pump Control for several seconds.
When the Sample Loop and Valve are emptied turn Off. See the Qtegra section below.

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5 Standard 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. ▲
Gloves must be worn when handling glass or ceramic torches as handprints will reduce the life of
the torch and may cause the torch not to light.
5.1 Duo and Radial Torch Assembly
The O-rings in the metal torch mount (3 internal & 2 external) should be inspected and replaced if
any wear, or damage, is visible.
Gloves must be warn when handling a torch as contamination from hands will make the torch
harder to light and reduce its life.
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.
The alignment of the torch markings in accordance with the torch holder assembly are essential
in order to ensure that the optical radial view hole on a duo torch and gas holes are correctly
aligned. Incorrect assembly of the torch can result in damage and reduced torch lifetime.

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5.2 Center Tube Options
5.2.1 1mm with 2 RED bands centre tube
Used for organic solvents. Used for both radial and duo instruments.
This is to reduce the amount of sample reaching the plasma as larger center tubes result in too
much sample reaches the plasma and the plasma may go out.
5.2.2 1.5mm RED band centre tube
Best compromise for a radial instrument,
5.2.3 2mm Blue band centre tube
Best Compromise for a duo instrument.
5.2.4 2mm Ceramic centre tube
Used for specific sample types (for example hydrofluoric acid digests)
5.3 Centre tube holder
Check the 4 o-rings in the Center tube holder are not damaged. Insure the centre tube is inserted
fully into the plastic centre tube holder.
Note: the tip of the centre tube holder will discolor with use. This discoloration is normal and will
not affect the performance of the torch holder assembly. ▲

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5.4 Centre tube insertion into torch holder
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.
When fitted the center tube should be 1-3mm lower than the intermediate tube as shown above.
5.5 Torch holder insertion into the torch box
Insert the torch holder into the
torch box and turn the metal torch holder clockwise until the red orientation lock self locates in the
torch box casting.
5.6 Positioning of the spray chamber drain
Insert the white plastic tubing connector and wide bore tubing (0.79mm inner diameter) into the
spray chamber drain tube. The drain and spray chamber should be positioned so that no pulsing

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occurs during the liquid removal.
5.7 Position of the nebulizer in the spray chamber
Liquid should be delivered to the nebulizer using an identical plastic tubing connector but with
narrow bore tubing (0.50mm inner diameter). Push the white plastic tubing connector with the
attached narrow bore sample tubing into the rear of the nebulizer as far as possible without
exerting undue pressure.
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 nozzle is
level with the arc of the edge of the spray chamber. Small movements in and out are required to
optimize the measurement precision.
Modern designs of nebulizers have a collar to set the depth into the spray chamber. By inserting
the nebulizer into the spray chamber so that the collar is a tight fit the nebulizer will have the
insertion depth optimized and this will aid reproducibility of results.
Attach the quartz glass spray chamber adaptor to the spray chamber with the fitting clamp
provided.
Warning: The adaptor provided with the instrument is specially designed to prevent UV radiation
escaping from the torch box. ▲

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5.8 Connection of spray chamber adaptor to torch assembly
Insert spray chamber adaptor fitting into torch assembly holder as far as it will go, and connect up
the Nebulizer gas supply to the push-fit fitting.
After assembly of the sample introduction system and prior to ignition of the plasma checks
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 adaptor 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.
WARNING: It is extremely important that the correct Thermo Scientific parts are used for the
sample introduction system. In addition interlocks on the torch holder and other parts of the
instrumentation are there for safety and must not be bypassed. Operators could be exposed to
dangerous UV and radio frequency radiation if alternate parts are used for the spray chamber
adaptor. ▲

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5.9 Connection of pump tubing
The following figure shows the peristaltic pump and 2-stop windings are typical of the iCAP 7200.
iCAP 7200 sample pump tubing has white and orange stops and the drain tubing has white and
white stops.
The iCAP 7400 and 7600 instrumentation has a Mini Pump and 3-stop windings (providing two
sections for reduced running costs.
The sample pump tubing has yellow, white and yellow stops. The drain pump tubing has white,
blue and white stops.
For all instrumentation the assembly procedure is similar:
• Feed the sample capillary tubing from the rear of the nebulizer through the upper holder
in the cover and towards the pump.
• Ensure there are no twists or bends in the nebulizer and drain PTFE tubing that may
prevent flow of the sample.
• Pass the drain capillary tubing through the lower holder in the cover and towards the
pump. The lower 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.
• Insert the sample and drain PTFE tubing into their respective peristaltic pump tubes.

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Note: the drain tubing should be connected correctly to the peristaltic pump to account for the
anticlockwise flow.
• 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.
• For a freely aspirating nebulizer. 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.

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5.10 Radial view window on a Duo instrument.
For a Duo instrument check that the radial view bucket shaped window is in place and clean. It is
possible to rotate the window holder to gain access (take the torch out before inspection). When
assembling the torch and radial view window insure the window is located against the torch as
shown below:

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5.11 iCAP Sprint Valve installation guide (iCAP 7600 only)
5.11.1 Connecting the tubing
Fit the drain fitting to the spray chamber
(black ringed), insert the fittings capillary
tube into the yellow/blue peristaltic pump
tubing and attach it to the pump so that the
waste runs counter clockwise across the
pump: Cut a length of the supplied drain
tubing so it can reach between the pump
tubing and the waste container.

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Inset the tubing with the green valve fitting
and the carrier uptake tube (bubbler) into
the white/white peristaltic pump tubing:
Attach the pump tubing onto the peristaltic
pump so that the bubbler runs counter
clockwise across the pump:
Screw the green valve fitting into port 5 on
the valve head:
Next take the white valve fitting tube and
attach one end to port 3 on the valve head:

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Screw the other end of the fitting tube into
the vacuum valve connector on the iCAP:
Attach the vacuum pump waste tubing to
the waste out connector on the iCAP, and
insert the other end into the waste
container:
Screw the autosampler probe valve fitting
into port 2 on the valve head:
Attach the sample loop into ports 1 and 4
on the valve head (this is the same as the
loop provided in the Field Service Test Kit):

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Screw the fitted nebulizer tube into port 6:
Attach the other end on the nebulizer line
and the nebulizer gas fitting onto the
nebulizer:
5.11.2 Manual sampling using the Sprint Valve
Manual sampling uses the Inject position (5) with a standard or non-aerating sample probe.