iCAP 7000 Series ICP-OES User Guide PDF

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The manual discusses operation, maintenance, optimization and safety procedures for an ICP-OES system.

The manual mentions components like the plasma source, optical system, sample introduction system and nebulizer options.

Sample introduction options discussed include ultrasonic nebulizers, V-groove nebulizers and hydride generation kits.

Thermo Scientific

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iCAP 7000 Series
ICP-OES
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Users Guide
Version 1.0 May 2013

part-number Revision A April 2009


Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use in the product
operation. This document is copyright protected and any reproduction of the whole or any part of this document is
strictly prohibited, except with the written authorization of Thermo Fisher Scientific Inc.

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
and assumes no responsibility and will not be liable for any errors, omissions, damage or loss that might result
from any use of this document, even if the information in the document is followed properly.

This document is not part of any sales contract between Thermo Fisher Scientific Inc. and a purchaser. This document
shall in no way govern or modify any Terms and Conditions of Sale, which Terms and Conditions of Sale shall govern
all conflicting information between the two documents.

Save to the extent permitted by law, the customer hereby undertakes not to alter or modify the whole or any part of
the software incorporated in the products in any way whatever nor permit the whole or any part of the software to be
combined with or become incorporated in any other programs nor decompile disassemble or reverse engineer the same
nor attempt to do any other such things.

In no event shall Thermo Fisher Scientific have any obligation to repair or replace in accordance with any warranties
given with the product in whole or in part, as the result of
• Accident, disaster or event of force majeure
• Customers misuse, fault or negligence by or on the customer’s behalf
• Use of the software in a manner for which it was not designed
• Causes external to the software such as, but not limited to, power failure or electrical power surges
• Use of the software in combination with equipment or software not supplied by Thermo Fisher Scientific or with
which it is incompatible.

The warranty shall not apply to any software which the Customer alters or modifies.

Thermo Fisher Scientific does not warrant that the software is error-free, will accomplish any particular result or is fit
for any particular purpose of or intended use by the customer and it is for the customer to satisfy themselves that the
software is so fit.

The photographs used in this manual can differ from the actual module and set-up. All photographs, drawings and
diagrams are for illustrative purposes only.

The content of this manual is protected by copyright.

All efforts have been made to ensure the accuracy of the contents of this manual. However, should any errors be
detected then Thermo Fisher Scientific would appreciate being informed.

The above notwithstanding Thermo Fisher Scientific can assume no responsibility for any errors in this manual or their
consequences.

For more information, please visit our website at http://www.thermo.com/

Any use of this manual other than intended by the producer is prohibited without the prior written permission of
Thermo Fisher Scientific.

© 2013, Copyright reserved by Thermo Fisher Scientific, Cambridge, UK

ii           iCAP 7000 Series ICP-OES Users Guide Thermo  Scientific


EC DECLARATION OF CONFORMITY

No. : DEC0002

The undersigned, representing the following manufacturer

Manufacturer or
Authorised Representative:
Representative Thermo Electron Manufacturing Ltd
Address : SOLAAR House, 19 Mercers Row, Cambridge
CB5 8BZ, UK

herewith declares that the product

Product Identification
dentification : iCAP 7000
000 Series Inductively Coupled Plasma
Spectrometer

is in conformity with the provisions of the following EC directive(s)

Reference No Title
2006/95/EC Low Voltage Directive
2004/108/EC EMC Directive

and that the standard(s) and/or technical specifications referenced


overleaf have been applied.

Last two digits of the year in which the CE marking was affixed : 13

Place : Cambridge, UK Date : 9th April 2013

Signature :

Name : Dr Neil C. Bird Function : R&D Director

Thermo Scientific iCAP 7000 Series ICP-OES Users Guide            iii


EC DECLARATION OF CONFORMITY

No. : DEC0002

References of standards and/or technical specifications applied for this


declaration of conformity, or parts thereof :

- harmonized standards :

number title result


safety:
BS EN 61010-1:2001 Safety Requirements for Electrical Equipment for Measurement, Control Pass
and Laboratory Use. General Requirements.
IEC 61010-2-061:2003 Safety Requirements for Electrical Equipment for Measurement, Control Pass
and Laboratory Use. Particular Requirements for Laboratory Atomic
Spectrometers with Thermal Atomization and Ionization.
BS EN 6010-2- Safety Requirements for Electrical Equipment for Measurement, Control
081:2001/A1:2003 and Laboratory Use. Particular Requirements for Automatic and Semi-
automatic Laboratory Equipment for Analysis and other purposes Pass

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 :

Other references or information required by the applicable EC directive(s):


The documentation relating to this declaration is on 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.

iv           iCAP 7000 Series ICP-OES Users Guide Thermo  Scientific


WEEE Compliance

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:

Thermo Fisher Scientific hat Vereinbarungen mit Verwertungs-/Entsorgungsfirmen in allen EU-Mitgliedsstaaten


getroffen, damit dieses Produkt durch diese Firmen wiederverwertet oder entsorgt werden kann. Mehr Information
über die Einhaltung dieser Anweisungen durch Thermo Fisher Scientific, über die Verwerter, und weitere Hinweise,
die nützlich sind, um die Produkte zu identifizieren, die unter diese RoHS Anweisung fallen, finden sie unter
www.thermo.com/WEEERoHS.

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
l’union européenne et ce produit devrait être collecté ou recyclé par celles-ci. Davantage d’informations sur la
conformité de Thermo Fisher Scientific à ces directives, les recycleurs dans votre pays et les informations sur les pro-
duits Thermo Fisher Scientific qui peuvent aider la détection des substances sujettes à la directive RoHS sont disponi-
bles sur www.thermo.com/WEEERoHS.

Thermo Scientific iCAP 7000 Series ICP-OES Users Guide            v


Warning Signs
CAUTION Symbol CAUTION VORSICHT ATTENTION PRECAUCION AVVERTENZA
Electric Shock: This instrument uses Elektroschock: In diesem Gerät werden Choc électrique: L’instrument utilise des Descarga eléctrica: Este instrumento Shock da folgorazione. L’apparecchio è
high voltages that can cause personal Hochspannungen verwendet, die tensions capables d’infliger des blessures utiliza altas tensiones, capaces de alimentato da corrente ad alta tensione
injury. Before servicing, shut down the Verletzungen verursachen können. Vor corporelles. L’instrument doit être arrêté et producir lesiones personales. Antes de che puo provocare lesioni fisiche. Prima di
instrument and disconnect the instrument Wartungsarbeiten muß das Gerät débranché de la source de courant avant dar servicio de mantenimiento al effettuare qualsiasi intervento di
from line power. Keep the top cover on abgeschaltet und vom Netz getrennt tout intervention. Ne pas utiliser instrumento, éste debera apagarse y manutenzione occorre spegnere ed isolare
while operating the instrument. Do not werden. Betreiben Sie Wartungsarbeiten l’instrument sans son couvercle. Ne pas desconectarse de la línea de alimentacion l’apparecchio dalla linea elettrica. Non
remove protective covers from PCBs. nicht mit abgenommenem Deckel. Nehmen enlever les étuis protecteurs des cartes de eléctrica. No opere el instrumento sin sus attivare lo strumento senza lo schermo
Sie die Schutzabdeckung von Leiterplatten circuits imprimés. cubiertas exteriores quitadas. No remueva superiore. Non togliere i coperchi a
nicht ab. las cubiertas protectoras de las tarjetas protezione dalle schede di circuito
de circuito impreso. stampato (PCB).
Chemical: This instrument might contain Chemikalien: Dieses Gerät kann Chimique: Des produits chimiques Química: El instrumento puede contener Prodotti chimici. Possibile presenza di
hazardous chemicals. Wear gloves when gefährliche Chemikalien enthalten. Tragen dangereux peuvent se trouver dans productos quimicos peligrosos. Utilice sostanze chimiche pericolose
handling toxic, carcinogenic, mutagenic, Sie Schutzhandschuhe beim Umgang mit l’instrument. Portez des gants pour guantes al manejar productos quimicos nell’apparecchio. Indossare dei guanti per
or corrosive or irritant chemicals. Use toxischen, karzinogenen, mutagenen oder manipuler tous produits chimiques tóxicos, carcinogenos, mutagenos o maneggiare prodotti chimici tossici,
approved containers and proper ätzenden/reizenden Chemikalien. toxiques, cancérigènes, mutagènes, ou corrosivos/irritantes. Utilice recipientes y cancerogeni, mutageni, o
procedures to dispose waste oil. Entsorgen Sie verbrauchtes Öl corrosifs/irritants. Utiliser des récipients procedimientos aprobados para corrosivi/irritanti. Utilizzare contenitori
entsprechend den Vorschriften in den et des procédures homologuées pour se deshacerse del aceite usado. aprovo e seguire la procedura indicata per
vorgeschriebenen Behältern. débarrasser des déchets d’huile. lo smaltimento dei residui di olio.
Heat: Before servicing the instrument, Hitze: Warten Sie erhitzte Komponenten Haute Temperature: Permettre aux Altas temperaturas: Permita que lop Calore. Attendere che i componenti
allow any heated components to cool. erst nachdem diese sich abgekühlt haben. composants chauffés de refroidir avant componentes se enfríen, ante de efectuar riscaldati si raffreddino prima di
tout intervention. servicio de mantenimiento. effetturare l’intervento di manutenzione.
Fire: Use care when operating the system Feuer: Beachten Sie die einschlägigen Incendie: Agir avec précaution lors de Fuego: Tenga cuidado al operar el Incendio. Adottare le dovute precauzioni
in the presence of flammable gases. VorsichtsmaBnahmen, wenn Sie das l’utilisation du système en présence de sistema en presencia de gases quando si usa il sistema in presenza di gas
System in Gegenwart von entzündbaren gaz inflammables. inflamables. infiammabili.
Gasen betreiben.
Eye Hazard: Eye damage could occur Verletzungsgefahr der Augen: Danger pour les yeux: Des projections Peligro par los ojos: Las salicaduras de Pericolo per la vista. Gli schizzi di
from splattered chemicals or flying Verspritzte Chemikalien oder kleine chimiques, liquides, ou solides peuvent productos químicos o particulas que prodotti chimici o delle particelle presenti
particles. Wear safety glasses when Partikel können Augenverletzungen être dangereuses pour les yeux. Porter des salten bruscamente pueden causar nell’aria potrebbero causare danni alla
handling chemicals or servicing the verursachen. Tragen Sie beim Umgang mit lunettes de protection lors de toute lesiones en los ojos. Utilice anteojos vista. Indossare occhiali protettivi quando
instrument. Chemikalien oder bei der Wartung des manipulation de produit chimique ou pour protectores al mnipular productos si maneggiano prodotti chimici o si
Gerätes eine Schutzbrille. toute intervention sur l’instrument. químicos o al darle servicio de effettuano interventi di manutenzione
mantenimiento al instrumento. sull’apparecchio.
General Hazard: A hazard is present that Allgemeine Gefahr: Es besteht eine Danger général: Indique la présence Peligro general: Significa que existe un Pericolo generico. Pericolo non
is not included in the above categories. weitere Gefahr, die nicht in den d’un risque n’appartenant pas aux peligro no incluido en las categorias compreso tra le precedenti categorie.
Also, this symbol appears on the vorstehenden Kategorien beschrieben ist. catégories citées plus haut. Ce symbole anteriores. Este simbolo también se utiliza Questo simbolo è utilizzato inoltre
instrument to refer the user to instructions Dieses Symbol wird im Handbuch figure également sur l’instrument pour en el instrumento par referir al usuario a sull’apparecchio per segnalare all’utente
in this manual. auBerdem dazu verwendet, um den renvoyer l’utilisateur aux instructions du las instrucciones contenidas en este di consultare le istruzioni descritte nel
Benutzer auf Anweisungen hinzuweisen. présent manuel. manual. presente manuale.
When the safety of a procedure is Wenn Sie sich über die Sicherheit eines Si la sûreté d’une procédure est Cuando la certidumbre acerca de un Quando e in dubbio la misura di sicurezza
questionable, contact your local Technical Verfahrens im unklaren sind, setzen Sie incertaine, avant de continuer, contacter procedimiento sea dudosa, antes de per una procedura, prima di continuare, si
Support organization for Thermo Fisher sich, bevor Sie fortfahren, mit Ihrer le plus proche Service Clientèle pour les proseguir, pongase en contacto con la prega di mettersi in contatto con il
Scientific San Jose Products. lokalen technischen produits de Thermo Fisher Scientific San Oficina de Asistencia Tecnica local para Servizio di Assistenza Tecnica locale per i
Unterstützungsorganisation für Thermo Jose. los productos de Thermo Fisher Scientific prodotti di Thermo Fisher Scientific San
Fisher Scientific San Jose Produkte in San Jose. Jose.
Verbindung.
vi         
iCAP 7000 Series ICP-OES Users Guide Thermo  
Scientific
CAUTION Symbol CAUTION

Electric Shock: This instrument uses


high voltages that can cause personal
injury. Before servicing, shut down the
instrument and disconnect the instrument
from line power. Keep the top cover on
while operating the instrument. Do not
remove protective covers from PCBs.

Chemical: This instrument might contain


hazardous chemicals. Wear gloves when
handling toxic, carcinogenic, mutagenic,
or corrosive or irritant chemicals. Use
approved containers and proper
procedures to dispose waste oil.
Heat: Before servicing the instrument,
allow any heated components to cool.

Fire: Use care when operating the system


in the presence of flammable gases.

Eye Hazard: Eye damage could occur


from splattered chemicals or flying
particles. Wear safety glasses when
handling chemicals or servicing the
instrument.

General Hazard: A hazard is present that


is not included in the above categories.
Also, this symbol appears on the
instrument to refer the user to instructions
in this manual.

When the safety of a procedure is


questionable, contact your local Technical
Support organization for Thermo Fisher
Scientific San Jose Products.

hermo  Scientific             iCAP 7000 Series ICP-OES  Users  Guide  vii


Preface

ISO 9001 certification


The Thermo Scientific iCAP 7000 Series ICP-OES has been designed and manufactured in
accordance with the following standards.
• ISO 9001 (2000: Quality Management Systems –Requirements)
• ISO 3864 (Safety colours and safety signs)

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.

viii          iCAP 7000 Series ICP-OES Users Guide Thermo  Scientific


C

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

Sample Introduction System Set-up.....................................................................................................29


Centre Tube Options..............................................................................................31
Nebulizer Options..................................................................................................31
Pumping Pump Tubing Options.............................................................................31
Internal Standards...................................................................................................32
Organic Solvent Analysis.........................................................................................33
Light Organic Samples............................................................................................33
Heavy Organic Samples..........................................................................................33
Volatile Organic Samples........................................................................................34
High Dissolved Solid Samples.................................................................................34
Argon Humidifier...................................................................................................34
Installation of your Argon Humidifier Accessory.....................................................35
Daily Operation of your Argon Humidifier Accessory.............................................35
Maintenance of your Argon Humidifier Accessory..................................................36
AeroSalt Nebulizer..................................................................................................37
V-Groove Nebulizer................................................................................................37
HF Samples ...........................................................................................................37

Autosampler Use......................................................................................................................................39
Autosampler Installation.........................................................................................41
Autosampler Set-up................................................................................................41

Thermo Scientific  iCAP 7000 Series ICP-OES Users Guide            ix


Contents

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

x          iCAP 7000 Series  ICP-OES Users Guide Thermo  Scientific


Figures
Figure 1. Duo torch assembly - metal torch mount...................................................................15
Figure 2. Torch assembly - torch body......................................................................................15
Figure 3. Torch assembly - centre tube......................................................................................15
Figure 4. Torch assembly - centre tube insertion.......................................................................16
Figure 5. Insertion of centre tube into torch assembly...............................................................16
Figure 6. Insertion of the torch assembly into the box...............................................................16
Figure 7. Spray chamber drain..................................................................................................17
Figure 8. Nebulizer/spray chamber assembly.............................................................................17
Figure 9. Spray chamber/adapter assembly................................................................................18
Figure 10. Spray chamber fitted..................................................................................................18
Figure 11. Sample capillary tubing scheme.................................................................................19
Figure 12. Sample capillary tubing..............................................................................................19
Figure 13. Pump tubing ...........................................................................................................20
Figure 14. Radial torch - metal torch mount...............................................................................21
Figure 15. Radial torch assembly................................................................................................21
Figure 16. Torch assembly - spray chamber adapter....................................................................21
Figure 17. Centre tube holder assembly......................................................................................21
Figure 18. Torch assembly - centre tube to torch mount.............................................................21
Figure 19. Torch installation in the torch box.............................................................................22
Figure 20. Cyclone spray chamber..............................................................................................22
Figure 21. Nebulizer to spray chamber.......................................................................................23
Figure 22. Torch/spray chamber assembly...................................................................................23
Figure 23. Sample capillary tubing..............................................................................................24
Figure 24. Pump tubing ...........................................................................................................25
Figure 25. Torch Alignment procedure.......................................................................................26
Figure 26. Auto Peak procedure .................................................................................................27
Figure 27. Auto Peak procedure result........................................................................................27
Figure 28. Torch centre tube options..........................................................................................31
Figure 29. Internal Standards Mixing Kit....................................................................................32
Figure 30. Baffled cyclonic spray chamber..................................................................................33
Figure 32. IsoMist - temperature controllable spray chamber.......................................................... 34
Figure 33. Schematic of fully assembled Argon Humidifier.........................................................34
Figure 34. Dispersion tube assembly for glass vessel....................................................................36
Figure 35. HF sample introduction configuration.......................................................................37
Figure 36. Autosampler Tubing Set-up.......................................................................................41

Thermo Scientific  iCAP 7000 Series  ICP-OES Users Guide           xi


Contents

Figure 38. Integrated hydride generation kit...............................................................................46


Figure 40. iCAP 7000 Series ICP-OES power on/off..................................................................57
Figure 41. Get Ready window.....................................................................................................62
Figure 42. Creating new LabBooks window................................................................................62
Figure 43. Methods Parameters of the LabBook..........................................................................63
Figure 44. Manual Sample Control page.....................................................................................63
Figure 45. Autosampler settings..................................................................................................64
Figure 46. Sample list page.........................................................................................................64
Figure 47. Running a LabBook...................................................................................................65
Figure 48. System shut down......................................................................................................65
Figure 49. Additional Gas Accessory Aux Gas Connections........................................................69
Figure 50. 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

xii          iCAP 7000 Series  ICP-OES Users Guide Thermo  Scientific


1

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

Thermo Scientific iCAP 7000 Series ICP-OES Users Guide            1


1  Overview

This page is intentionally blank.

2  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


1  Overview

Most samples are liquids that are pumped through a nebulizer 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. The residual sample is decomposed to atoms
and ions that become excited and emit characteristic light which
is measured, giving a measurement of the concentration of each
element type in the original sample.
Control of the spectrometer is provided by PC-based Thermo
Scientific Qtegra™ Intelligent Scientific Data Solution™ (ISDS).
To avoid loss of analytical performance and compromising safety
only Thermo Scientific specified parts should be used.

Table 1. System Configuration

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

The iCAP 7000 Series ICP-OES consists of several major components:


• optical system
• radio frequency power generator
• CID detector with thermoelectric cooling
• interlocks
• plasma torch and sample introduction parts

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  3


1  Overview

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.

4  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


2

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

Thermo Scientific iCAP 7000 Series  ICP-OES Users Guide            5


2  Technical Specification

This page is intentionally blank.

6  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


2  Technical Specification - Optical System

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.

Focal Length: Effective focal length 383 mm;

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.

Grating: 52.91 grooves/mm, 63.5° blaze angle manufactured using exclusive


high resolution interferometric ruling technology.

Cross dispersion: 9.5 degree prism. Ultra pure ultraviolet fused silica.

Spectral Bandpass: 7 pm at 200 nm, 3.5 pm per pixel.

Wavelength Coverage: iCAP 7400 ICP-OES and iCAP 7600 ICP-OES


instruments have a wavelength range from 166 nm to 847 nm. iCAP 7200
ICP-OES instruments cover 175 nm to 847 nm.

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 Cooling: High efficiency triple stage thermoelectric cooling device


maintains the detector at a constant - 45° C. Interlocks are provided for purge
gas and cooling water to prevent possible damage should a failure of the services
occur.

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.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  7


2  Technical Specification - Plasma Viewing

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.

To maximize performance the viewing height can either be selected by the


operator or automatically optimized using a software routine.

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 %.

Nominal Frequency: 27.12 MHz

Operation: Plasma ignition and operation are fully automated and pc


controlled. Directly coupled autotune with swing frequency impedance
control. Power regulation better than 0.1 %.

Power Output: iCAP 7200 ICP-OES power is pre-optimized at 1150 watts.


iCAP 7400 ICP-OES 750 - 1500 watts computer controlled in steps of 25
watts. iCAP 7600 ICP-OES 750 - 1600 watts computer controlled in steps of
25 watts. The iCAP 7400 ICP-OES Duo and the iCAP 7600 ICP-OES
instruments are restricted to a maximum of 1350 watts.

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.

Sample Pump: The iCAP 7200 ICP-OES - high precision 12 roller, 3


channel pump with speed adjustable from 0 - 125 rpm. Standby mode
prevents damage to pump tubing when the plasma is shutdown. iCAP 7200
ICP-OES has a fixed pump speed of 45 rpm.

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.

8  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


2  Technical Specification - Sample Introduction

Integrated Sprint Valve: The iCAP 7600 ICP-OES incorporates an integrated


sample loop, delivering the sample to the plasma in the most efficient method to
drive increased productivity.

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.

The iCAP 7600 ICP-OES - The nebulizer gas is computer-controlled through


an MFC with options from 0 - 1.5 L/min with increments of 0.1 L/min. The
auxiliary gas is computer controlled through an MFC with options from 0 - 2 L/
min in 0.1 L/min increments. The coolant flow is computer controlled through
an MFC from 0 - 20 L/min with increments of 1 L/min

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  9


2  Technical Specification

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10  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


3

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.

Thermo Scientific iCAP 7000 Series  ICP-OES Users Guide            11


3  Safety

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12  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


4

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

Thermo Scientific iCAP 7000 Series  ICP-OES Users Guide            13


4  Spectrometer Installation

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14  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


4  Spectrometer Installation

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.

Standard Sample WARNING: Appropriate care and safety procedures should be


Introduction followed to avoid breaking any glassware and causing injury
to the operator. Broken glassware should be handled with
Glassware Assembly appropriate care. 

Duo Torch Assembly

Figure 1. Duo torch assembly - metal torch mount


The O-rings in the metal torch mount (3 internal & 2 external) should be
inspected and replaced if any wear, or damage, is visible.

The quartz body of the torch should be pushed into the metal torch mount.
Ensure the torch body is pushed fully into the metal torch mount. The marked
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.

Figure 2. Torch assembly - torch body


The alignment of the torch markings in accordance with the torch holder
assembly are essential in order to ensure that the radial view hole and gas holes
are correctly aligned.

Figure 3. Torch assembly - centre tube


Insert the centre tube fully into the plastic centre tube holder.

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. 

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  15


4  Torch Assembly

Figure 4. Torch assembly - centre tube insertion


Insert the centre tube assembly into the metal torch holder.

Figure 5. Insertion of centre tube into torch assembly


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 6. Insertion of the torch assembly into the 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.

16          iCAP 7000 Series  ICP-OES Users Guide Thermo  Scientific


4  Torch Assembly

Figure 7. Spray chamber drain

Figure 8. Nebulizer/spray chamber assembly


Insert the white plastic tubing connector and wide bore tubing (0.79mm inner
diameter) into the spray chamber drain tube.

Liquid should be delivered to the nebulizer using an identical plastic tubing


connector but with narrow bore tubing (0.50mm i.d.) 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 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 collar is a tight fit. The collar will set the insertion depth
and aid reproducibility of results.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  17


4  Torch Assembly

Figure 9. Spray chamber/adapter assembly


Attach 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.

Figure 10. Spray chamber fitted


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 a check should be made for correct assembly:
•• Make sure the torch is fully rotated and locked in place.
•• Make sure the centre tube holder is fully rotated and locked into
the torch.
•• Make sure the spray chamber 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 part is used for the spray chamber adaptor. In addition,
systems interlocks on the torch holder and elsewhere are there
for safety reasons and must not be bypassed. Operators could
be exposed to dangerous UV and radio frequency radiation if
alternate parts are used for the spray chamber adaptor. 

18  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


4  Torch Assembly

Figure 11. Sample capillary tubing scheme


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.

Figure 12. Sample capillary tubing


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.
Please note: the drain tubing should be connected correctly to the peristaltic
pump to account for the anticlockwise flow.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  19


4  Torch Assembly

Figure 13. Pump tubing


Release the pump tubing clamps and locate the sample and drain pump
tubing over the pump rollers, locking the lugs on the pump tubing into the
left and right clamps.

Connect the sample pump tubing to the sample capillary tubing and the drain
pump tubing to the drain capillary tubing; remember to allow for the
direction of flow.

Pump tubing should be inspected before each analysis and should be replaced
if there are indications of wear.

Additional lengths of capillary tubing should be used to allow connection to


the input of the sample pump tubing to the sample and the output of the
drain pump tubing to a waste container.

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.

20  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


4  Radial Torch Assembly

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.

Figure 15. Radial torch assembly


The quartz body of the torch should be pushed fully into the metal torch
mount.

Figure 16. Torch assembly - spray chamber adapter


Insert the spray chamber adaptor (ground glass joint) into the rear of the centre
tube holder

Figure 17. Centre tube holder assembly


Insert the centre tube fully into the 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.

Figure 18. Torch assembly - centre tube to torch mount


Insert the centre tube assembly into the torch mount assembly. Screw the centre
tube holder in a clockwise direction into the base of the torch holder assembly
until the O-ring is compressed. Do not over tighten as this will reduce the
lifetime of the O-ring seal.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  21


4  Radial Torch Assembly

Figure 19. Torch installation in the torch box


Push the torch assembly up into the torch box and twist clockwise until the
red orientation lock locates in the torch box casting.

Figure 20. Cyclone spray chamber


Insert the white plastic tubing connector and wide bore tubing (0.79mm i.d.)
into the spray chamber drain tube.

Liquid should be delivered to the nebulizer using an identical plastic tubing


connector but with narrow bore tubing (0.50mm i.d.) 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 nebulizer as far as
possible without exerting undue pressure.

22  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


4  Radial Torch Assembly

Figure 21. Nebulizer to spray chamber


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.

Figure 22. Torch/spray chamber assembly


Connect spray chamber and nebulizer assembly to the torch assembly and lock
in to place in the instrument using the stainless steel clamp. The torch
compartment door must be closed before use.

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.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  23


4  Radial Torch Assembly

WARNING: It is extremely important that the safety interlocks are


not disabled. This could result in exposure to dangerous radio and
UV frequency radiation. 

Figure 23. Sample capillary tubing


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 that may prevent flow of the sample.

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.

24  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


4  Radial Torch Assembly

Figure 24. Pump tubing


Release the pump tubing clamps and locate the sample and drain pump tubing
over the pump rollers, locking the lugs on the pump tubing into the left and
right clamps.

Connect the sample pump tubing to the sample capillary tubing and the drain
pump tubing to the drain capillary tubing; remember to allow for the direction
of flow. Pump tubing should be inspected before each analysis and 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.

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.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  25


4  Torch Alignment

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.

Click on “Qtegra” to open the program. In the “Dashboard Page”, click


“Torch Alignment” to start the procedure. Introduce a “loaded Blank” sample
(2 ppm Zn solution). And ensure you leave enough time for the sample to
enter the plasma before clicking “ok”. Aspirate until the process is finished.
The result of the test is displayed in the bottom (right side) of the page.

Figure 25. Torch Alignment procedure

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”.

26  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


4  Torch Alignment

Figure 26. Auto Peak procedure


Introduce the sample “Method development standard” (high standard
concentration solution of the selected element(s)). Ensure you leave enough
time for the sample to enter the plasma and then click ok. This procedure will
set the default position for this line until the next auto peak adjustment takes
place. If all elements are not in the same solution then multiple standards may
be used.

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.

Figure 27. Auto Peak procedure result

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  27


4  Torch Alignment

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28  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


5

Sample Introduction System Set-up

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

Thermo Scientific iCAP 7000 Series  ICP-OES Users Guide            29


5  Sample Introduction System Set-up

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30  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


5  Centre Tube Options

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

Figure 28. Torch centre tube options

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).

Solvent Flex – recommended for oils and many organic solvents.

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.

Typically, the peristaltic pump is operated at a speed of approximately 45 rpm in


an iCAP 7000 Series ICP-OES. However, it may be necessary to reduce the
pump speed to between 35-45 rpm should analysis of samples containing high
concentrations of dissolved solids or volatile organic constituents be required.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  31


5  Internal Standards

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.

Figure 29. 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 may
vary. 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


analyzed it is possible to add it automatically on-line using the Internal
Standards Kit.

To minimize sample dilution, the tubing for the internal standard solution has
a smaller bore than that of the sample solution.

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
manner to the sample tube - as previously described.

32  iCAP 7000 Series ICP-OES Users  Guide Thermo Scientific


5  Organic Solvent Analysis

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.

A specific sample introduction system should be used for organic samples.

WARNING: Organic solvents are a fire hazard and no build up is


permitted in the sample introduction system, or vicinity. 

Light Organic Samples

Figure 30. Baffled cyclonic spray chamber


The organic sample spray chamber has a baffle tube inside. This will reduce the
sample aerosol density; an organic centre tube is also used.

Heavy Organic Samples

Figure 31. V-groove nebulizer for heavy organic sample analysis

In addition to the sample introduction options for light organic samples a


quartz V-groove nebulizer is essential for heavy organic samples.

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.

The V-groove nebulizer should be configured in the cyclonic spray chamber


with the gas connection pointing vertically downwards as shown on the left
hand side in Figure 5-5. The orientation of the nebulizer is essential to enable
successful sample aspiration.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  33


5  Volatile Organic Samples

Volatile Organic Samples

Figure 32. IsoMist - temperature controllable spray chamber


The analysis of organic samples which exhibit a high vapor pressure may
require the use of a cooled spray chamber in order to control the sample
loading of the plasma. An efficient and flexible approach to ensure control
over the spray chamber temperature is to use a programmable temperature
controlled device such as a Peltier unit.
Figure 5-5 shows a photograph of the IsoMist programmable temperature
control device from Glass Expansion, which can be used effectively with iCAP
7000 Series ICP-OES for applications with volatile organic solvents.

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.

Figure 33. Schematic of fully assembled Argon Humidifier

34  iCAP 7000 Series ICP-OES Users  Guide Thermo Scientific


5  Installation of the Argon Humidifier Accessory

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.

WARNING: Do not operate the argon humidifier accessory if any


evidence of surface damage to the glass vessel is observed or if any
parts are damaged. 

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.

WARNING: The shield lid must be locked to the containment shield


before operating this accessory. It is preferable to position the argon
humidifier on the drip tray within the sample introduction area of
the instrument and to operate the unit with the outer door of the
instrument closed. 

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.

Accessory 1. Switch the two-way switch (Figure 7-8) to ‘ON-LINE’.


2. Switch on the nebulizer gas flow from the ICP and set the flow in
the range of 0.5 to 0.8 L/min (0.1 to 0.35MPa). Wait for 1 minute
before proceeding to step 3.

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. 

3. Switch the two-way switch to ‘BYPASS’.


4. Ignite the plasma using the standard plasma ignition procedure
with the two way switch in ‘BYPASS’.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  35


5  Maintenance of the Argon Humidifier Accessory

5. Allow the instrument to perform its Spectrometer Optimization


procedures.
6. When the Spectrometer Optimization procedure has been
completed, switch to ‘ONLINE’ and proceed with the required
sample analysis.
NOTE: If an AutoPeak routine is required, ensure that the switch is set
to BYPASS. When the routine is completed, switch to ‘ONLINE’ as
required before proceeding with sample analysis. 

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.

WARNING: Do not attempt to remove the glass vessel from the


plastic containment shield until the gas pressure inside the glass
vessel has been released. 
3. Perform routine maintenance operations as required.
NOTE: When re-fitting the dispersion tube to the plastic lid of the glass
vessel, ensure that the plastic nut and O-rings are fitted over the tube
as shown in Figure 5-7. Ensure that the tube is pushed fully into the
plastic lid of the glass vessel before screwing the nut into the plastic
lid. Do not over tighten the nut as this may break the dispersion tube. 

Figure 34. Dispersion tube assembly for glass vessel

36  iCAP 7000 Series ICP-OES Users  Guide Thermo Scientific


5  Maintenance of the Argon Humidifier Accessory

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

Figure 35. HF sample introduction configuration


For certain applications hydrofluoric (HF) has to be used to dissolve a sample.
HF will react and dissolve the standard sample introduction glassware supplied
with an iCAP 7000 Series ICP-OES. Most of the glassware will have to be
replaced with optional HF resistant components. Replacing the components
follows the same procedure as detailed for the standard sample introduction
parts.

The components that must be exchanged are: Ceramic centre tube, HF resistant
nebulizer and HF resistant spray chamber with spray chamber adaptor.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  37


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38  iCAP 7000 Series ICP-OES Users  Guide Thermo Scientific


6

Autosampler Use

The autosampler can be configured to suit an application, or several applications.


The volume, number and type of sample will all influence the setup of the autosampler

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6  Autosampler Use

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40  iCAP 7000 Series ICP-OES Users  Guide Thermo Scientific


6  Autosampler Installation

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

Figure 36. Autosampler Tubing Set-up


For analysis with an autosampler the capillary tubing attached to the end of the
autosampler probe should be attached to the end of the sample pump tubing on
the iCAP 7000 Series ICP-OES. To minimize the sample volume required the
length of the capillary tubing should be minimized, but should allow free
movement over the whole sample area of the autosampler.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  41


6  Autosampler Installation

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42  iCAP 7000 Series ICP-OES Users  Guide Thermo Scientific


7

Hydride Generation

Contents
•• On-line Hydride Generation Kit
•• Integrated Hydride Generation Kit
•• Gas Liquid Separator
•• Pump Tubing

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7  Hydride Generation

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44  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


7  On-line Hydride Generation Kit

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.

Figure 37. On-line hydride generation kit with mixing loop

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.

For best plasma stability it is recommended that sodium borohydride and an


acidified wash solution are pumped continuously between measurements.

Ignite the plasma and set the following operating parameters using the plasma
control dialogue:

Table 2. Operating parameters for on-line hydride generation

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.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  45


7  Integrated Hydride Generation Kit

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.

If better sensitivity is required for a particular element then that element


should be used for optimization.

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.

Set-up ❖❖ Assembly of Integrated Hydride Generation Accessory


• The unit is supplied with all the pump tubing connected.
• The user will need to attach the pump tubing to the
peristaltic pump on the ICP-OES and set up the Gas
Liquid Separator.
• The unit should sit comfortably in the kitchen area of the
ICP (to the left of the peristaltic pump), and the lengths of
Tygon peristaltic pump tubing supplied are sufficiently long
so that the acid blank (orange/yellow) and reductant (black)
pump tubing will go directly into their respective solution
containers.
• The sample and drain Tygon peristaltic tubing are supplied
connected to the Ultem sampling probe and 3 mm ID PTFE
drain tubing respectively.
• The Gas Liquid Separator needs to be prepared as described
below before use.

Figure 38. Integrated hydride generation kit

46  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


7  Gas Liquid Separator (GLS)

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.

❖❖ To prepare the Gas Liquid Separator

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.

Figure 39. Schematic of the Gas Liquid Separator

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  47


7  Pump Tubing

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:

Table 3. Colour coded connectors on a Gas Liquid Separator unit


Colour Pump tubing
Black Drain
Green Yellow Sample
Red Reductant reagent
Blue Acid reagent

The peristaltic pump of the ICP-OES operates in an anti-clockwise direction.

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.

48  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


7  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.

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7  Hydride Generation

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8

Ultrasonic Nebulizer

Using an ultrasonic nebulizer can provide a 5 to 20 fold enhancement in detection limit


performance, when compared to a standard sample introduction.

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8  Ultrasonic Nebulizer

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52  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


8  Ultrasonic Nebulizer Installation

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.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  53


8  Ultrasonic Nebulizer

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54  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


9

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

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9  System Operation

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56  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


9  Preparing the System for use

The instrument is powered via an on/off switch at the rear of the left side.

Figure 40. iCAP 7000 Series ICP-OES power on/off

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.

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9  System Operation

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58  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


10

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

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60  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


10  Method Optimization

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

Lighting the Plasma Click on “Qtegra” to open the program.

On the Dashboard Page, click on the “Get Ready” icon to open the window.

Define warm up time. Click “ok”.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  61


10  Setting up Analyses

Figure 41. Get Ready window.


The plasma is switched on and a spectrometer optimization is performed.
During these procedures the remaining warm-up time is shown in the
Dashboard page.

NOTE: To allow the plasma to stabilize leave Plasma on with


blank solution running for about 10 minutes before carrying out
an analysis. 

Setting up Analyses Click on “Qtegra” to open the program.


On the Homepage page, click “LabBooks”. The LabBooks page of Qtegra
opens.
When creating a new LabBook enter a name and select a Location.
LabBooks can be created from blank Templates, existing Templates or from
existing LabBooks.

Figure 42. Creating new LabBooks window

62  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


10  Setting up Analyses

When creating LabBooks from blank Templates, Methods Parameters need


to be defined.

Figure 43. Methods Parameters of the LabBook


If using the Manual Sample Control define Uptake and wash times.

Figure 44. Manual Sample Control page

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  63


10  Setting up Analyses

If using an Autosampler define the autosampler settings.

Figure 45. Autosampler settings

On the sample list define the samples to be analyzed. If using an autosampler


do not forget to identify the rack and vial for each sample.

Figure 46. Sample list page

64  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


10  Shutting Down the System

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.

Figure 47. Running a LabBook

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.

Click on “Qtegra” to open the program.

On the Dashboard Page, click on the “Get Ready” icon.

Figure 48. System shut down


Release the tension on the sample pump platens.

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.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  65


10  Shutting Down the System

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66  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


11

Advanced Hardware

Contents
•• Additional Gas Accessory
•• Sprint Valvve
•• Safety Notices
•• Description of Timings
•• Manual Control Features

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68  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


11  Additional Gas Accessory

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.

For best performance it is recommended that the addition is made to the


auxiliary gas in preference to the nebulizer gas (this is the standard
configuration).

Figure 49. Additional Gas Accessory Aux Gas Connections


Connect the “unequal” T-piece provided to Additional Gas connection fitting
using the short length of 6mm tubing provided. Connect the nebulizer gas
fitting to the T-piece with a second piece of 6mm tubing. Finally re-connect the
nebulizer tubing to the remaining port on the T-piece.

WARNING: Appropriate precautions that are dependent on the gas


used should be followed. These precautions must comply with local
and national safety requirements and guidelines. 

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.

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  69


11  Explanaton of Notices

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:

•• Predominantly aqueous solutions of strong acids (less


than 40%).
•• Common organic solvents such as acetone, alcohols, ethyl acetate,
Methylethylketone (MEK), petroleum oils and derived fuels,
tetrachloroethylene, toluene, and xylene.

NOTE: Prolonged or repeated exposure to temperatures greater


than 135°C and to the following substances can cause failure of
the flow path components:
•• Solutions of concentrated acids (greater than 40%)
•• Partially halogenated hydrocarbons or extremely aggressive
organic solvents (chloroform, methylene dichloride,
1,1,2-trichloroethane) 
Where to find more information
•• iCAP 7600 ICP-OES Sprint valve installation guide
•• iCAP 7600 ICP-OES Sprint valve maintenance guide

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.

70  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


11  Explanaton of Notices

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:

Now click “Connect to Sprint Valve”:

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11  Explanaton of Notices

The screen will now look like this:

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.

72  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


11  Description of Timings

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

Time spent evacuating the loop before the sample is loaded


Time spent evacuating the loop before the sample is loaded
Enables rinse solution to be pumped through the loop

Time taken to perform ‘extra rinse’


Enables rinse solution to be pumped through the loop

Time for vacuum pump to load sample loop


Time taken to perform ‘extra rinse’
Time to let the sample ‘settle’ in the loop, before the valve is
switched
When using the ASX 1400 stirring autosampler, time required to
Time for vacuum pump to load samplestir loop
the sample
Time to drain probe before rinse

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

When using the ASX 1400 Enables/disables


stirring autosampler, timetimeout
the pump required to feature
safety
stir the sample
Maximum time allowed between pump operations, before the
analysis is aborted
Time taken to refill the rinse station, after a ‘pump timeout’
Time to drain probe before rinse
Activates option to have the autosampler probe to wait over the
sample being analysed, after rinse operations are complete. This can
reduce analysis time by several seconds
Rinse time using the autosampler rinse, during analysis

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  73


11  Description of Manual Control Features

A Description of
the Manual Control In order to access the manual control features, click the button, the

Features following options will appear, allowing for manual control:

Sends the autosampler to the home position (above the rinse)

Turns autosampler rinse pump on and off

Switches the valve between load and inject

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

Sets the manual cycle to be performed with rinse solution

Gets the valve/autosampler to perform a complete cycle

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:

Figure 50. Manual Sampling

74  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific


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Index

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I  Index

A-D Setting up Analyses...................................................................... 62


Acid................................................................................................. 48 Set-up............................................................................................. 46
Additional Gas Accessory........................................................... 69 Shutting Down the System.......................................................... 65
Advanced Hardware.................................................................... 67 Sprint valve.................................................................................... 69
AeroSalt Nebulizer........................................................................ 37 Standard Sample Introduction Glassware Assembly............. 15
Argon Humidifier........................................................................... 34 Supported Autosamplers............................................................. 70
Auto Peak Adjust.......................................................................... 26 System Operation.......................................................................... 55
Autosampler Installation............................................................. 41 T -Z
Autosampler Set-up..................................................................... 41
Centre Tube Options..................................................................... 31 To fit the pump tubing:.................................................................. 49
Daily Operation of your Argon Humidifier Accessory.............. 35 Torch Alignment............................................................................ 26
Detector Modes.............................................................................. 7 Ultrasonic Nebulizer Installation................................................ 53
Detector............................................................................................ 7 Ultrasonic Nebulizer Setup.......................................................... 53
Description of the Manual Control Features............................ 74 Ultrasonic Nebulizer..................................................................... 51
Description of the Timings........................................................... 73 V-Groove Nebulizer...................................................................... 37
Drain................................................................................................ 48 Volatile Organic Samples............................................................. 34
Duo Torch Assembly..................................................................... 15 Who Should Read This Book...................................................... 70

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

Thermo Scientific iCAP 7000 Series ICP-OES  Users  Guide  III


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IV  iCAP 7000 Series ICP-OES  Users  Guide Thermo Scientific

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