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Prodigy7 User Manual

Part Number: 150-00371


Rev: A, July - 2014
Copyright © 2014 Teledyne Technologies Incorporated

All rights reserved. Reproduction, adaptation, or translation without permission is prohibited, except as allowed under copy-
right laws. Printed in the U.S.A.

Updated Information
The information contained in this document is subject to change without notice.

Trademarks
The companies indicated own the following trademarks:

Prodigy7............................................................................................................................................Teledyne Leeman Labs


Salsa Software.................................................................................................................................Teledyne Leeman Labs
Twist-n-Lock Auto-Aligning Sample Introduction System.............................................Teledyne Leeman Labs
Full Spectral Access.......................................................................................................................Teledyne Leeman Labs
All other brands or product names are trademarks or registered trademarks of their respective owners.

Teledyne Leeman Labs


110 Lowell Road
Hudson, NH 03051 U.S.A
www.teledyneleemanlabs.com

Sales Support: 800-634-9942


Main: 603-886-8400
Fax: 603-886-9141
Prodigy7 User Manual
Table of Contents

General Warnings
Notations and Hazard Severity Levels
Prodigy7 ICP Safety Labels
Chapter 1: Introduction
1.1 Prodigy7 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
1.1.1 Site Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
1.1.2 System Specifications. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
1.2 Twist-n-Lock, Auto-Aligning Sample Introduction System . . . . . . . . . . . . . 1-3
1.3 High-Energy, High-Performance Optical System. . . . . . . . . . . . . . . . . . . . 1-3
1.4 CMOS Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
1.5 Salsa Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
1.5.1 Overview. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
1.5.2 Common Tasks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
1.5.3 Advanced Tasks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-5
1.5.4 Quantitative Full Frame Feature . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6
1.6 View Configurations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
1.6.1 Axial View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
1.6.2 Dual-View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
1.6.3 Radial View. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-8
1.7 Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-9
Chapter 2: Standard Operating Procedures
2.1 Sample Introduction System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
2.1.1 Sample Introduction and Sample Types. . . . . . . . . . . . . . . . . . . . . . 2-2
2.1.2 Peristaltic Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Set-Up and Adjustment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
2.1.3 Torch - Installation and Removal . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Axial and Dual-View Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Radial Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
Torch Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
Torch Injector Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
Torch Position . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-11
2.1.4 Torch Adjustment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
Axial and Dual-View Torch Adjustment . . . . . . . . . . . . . . . . . . . . . 2-12
Dual-View Mirror Positioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-14
Radial System Torch Adjustment . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
2.1.5 Spray Chamber. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-16
Spray Chamber Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-16
Installing and Adjusting the Spray Chamber . . . . . . . . . . . . . . . . . 2-16
2.1.6 Nebulizer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-17
Nebulizer Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-17
Installing and Adjusting the Nebulizer . . . . . . . . . . . . . . . . . . . . . . 2-18
2.1.7 Optimizing the Sample Introduction System. . . . . . . . . . . . . . . . . . 2-19
Sample Introduction Optimization by Sample Type . . . . . . . . . . . . 2-19
2.2 Mix Standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-20
2.3 Salsa Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-21
2.3.1 Salsa Application Tabs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-22

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2.4 Create an Analytical Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-22
2.4.1 Method Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-22
Axial or Radial View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-22
Entering Elements and Wavelengths . . . . . . . . . . . . . . . . . . . . . . . 2-23
2.5 Setting Analytical Parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-26
2.6 Igniting the Plasma . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-27
2.6.1 Plasma Manual Ignition. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-27
2.6.2 Plasma Auto Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-27
2.7 Position the Plasma (Peak Source) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-29
2.7.1 Axial View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-30
2.7.2 Radial View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-30
2.8 Align the Spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-31
2.8.1 Manual Alignment Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-31
2.8.2 Auto Alignment Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-33
2.9 Align Wavelengths . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-34
2.9.1 Manual Alignment Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-34
2.9.2 Auto Alignment Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-38
2.10 Collect Wavelength Spectra . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-41
2.11 Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-41
2.11.1 Add Calibration Standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-41
2.11.2 Modify Calibration Standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-43
Modify the Standard Concentration and Unit of Concentration . . . 2-43
Change the Standard Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-44
2.11.3 Delete a Calibration Standard . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-44
2.11.4 Run Calibration Standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-44
Without an Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-44
With Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-45
2.11.5 Reviewing the Calibration Data. . . . . . . . . . . . . . . . . . . . . . . . . . . 2-46
2.12 Quality Control Checks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-48
2.12.1 Add Quality Control Check Standards . . . . . . . . . . . . . . . . . . . . . 2-48
2.12.2 Modify Quality Control Check Standards . . . . . . . . . . . . . . . . . . . 2-49
Modify the Standard Concentration and Unit of Concentration . . . 2-49
Change the Standard Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-49
2.12.3 Delete a Quality Control Check Standard . . . . . . . . . . . . . . . . . . . 2-49
2.12.4 Run Quality Control Check Standards . . . . . . . . . . . . . . . . . . . . . 2-50
Without an Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-50
With an Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-50
2.13 Sample Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-52
2.13.1 Add Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-52
2.13.2 Run Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-52
Without an Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-52
With an Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-53
2.14 Build Sequences. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-54
2.15 Review and Report Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-56
2.15.1 Reviewing Numerical Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-56
2.15.2 Recalculating Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-57
Recalculating Calibration Standards. . . . . . . . . . . . . . . . . . . . . . . . 2-57
Recalculating for Weight and Volume. . . . . . . . . . . . . . . . . . . . . . . 2-58
2.15.3 Reporting Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-59
CSV File Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-61
Paper Reports Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-61
Exporting Data to LIMS. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-61
Chapter 3: Method Development
3.1 Overview. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1

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3.1.1 Method and Analysis Chapters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
3.1.2 Method Complexity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
3.1.3 Compromise Operating Conditions. . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
3.2 Selecting Wavelengths for the Method . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
3.2.1 Wavelength Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
3.2.2 Collect Wavelength Spectra . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
3.2.3 Collecting Spectral Information for Standards . . . . . . . . . . . . . . . . . 3-4
Scan a Calibration Standard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
3.2.4 Collecting Spectral Information for Samples. . . . . . . . . . . . . . . . . . . 3-5
Scan a Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5
3.2.5 Examining Wavelength Scans . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
Viewing Wavelength Scans using the Profiles Tab . . . . . . . . . . . . . 3-7
Sensitivity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8
Linear Dynamic Range. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8
Freedom from Interferences. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
Atomic vs. Ionic Lines. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
Automated Wavelength Scans . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9
3.3 Estimating Analyte Concentrations in Samples . . . . . . . . . . . . . . . . . . . . 3-10
3.4 Selecting Parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11
3.4.1 Integrations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-11
3.4.2 Rinse Time . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12
3.4.3 Uptake Time . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12
3.4.4 Peaking Line . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12
3.4.5 Plasma Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13
Plasma Parameter Settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
RF Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14
Nebulizer Pressure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-15
Coolant Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-15
Auxiliary Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-16
Sample Uptake Rate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-17
Chapter 4: Salsa Software Overview
4.1 Startup Login . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
4.2 Menu Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3
4.3 Tool Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-5
4.4 Instrument Control Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
4.4.1 Maintenance Button . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
Scheduled Maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
Required Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
4.4.2 Interlocks Button . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
4.5 Application Tabs. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
4.6 Navigation Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
4.6.1 Method Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
4.6.2 Sequence Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
4.6.3 Analysis Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
4.7 Display Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
4.8 Status Panel. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
Chapter 5: Method
5.1 Method Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
5.2 Creating a Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2
5.3 Opening an Existing Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2
5.4 Instrument Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
5.4.1 Autosampler Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
5.4.2 Diagnostics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
5.4.3 Optimize Sample Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5

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5.4.4 Plasma Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Auto Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-7
Manual Start . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Extinguish . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-9
Extinguish After Rinse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-9
Gas Knife . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-9
5.4.5 Peristaltic Pump Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
5.4.6 Spectrometer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
5.4.7 Torch Gas Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
5.5 Element Selection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12
5.5.1 Add a Line to the Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12
5.5.2 Line Specific Information. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-13
5.5.3 General Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-14
5.5.4 Calibration Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-16
5.5.5 Align Wavelength Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-17
Automatic Alignment of Wavelengths . . . . . . . . . . . . . . . . . . . . . . . 5-18
5.5.6 Interfering Element Corrections (IEC) Tab . . . . . . . . . . . . . . . . . . . 5-20
5.6 Standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-20
5.6.1 Add a Standard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-20
5.6.2 Modify a Standard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21
5.6.3 Delete a Standard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-22
5.6.4 Update Standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-22
Add/Modify an Update . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-22
Running Updates Using Assigned Frequencies . . . . . . . . . . . . . . . 5-23
Running Updates using Cup Macros . . . . . . . . . . . . . . . . . . . . . . . 5-23
Update Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-24
Overwriting Replicates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-24
5.6.5 Internal Standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-25
5.6.6 Method of Standard Additions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-25
5.7 Concentration Ratio . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-25
5.8 Quality Control Checks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-26
5.8.1 Add a QC Check . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-27
5.8.2 Modify QC Check Criteria . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-27
5.8.3 Modifying QC Acceptance Criteria . . . . . . . . . . . . . . . . . . . . . . . . . 5-27
5.8.4 Delete QC Check . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-27
5.8.5 Extra Volumes for Check Standards . . . . . . . . . . . . . . . . . . . . . . . . 5-28
5.9 QC Automation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-28
5.9.1 Initial - QC Standards Before Samples Run . . . . . . . . . . . . . . . . . . 5-29
Automatic Assignment of QC Standard Locations . . . . . . . . . . . . . 5-29
Custom Assignment of QC Standard Locations . . . . . . . . . . . . . . . 5-30
Shared Cup Locations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-30
5.9.2 Continuous - QC Standards During Sample Run . . . . . . . . . . . . . . 5-31
5.9.3 Final - QC Standards After Samples are Run . . . . . . . . . . . . . . . . . 5-31
5.9.4 Post-Calibration Action . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-32
5.10 Analytical Parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-32
5.11 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-34
5.12 Creating a SemiQuant Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-34
Chapter 6: Sequence
6.1 Sequence Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1
6.1.1 Editing Tools . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
6.1.2 Sample List Table . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
Sample Weights, Volumes, and Dilutions . . . . . . . . . . . . . . . . . . . . . 6-3
Correction Factors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
6.1.3 Sequence Navigation Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4

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6.1.4 Rack Map . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
6.1.5 Editing the Rack While Running a Sequence . . . . . . . . . . . . . . . . . . 6-5
6.2 Sequence Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
6.2.1 Set-Up a Sequence Method Run . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-7
6.3 Cup Macros (Flexible QC Automation) . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11
6.3.1 Available Cup Macros. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11
6.3.2 Cup Macro Examples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11
Example 1: A typical Cup Macro Action Indicator List . . . . . . . . . . 6-11
Example 2: Use of the "CP" Action . . . . . . . . . . . . . . . . . . . . . . . . 6-11
6.3.3 Multiple Updates Using Cup Macros . . . . . . . . . . . . . . . . . . . . . . . 6-12
6.4 Synchronizing External Hardware to Sample Sequence . . . . . . . . . . . . . 6-13
Chapter 7: Analysis
7.1 Analysis Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
7.2 Results Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
7.2.1 Show/Hide Items in the Analysis Tree . . . . . . . . . . . . . . . . . . . . . . . 7-2
Hide Items . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2
Show Items. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3
7.2.2 Renaming Samples and Analysis Items . . . . . . . . . . . . . . . . . . . . . . 7-3
7.2.3 Display Modes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-4
7.2.4 Searching for Existing Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
7.3 Scans Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6
7.4 Profiles Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-8
7.5 Calc. Validation Tab (Raw Data) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-8
7.6 Image Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-10
7.6.1 Fingerprint Spectra (QA Mode). . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-11
7.7 Control Chart (Crtl Chrt) Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-13
7.8 Report Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-14
7.8.1 Report Control and Filtration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-16
7.8.2 Report Limits and Averaging . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-17
7.8.3 Report Precision Customization . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-17
7.8.4 Report Formats and Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19
7.8.5 Saving/Loading/Deleting Report Specs . . . . . . . . . . . . . . . . . . . . . 7-22
Save a Report Spec . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-22
Load a Saved Report Spec . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-22
Delete a Saved Report Spec . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-22
7.8.6 Quick Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-22
7.8.7 Sequence Reporting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-23
7.9 Recalculate Tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-25
7.10 Collecting Echellograms. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-27
7.11 Archiving Analytical Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-27
Chapter 8: Maintenance Procedures
8.1 Routine Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1
8.2 Instrument Maintenance Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-2
8.3 Maintenance Schedule. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3
8.3.1 Attention Items . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3
8.3.2 Prior to Start Up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-3
8.3.3 At End of Day . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-4
8.3.4 Daily . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-4
8.3.5 Weekly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-4
8.3.6 Monthly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-5
8.3.7 Every 2 Months. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-5
8.3.8 Every 6 Months. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-5
8.3.9 Annually . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-5
8.4 Maintenance Procedures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6

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8.4.1 Powering OFF the Instrument Before Servicing . . . . . . . . . . . . . . . . 8-6
8.4.2 Prodigy7 Access Panels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-7
8.4.3 Front Access Panel Removal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-8
8.4.4 Camera Purge Gas Dehydrator Replacement . . . . . . . . . . . . . . . . . 8-9
8.4.5 Purge Gas Cylinders Replacement. . . . . . . . . . . . . . . . . . . . . . . . . 8-10
8.4.6 Plasma Viewing Windows - Removal, Cleaning and Replacement 8-11
8.4.7 Lubricating the Peristaltic Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-14
8.4.8 Cleaning the Spray Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-14
8.4.9 Cleaning the Nebulizer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-15
Concentric Nebulizer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-15
V-Groove Nebulizer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-15
Hildebrand Grid Nebulizer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-15
8.4.10 Cleaning Labware . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-17
8.4.11 Torch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-18
8.4.12 Changing Torch Injectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-18
8.4.13 Cleaning the Torch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-19
8.4.14 Autosampler Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-19
8.4.15 Camera Water Cooling System. . . . . . . . . . . . . . . . . . . . . . . . . . . 8-20
Camera Water Cooling System Fill Procedure . . . . . . . . . . . . . . . . 8-20
8.4.16 Water Recirculation System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-21
Water Recirculation System Water Change . . . . . . . . . . . . . . . . . . 8-21
Water Recirculation System Filter Cleaning and Replacement . . . 8-22
Water Recirculation System Backflush Procedure . . . . . . . . . . . . . 8-22
Water Recirculation System Chemical Wash . . . . . . . . . . . . . . . . . 8-24
8.4.17 Cleaning Air Filters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-24
8.4.18 Ventilation Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-25
8.5 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-25
8.5.1 Peristaltic Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-25
8.5.2 Plasma Ignition Issues . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-25
Plasma Will Not Ignite. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-25
Plasma Ignition Troubleshooting Checklist . . . . . . . . . . . . . . . . . . . 8-26
8.5.3 Check Standard Failures. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-26
8.5.4 Interlocks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-28
8.5.5 Camera Full Echellogram Shows Unusual Shapes in Continuum . 8-29
8.5.6 Instability (High RSDs) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-30
Sample Introduction System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-30
Nebulizer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-30
Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-30
Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-30
Leaks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-31
8.5.7 Chemistry and Labware . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-31
8.5.8 Water Recirculation System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-31
8.6 Diagnostics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-32
8.6.1 Installation Test Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-32
8.6.2 Autosampler Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-32
8.6.3 Resetting Source Mirror . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-32
8.7 Instrument Set-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-34
8.7.1 Installation Short Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-34
Internal Camera Chiller Startup Procedure. . . . . . . . . . . . . . . . . . . 8-35
On the Instrument Control Panel . . . . . . . . . . . . . . . . . . . . . . . . . . 8-36
8.7.2 Reducing Power and Gas Consumption . . . . . . . . . . . . . . . . . . . . . 8-37
8.7.3 Installation of the Cetac ASX500 Series Autosampler . . . . . . . . . . 8-40
SartUp.INI Parameters for Cetac ASX500 . . . . . . . . . . . . . . . . . . . 8-40
8.8 Teledyne Leeman Lab’s Contact Information . . . . . . . . . . . . . . . . . . . . . . 8-41
8.8.1 Teledyne Leeman Labs. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-41

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8.8.2 Sales. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-41
Representatives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-41
8.8.3 Technical Support. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-41
8.8.4 Replacement Parts and Consumables . . . . . . . . . . . . . . . . . . . . . . 8-41
8.8.5 Plasma-Pure Laboratories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-41
Appendix A: Advanced User Reference
A.1 Spectral Interferences . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1
A.1.1 Background Correction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1
A.1.2 Background Correction Types . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3
Simple Background Shift . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3
Sloping Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3
Curved Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-4
Complex Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-5
A.1.3 Spectral Overlap and Interfering Element Correction (IEC) . . . . . . . A-5
Partial And Direct Spectral Overlap . . . . . . . . . . . . . . . . . . . . . . . . . A-6
A.1.4 Interfering Element Correction (IEC) Factors . . . . . . . . . . . . . . . . . . A-7
Determine the Identity of the Interfering Element. . . . . . . . . . . . . . . A-7
Calculate the Interfering Element Correct Factor (IEC) . . . . . . . . . . A-7
A.1.5 IEC Practical Example . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-8
A.1.6 Interfering Element Corrections (IEC) . . . . . . . . . . . . . . . . . . . . . . A-11
How to Apply an IEC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-11
A.2 Matrix Interferences . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-12
A.2.1 Sample Introduction System Matrix Effects . . . . . . . . . . . . . . . . . . A-13
A.2.2 Plasma Matrix Effects. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-13
A.2.3 Determining if Matrix Effects are a Problem. . . . . . . . . . . . . . . . . . A-14
A.2.4 Coping with Matrix Effects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-16
Matrix Matching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-16
Method of Standard Addition (MSA). . . . . . . . . . . . . . . . . . . . . . . . A-16
A.2.5 Adding a Method of Standard Additions. . . . . . . . . . . . . . . . . . . . . A-18
A.2.6 Running MSA Additions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-19
A.2.7 Internal Standard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-21
A.3 Internal Standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-23
A.4 Import/Export of Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-24
A.4.1 Export a Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-24
A.4.2 Importing a Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-25
A.5 Database Manager . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-27
A.5.1 Archiving Databases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-27
A.5.2 Viewing Archived Databases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-30
A.5.3 Reusing a Database Archive . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-32
A.6 Synchronizing External Hardware to Sample Sequence . . . . . . . . . . . . . A-33
A.6.1 SampSync Special Characters or String Commands. . . . . . . . . . . A-34
A.7 Creating a Custom Line Library . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-35
A.8 Salsa Computation Mathematics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-38
A.8.1 Concentration of Unknown Sample Calculations . . . . . . . . . . . . . . A-38
A.8.2 Update Intercept and Update Slope Calculations . . . . . . . . . . . . . A-39
A.8.3 Internal Standard Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-39
A.8.4 IEC Calculations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-40
A.8.5 Duplicate Sample Calculations. . . . . . . . . . . . . . . . . . . . . . . . . . . . A-41
A.8.6 Spike Recovery and Percent Recovery Calculations . . . . . . . . . . . A-41
A.8.7 Concentration, Calibration, and Ratio Calculations . . . . . . . . . . . . A-42
A.8.8 Concentration Ratio Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . A-43
A.8.9 Concentration Ratios and Updates . . . . . . . . . . . . . . . . . . . . . . . . A-43
A.8.10 Concentration Ratios and Sample Calculations . . . . . . . . . . . . . . A-46
A.8.11 Calculation Sequence and Protocol . . . . . . . . . . . . . . . . . . . . . . . A-46

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A.9 Diagnostics. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-47
A.9.1 Motors Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-47
A.9.2 A/D Channels Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-48
A.9.3 Optics Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-48
A.9.4 Set Points . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-48

List of Figures
1-1 Prodigy7 schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
1-2 Twist-n-Lock system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
1-3 Prodigy7 optical system . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
1-4 CMOS Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
1-5 Salsa home screen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-4
1-6 Full frame feature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-6
1-7 Axial torch configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
1-8 Dual-view torch configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-7
1-9 Radial torch position . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-8
1-10 Cetac ASX-520, Hildebrand grid nebulizer, and cyclonic spray chamber 1-9
2-1 Peristaltic pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
2-2 Routing pump tubing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
2-3 Pump clamps contacting pump platens . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
2-4 Adjusting pump clamp tension . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
2-5 Axial torch mount . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
2-6 Loosen the torch lock lever. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
2-7 Twist the torch bayonet in a counter-clockwise direction . . . . . . . . . . . . . . 2-7
2-8 Rotate until the alignment pin disengages from the alignment slot . . . . . . 2-7
2-9 Withdraw the torch body from the mount . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
2-10 Radial torch mount . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-8
2-11 Loosen the torch lock lever. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-9
2-12 Twist the torch body in a counter-clockwise direction . . . . . . . . . . . . . . . 2-9
2-13 Rotate until the alignment pin disengages from the alignment slot . . . . 2-10
2-14 Withdraw the torch body from the mount . . . . . . . . . . . . . . . . . . . . . . . . 2-10
2-15 Axial torch box overview. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
2-16 Axial torch mount . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-12
2-17 Torch lock Lever . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-13
2-18 Torch body adjustment knob . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-13
2-19 Torch vernier scale . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-14
2-20 Dual-view mirror . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-14
2-21 Radial torch box overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
2-22 Radial torch mount . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
2-23 Mounting the cyclonic spray chamber on an axial system . . . . . . . . . . . 2-16
2-24 Mounting the cyclonic spray chamber on a radial system . . . . . . . . . . . 2-17
2-25 Salsa main screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-21
2-26 New method dialog. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-22
2-27 Element selection from the Periodic Table . . . . . . . . . . . . . . . . . . . . . . . 2-24
2-28 Setting the view for individual or all wavelengths . . . . . . . . . . . . . . . . . . 2-25
2-29 Setting analytical parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-26
2-30 Instrument control screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-27
2-31 Instrument interlocks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-28
2-32 Instrument control screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-29
2-33 Position plasma results for axial view. . . . . . . . . . . . . . . . . . . . . . . . . . . 2-30
2-34 Diagnostic display. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-32
2-35 Update Hg deltas message . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-33
2-36 Auto wavelength alignment dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-33

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2-37 Echellogram viewed in the align wavelength tab . . . . . . . . . . . . . . . . . . 2-35
2-38 Echellogram with too short of an exposure time . . . . . . . . . . . . . . . . . . 2-36
2-39 Echellogram with too long of an exposure time . . . . . . . . . . . . . . . . . . . 2-36
2-40 Alignment of a wavelength. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-37
2-41 Automatic wavelength alignment window . . . . . . . . . . . . . . . . . . . . . . . 2-39
2-42 Automatic wavelength alignment window . . . . . . . . . . . . . . . . . . . . . . . 2-40
2-43 Automatic wavelength alignment (dX and/or dY values 3 or higher) . . . 2-40
2-44 Calibration standards screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-41
2-45 Adding calibration standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-42
2-46 Adding calibration standards - “blank” standard lines added . . . . . . . . . 2-42
2-47 Adding calibration standards - adding standard 1 . . . . . . . . . . . . . . . . . 2-43
2-48 Modify standard dialog. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-44
2-49 Run standard dialog. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-44
2-50 QC Automation window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-46
2-51 Calibration curve display . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-46
2-52 Add QC window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-48
2-53 Modify standard dialog. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-49
2-54 Run a QC dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-50
2-55 QC Automation screen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-51
2-56 Run a sample dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-52
2-57 Sequence overview window. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-53
2-58 Building sequences . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-55
2-59 Sequence prompt. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-56
2-60 Data recalculation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-58
2-61 Reporting data with replicate and statistical information . . . . . . . . . . . . 2-60
3-1 Element selection screen. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-3
3-2 Wavelength scan screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
3-3 Run standard dialog. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4
3-4 Run a sample dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5
3-5 Scans tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6
3-6 Wavelength scan window illustrating shifted ROI . . . . . . . . . . . . . . . . . . . 3-7
3-7 Thumbnail profile display . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8
3-8 Selecting scans for estimating concentrations. . . . . . . . . . . . . . . . . . . . . 3-10
3-9 Estimating concentrations using the selected wavelength scans . . . . . . 3-11
4-1 Salsa main screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
4-2 Login prompt . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
4-3 Menu bar (with method tab selected). . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-3
4-4 Instrument control bar (left side) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
4-5 Instrument control bar (right side) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
4-6 Scheduled maintenance dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-7
4-7 Application tabs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8
4-8 Status panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9
5-1 Home screen with method tab selected. . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
5-2 New method dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2
5-3 Open method dialog. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-3
5-4 Instrument control screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
5-5 Autosampler control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
5-6 Instrument diagnostics dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
5-7 Instrument control screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
5-8 Optimize sample intro dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
5-9 Plasma auto start flowchart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
5-10 Plasma controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-9
5-11 Pump controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-10
5-12 View control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11
5-13 Torch gas control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-11

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5-14 Element selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-12
5-15 Method tree . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-13
5-16 General tab containing wavelength information . . . . . . . . . . . . . . . . . . . 5-14
5-17 Wavelength view selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-15
5-18 Calibration tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-16
5-19 Aligning wavelength tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-17
5-20 Mercury lamp alignment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-18
5-21 The mercury (Hg Ref) lamp aligned and accepted. . . . . . . . . . . . . . . . . 5-19
5-22 Newly aligned wavelengths aligned and accepted . . . . . . . . . . . . . . . . . 5-19
5-23 Adding a calibration standard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-20
5-24 Entering calibration standard concentrations . . . . . . . . . . . . . . . . . . . . . 5-21
5-25 Modifying standard dialog. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-21
5-26 Multiple updates in a method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-22
5-27 Specifying update frequencies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-23
5-28 Using cup macros for updates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-23
5-29 Display update data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-24
5-30 Running a specific replicate for a calibration standard . . . . . . . . . . . . . . 5-24
5-31 Setting the base element for concentration ratio . . . . . . . . . . . . . . . . . . 5-25
5-32 Calibration curve using concentration ratio . . . . . . . . . . . . . . . . . . . . . . 5-26
5-33 Viewing quality control standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-26
5-34 Setting up extra volumes for QC standards . . . . . . . . . . . . . . . . . . . . . . 5-28
5-35 QC Automation screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-29
5-36 Automatic assignment of QC standard locations . . . . . . . . . . . . . . . . . . 5-29
5-37 Custom assignment of QC standard locations . . . . . . . . . . . . . . . . . . . . 5-30
5-38 Custom QC standard locations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-30
5-39 Example of mismatch shared QC standard error message . . . . . . . . . . 5-31
5-40 Post calibration action . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-32
5-41 Analytical parameter screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-33
5-42 Sample uptake timer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-33
5-43 Method data summary screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-34
5-44 New method dialog - semiquant . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-35
5-45 Running a semiquant update standard. . . . . . . . . . . . . . . . . . . . . . . . . . 5-36
5-46 Calculating semiquant ratios . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-36
6-1 Sequence tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1
6-2 Rack edit tools . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
6-3 Weight and volume corrections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3
6-4 Sequence tree . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
6-5 Autosampler rack map . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-4
6-6 Sample sequence “locked in” . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5
6-7 Additional sample added to sequence . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-5
6-8 QC Standard locations set in two methods . . . . . . . . . . . . . . . . . . . . . . . . 6-6
6-9 Standard or QC mismatch error message . . . . . . . . . . . . . . . . . . . . . . . . . 6-6
6-10 Select the first sequence method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-7
6-11 Select set sequence method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-7
6-12 Select the second method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-8
6-13 Second method standards and QCs added to rack map . . . . . . . . . . . . . 6-8
6-14 Samples added for the first method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-9
6-15 Samples added for the second method . . . . . . . . . . . . . . . . . . . . . . . . . 6-10
6-16 Setting the extinguish plasma option . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-10
6-17 Using cup macros. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-12
6-18 Using the “CP” cup marco command . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-13
7-1 Analysis tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
7-2 Results tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2
7-3 Hidden items. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3
7-4 Renaming samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3

Table of Contents
TOC - 10
Prodigy7 User Manual
7-5 Sample renaming history - traceable renaming structures . . . . . . . . . . . . 7-4
7-6 “Single” display tab results. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
7-7 “All” display tab results. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5
7-8 Sample search results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6
7-9 Overlaying wavelength scans . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-7
7-10 Thumbnail wavelength scan profile . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-8
7-11 Raw subarray data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-9
7-12 Example of full frame image . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-10
7-13 Selecting a full frame for QA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-12
7-14 QA probability report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-12
7-15 Control chart data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-14
7-16 Report criteria . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-14
7-17 Report control menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-16
7-18 Selecting the report type . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-17
7-19 Changing the report precision mode . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-18
7-20 Scientific notation mode. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-18
7-21 Blank subtraction set-up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19
7-22 Format 1 report example . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-20
7-23 Printed example of format 1 report data . . . . . . . . . . . . . . . . . . . . . . . . 7-20
7-24 Format 2 report data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-21
7-25 Printed example of format 2 report data . . . . . . . . . . . . . . . . . . . . . . . . 7-21
7-26 Report spec options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-22
7-27 Creating a quick report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-23
7-28 Starting sequence reporting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-23
7-29 Open sequence reporting method dialog. . . . . . . . . . . . . . . . . . . . . . . . 7-24
7-30 Sequence reporting mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-24
7-31 Report generated using sequence reports. . . . . . . . . . . . . . . . . . . . . . . 7-25
7-32 Sequence reporting error message . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-25
7-33 Recalculation tab . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-26
7-34 Run full frame image dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-27
8-1 Shutting off the main power breaker . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
8-2 Unplug power cord from wall . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-6
8-3 Prodigy7 front. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-7
8-4 Prodigy7 left side . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-7
8-5 Front panel removal sequence . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-8
8-6 Locating the gas dehydrator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-9
8-7 Window cassette . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-11
8-8 Window cassette removal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-12
8-9 Torch cassette o-rings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-12
8-10 Unscrew torch cap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-18
8-11 Withdraw torch injector tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-18
8-12 Remove the injector tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-19
8-13 Camera water cooling reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-20
8-14 Air filter location . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-24
8-15 Ice crystal on detector chip . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-29
8-16 Peak source dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-33
8-17 Reset mirror message . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-33
8-18 Camera water cooling reservoir . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-35
8-19 Instrument control panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-36
A-1 A) Illustration of the concept of net signals . . . . . . . . . . . . . . . . . . . . . . . . A-2
A-2 B) Illustration of the concepts of matrix-induced background shift . . . . . . A-2
A-3 Simple background shift . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3
A-4 Sloping background. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-4
A-5 Curved background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-4
A-6 Complex background. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-5

Table of Contents
TOC - 11
Prodigy7 User Manual
A-7 Spectral scans for pure Zn, mixed Zn and Ni and pure Ni solutions . . . . . A-6
A-8 Formula 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-7
A-9 Formula 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-8
A-10 IEC Practical example - setting up an IEC correction . . . . . . . . . . . . . . . A-8
A-11 IEC Practical example - running an IEC standard . . . . . . . . . . . . . . . . . . A-9
A-12 IEC Practical example - using IECs in a method . . . . . . . . . . . . . . . . . . A-10
A-13 Selecting an interfering element. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-11
A-14 Running an IEC standard. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-12
A-15 Adding a spiked QC for spike recovery analysis . . . . . . . . . . . . . . . . . . A-14
A-16 Sequence recovery commands . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-15
A-17 Method of standard addition calibration plot . . . . . . . . . . . . . . . . . . . . . A-16
A-18 Sample placement for method of standard additions. . . . . . . . . . . . . . . A-18
A-19 Selecting the MSA mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-19
A-20 Running an MSA sample manually . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-20
A-21 MAS results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-20
A-22 Displaying an MSA calibration curve . . . . . . . . . . . . . . . . . . . . . . . . . . . A-21
A-23 Assigning internal standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-22
A-24 Assigning internal standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-23
A-25 Export method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-24
A-26 Method export “save as” . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-25
A-27 Import method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-25
A-28 Import method dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-26
A-29 Open method dialog. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-26
A-30 Import method error display . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-27
A-31 Open database manager . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-28
A-32 Database manager. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-28
A-33 Delete full frame images prompt . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-28
A-34 Open database archive dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-29
A-35 Comparison of analysis tree before and after archiving. . . . . . . . . . . . . A-29
A-36 Open database manager . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-30
A-37 Database manager. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-30
A-38 Open archive dialog . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-31
A-39 Database in archive view . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-31
A-40 Open database manager . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-32
A-41 Database manager. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-32
A-42 Using sampsync. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-33
A-43 Instrument diagnostics screen . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-47

List of Tables
1-1 Hazard Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-3
1-1 Prodigy 7 Site Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
1-2 Prodigy7 System Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
2-1 Sample Introduction Optimization Recommendations . . . . . . . . . . . . . . . 2-19
2-2 Recommended Analytical Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-26
2-3 Calibration Values . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-47
2-4 Data Reporting Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-59
3-1 Recommended Peaking Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13
3-2 Plasma Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-13
3-3 Recommended Plasma Parameters for Aqueous Samples . . . . . . . . . . . 3-14
3-4 Recommended RF Power by Sample Type . . . . . . . . . . . . . . . . . . . . . . . 3-14
3-5 Recommended Nebulizer Pressure by Sample Type. . . . . . . . . . . . . . . . 3-15
3-6 Recommended Coolant Flow by Sample Type . . . . . . . . . . . . . . . . . . . . 3-16
3-7 Recommended Auxiliary Flow by Sample Type . . . . . . . . . . . . . . . . . . . . 3-16

Table of Contents
TOC - 12
Prodigy7 User Manual
3-8 Recommended Sample Uptake Rates. . . . . . . . . . . . . . . . . . . . . . . . . . . 3-17
4-1 Privilege Levels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
6-1 Cup Macro Commands . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11
7-1 Control Chart Button Functions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-13
7-2 Report Data Selection Button . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-15
7-3 Report/Output Button Functions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19
7-4 Recalculate Button Functions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-25
8-1 Maintenance Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-2
8-2 Recommended Nebulizer Cleaning Procedures . . . . . . . . . . . . . . . . . . . 8-16
8-3 Plasma Ignition Troubleshooting Checklist . . . . . . . . . . . . . . . . . . . . . . . 8-26
8-4 Interlock Diagnosis and Corrective Action . . . . . . . . . . . . . . . . . . . . . . . . 8-28
8-5 Leak Points . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-31
8-6 Instrument Inspection. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-34
8-7 Power Consumption Settings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-38
8-8 Gas Consumption Settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-39
8-9 Cetac ASX500 Series Autosampler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-40
A-1 Cup Macro Codes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-15
A-2 Wavelength for Library Fit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-35

Table of Contents
TOC - 13
Prodigy7 User Manual
Table of Contents
TOC - 14
Prodigy7 User Manual
Prodigy7 ICP
Safety

General Warnings
Before installing, operating, or maintaining this equipment, it is imperative that all
hazards and preventive measures are fully understood. While specific hazards may vary
according to location and application, take heed of the following general warnings:

WARNING
Liquids associated with this instrument may be classified as carcinogenic,
biohazard, flammable, or radioactive. Should these liquids be used, it is
highly recommended that this application be accomplished in an isolated
environment designed for these types of materials in accordance with
federal, state, and local regulatory laws, and in compliance with your
company’s chemical/hygiene plan in the event of a spill.

WARNING
Eviter de répandre des liquides dangereux. Les liquides qui sont analysés
dans cet instrument peuvent être cancérigènes, hasards biologiques,
inflammables, ou radioactifs. Si vous devez utiliser tels liquides, il est très
recommandé que vous le faites à l'intérieur d'un environnement isolé
conçu pour tels liquides. Cet environnement isolé devrait être construit
selon les règlements fédéraux, provinciaux, et locaux, aussi que le plan de
votre compagnie qui concerne l'évènement d'un accident avec les
matières hasardeuses.

WARNING
Avoid hazardous practices! If you use this instrument in any way not
specified in this manual, the protection provided by the instrument may
be impaired.

WARNING
Éviter les usages périlleux! Si vous utilisez cet instrument d’une manière
autre que celles qui sont specifiées dans ce manuel, la protection fournie
de l’instrument peut être affaiblie; cela augmentera votre risque de
blessure.
WARNING
If this system uses flammable organic solvents, Teledyne Leeman Labs
recommends that you place this system in a well-ventilated environment,
designed for these types of materials. This environment should be
constructed in accordance with federal, state, and local regulations. It
should also comply with your organization’s plan concerning chemical and
hygiene mishaps. In all cases use good laboratory practices and standard
safety procedures.

WARNING
Ce système peut utiliser des dissolvants organiques inflammables. Pour
réduire le péril qui peut être causé par l'accumulation des vapeurs
explosives, Teledyne Leeman Labs recommande que vous installez ce
système dans un environnement bien-aéré qui est conçu pour les matières
hasardeuses. Cet environnement devrait être construit selon les
règlements fédéraux, provinciaux, et locaux. Aussi, il devrait se conformer
au plan de votre organisation qui concerne les mésaventures de l'hygiène
ou de chimique. En tout cas, utilisez toujours de pratiques bonnes de la
laboratoire et des procédures standardes de la sûreté.
Notations and Hazard Severity Levels
This manual uses Notations and Hazard Severity Levels to emphasize information that is
important for instrument functionality and user and instrument safety. The four levels:

NOTE
Note is used for information and descriptions to ensure correct usage to
prevent damage of the instrument.

Caution

Cautions identify a potential hazard, which if not avoided, may result in minor
or moderate injury. This category can also warn you of unsafe practices, or
conditions that may cause property damage.

WARNING
Warnings identify a potentially hazardous condition, which if not avoided,
could result in death or serious injury.

DANGER
DANGER – limited to the most extreme situations to identify
an imminent hazard, which if not avoided, will result in death
or serious injury.
Prodigy7 ICP Safety Labels
The Prodigy7 ICP is labeled to meet with safety standards of CE compliance. The
following signal words contained in this chapter are used in the manual and on
instrument labels.
The equipment and this manual use symbols to warn of hazards. The symbols are
explained below.

Table 1-1 Hazard Symbols


Warnings and Cautions
The exclamation symbol alerts the user to important instructions in the
instrument’s user manual.

The lightning flash symbol indicates “dangerous voltage” inside the


product.

The extreme heat warning symbol indicates a part or component that


may be heated to high temperature and result in burns to skin, clothing,
and other materials.

The UV light symbol represents a part or component that gives off


Ultraviolet Light and could cause harm to vision.

The eye protection symbol indicates a procedure requiring that the


instrument user wear eye protection to prevent harm to eyes.

The electrical chassis ground symbol indicates that the instrument


component is connected to an electrical ground.

Symboles de sécurité
Ce symbole signale l’existence d’instructions importantes relatives au
produit dans ce manuel.

Ce symbole signale la présence d’un danger d’électocution.

Warnungen und Vorsichtshinweise


Das Ausrufezeichen in Dreieck ist ein Warnzeichen, das Sie darauf
aufmerksam macht, daß wichtige Anleitungen zu diesem Handbuch
gehören.

Der gepfeilte Blitz im Dreieck ist ein Warnzeichen, das Sei vor “gefährli-
chen Spannungen” im Inneren des Produkts warnt.
Table 1-1 Hazard Symbols (Continued)
Advertencias y Precauciones
Esta señal le advierte sobre la importancia de las instrucciones del man-
ual que acompañan a este producto.

Esta señal alerta sobre la presencia de alto voltaje en el interior del


producto.
Prodigy7 User Manual
Chapter 1: Introduction
1.1 Prodigy7 Overview
The Prodigy7 comprises the most sophisticated solid-state detection ICP-OES system
ever developed and is a complete solution for elemental analysis. This system is capable
of wide dynamic range, low detection limits, excellent wavelength resolution, long term
stability, and true simultaneous measurement of all important elemental lines. The
Prodigy7 ICP covers wavelengths from 165-1100 nm. This includes the cesium 894 nm
line which is 60 times more sensitive than previously found lines on any ICP-OES.
The Prodigy7 is the synthesis of advanced technology and user simplicity. The
summation of years of refinement, the Prodigy7 has distinct advantages over other ICPs:
 Twist-n-Lock, Auto-Aligning Sample Introduction System
 High-Energy, High-Performance Optical System
 Full wavelength coverage from 165 nm - 1100 nm
 500 mm, Low Stray Light Optics (0.007 nm resolution @200 nm)
 Large format, advanced CMOS Array Detector for true simultaneous
measurement
 Simple to use Salsa Software
 Full Spectral Access (FSA) that captures the entire wavelength spectrum in a
single reading
 Compact benchtop design
 Fast system startup and reduced gas consumption
 Axial, Radial, and Dual-View configurations

1.1.1 Site Requirements

Table 1-1 Prodigy 7 Site Requirements


Length 48.0 in (1220 mm)
Depth 27 in (682 mm)
Height 27.5 in (698 mm)
Weight 231 lbs (105 Kg)
Shipping Weight 445 lb (202 Kg)
Electrical Grounded Singe-Phase Power Supply 190-230 V, 30 A, 50/60 Hz
Exhaust Venting 100 ft3/min (2.83 m3/min)

1-1
Figure 1-1 Prodigy7 schematic

1.1.2 System Specifications

Table 1-2 Prodigy7 System Specifications


Optical Design High-Energy Echelle Polychromator Detector Type CMOS
Focal Length 500 mm Size 28 mm x 28 mm
Dispersion 0.1 nm/mm @ 200 nm Number of Pixels 3.38 million (1840 x 1840)
Optical Resolution 0.007 nm @ 200 nm Pixel Size 15 µm
Pixel Resolution 0.0015 nm@ 200 nm Active Area 100%
Wavelength Range 165 - 1100 nm Standard Measurement Mode Simultaneous

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1.2 Twist-n-Lock, Auto-Aligning Sample Introduction System
The Prodigy7’s Twist-n-Lock sample introduction system ensures consistent and
reproducible high-quality results. By designing the torch mount to twist and lock into
place, leak-proof gas connections are automatically made and the torch is returned
precisely to its optimum position. Fine-tuning of the torch position can be made while
the plasma is running simplifying optimization of the sample introduction system.

Figure 1-2 Twist-n-Lock system

1.3 High-Energy, High-Performance Optical System


The Prodigy7’s high-energy, high-resolution Optical System complements its advanced
CMOS Detector. The small internal volume reduces on purge gas consumption
(1 L/min), while still providing the widest wavelength range of any ICP system available.
With a focal length of 500 mm it provides a resolution of 0.007 nm @ 200 nm, and affords
exceptional flexibility in wavelength selection. Because the entire Optical System is
maintained at a constant temperature, its alignment has exceptional, long-term stability.

Figure 1-3 Prodigy7 optical system

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1.4 CMOS Detector
The cutting edge solid-state detector is designed specifically for ICP-OES, and exclusive
only to the Prodigy7 ICP. The largest in the industry (28 mm 2 ) and containing 3.38
million pixels, the CMOS Detector is capable of capturing the entire ICP spectrum in a
single exposure, at a speed 10x faster than older, less advanced devices. All of which
means greater linearity, and the ability to determine the concentration of any element
within a single full-frame acquisition. The CMOS Detector’s unparalleled capabilities
make it the new standard for ICP-OES.
The challenge in creating any ICP method is choosing the proper wavelengths. The
combination of Prodigy7’s broad wavelength range and powerful CMOS camera with
Full Spectral Access (FSA), allows wavelengths to be selected quickly without trial and
error.

Figure 1-4 CMOS Detector

1.5 Salsa Software

Figure 1-5 Salsa home screen

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1.5.1 Overview

The Salsa software is designed around the four components of ICP analysis:
1. Select a method
2. Prepare the Sequence (Place samples into the autosampler)
3. Start the Sequence) (Analyze the samples)
4. Report the data
These components are mirrored in Salsa’s three primary tabs:
 A METHOD TAB for development of the analytical method
 A SEQUENCE TAB for building the automated series of analytical events
 An ANALYSIS TAB for the resulting data

1.5.2 Common Tasks

The following common tasks are easily accomplished in the Prodigy7’s Salsa software.
Refer to Chapter 2: "Standard Operating Procedures" for more information on
conducting the following:
 Create an analytical Method as well as convenient access to saved Methods
 Add, modify and delete Standards in the Method
 Set Analytical Parameters
 Position the Plasma
 Align the Spectrometer
 Align Wavelengths
 Collect Wavelength Spectra
 Run a Calibration
 Add Quality Control Checks
 Build Sequences
 Analyze Samples
 Review, report, and export results

1.5.3 Advanced Tasks

Salsa is fully capable of conducting the following advanced tasks in a logical,


straightforward manner. Refer to Chapter 5: "Method", Chapter 6: "Sequence", and
Chapter 7: "Analysis" for more information on accomplishing the following:
 Create a unique method tailored to specific analytical requirements
 Fine tune an existing method to achieve superior analysis results for a
challenging sample type
 Perform a highly detailed review of results for a specific sample or series of
samples
 Take advantage of the Full Spectral Access (FSA) capability to determine the
concentration of components not targeted in the original analysis

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1.5.4 Quantitative Full Frame Feature

The Prodigy7 offers the operator the unprecedented capability to immediately


determine the concentration of any element in a sample without having the element in a
method itself. This is only possible with the new, high speed CMOS detector.

Figure 1-6 Full frame feature

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1.6 View Configurations

1.6.1 Axial View

Axial and dual-view instruments consists of a RF load coil oriented horizontally. The
torch body is placed horizontally through the center of the load coil by installing the
torch body from the right with a clockwise rotation into position (Figure 1-7).

Figure 1-7 Axial torch configuration

1.6.2 Dual-View

Dual-view systems have a radial mirror mounted to the side of the air knife spacer
(Figure 1-8).

Figure 1-8 Dual-view torch configuration

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1.6.3 Radial View

Sample introduction for radial view instruments consists of a RF load coil oriented
vertically. The torch body is placed vertically through the center of the load coil by
installing the torch body from the bottom with a clockwise rotation into position as
shown in Figure 1-9.

Figure 1-9 Radial torch position

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1.7 Accessories
Teledyne Leeman Labs offers a full range accessories and consumables for the Prodigy7
including CETAC autosamplers, application specific nebulizers, spray chambers and
specialized torch assemblies. Refer to the Teledyne Leeman Lab’s website
(www.teledyneleemanlabs.com) for more information on consumables, spare parts and
accessories.

Figure 1-10 Cetac ASX-520, Hildebrand grid nebulizer, and cyclonic spray
chamber

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Chapter 2: Standard Operating Procedures

NOTE
For information on setting up the Prodigy7, refer to Section 8.7.1 "Installation
Short Procedure".

NOTE
For information on setting up the CETAC ASX500 series autosampler, refer to
Section 8.7.3 "Installation of the Cetac ASX500 Series Autosampler".

The objective of this chapter is to enable an operator who possesses a basic


understanding of analysis by ICP a convenient resource for familiarizing themselves
with the Prodigy7 and its Salsa software. This chapter explains how to:
 Set-up and adjust the Sample Introduction System
 Mix standards
 Salsa software overview
 Create an analytical Method
 Add, modify and delete standards in the Method
 Set analytical parameters
 Ignite and position the plasma
 Align the Spectrometer
 Align wavelengths
 Collect wavelength spectra
 Run a calibration
 Add quality control checks
 Build sequences
 Analyze samples
 Review and report results
The Prodigy7 is available in radial, axial, or dual-view torch configuration and may be
operated with and without an autosampler. Configuration and procedural differences
dependant upon the torch configuration and autosampler are noted, and references will
be made to each specific configuration exception, when necessary.

2-1
2.1 Sample Introduction System
The sample introduction system transports the liquid sample to be analyzed to the
plasma. Along the way it is converted from a liquid with dissolved metals into gaseous
atoms and ions. The Sample introduction System consists of:
 Peristaltic Pump and tubing
 Spray Chamber
 Nebulizer
 Torch
 Torch Body (inclusive of torch)

2.1.1 Sample Introduction and Sample Types

Select the type of sample introduction suited to the sample type to be analyzed. Typical
sample introduction setups are:
 Aqueous (usually in acids)
 Aqueous with high dissolved solids (i.e. lithium borate fusions, sea water,
soils)
 Organic (i.e. wear metals in oils, edible oils, kerosene solubilized, xylene
solubilized)
 Hydrofluoric acid (i.e. mineralogy, ceramic, glasses)

2.1.2 Peristaltic Pump

The peristaltic pump conducts samples to the instrument and waste to the drain. the
peristaltic pump consists of:
1. Rotating Cylinder
2. Pump Platens
3. Clamps
4. Tubing

Figure 2-1 Peristaltic pump

Pump Platens

Pump Clamps

Rotating Cylinder

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Different types of tubing can be used on the peristaltic pump according to the type of
analysis. Each type of tubing is a different polymer compound that is conducive to the
liquid matrix of the application. Refer to the Teledyne Leeman Lab’s website
(www.teledyneleemanlabs.com) for more information on consumables, spare parts and
accessories.

Set-Up and Adjustment


1. Route the uptake and drain tubing neatly up and over the cylinder and in-line with
the pump platens. The pump rotates in a counter-clockwise rotation and conducts
the flow of liquid in the same direction (Figure 2-2).

Figure 2-2 Routing pump tubing

2. Once the tubing is routed, lower the pump platens so that they press down onto
the tubing (Figure 2-2).
3. Swivel the pump clamps so they contact the pump platens (Figure 2-3).

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Figure 2-3 Pump clamps contacting pump platens

4. Gradually tighten the pump clamp by turning the adjustment knob located at the
end of the clamp (Figure 2-4).
The tendency, when adjusting the pump, is to quickly crank down the tension until
there is uptake and drain. This will usually result in too much pressure leading to
reduced tubing life and poor precision in the data. Be patient and adjust the pump
clamp tension in small increments.

NOTE
Pump flow and nebulizer stability is the most common cause of instability in
results.

5. To ensure that the sample flow and drain are smooth and consistent, lift the
sample tip out of the rinse solution, then place it back in. By creating an air pocket,
the bubble can be followed up the length of the tubing. “Hitching”, or hesitation in
the bubble, indicates that the clamp tension requires adjustment.

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Figure 2-4 Adjusting pump clamp tension

6. Once smooth uptake and drainage have been achieved, wait 15 to 20 minutes and
check both again. During this time, the tubing will be worked by the rollers and it
will be more flexible. It will also stretch, changing the diameter of the tubing.

NOTE
When using new tubing, allow the peristaltic pump to run solution through
the tubing then adjust the pressure on the pump platens as needed, before
igniting the plasma.

7. When rechecking the uptake, it may be necessary to increase or decrease the


tension by 1/4 turn on the pump clamps to maintain a steady flow after the tubing
has been broken in.

NOTE
Occasionally check the sample uptake (black/black) and drain (red/red) tubing
for tears or excess wear and replace if needed. Operating with excessively
worn tubing may produce leaking which can damage the pump.

2.1.3 Torch - Installation and Removal

The Prodigy7’s Twist-n-Lock Auto-Aligning Sample Introduction System allows the


operator to obtain consistent, high-quality results by retaining its settings if removed.
Additionally, the twist-n-lock system permits fine-tuning of the torch position while the
plasma is running.

NOTE
The Prodigy7’s is designed for demountable “hybrid” torches. Usage of hybrid
torches can significantly reduce argon gas consumption.

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The Torch mount is designed to twist and lock into place simplifying torch installation
and removal. Once locked into position the mount makes leak-proof gas connections
and returns the torch precisely to its optimum position. Twist-n-lock functionality is
detailed for axial and radial configurations below.

Axial and Dual-View Systems

Figure 2-5 Axial torch mount

Torch Lock Lever Torch Adjustment


Knob

Torch Bayonet
Alignment Pin
Vernier Scale
Ball Joint

To use the axial and dual-view twist-n-lock system:


1. Loosen the torch lock lever by rotating it counter-clockwise (Figure 2-6).

Figure 2-6 Loosen the torch lock lever

2. With the torch lock lever loose, rotate the torch bayonet in a counter-clockwise
direction, disengaging the alignment pin (Figure 2-7).

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Figure 2-7 Twist the torch bayonet in a counter-clockwise direction

3. Continue rotating the torch bayonet until the alignment pin is out of the alignment
slot (Figure 2-8).

Figure 2-8 Rotate until the alignment pin disengages from the alignment slot

4. With the alignment pin disengaged from the slot, withdraw the torch bayonet
(Figure 2-9).

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Figure 2-9 Withdraw the torch body from the mount

5. Reverse the procedure for installation.

NOTE
For information on adjusting the torch refer to Section 2.1.4 "Torch
Adjustment". For procedures on disassembling the torch from the torch
bayonet refer to Section 8.4.11 "Torch".

Radial Systems
The radial twist-n-lock torch mount is similar in functionality to the axial and dual-view
twist-n-lock system.

Figure 2-10 Radial torch mount

Torch Adjustment
Knob

Torch Lock Lever


Vernier Scale
Alignment Pin

Torch Bayonet
Ball Joint

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To use the radial twist-n-lock system:
1. Loosen the torch lock lever by rotating it counter-clockwise (Figure 2-11).

Figure 2-11 Loosen the torch lock lever

2. With the torch lock lever loose, rotate the torch bayonet in a counter-clockwise
direction, disengaging the alignment pin (Figure 2-12).

Figure 2-12 Twist the torch body in a counter-clockwise direction

3. Continue rotating the torch bayonet until the alignment pin is out of the alignment
slot (Figure 2-13).

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Figure 2-13 Rotate until the alignment pin disengages from the alignment slot

4. With the alignment pin disengaged from the slot, withdraw the torch bayonet
(Figure 2-14).

Figure 2-14 Withdraw the torch body from the mount

5. Reverse the procedure for installation.

NOTE
For information on adjusting the torch refer to Section 2.1.4 "Torch
Adjustment". For procedures on disassembling the torch from the torch
bayonet refer to Section 8.4.11 "Torch".

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NOTE
Maintenance procedures for removing the torch, cleaning the torch and
changing torch injectors are located in Chapter 8: "Maintenance Procedures".

Torch Selection
The Prodigy7 uses the same torch design for radial, axial, and dual-view configurations.
Torch selection is typically based on the application. Torches are available in HF
resistant design for samples containing hydrofluoric acid. Refer to the Teledyne Leeman
Lab’s website (www.teledyneleemanlabs.com) for more information on consumables,
spare parts and accessories.

NOTE
Refer to Section 8.4.11 "Torch" for information on changing the Torch.

Torch Injector Selection


Torch injector selection is typically based on the application. The narrower the injector
bore the faster the aerosol travels through the plasma. The general rule is to use large
bore for aqueous samples and narrow bores for organics. Refer to the Teledyne Leeman
Lab’s website (www.teledyneleemanlabs.com) for more information on consumables,
spare parts and accessories.

NOTE
Refer to Section 8.4.12 "Changing Torch Injectors" for information on changing
Torch Injectors.

Torch Position
Torch position can optimize conditions based on the user’s goal. If the best precision is
required, the torch should have the injector placed near to the plasma. A starting
position of approximately 3 mm away from the load coil is good for alkalis and “soft”
lines.
If the lowest detection limits are needed for hard lines, such as, Arsenic (As) and
Selenium (Se) the torch injector should be placed farther away from the load coil. A
starting position of approximately 6 mm is a good starting point. This position may
cause a flickering plasma; however, the plasma instability is “shot noise” and is easily
averaged by longer integration times of 20 seconds or more.

NOTE
At ~6 mm the torch is further away from the plasma and aerosol is increased.
Positioning the torch ~6 mm or greater from the plasma may cause plasma
blowout.

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2.1.4 Torch Adjustment

Axial and Dual-View Torch Adjustment

Figure 2-15 Axial torch box overview

Torch

RF Load Coil Torch Injector Tube

Figure 2-16 Axial torch mount

Torch Lock Lever Torch Adjustment


Knob

Torch Bayonet
Alignment Pin
Vernier Scale
Ball Joint

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The torch body can be moved in and out of the load coil via the torch adjustment knob
and lock lever. To adjust the torch body:
1. Release the lock lever by turning counter-clockwise (when viewed from the top)
(Figure 2-17).

Figure 2-17 Torch lock Lever

2. Use the torch body adjustment knob to change the position of the torch
(Figure 2-18).

Figure 2-18 Torch body adjustment knob

NOTE
The torch is typically set to approximately 2 mm from zero measured on the
vernier scale (Figure 2-19).

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Figure 2-19 Torch vernier scale

3. Once the torch is properly adjusted, lock it into position by turning the lock lever
clockwise (Figure 2-17).

NOTE
If the end of the torch is too close to the air knife, the torch will overheat and
will shorten its useful life. When the air knife is in position, the purge tube
should be moved to the right until it is flush with the left edge of the air knife.

Dual-View Mirror Positioning

Figure 2-20 Dual-view mirror

Torch

Torch Injector Tube

RF Load Coil

Dual-View Mirror

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Dual-view systems have a radial mirror mounted to the side of the air knife spacer
(Figure 2-20). The mirror can be moved to the right (toward the torch) or slightly left
(toward the air knife) by loosening a small thumbscrew on the arm of the mirror. The
mirror positioned near the middle of its range of travel is generally sufficient.

Radial System Torch Adjustment

Figure 2-21 Radial torch box overview

RF Load Coil Torch

Torch Injector Tube

Figure 2-22 Radial torch mount

Torch Adjustment
Knob

Torch Lock Lever


Vernier Scale
Alignment Pin

Torch Bayonet
Ball Joint

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Radial torch configurations are adjusted in a similar manner as axial and dual-view
systems with the exception that the adjustment knob and lock lever are located beneath
the torch box. Refer to "Axial and Dual-View Torch Adjustment".

2.1.5 Spray Chamber

NOTE
For spray chamber maintenance procedures refer to Section 8.4.8 "Cleaning
the Spray Chamber" in Chapter 8: "Maintenance Procedures".

Spray Chamber Selection


Spray chamber selection can be used to optimize precision and detection limits. Spray
chambers should be chosen according to the sample type and nebulizer used. Refer to
the Teledyne Leeman Lab’s website (www.teledyneleemanlabs.com) for more
information on consumables, spare parts and accessories.

Installing and Adjusting the Spray Chamber

Axial and The spray chamber is mounted to the right of the torch with a ball joint connection
Dual-View (Figure 2-16) to allow liquid to drain from the spray chamber and aerosol to travel up
Systems through the top of the spray chamber to the torch. A close-up view of a glass cyclonic
spray chamber properly mounted to an axial torch is illustrated in the Figure 2-23.

NOTE
The spray chamber should be fitted with the desired nebulizer prior to
securing it to the torch. If the nebulizer needs to be adjusted, it should be
adjusted prior to installing it into the spray chamber.

Figure 2-23 Mounting the cyclonic spray chamber on an axial system

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The cyclonic spray chamber is light enough to mount onto the end of the torch without
supporting hardware; however, heavier spray chambers (such as the HF resistant spray
chamber) require the use of appropriate hardware to provide support and relieve the
strain on the torch stem.

Radial Systems The spray chamber is mounted below the torch with a ball joint connection
(Figure 2-22)to allow liquid to drain from the spray chamber and to allow the aerosol to
travel vertically to the torch. A glass cyclonic spray chamber properly mounted to a
radial torch is shown in Figure 2-24.

NOTE
The spray chamber should be fitted with the desired nebulizer prior to
securing it to the torch. If the nebulizer needs to be adjusted, it should be
adjusted prior to installing it into the spray chamber.

Figure 2-24 Mounting the cyclonic spray chamber on a radial system

2.1.6 Nebulizer

NOTE
For nebulizer maintenance procedures refer to Section 8.4.9 "Cleaning the
Nebulizer" in Chapter 8: "Maintenance Procedures".

Nebulizer Selection
Nebulizers should be chosen according to the sample type and spray chamber used.
Refer to the Teledyne Leeman Lab’s website (www.teledyneleemanlabs.com) for more
information on consumables, spare parts and accessories.

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Installing and Adjusting the Nebulizer
Nebulizer adjustment varies according to the type of nebulizer.

NOTE
Pump flow and nebulizer stability is the most common cause of instability in
results.

NOTE
The nebulizer should be adjusted prior to installing it into the spray chamber.

Concentric Typically, the primary adjustment of the concentric nebulizer is depth when used in
Nebulizer combination with a cyclonic spray chamber. In this case, the nebulizer tip should extend
into the circular section of the spray chamber so that it will be cleaned by the circling gas
stream. It is usually best to simply push the nebulizer all the way into the o-ring mount
of the spray chamber.

V-Groove The V-groove nebulizer does not require any adjustment.


Nebulizer

Hildebrand Grid The spacing between the two Pt-Ir screens of the Hildebrand nebulizer is critical. Rotate
Nebulizer the cap until a fine mist results. The Prodigy7 ICP is less susceptible to inaccurate
(HGN) adjustment of the nebulizer, because longer integration times are used as compared
those used with a PMT based ICP (such as the Teledyne Leeman Lab’s Profile).
To achieve optimal performance and analytical reliability of data, adjusting the HGN to
obtain a consistent flow is essential to successful analysis. The Hildebrand Grid
Nebulizer (HGN) flow is affected by:
1. Pump rate.
2. Nebulizer pressure (adjusted changing the distance between the two platinum
screens).
Optimizing Without Plasma – Proper adjustment should achieve a smooth, continuous
flow through the nebulizer. To optimize the nebulizer:
1. Increase or decrease the pump rate in 5 rpm increments, and observe the
nebulizer spray pattern.
 Droplets or excess liquid forming at the end cap, represent too much
sample flow.
 When the spray is too fine or thin, the sample flow is too low.
2. If adjusting the flow rate has no effect, adjust the nebulizer pressure:
 Up if droplets occur.
 Down if mist is too fine.
Optimizing in Plasma – To optimize the nebulizer in the plasma,
1. Run multiple fast (1 second) integrations on a high standard (~10 ppm).
2. With the ANALYSIS TAB active, select the RESULTS TAB.
3. Click the STATISTICS BUTTON.

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4. To modify the pump rate and nebulizer pressure, make the METHOD TAB active and
then select INSTRUMENT CONTROL in the NAVIGATION PANEL. Repeat the adjustments
until a good precision in data is obtained (<1-2%).

2.1.7 Optimizing the Sample Introduction System

Sample introduction optimization is best performed by using the SAMPLE INTRODUCTION


OPTIMIZER. For more information on the SAMPLE INTRODUCTION OPTIMIZER refer to Section
5.4.3 "Optimize Sample Introduction". Operate optimization with the plasma ON and
running a high standard (~10ppm).
1. With the METHOD TAB active, select INSTRUMENT CONTROL in the NAVIGATION PANEL.
2. Click the OPTIMIZE SAMPLE INTRO BUTTON.
3. Select a line from the method and click START.
4. The software will begin reading the selected line and calculating various metrics
for optimization.
5. While observing the selected metric (i.e. precision, or detection limit) adjust the
instrument conditions. Make adjustments in the following sequence:
1. Pump flow rate.
2. Nebulizer pressure (this will optimize the nebulizer).

Sample Introduction Optimization by Sample Type


Suggestions for optimizing the sample introduction system according to sample type are
given in theTable 2-1 "Sample Introduction Optimization Recommendations".

Table 2-1 Sample Introduction Optimization Recommendations


Sample Type Recommended for Optimization
Aqueous Applications The auxiliary flow is not always needed. A larger bore injector
attains better detection limits of VUV lines.
Organic Applications Auxiliary is necessary to avoid carbon buildup near the injector. A
smaller bore injector is recommended to achieve a higher velocity
through the plasma.
Alkalis Increase the nebulizer pressure. A smaller bore injector bore may
improve results.
“Hard” Lines Lower nebulizer pressure and increasing the pump flow rate.
Increase RF powera.
Very “Hard” Lines Increase RF power.
(phosphorus, and
aluminum 167 nm)
For Improved Alkali Decrease RF powerb
Detection Limits
For Precision Increase nebulizer pressure
For Lower Detection Limits Lower nebulizer pressure and increasing the pump flow rate.
Increase RF power.
Plasma Stability Increase Coolant Flowc
a. Increased RF power also improves desolvation of the aerosol and promotes stability. Increased RF
power reduces the life of the torch. The coolant flow should be increased with increased RF power.
b. Decreased RF power increases torch life.
c. Increased coolant flows pull the plasma back toward the injector. This may require the use of an
auxiliary gas flow to push the plasma away from the injector.

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2.2 Mix Standards
To make standards for use with this tutorial, use a 100 ppm QC Soup as a stock solution.
Make a calibration blank and 3 standards containing 0, 1, 5 and 10 ppm of the elements
in the QC Soup solution. Make all standards in a 2% nitric acid matrix. If an autosampler
is to be used, fill the rinse reservoir with 2% nitric acid.

NOTE
If the semiquant option is to be used (selected on the New Method Dialog),
the standards should be made in two solutions: Set 1 (34 elements) and Set 2
(36 elements). For pre-made standards refer to the Teledyne Leeman Lab’s
website (www.teledyneleemanlabs.com) for more information on
consumables, spare parts and accessories.

NOTE
The SemiQuant check box (selected on the New Method Dialog) configures a
method as a semi-quantitative analysis method. A semi-quantitative method
includes the best wavelengths for each of 70 elements and an estimated
calibration curve based on Teledyne Leeman Lab’s semi-quantitative
standards. For pre-made standards refer to the Teledyne Leeman Lab’s website
(www.teledyneleemanlabs.com) for more information on consumables, spare
parts and accessories.

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2.3 Salsa Overview
Refer to Section 4.1 "Startup Login"for information on logging in to the Salsa software.
When the software is started, the HOME screen is displayed:

Figure 2-25 Salsa main screen

The Salsa main screen contains:


1. A MENU BAR with drop-down menus that provide access to all application
functions in Salsa.
2. A TOOL BAR containing buttons that provide access to commonly used functions.
3. An INSTRUMENT CONDITIONS BAR where the current instrument control parameters
(power, coolant flow, nebulizer flow, pump flow, etc.) are displayed.
4. A NAVIGATION PANEL that contains features or selections relating to the application
tab selected (METHOD, SEQUENCE, or ANALYSIS). Information in the NAVIGATION
PANEL is organized in a tree structure according to the application tab selected
(METHOD TREE, SEQUENCE TREE, ANALYSIS TREE). Make selections in the NAVIGATION
PANEL by highlighting, or placing a check mark in the box to the left of each item
(depending upon the function). Selecting an item in the NAVIGATION PANEL will add
it to the DISPLAY PANEL.
5. APPLICATION TABS which allow the user to navigate between application areas
(METHOD, SEQUENCE and ANALYSIS).
6. A DISPLAY PANEL which actively displays the feature or item selected in the
NAVIGATION PANEL.
7. A STATUS BAR which displays text in the lower left of the screen to indicate the
operation currently being performed.

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2.3.1 Salsa Application Tabs

The Salsa program has three main application areas:


 The METHOD TAB provides access to all functions related to method
development and application. This includes: creating methods, opening and
using pre-existing methods to perform routine analytical tasks, and modifying
existing methods to meet new application requirements.
 The SEQUENCE TAB provides tools to define an analysis sequence. This
SEQUENCE TAB can include blanks, standards, check solutions and samples, and
allows the solutions to be analyzed using an autosampler or manually with
appropriate prompts.
 The ANALYSIS TAB provides access to all functions related to processing and
reporting data. These functions include: displaying data (both numerically and
graphically), recalculating data (if necessary), generating reports and printing
results.
In depth information on the Salsa software including screens, tabs, buttons, and use of
the application areas can be found in Chapter 4: "Salsa Software Overview".

2.4 Create an Analytical Method


This section will illustrate the steps necessary to create and use a method. For more
detailed information on method development refer to Chapter 3: "Method
Development" in the manual.

2.4.1 Method Setup

Axial or Radial View


1. With the METHOD TAB active, select METHOD>NEW from the MENU BAR. The NEW
METHOD DIALOG will appear (Figure 2-26).

Figure 2-26 New method dialog

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2. Type “Tutorial” into the text box under METHOD name field and type the current
date into the text box under ANALYSIS CHAPTER NAME. Type any comments in the
METHOD NOTES if desired. Leave the SEMIQUANT check box at the bottom of the
window unchecked.

NOTE
The SemiQuant check box configures a method as a semi-quantitative analysis
method. A semi-quantitative method includes the best wavelengths for each
of 70 elements and an estimated calibration curve based on Teledyne Leeman
Lab’s semi-quantitative standards. Refer to Section 2.2 "Mix Standards" for
information on the standards used with semi-quantitative analysis.

3. Click OK and a new method named “Tutorial” will be created.

Entering Elements and Wavelengths


1. When the new method has been created, the method name appears at the top of
the NAVIGATION PANEL. A small box with a “+” appears to the left of the method
name to indicate that the METHOD TREE is minimized. Click on the box to expand
the tree.
2. Select ELEMENT SELECTION in the NAVIGATION PANEL to display the PERIODIC TABLE OF
ELEMENTS.
3. On the PERIODIC TABLE, click “Cu” in the PERIODIC TABLE. When this element is
selected, information appears in the AVAILABLE LINES and INTERFERENTS TABLES at
the top of the window (Figure 2-27).
The table on the left contains five columns of information:
 The first column is unlabeled and contains asterisks to indicate the
preferred order in which wavelengths should be added to a method.
Wavelengths with asterisks are the most preferred.
 The second column contains copper wavelengths from the line library.
 The third column contains the atomic species (“I” represents an atomic
state and “II” represents an ionic state).
 The fourth and fifth columns contain the signal-to-background ratio and
alignment status for each wavelength, respectively.

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Figure 2-27 Element selection from the Periodic Table

4. Highlight the 324.754 wavelength and note that the INTERFERENTS TABLE now
contains spectral information for nearby interfering elements. The INTERFERENTS
TABLE is illustrated as a bar graph spanning the area beneath the AVAILABLE LINES
and INTERFERENTS TABLES. The pink-colored bar represents the wavelength
highlighted in the AVAILABLE LINES TABLE. All other bars represent the nearby
interfering elements in the INTERFERENTS TABLE.
5. Click the ADD LINE BUTTON to add this wavelength to the method.

NOTE
Double-clicking on the Add Line Button, with an element selected, will
automatically add the preferred line for a particular element without the need
to highlight the desired line.

6. The added wavelength will appear under ELEMENT SELECTION in the NAVIGATION
PANEL.
7. Similarly, add a wavelength for each of the following elements from the PERIODIC
TABLE: As, Ba, Fe, Mn and Zn. For each element, select the wavelength with two
stars to add the “most preferred” wavelength to the method.

NOTE
If the user wishes to select a wavelength that is not listed in the Preferred List
of wavelengths, all wavelengths in the line library can be accessed by selecting
the All Lines Button at the bottom right corner of the window.

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For Dual-View Wavelengths are added to a method in axial view by default. If the radial view is
Instruments preferred, highlight the wavelength of interest and select the RADIAL BUTTON under the
GENERAL TAB. If the user wishes to change the view for all wavelengths in the method,
highlight any wavelength in the NAVIGATION PANEL, hold down the Shift key and select
the RADIAL BUTTON. All wavelengths can be changed back to the axial view position in a
similar manner.

NOTE
For a dual-view instrument, add 2 wavelengths for Ba and 2 wavelengths for Fe
to the method. Choose a sensitive Ba wavelength (i.e., high S/B ratio) and set
the view to radial. Choose a Ba wavelength with less sensitivity (i.e. low S/B
ratio) and keep the view for this wavelength axial. For Fe, add the most
preferred Fe wavelength twice (this should be the 259.940 nm wavelength)
and set one of the 259.940 nm wavelengths to the radial view.

For Radial and Wavelength selections will be added to the method according to the view of the
Axial View instrument.
Instruments

Figure 2-28 Setting the view for individual or all wavelengths

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2.5 Setting Analytical Parameters
1. With the METHOD TAB active, select ANALYTICAL PARAMETERS in the NAVIGATION PANEL
to set the analytical parameters (integration time, number of integrations, uptake
and rinse times, etc.) for sample analysis.

NOTE
If the instrument is dual-view, there will be text boxes to set both the axial and
radial integration times.

2. Type the values shown in Table 2-2 "Recommended Analytical Parameters" into
the respective text boxes on the ANALYTICAL PARAMETERS SCREEN according to the
instrument configuration.

Table 2-2 Recommended Analytical Parameters


Inst. Integration Pump Computationa
Config Axial Radial Integrations Uptake Rinse Use Wt. Use Vol.
Axial 60 sec - 1 60 sec 40 sec Select Select
Radial - 10 sec 1 60 sec 40 sec Select Select
Dual 60 sec 10 sec 1 60 sec 40 sec Select Select
a. Checking the “Use Weight and Volume” option, regardless of whether it will be employed, allows
the user the flexibility of using (or not using) weight and volume correction factors.

3. The ANALYTICAL PARAMETERS SCREEN should now look similar to the one illustrated
in Figure 2-29.

Figure 2-29 Setting analytical parameters

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2.6 Igniting the Plasma

NOTE
It is recommended to give the plasma sufficient time to warm up. Under
general operating conditions provide 10-20 minutes for the plasma to
stabilize.

NOTE
For plasma ignition issues, refer to Section 8.5 "Troubleshooting".

2.6.1 Plasma Manual Ignition

For information on igniting the plasma manually, refer to Section 5.4.4 "Plasma
Controls".

2.6.2 Plasma Auto Start

The Prodigy7 plasma can be ignited manually or automatically. Automatic plasma


ignition is recommend. For the sequence of events taking place during the auto start
sequence refer to Section 5.4.4 "Plasma Controls".
1. With the METHOD TAB active, select INSTRUMENT CONTROL in the NAVIGATION PANEL
(Figure 2-30).

Figure 2-30 Instrument control screen

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2. If not already ON, turn ON the ICP exhaust vent and external water recirculator.
3. Make sure the sample introduction system (torch, spray chamber, and nebulizer)
is properly assembled.
4. Make sure that the pump platens and clamps have secured the pump tubing and
are properly adjusted.

NOTE
Refer to Section 2.1 "Sample Introduction System" for information on
adjusting the Sample Introduction System.

5. Check the INTERLOCK BUTTON. Refer to Section 8.5.4 "Interlocks" for information on
resolving interlocks issues.

NOTE
With the exception of the Air knife interlock, all interlock errors must be
satisfied before the plasma can be lit. The Air Knife interlock will automatically
clear when the Plasma Startup Button is clicked.

Figure 2-31 Instrument interlocks

6. Make sure the instrument conditions (RF power, coolant flow, nebulizer pressure,
pump flow, etc.) are set appropriately and click the AUTO START Button. As the auto
start sequence proceeds, the status of the air knife, torch gases, RF power, igniter,
and peristaltic pump will change.
7. While the plasma is warming up, continue with the following sections.

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2.7 Position the Plasma (Peak Source)
Before the calibration can be started, the source mirror needs to be positioned to collect
the maximum light emission from the plasma for each view (axial and radial) used
during sample analysis. The position plasma or PEAK SOURCE feature does this by
scanning the plasma, both horizontally and vertically, while a solution is aspirated into
the plasma. Perform the procedures below according to your instrument’s plasma view
configuration. A histogram similar to those depicted verifies a successful positioning of
the source mirror has been accomplished.

NOTE
Differences in numerical intensity in the upper right-hand corner of the
histogram window will occur from instrument to instrument, and do not
reflect a failure in positioning the source mirror.

Begin with the general procedure for positioning the plasma below and then continue to
the appropriate section according to instrument configuration.
1. With the METHOD TAB active, select INSTRUMENT CONTROL in the NAVIGATION PANEL
(Figure 2-32).

Figure 2-32 Instrument control screen

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2. Place the sipper probe in Standard 3 (a solution containing the necessary
positioning element or elements.

NOTE
If the autosampler is being used, place the “Standard 3” solution in a cup in the
standards rack on the autosampler and move the autosampler probe to that
cup. Do this by selecting the appropriate rack and cup locations at the bottom
left-hand section of the window. Under Move Tip, click the Cup Button to
initiate the movement of the probe. Wait until the solution has reached the
plasma. For more information on configuring the autosampler refer to Section
5.4.1 "Autosampler Controls".

3. Click the PEAK SOURCE BUTTON, located in the SPECTROMETER section of the
INSTRUMENT CONTROL SCREEN. A window labeled POSITION SOURCE will appear.
Follow the appropriate section below according to instrument configuration.

2.7.1 Axial View

1. Select the wavelength to be used to optimize the plasma view from the PEAKING
LINE MENU. Mn 257.610 nm is often used to position the plasma in view; however,
the user can select another wavelength if desired. For purposes of example, choose
the Mn 257.610 nm wavelength from the PEAKING LINE MENU.
2. Click the PEAK SOURCE BUTTON and the positioning routine begins.
3. Once completed, the resulting purple histogram should have a pattern similar to
the one displayed below.

Figure 2-33 Position plasma results for axial view

2.7.2 Radial View

1. Select a radial wavelength (indicated by an “r”) from the PEAKING LINE MENU to
position the plasma for the radial view. For purposes of example, choose the Fe
259.940r wavelength.
2. Click the PEAK PLASMA BUTTON and the positioning routine begins.

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2.8 Align the Spectrometer
The spectrometer line library is based on the Mercury Hg 253.652 nm line as a reference
position on the camera. Small deviations from a perfect alignment can be corrected by
realigning to this reference wavelength. When changes are made to this wavelength, the
offsets are applied globally to all wavelengths in the line library. The Prodigy7 has an
onboard Mercury (Hg) lamp that produces the Hg 253.652 nm line to which the
spectrometer is aligned.
The alignment is performed upon installation and can be corrected throughout the life
of the instrument. Small corrections may be made every week to improve the accuracy
of wavelength alignment. Parameters that affect spectral movement are temperature
and flow rate of the purge gas. It is important to keep the same purge flow rate whenever
checking the reference alignment.
There are two methods available for aligning the spectrometer. The manual method is
typically reserved for extreme cases where the automatic method does not work. The
automatic method is almost always the method of preference.

2.8.1 Manual Alignment Method

1. Add the Hg 253.652 nm wavelength to the current method or open a method in


which Hg 253.652 nm has already been added. With the METHOD TAB active, look at
the Hg wavelength under ELEMENT SELECTION and make sure the Hg 253.652 nm
wavelength has an “m” to the right of it to indicate that data for this wavelength will
be collected using the Hg lamp. If no “m” appears, highlight this wavelength and
click on the GENERAL TAB. Select the HG LAMP BUTTON under TORCH VIEW and an
“m” will appear to the right of the wavelength.
2. With the METHOD TAB active, select INSTRUMENT CONTROL in the NAVIGATION PANEL.
3. Click the DIAGNOSTICS BUTTON and the resulting window will appear (Figure 2-34).
The DIAGNOSTICS DISPLAY provides access to several features and functions within
Salsa including:
 Manual control of the source mirror motors
 Manual control of the autosampler probe
 Control of the offsets applied to the Hg reference wavelength
 Control over the “optimal” source mirror position for each view available
on the instrument
 Ability to turn the camera’s TE cooler ON and OFF
 Real-time view of several instrument hardware parameters (temperatures
of the optics tank, camera, and water recirculating through the camera,
purge gas flow rate inside the optics tank, the purge gas flow through the
camera, etc.).

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Figure 2-34 Diagnostic display

4. To reset the offset values for the Hg reference wavelength, type “0” into each of the
text boxes labeled X and Y in the top right-hand portion of the window labeled
OPTICS.
5. Click OK.
6. A message will be displayed: “Opening Method Lines updating from Library.” Click
OK. This will reset the theoretical location of the Hg 253.653 nm wavelength.
7. Click the CLOSE BUTTON at the bottom of the DIAGNOSTICS DISPLAY.
On the I NSTR UMENT C ONTROL S CREEN , select the H G L AMP B UTTON under
SPECTROMETER>VIEW SECTION.

8. Click on the FULL SPECTRUM BUTTON to obtain an echellogram of the Hg


lamp. Set the exposure time to 0.05 seconds and deselect the boxes for UPTAKE TIME
and for the EXTENDED RANGE. Name the echellogram something useful such as “Hg
0.05 s” and click OK to acquire the echellogram.
9. When the echellogram has been acquired, highlight the Hg 253.652 wavelength
under ELEMENT SELECTION and click on the ALIGN WAVELENGTH TAB. Select the top
image from the ECHELLE IMAGES TABLE and the image will appear in the display
window.
10. Click the AUTO BUTTON on the upper right-hand side of the window.
11. Once the subarray has moved, an ACCEPT BUTTON will appear on the right-hand
side of the window. Click ACCEPT.
12. When the ACCEPT BUTTON is clicked, a message will appear to indicate that the Hg
peaking line array cannot be moved and Delta X and Delta Y values will be
provided. Click YES to accept the improved Hg 253.652 wavelength position on the
camera (Figure 2-35).

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Figure 2-35 Update Hg deltas message

NOTE
If the X and Y offset values exceed 15 pixels, contact Teledyne Leeman Lab’s
Customer Support. Refer to Section 8.8 "Teledyne Leeman Lab’s Contact
Information".

2.8.2 Auto Alignment Method

1. Open any existing method.

2. Click the AUTO ALIGN BUTTON.


3. An AUTO WAVELENGTH ALIGNMENT window similar to the one depicted in Figure
2-36 will appear. The Hg Ref line appears on the wavelength list as Hg Ref. Make
sure this is checked in the left column.

Figure 2-36 Auto wavelength alignment dialog

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4. Click the AUTO ALIGN BUTTON. The software will automatically align the Hg 253.653
nm line labeled “Hg Ref.”
5. When the alignment is complete, an ACCEPT BUTTON will appear under the AUTO
ALIGN BUTTON. Click ACCEPT, then click the CLOSE BUTTON.
6. A prompt dialog may appear asking to accept the “Opening Method lines Updating
from Library”. Click OK.
For more information on aligning to the Hg 253.653 wavelength and aligning element
wavelengths thereafter, refer to Section 5.5.5 "Align Wavelength Tab". To create a custom
line library refer to Section A.7 "Creating a Custom Line Library".

2.9 Align Wavelengths


When a wavelength is added to a method, the spectrometer uses information in the
system Line Library to predict the location of the wavelength on the detector. The
location will vary from instrument to instrument and newly selected lines should be
aligned before use. If a wavelength is being aligned for the first time, it should be done by
following Section 2.9.1 "Manual Alignment Method". Previously aligned wavelengths
can be aligned using either the manual alignment method in Section 2.9.1 "Manual
Alignment Method"or the auto alignment method in Section 2.9.2 "Auto Alignment
Method".

2.9.1 Manual Alignment Method

1. Aspirate a solution containing the element(s) to be aligned. Solutions used for


alignment should contain relatively high concentrations of each element (10 ppm
or higher) to ensure that each wavelength is properly aligned.

2. Click the acquire FULL SPECTRUM BUTTON to obtain an echellogram.


3. Type an appropriate name in the text box labeled SAMPLE TITLE.
4. Type an appropriate exposure time in the text box labeled EXPOSURE TIME
(a 1 second exposure is recommended). The 40 SEC. UPTAKE and EXTENDED RANGE
will be checked by default. These options are defined below:
 The 40 Second Uptake time is a delay period that allows the sample to
equilibrate (before the reading commences) after traveling from the sample
filter tip, through the pump tubing and spray chamber, and into the
plasma.

NOTE
A normal uptake time is approximately 30-45 seconds.

NOTE
If an autosampler is not in use, the uptake time must also be long enough to
ensure equilibration of the Sample Introduction System. When manual
readings are selected, the operator can override the uptake time by clicking
the uptake time check box in the Run Full Frame Image Dialog.

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 The Extended Range feature takes a few more seconds to acquire an
echellogram and is used for generating an image with more dynamic range.
This makes it easier to see visible emission lines (which tend to be very
strong) in the same image with UV emission lines (which tend to be
significantly weaker in intensity).
5. If either of these options is not desired, deselect the option and click OK. Wait for
the exposure to be completed.
6. With the METHOD TAB active, highlight one of the wavelengths to be aligned in the
NAVIGATION PANEL. Select the ALIGN WAVELENGTH TAB and select the top image from
the ECHELLE IMAGES TABLE.

Figure 2-37 Echellogram viewed in the align wavelength tab

An example echellogram is illustrated above in Figure 2-24. The image contains a blue 3 x 29
pixel subarray with short, light blue lines to indicate the positions of background correction
points and the peak region of interest. This subarray is represented in a histogram at the
bottom of the window, where blue boxes represent left and right background correction points
(each 2 pixels in width) and a green box represents the peak region of interest (5 pixels in
width). The left and right background correction points are at pixel positions 2 & 3 and 27 & 28,
respectively, and the peak region of interest is at pixel positions 13 through 17.

NOTE
The default subarray is 3 pixels in height and 29 pixels in width. The height can
be changed to 1, 3, 5, and 7 pixels and the width may be changed to 29 or 57
pixels using radio buttons on the upper left side of the Align Wavelength Tab.
A 3 x 29 pixel size is suitable for most analytical methods, however, some
applications may require the analysis of many wavelengths in a highly
challenging matrix. Altering the size of the subarray provides more flexibility in
the choice of wavelengths used and in the placement of background
correction points.

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7. If the exposure time was not chosen correctly, the resulting echellograms will look
like those illustrated in Figure 2-38 and Figure 2-39.
a. If the echellogram looks like that in Figure 2-38, a new echellogram needs to be
taken with a longer exposure time (30-60 sec).
b. If the echellogram looks like that in Figure 2-39, a shorter exposure time
(0.01-0.1 sec) needs to be chosen.

Figure 2-38 Echellogram with too short of an exposure time

Figure 2-39 Echellogram with too long of an exposure time

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8. To align the subarray, click the AUTO BUTTON on the upper right side of the window.
If the wavelength is out of alignment, the subarray should move to position itself as
shown in Figure 2-40. If the subarray does not move to the correct (aligned)
position, click the CANCEL BUTTON and use the arrow buttons on the right side of
the ALIGN WAVELENGTH TAB to move the subarray to the desired location. These
arrow buttons can be used at any time to move the subarray manually.

NOTE
Use extreme caution when doing wavelength alignments with multi-element
solutions. Multiple elements may emit light at similar locations on the detector
leading to the possible alignment of subarrays on the wrong wavelengths. If
the alignment of the subarray is in doubt, take echellograms of single-element
solutions to perform the alignment.

Figure 2-40 Alignment of a wavelength

9. Once the subarray is aligned, click the ACCEPT BUTTON to accept the change.

NOTE
The Accept and Cancel Buttons only appear if the subarray has moved.

10. Repeat the steps above for all analytical wavelengths that require alignment. If
multiple echellograms have been acquired using different exposure times, choose
the most appropriate echellogram when aligning each wavelength.

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2.9.2 Auto Alignment Method

1. Aspirate a solution containing the element(s) to be aligned. Solutions used for


alignment should contain relatively high concentrations of each element (10 ppm
or higher) to ensure that each wavelength is properly aligned.
2. Click the AUTO ALIGN BUTTON .

3. An AUTO WAVELENGTH ALIGNMENT DIALOG will open (Figure 2-36). The Hg Ref line
appears on the wavelength list as Hg Ref and should be checked.

NOTE
Ensure the Hg Ref line is checked in the left column.

4. Click the AUTO ALIGN BUTTON. The software will automatically align the Hg 253.653
nm line labeled “Hg Ref.”
5. When the alignment is complete, an ACCEPT BUTTON will appear under the AUTO
ALIGN BUTTON. Click the ACCEPT button and all other wavelengths in the window
will no longer be grayed out.
6. Place a check mark beside each wavelength to be aligned. If all wavelengths are to
be aligned, click the CHECK ALL BUTTON.
7. Click the AUTO ALIGN BUTTON and wait for the software to automatically align the
element lines that are checked off in the left column.
8. When the alignment is complete, the table will fill with appropriate dX, dY and
time values, and an ACCEPT BUTTON will appear under the AUTO ALIGN BUTTON
(Figure 2-41).

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Figure 2-41 Automatic wavelength alignment window

9. The values in the dX and dY columns indicate how far each subarray will need to
be moved for alignment, and the time column indicates the exposure time for each
echellogram.
 If the auto alignment results produce dX and/or dY values of 3 or less, the
result will be written in blue text (Figure 2-42).
 If the auto alignment results produce dX and/or dY values of 3 or higher, the
result will be written in red text (Figure 2-43). If the suggested movement of
the subarray movement is this large, this line should not be accepted and
the wavelength should be manually aligned.
 A “U” to the left of the wavelength indicates that the alignment has not
been accepted (Figure 2-42). To view the image on the detector for any
specific wavelength, highlight that wavelength. The image will appear in
the small box at the bottom of the window.
 A “?” to the left of one of the wavelength indicates a significant amount of
light reached the detector despite using the shortest possible exposure
time. This is often the case with wavelengths having very strong emission
signals. If the highlighted image looks similar to that in Figure 2-42, and the
dX and dY values are each relatively small (less than 3), the alignment for
that wavelength should be accepted. Alternatively, the user may opt to
leave the wavelength unaccepted and perform a manual alignment once
the auto alignment has been performed for all other wavelengths.

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Figure 2-42 Automatic wavelength alignment window

Figure 2-43 Automatic wavelength alignment (dX and/or dY values 3 or higher)

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10. Once the ACCEPT button has been clicked, a dialog window may appear to inform
the user that the software is “Opening Lines Updating from Library”. Click the OK
button. This updates the wavelengths in the line library.
11. Click CLOSE to exit the AUTO WAVELENGTH ALIGNMENT DIALOG.

2.10 Collect Wavelength Spectra


Collecting and examining wavelength scans is an important part of method
development. These scans will illustrate potential interferences and are indispensable
when determining how many background correction points to use, where to place the
background correction point(s) and how many pixels in width each background
correction point should be. Scans should be collected for the blank, a representative
calibration standard, and representative samples. If all the samples to be analyzed are
similar in matrix and elemental composition, only one sample needs to be scanned.
Refer to Section 3.2.2 "Collect Wavelength Spectra" for information on collecting
wavelength spectra.

2.11 Calibration

2.11.1 Add Calibration Standards

Some applications may require that the instrument be calibrated over different
concentration ranges for different elements. The Salsa software allows the user to add
multi-element standards to a method in which elements can be present at widely
different concentrations.
1. With the METHOD TAB active, select STANDARDS/MSA in the NAVIGATION PANEL. The
DISPLAY PANEL should look similar to Figure 2-44 below, except that the STANDARD
NAME box should be empty.

Figure 2-44 Calibration standards screen

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2. Click the ADD STANDARD BUTTON and the ADD STANDARD DIALOG will appear:

Figure 2-45 Adding calibration standards

3. Type “Blank” in the text box labeled STANDARD NAME, “0.0” in the text box labeled
CONCENTRATION and “ppm” in the text box labeled SET UNITS. Under UPDATE TYPE,
the NOT AN UPDATE BUTTON will remain selected. Click OK to add this standard.

NOTE
If this standard is to be used to update the calibration intercept values, the
Intercept Button should be selected.

4. The STANDARD LINES TABLE on the right will automatically be populated with all the
analytical wavelengths at the concentration of 0 ppm as shown in Figure 2-46.

Figure 2-46 Adding calibration standards - “blank” standard lines added

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5. Once again, use the ADD STANDARD BUTTON again to add Standard 1 with a
concentration of 1.0 ppm as shown in Figure 2-47.

Figure 2-47 Adding calibration standards - adding standard 1

6. Similarly add Standard 2 with a concentration of 5.0 ppm, and Standard 3 with a
concentration of 10.0 ppm.
7. To set the number of integrations to be used for analyzing standards, select the
number of integrations from the NUMBER OF INTEGRATIONS MENU. Choose between
1 and 5 integrations (3 integrations is recommended). For more information on
running standards refer to Section 2.11.4 "Run Calibration Standards".

2.11.2 Modify Calibration Standards

Modify the Standard Concentration and Unit of Concentration


1. Highlight the standard in the STANDARD NAME TABLE (Figure 2-44).
2. Click the MODIFY STANDARD BUTTON.
3. Make any necessary changes in the MODIFY STANDARD DIALOG (Figure 2-48).
4. Click OK.
5. Changes will be reflected in the STANDARD LINES TABLE on the right.

NOTE
Element concentrations in the Standard Lines Table should reflect the
concentrations present in the standard solution used.

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Figure 2-48 Modify standard dialog

Change the Standard Lines


1. Highlight the standard in the STANDARD NAME TABLE (Figure 2-44).
2. In the STANDARD LINES TABLE select/deselect the standard lines included in that
standard.
3. Click the MODIFY STANDARD BUTTON to display the MODIFY STANDARD DIALOG
(Figure 2-48).
4. Click OK.

2.11.3 Delete a Calibration Standard

1. Highlight the standard in the STANDARD NAME TABLE (Figure 2-44).


2. Click the DELETE STANDARD BUTTON.

2.11.4 Run Calibration Standards

Without an Autosampler
1. Place the sipper probe in the blank solution.

2. Click on the RUN STANDARD BUTTON to display the RUN STANDARD DIALOG
(Figure 2-49).

Figure 2-49 Run standard dialog

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 Select “Blank” from the STANDARD ID MENU.
 Select three integrations under INTEGRATION NUMBER by
selecting/deselecting each integration.
 If the solution has reached the plasma, deselect the UPTAKE TIME option. If it
has not reached the plasma, leave the box checked and click OK.
3. Once the analysis is complete, put the autosampler probe in the rinse solution and
let the instrument rinse for 30-60 seconds.
4. Repeat the steps above for all remaining standards in the method.

With Autosampler
If an autosampler is being used for calibration, all calibration curves will automatically
be accepted with a linear fit type by default. If the user wishes to have failure criteria for
the calibration curves, the following actions must be taken:
1. In the calibration display window, type a number into the text box labeled
MINIMUM RHO (sequences) to indicate the minimum Rho value that must be met
for the calibration curve to be accepted. Minimum Rho values can be added to
each wavelength individually or the same minimum Rho value can be added to all
the wavelengths in the method by clicking the SET ALL BUTTON
2. Select QC AUTOMATION in the NAVIGATION PANEL and place a check mark beside the
blank and each calibration standard to be used for generating the calibration
curve.
3. The last standard checked will have the default Action as “Continue.” in the ACTION
column. Click in this text box to display the drop-down list of failure actions:
 Stop on failure
 Recalibrate & Rerun on failure
 Prompt on failure
4. Choose the failure action desired.

NOTE
When running a calibration with an autosampler, the only acceptance criteria
available for a calibration curve is meeting a minimum Rho value. If there are
concerns about the precision or the accuracy of calibration data, the user
should consider running the calibration standards manually or should select
the “Pause” failure action which will pause the sequence after calibration and
allow the user to examine the calibration curves before any samples or check
standards are analyzed.

5. Place the blank and standard solutions into appropriate places in the standards
rack.
6. With the METHOD TAB active select QC AUTOMATION.
7. Place a check mark beside the blank and each calibration standards to be used for
generating the calibration curve. Leave the default action item as CONTINUE. The
QC AUTOMATION window will look similar to Figure 2-50.

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Figure 2-50 QC Automation window

8. With the SEQUENCE TAB active, click the RUN SEQUENCE BUTTON.
For more detailed information on the use of an autosampler to run calibration and
sample sequences, refer to Chapter 6: "Sequence".

2.11.5 Reviewing the Calibration Data

1. With the METHOD TAB active, highlight one of the wavelengths listed under
ELEMENT SELECTION in the NAVIGATION PANEL.
2. Click the CALIBRATION TAB and examine the calibration data in the DISPLAY PANEL.
An example calibration curve is shown in Figure 2-51.

Figure 2-51 Calibration curve display

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3. Examine the calibration curve for each wavelength to determine whether the data
is acceptable to proceed with sample analysis. When examining calibration data
and choosing the fit type, pay close attention to the “Calc” values, the “%RSD”
values and the “Rho” value. Table 2-3 "Calibration Values" explains what each
value indicates.

Table 2-3 Calibration Values


Value Meaning
Conc These values represent the concentration of each Standard.
Calc These values indicate the calculated concentration of each stan-
dard, based on the measured intensities and the fit type chosen.
Ideally, the “Calc” values will be very close to the “Conc” values
Dev The deviation from the actual concentration. The deviation is the
Calc minus the Conc.
Mean The mean intensity based on the average of the replicate readings.
SD or %RSD These values indicate the precision with which each standard was
measured. Poor precision (i.e. high %RSD values), might indicate
problems with the analysis that should be addressed prior to ana-
lyzing samples (memory effects, uptake time is too short, nebu-
lizer is slowly clogging over the course of 3 replicate
measurements, etc.)
Rho These values indicate the correlation coefficient of the calibration
fit. A Rho value of 1.0 indicates a perfect fit between the calibra-
tion fit type and the data points in the curve.

NOTE
To quickly step through wavelength calibration displays for each wavelength,
highlight a wavelength in the Navigation Panel and use the up and down
arrow keys.

NOTE
Calibration data can be accepted individually, by clicking the Accept Button
for each wavelength, or for all wavelengths by clicking the Accept All Button.

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2.12 Quality Control Checks
Quality Control (QC) check standards are used before, between, and after the analysis of
samples to ensure the accuracy of the instrument. If the results for the QC checks are
within acceptable parameters, the sample results will be accepted. If the QC check
results fail, the action set for QC failure in the QC AUTOMATION SCREEN will be taken:
 Continue
 Stop on Failure
 Rerun Cup on Failure
 Recalibrate and Rerun on Failure
 Update and Rerun
This section will cover how to add and run a quality control check.

2.12.1 Add Quality Control Check Standards

1. With the METHOD TAB active, select QUALITY CONTROL CHECKS in the NAVIGATION
PANEL.
2. Click the ADD QC BUTTON to display the ADD QC DIALOG (Figure 2-52)

Figure 2-52 Add QC window

3. Type the check standard name into the QC NAME field.


4. There are 3 types of check standards available:
 Check standards
 Spikes
 Duplicates
5. Make sure “Check standard” is selected as the QC TYPE.
6. Enter the target concentration in to the TARGET field.
7. Select the RELATIVE BUTTON and enter 10 into the LOW and HIGH text boxes.
8. Click OK and the check standard name will appear in the CHECK STANDARD list.
9. Click on the CHECK STANDARD TABLE entry to see the wavelengths, target
concentrations and acceptance limits for the check standard. The check marks in
to the left of the wavelengths indicate that the results for all wavelengths will be
checked for acceptance.

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2.12.2 Modify Quality Control Check Standards

Modify the Standard Concentration and Unit of Concentration


1. Highlight the standard in the STANDARD NAME TABLE.
2. Click the MODIFY STANDARD BUTTON as shown in Figure 2-44.
3. Make any necessary changes.
4. Click the OK button in the MODIFY STANDARD DIALOG (Figure 2-53).
5. Changes will be reflected in the STANDARD LINES TABLE on the right.

NOTE
Element concentrations in the Standard Lines Table should reflect the
concentrations present in the standard solution used.

Figure 2-53 Modify standard dialog

Change the Standard Lines


1. Highlight the standard in the STANDARD NAME TABLE.
2. In the STANDARD LINES TABLE select/deselect the standard lines to include in that
standard.
3. Click the MODIFY STANDARD BUTTON to display the MODIFY STANDARD DIALOG.
4. Click OK.

2.12.3 Delete a Quality Control Check Standard

1. Highlight the standard in the STANDARD NAME TABLE.


2. Click the DELETE STANDARD BUTTON.

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2.12.4 Run Quality Control Check Standards

Without an Autosampler
1. After the calibration standards have been run and the calibration curves have been
accepted, place the sipper probe in a check standard solution.

2. Click on the QC CHECK BUTTON to display the RUN A QC CHECK DIALOG.

Figure 2-54 Run a QC dialog

3. Select the CHK STD BUTTON and select the check standard from the CHK STD ID
MENU.
4. Click OK to run the check standard.

With an Autosampler
Quality control checks can be run automatically from METHOD TAB>QC AUTOMATION.
1. With the METHOD TAB active, select QC AUTOMATION in the NAVIGATION PANEL.
2. Place a check mark beside the check standard under the INITIAL – BEFORE SAMPLES
ARE RUN TABLE.

3. The CONTINUOUS – DURING SAMPLE RUN TABLE allows the user to periodically run
quality control checks over the course of an automated sample run. The column
labeled FREQ (frequency) defines the number of samples to be analyzed before
repeating the check standard analysis. Put a check in the check box in the
CONTINUOUS – DURING SAMPLE RUN TABLE and type “10” into the FREQ cell for check
standard. The check standard will be run after every 10 samples are analyzed.
4. The FINAL – AFTER SAMPLES ARE RUN TABLE allows the user to analyze quality control
checks at the end of the sample sequence. This ensures that the selected checks
will be analyzed at the end of analysis, regardless of the number of samples
preceding them. This table excludes calibration and update standards. For
purposes of this example, put a check in the check box in the FINAL – AFTER SAMPLES
ARE RUN TABLE for the check standard.

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5. Each QC check standard has a drop-down menu in the ACTION column containing
a list of failure actions associated with it. The QC AUTOMATION SCREEN should now
look similar to the one Figure 2-55.

NOTE
If a calibration curve has already been generated and the user does not wish to
re-run the calibration standards before running the QC check standard,
deselect the blank and calibration standards in the Initial window.

Figure 2-55 QC Automation screen

6. Place a portion of the check standard into an autosampler cup and load it into the
cup location in the sample rack.

NOTE
Click on the Sequence Tab and look at the graphical display of the standards
rack to double check the position of the check standard.

7. Click on the SEQUENCE TAB and the quality control check will be listed in the
ANALYSIS TREE in the NAVIGATION PANEL.
8. Click the RUN SEQUENCE BUTTON to analyze the quality control check.

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2.13 Sample Analysis
After the instrument has been calibrated, samples can be added and their analysis
performed. Sample analysis can be performed with or without an autosampler.

2.13.1 Add Samples

 When analyzing samples without an autosampler, samples are added as they


are run.
 If samples are to be run with an autosampler refer to Section 2.14 "Build
Sequences"

2.13.2 Run Samples

Without an Autosampler
1. Place the sipper probe in the appropriate sample solution.
2. Select the RUN SAMPLES BUTTON to display the RUN A SAMPLE DIALOG
(Figure 2-56).

Figure 2-56 Run a sample dialog

3. Enter an appropriate name in the SAMPLE TITLE field. Enter weight and volume
correction factors if applicable.

NOTE
The check boxes and value fields for Weight, Volume and Dilution are visible
only after they are set on the Analytical Parameters Screen.

4. Ensure the UPTAKE option is selected if a delayed integration is required.


5. Click OK to analyze the sample.

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With an Autosampler

NOTE
This section requires the use of a prebuilt sequence. Refer to Section 2.14
"Build Sequences" prior to accomplishing this section.

1. Load the sample into the first cup in the sample rack

2. Click the RUN SEQUENCE BUTTON to begin the analysis.

NOTE
The Figure 2-57 indicates that calibration standards will be run prior to the
sample. If the user has already run calibration standards and does not wish to
re-run them, uncheck each of the standards in the QC Automation section of
the Method Tab.

Figure 2-57 Sequence overview window

3. Once results are collected, they may be viewed under the ANALYSIS TAB. For
information on reviewing analysis results refer to Section 2.15.1 "Reviewing
Numerical Data".
4. Results may be printed at any time during data collection. With the ANALYSIS TAB
ACTIVE, select the RESULTS TAB. Click the PRINT BUTTON.

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2.14 Build Sequences
Salsa allows the user to build automated sequences that can be run with or without an
autosampler. Building a full sequence before starting an analysis run allows the user to
ensure that all solutions will be analyzed in the proper order and with the necessary
frequency throughout the sample run. Sequences combined with an autosampler will
automatically perform all designated steps for calibration, quality control and sample
analysis. If a sequence is run without the use of an autosampler, the user will be
prompted throughout the run to move the sipper probe to the appropriate solution.
Refer to Chapter 6: "Sequence" for more information on customizing sequences.
1. Click on the METHOD TAB and select QC AUTOMATION. Make sure there are check
marks beside the blank and calibration standards, as well as the QC standard.
2. Click on the SEQUENCE TAB at the bottom of the NAVIGATION PANEL. The NAVIGATION
PANEL will display the calibration standards and the QC standards active in the
method.
3. Select the appropriate rack size from the RACK MENU on the top right-hand corner
of the window (the most commonly used size is the 44 rack). Ensure the size of the
sample racks in the display match the physical racks in the autosampler. If they do
not, select the appropriate sized rack.
4. The DISPLAY PANEL contains a table for defining samples to be analyzed. If an
autosampler is being used, the rack map at the bottom displays where the
standards, check standards, and samples are located in each autosampler rack.
Click in the first cell under the SAMPLE ID heading and type “Sample 1.”
5. Click the UPDATE BUTTON on the right-hand side of the window and note that
Sample 1 will be listed in the NAVIGATION PANEL.
6. If each sample has a unique sample name, the user will need to type each one into
the SAMPLE ID cells and click the UPDATE BUTTON when finished to load the entire
sequence into the NAVIGATION PANEL. If the sample IDs are not unique, place the
mouse cursor over the first cell under the CUP heading (the mouse cursor should
change to a black, horizontal arrow). Hold down the left mouse button and drag
the mouse down to highlight the first 18 rows in the sample table (clicking on the
first cup in the sequence, holding the shift key and then clicking on the last cup in
the sequence will also highlight cup positions).

7. With all thirty rows still highlighted, click the SEQUENCE BUTTON located
above the table, to show the SEQUENCE DIALOG. Make sure there is a “1” typed into
the text box labeled “Sequence cups by” and click OK.
8. The SEQUENCE TREE in the NAVIGATION PANEL will automatically update to display
the 18 samples and the appropriate check standard will be incorporated into the
sample sequence according to the settings applied through METHOD>QC
AUTOMATION TAB.
9. The rack map will automatically update to display the sample locations occupied
by the 18 samples entered into the sample sequence. The SEQUENCE SCREEN should
look similar to Figure 2-58.
10. Enter weight and volume correction factors for the samples if applicable.

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Figure 2-58 Building sequences

11. Click the RUN SEQUENCE BUTTON on the right-hand side of the DISPLAY PANEL
to begin the analysis.
12. At any point during the analysis, the sequence can be paused by clicking the PAUSE
SEQUENCE BUTTON

NOTE
When the Pause Sequence Button is selected, the instrument will complete
the analysis of the current cup, then move the autosampler sipper probe to
the rinse solution. The probe will remain in the rinse solution until the
sequence is resumed (by selecting the Pause Sequence Button again).

13. If a sequence is running without the use of an autosampler, the user will be
prompted throughout the run to move the sipper probe to the appropriate
solution. An example prompt is illustrated in Figure 2-59.

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Figure 2-59 Sequence prompt

2.15 Review and Report Results


Results can be reviewed in both numerical and in graphical form and recalculated if
needed (refer to Section 2.15.2 "Recalculating Data" for more information on
recalculating data). Once results have been reviewed, they can be reported using various
output formats.

2.15.1 Reviewing Numerical Data

1. With the ANALYSIS TAB active select the RESULTs TAB to review the numerical data for
all standards, quality control checks and samples. Use the DETAILED and
STATISTICS BUTTONS above the sample results to change how the results are
displayed:
 If the DETAILED BUTTON is selected, results will be displayed in terms of
individual replicates and the information will include: sample ID, element
symbol, element wavelength, calculated concentration, background
corrected peak intensity and the uncorrected concentration.
 If the STATISTICS BUTTON is selected, the statistical data for each standard
and sample will be displayed and the information will include: sample ID,
element symbol, element wavelength, mean calculated concentration,
standard deviation of the replicate measurements, %RSD of the replicate
measurements, the concentration units, and the uncorrected
concentration.

NOTE
Select the ALL or SINGLE radio buttons above the sample results will show the
results in either a running list of all the solutions that were analyzed or as a
truncated list with just the solution that is highlighted in the Navigation Panel.

NOTE
If the user wishes to print results directly from this display window, click the
Print Button.

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2.15.2 Recalculating Data

If data is reviewed and needs to be recalculated before it is reported, Salsa will perform a
recalculation of the method’s data according to the new parameters. This may occur due
to:
 Adjustments in weight
 Volume or dilution factors
 Incorrectly entered standard concentration
 Repositioning
 Adding or removing background correction points
 Removal of one or more standards from the calibration curves
 Removal of, or change to, an internal standard wavelength

NOTE
If data is being recalculated solely to adjust weight, volume, or dilution
correction factors, the calibration standards do not need to be recalculated.

Recalculating Calibration Standards


1. With the ANALYSIS TAB active, select the RECALCULATE TAB.
2. On the RECALCULATE TAB place a check mark beside the blank and calibration
standards that need to be recalculated.
3. Click the RECALCULATE BUTTON. A window will query whether the new calibration
curves should automatically be accepted.

NOTE
The user may click either the Yes or the No button; however, it should be noted
that if the user selects NO, the calibration curves must be manually accepted
prior to recalculating samples.

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4. As the calibration standards are recalculated, they will be appended to the ANALYSIS
TREE in the NAVIGATION PANEL. A red box indicates that the calibration standard has
been recalculated (Figure 2-60).

Figure 2-60 Data recalculation


.

5. Once the calibration standards have been recalculated, click on the METHOD TAB
and check each wavelength to make sure the recalibrated calibration curves did
not produce unexpected results.
6. If the calibration curves are acceptable, return to the RECALCULATE TAB and click the
CLEAR ALL BUTTON to clear the calibration standards from the RECALCULATION LIST,
and place a check mark beside all samples to be recalculated.
7. Click the RECALCULATE BUTTON and wait for the samples to be recalculated and
displayed in the NAVIGATION PANEL.

Recalculating for Weight and Volume

NOTE
If results are being reprocessed due to changes in weight, volume, or dilution
correction factors, these changes can only be made in the Recalculate Tab.

1. With the ANALYSIS TAB active, select the RECALCULATE TAB.


2. On the RECALCULATE TAB, put a check in the boxes labeled “Weight” and “Volume”
and enter weight and volume correction factors in the appropriate text fields.
3. Place a check mark beside the sample(s) to be recalculated.
4. Click the RECALCULATE BUTTON.

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2.15.3 Reporting Data

The Prodigy7’s Salsa software is designed to provide a wide range of flexibility when
reporting data. Users can select what samples are reported, what analytical data is
included in the report, and the organization of the report itself. This section shows how
to generate a basic report and output it in various formats. For more detailed
information on generating and customizing reports refer to Section 7.8 "Report Tab".
1. With the ANALYSIS TAB active, select the REPORT TAB.
2. Place a check mark beside all samples in the NAVIGATION PANEL to be included in
the report.

NOTE
To select multiple samples at once, place a check mark beside the first sample
at the top of the sample list, hold down the Shift key, and then check the last
sample included further down the list. All samples between the two will be
selected. Alternatively, placing a check mark beside the chapter folder
(represented by a red folder) will include all samples in that chapter.

3. Click on the appropriate radio button to indicate whether the data will be reported
as DETAILED, STATISTICS or LT (LONG-TERM) STATISTICS. Refer to Table 2-4 "Data
Reporting Options" for definitions of each report data sorting option.

Table 2-4 Data Reporting Options


Data Reporting Option Description
Detailed Results will be reported in terms of individual replicates and the
reported information will include items such as: calculated con-
centration, background corrected peak intensity, and uncorrected
concentration.
Statisticsa Statistical results will be reported and the information will include
items such as: mean calculated concentration, standard deviation
of the replicate measurements, %RSD of the replicate measure-
ments, and uncorrected concentration.
LT (long-term) Statistics LT Statistics radio button allows the user to report the concentra-
tion mean, standard deviation and %RSD for a sample that was
analyzed periodically over the course of 1 or more sample runs.
For example, statistics can be generated for a quality control check
that was measured twice a day, every day for a month to look at
the long-term accuracy and precision of the measured check stan-
dard.
Note: To successfully report long-term statistics, all samples
included in this report must have identical names.
a. When Statistics is chosen, a Stats Data reporting parameter, may been added. The Stats Data item
allows the user to report statistical data along with the measured concentration for each of the repli-
cates that were pooled together to generate the statistical data.

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4. Select which wavelengths to include in the report under the LINE TABLE. Selecting
the box to the left of each wavelength will include that wavelength. The ALL and
NONE BUTTONS under the LINE TABLE allow the user to select all or none of the
wavelengths to be reported.
5. Select which data parameters to include in the report by selecting the box to the
left of the appropriate item under the ITEMS TABLE. If the user is unsure of which
items to include, the DEFAULT BUTTON, located below the list provides a set of items
that are commonly reported with the DETAILED or STATISTICS BUTTON highlighted.
To generate a report with long-term statistical data, scroll to the bottom of the
ITEMS LIST and select LT MEAN CONC, LT SD CONC and LT RSD CONC. An example of
reporting parameters is depicted in Figure 2-61:

Figure 2-61 Reporting data with replicate and statistical information

6. Select the report format by clicking either the FORMAT 1 or FORMAT 2 BUTTON under
the REPORT section. FORMATS 1 and 2 report data in columns and tables.

NOTE
Saving Report Parameters: Once the report data parameters have been
chosen, the format can be saved and quickly loaded for future use. To save a
report, select the Save button beneath Report Spec. A dialog will prompt for
the New Report Spec Title. Saved reports can be quickly loaded using the Load
button, also located in the Report Spec section of the Report Tab. The Report
Spec will also save the wavelengths that are selected.

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CSV File Output
An electronic report can be generated by clicking the CSV FILE BUTTON under OUTPUT.
This will generate a comma separated file that can be saved, transferred and opened in
another program. This file can also be stored and printed at a later date.

Paper Reports Output


A paper report can be generated by clicking the PRINTER BUTTON under OUTPUT on the
REPORT TAB.

Exporting Data to LIMS


Interfacing data from Salsa to a LIMS can be performed using one of the methods
outlined below:
1. Real time data output to a local or network location. By placing a line into the
startup.ini file, (located in the /Salsa directory) a LIMS.TXT file will be generated in
designated location. The line has the form:

Lims LOCATION\FOLDER NAME\

Examples of acceptable lines:

Lims W:\ICPDATA\ (Folder ICPDATA on Drive W)


Lims \\MKDSVR\DATA (Folder DATA at location MKDSVR)

The folder and location must exist before data output is begun. The LIMS.TXT will
have data appended to it as samples, standards, etc., are analyzed.

Lims.txt file will contain Title, ExtId, Number of Reps, Weight, Volume, Dilution
Factor, Concentration, Intensity, Lines, Raw Intensity, Left Background point, and
Right Background point for each analysis item. Lims.txt will populate real time. If
the Start up file parameter is not set, the file will not be generated.
2. Output data as an ASCII file such as CSV output in post-run mode. Copy data onto
an external media and send via tied-in computer through the serial interface. The
“Parsing” software (supplied by vendor of the LIMS) then translates the data to the
LIMS. The user will have to customize what the “Parsing” does for each
instrument’s data it receives. This is a common approach taken and is one of the
more secure methods.
3. Output directly via the serial port to a “Parsing” software which translates the data
for LIMS (real time). This can be accomplished by setting up a generic printer on
Salsa computer as a serial output device. When the user selects this printer as the
default printer, all reported data will subsequently go to the “Parsing” system and
ultimately the LIMS. Because the generic printed is selected as “default”, hard
copies must be generated, post run, by selecting the real printer as default and
generating reports a second time.

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Chapter 3: Method Development
3.1 Overview
Anytime an unknown sample is analyzed by ICP a procedure must be followed to ensure
that the highest degree of accuracy and precision possible are achieved for the analytical
results. This procedure is referred to as “method development” and entails the following
steps:
1. Selecting wavelengths for determining the elements of interest.
2. Performing spectral scans of the blank, standards and the samples.
3. Estimating analyte concentrations using scan data or SemiQuant.
4. Selecting parameters for each line (background correction points, standard
concentrations, viewing mode, integration times, interfering element corrections,
etc.).
5. Confirming the accuracy and precision of the method with a check standard.

3.1.1 Method and Analysis Chapters

To perform an analysis, the Prodigy7 will rely on information contained in analytical


methods and analysis chapters. Both methods and analysis chapters are part of the Salsa
database.
 Methods contain the information the Prodigy7 ICP will use to calibrate the
system and run samples.
 Analysis chapters are where raw data for results is stored.

NOTE
Whenever a method is modified, a new copy of the method parameters is
copied to the active analysis chapter.

3.1.2 Method Complexity

The types of samples that will be analyzed determine the complexity of a method. The
purpose of developing a method is to ascertain what information needs to be included
in order to provide accurate and precise sample analysis results. For example, for a
simple analysis it may only be necessary to have wavelengths, integration times and
calibration standards. A more complicated analysis may require the addition of
background correction, interfering element correction and internal standards. While
each sample type may require different parameters, the basic procedure used to arrive at
those parameters is essentially the same.
Refer to Section 2.4.1 "Method Setup" for initial method set-up procedures when
creating a new method. The information contained in this chapter is designed to
address the analyst’s major considerations in developing a new method.

3-1
3.1.3 Compromise Operating Conditions

The properties of the ICP are such that, with very little compromise, determinations can
be performed under conditions where acceptable detection limits and few interferences
are obtained. This simplifies the task of method development since numerous sample
types can be analyzed under virtually identical plasma conditions. In fact, the outcome
of optimization schemes rarely results in any significant analytical improvement over
those obtained with the standard “compromise operating conditions”. In addition, the
actual plasma conditions obtained after an optimization scheme usually differ very little
from the original compromise conditions.

3.2 Selecting Wavelengths for the Method

3.2.1 Wavelength Selection

ICP is a multielement technique (more than one element can be measured in the same
solution) and provides a linear response over several orders of magnitude in
concentration. Therefore, in all but a few rare cases, it is possible to include all the
elements desired for the analysis in a single method. When selecting wavelengths (also
referred to as “lines”) for analysis, the following characteristics should be taken into
consideration:
 Sensitivity: the ratio of the net signal intensity to the background level.
 Linear Dynamic Range: range of concentrations over which a linear response is
obtained.
 Freedom from Interferences
 Atomic vs. Ionic Lines
Proper consideration of these points will result in the best wavelength line being chosen
for the analysis.
Refer to Figure 3-1. A list of recommended lines (indicated by two asterisks) appears in
the Salsa software line library. These lines are recommended for trace or routine level
work. The recommended line, however, does not always have the highest S/B ratio of the
element lines listed in the line library.
The recommendation takes into account characteristics such as S/B, freedom from
interferences and linear dynamic range. When creating a new protocol, the
recommended lines are a good place to start. It is also good practice to examine more
than one emission line for each element. When this is done, any spectral interference
that may exist will be found. For more information on spectral interference refer to
Section A.1.3 "Spectral Overlap and Interfering Element Correction (IEC)".

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Figure 3-1 Element selection screen

For the vast majority of analytical requirements, at least one of the emission lines listed
on the ELEMENT SELECTION display will be acceptable. The table from which the line was
chosen contains four columns of information:
1. The first column contains the element symbol and wavelength in units of
nanometers (nm).
2. The second column indicates whether the emission line originates from an atomic
(I) or ionic (II) species.
3. The third column list the signal to background ratio for the highlighted wavelength
4. The fourth column and whether or not this line has been peaked (designated by
“Aligned”), respectively.

3.2.2 Collect Wavelength Spectra

Collecting and examining wavelength scans is an important part of method


development. These scans will illustrate potential interferences and are indispensable
when determining how many background correction points to use, where to place the
background correction point(s) and how many pixels in width each background
correction point should be. When developing a method, scans should be collected for
the blank, a representative calibration standard, and representative samples. If all the
samples to be analyzed are similar in matrix and elemental composition, only one
sample needs to be scanned. For this example, wavelength scans will be collected for
both standards and samples.
Before any decisions can be made regarding which emission line to use, it is important
that spectral region around the wavelength (we call this spectral region a scan) be
examined for each line under consideration. The examination of scans should include
blanks, standards and some representative samples. Selecting emission lines without
first examining scans may lead to considerable inaccuracies in analytical results.

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Figure 3-2 Wavelength scan screen

3.2.3 Collecting Spectral Information for Standards

Scan a Calibration Standard


1. Choose the blank or calibration standard to be scanned.
 If an autosampler is not being used, place the sipper probe in the
appropriate solution.
 If the autosampler is being used, place the standard solution in a cup in the
standards rack on the autosampler and move the autosampler probe to that
cup. Do this by selecting the appropriate rack and cup locations at the
bottom left-hand section of the INSTRUMENT CONTROL SCREEN. Under MOVE
TIP, click the CUP BUTTON to initiate the movement of the autosampler
probe. Wait until the solution has reached the plasma.

2. Click on the RUN STANDARD BUTTON to display the RUN STANDARD DIALOG.

Figure 3-3 Run standard dialog

3. Select the STANDARD ID MENU. Standard 3 is the best choice because it contains the
highest concentration of all the elements in the method.

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4. Select the number of integrations under INTEGRATION NUMBER by
selecting/deselecting each integration.
5. If the solution has reached the plasma and an uptake time is not required, uncheck
the UPTAKE TIME option.
6. Click the OK to take the scan.

NOTE
Results for each scan will automatically populate the Navigation Panel when
the Analysis Tab is selected.

3.2.4 Collecting Spectral Information for Samples

Scan a Sample
1. Choose the sample to be scanned.
 If an autosampler is not being used, place the sipper probe in the
appropriate solution.
 If the autosampler is being used, place the sample solution in a cup in one
of the sample racks on the autosampler and move the autosampler probe to
that cup. Wait until the solution has reached the plasma.

2. Click on the RUN SAMPLE BUTTON to display the RUN A SAMPLE DIALOG.

Figure 3-4 Run a sample dialog

3. Enter an appropriate sample name in the SAMPLE TITLE field.

NOTE
The Integration time and number of integrations is set on the Analytical
Parameters page (Method Tab>Analytical Parameters).

4. If the solution has reached the plasma and an uptake time is not required, deselect
the UPTAKE TIME option.
5. Click OK to scan the sample.

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NOTE
Results for each scan will automatically populate the Navigation Panel when
the Analysis Tab is selected.

3.2.5 Examining Wavelength Scans

1. With the ANALYSIS TAB active, select the SCANS TAB.


2. Place check marks beside the samples or standards in the NAVIGATION PANEL to
view them on the SCANS TAB. As each sample or standard is selected, it is added to
the SCAN ID TABLE and a wavelength scan is displayed.

NOTE
Samples and wavelength scans are identified by coordinating colors.

3. To see the wavelength scans for each element, select the LINE MENU and select the
desired element (Figure 3-5).
4. Moving the cursor over the wavelength scan shows wavelength and intensity
information.
In Figure 3-5, four sample scans are being displayed for Mn 257.610 nm. A
maximum of twelve scans can be selected. For more information on the SCAN TAB
refer to Section 7.3 "Scans Tab".

Figure 3-5 Scans tab

The left and right


background correction
points are illustrated by the
blue boxes to the left and
right sides of the peak,
respectively. Each
background correction point
is 2 pixels in width.

The peak region of interest is illustrated


A list of potential spectral
by the green box and is located at pixel
interferences is listed in a table
positions 13 to 17 in the subarray.
at the bottom left corner of the
window.

Salsa provides the user with the option of shifting the pixels used to identify the
peak Region Of Interest (ROI) to any other place in the subarray. In Figure 3-5, the
region of interest has been shifted to pixel positions 22 to 25 to avoid a significant

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spectral interference. The left background correction point has been put at pixel
position 6 and 7 and the right background correction point has been eliminated.

Figure 3-6 Wavelength scan window illustrating shifted ROI

NOTE
Shifting the peak region of interest is only one of several options that might be
available when spectral interferences are encountered. Other options include
choosing another analytical wavelength from the line library and using
interfering element corrections (IECs). For more information on evaluating
wavelength, and background correction points for each element of interest,
refer to Appendix A: "Advanced User Reference".

Viewing Wavelength Scans using the Profiles Tab


An alternative, and convenient way to view wavelength scans is to use the PROFILES TAB.
1. With the ANALYSIS TAB active, select the PROFILES TAB.
2. Place a check mark beside the SAMPLE ID(S) in the NAVIGATION PANEL to display.
3. The PROFILES TAB will display thumbnail images of all the wavelengths for the
selected samples (Figure 3-7).

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Figure 3-7 Thumbnail profile display

Sensitivity
The sensitivity of the emission line chosen must match the concentration levels at which
the analysis will be performed. For most trace level work, a line with a high S/B ratio
should be chosen. An emission line with a high S/B ratio implies high sensitivity. This
means there will be sufficient signal at low concentrations. At high concentration levels,
lower S/B ratio lines are used.

Linear Dynamic Range


Linear dynamic range (LDR) is the concentration range over which an element may be
calibrated for at a particular wavelength. The LDR is dependent on the plasma
conditions and the detector. For most elements, the LDR is about 3 to 6 orders of
magnitude beginning at the detection limit. An emission line selected for analysis
should have an LDR sufficiently great enough to cover the range of concentrations that
may be present in the samples to be analyzed.
The LDR for extremely sensitive emission lines of some elements, particularly the
alkaline earths, may be short. An example of one such line is the Ca line at 393.366 nm.
For most analyses, the best line to use is the Ca line at 317.933 nm. This type of linearity
limit is a plasma physics limit imposed by the plasma conditions and is not due to any
detector limitation.
The solid-state CMOS Array Detector used in the Prodigy7 has considerable sensitivity
and dynamic range (approximately 8 orders of magnitude). In fact, the CMOS detector
has been tested to the same LDR as a Photomultiplier Tube (PMT). The limiting factor of
the LDR is governed more by the plasma than the detector. When the plasma is viewed
axially, the LDR is reduced as compared to a radial view of the plasma. The advantage of
an axially viewed plasma is a greater sensitivity, and therefore lower detection limits. To
improve accuracy when viewing the plasma axially, use a quadratic fit of the calibration
of a given line.

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There is a mathematical limit in the Salsa software for how high a count can be acquired.
The limit is near 4 billion counts. When this occurs the peak on a scan may show an
extreme negative peak. If this occurs, choose a less sensitive line or integrate for less
time. This is a very rare possibility, and should not occur in normal use. The result is not
a limit of the detector, instead, it is a limit of the memory size allocated for intensity.

Freedom from Interferences


The high temperature of the plasma discharge is also the cause one of the most common
types of interference found in ICP spectrometry. Because nearly every species present in
the ICP emits light, spectral interferences are encountered very frequently and occur as
both background shifts and interfering element effects. Of these two types of
interferences, the background shift is by far the most common. Fortunately,
compensating for spectral interferences in ICP is not difficult.
In order to detect spectral interferences, it is necessary to collect wavelength scans of the
standards and samples at the wavelengths under consideration. By overlapping the
scans and comparing them, it will be possible to see if any corrections are required.
The emission lines chosen for analysis should be those that exhibit either the fewest or
smallest levels of interference. The procedure for determining whether an interference
exists and how to make a correction is located in Appendix A: "Advanced User
Reference".

Atomic vs. Ionic Lines


Atoms in the plasma can emit light from either the atomic and/or ionic states. The
species responsible for a particular emission line is indicated in the line library by either
an “I” (atomic) or “II” (ionic) in the SP column.
Emission lines can be further categorized by being hard or soft.
 Hard lines are the atomic lines of elements with a first ionization potential
greater than 8 eV (electron volts) and all ionic lines with a second ionization
potential of more than 10 to 11 eV.
 Soft lines are all atomic lines of elements with first ionization potentials less
than 8 eV and ionic lines of elements with a low second ionization potential,
approximately 10 to 11 eV.
Generally, the highest S/B ratios and lowest detection limits are associated with hard
emission lines. Since the best lines for the majority of elements are hard, they are
preferred for analytical work. Whenever the choice exists, an operator should always
choose the hard emission line over a soft one. In most cases, this usually means selecting
an ionic line.
A quick way to determine experimentally if a particular emission line is hard or soft is to
increase the RF power. At the normal observation height, hard lines should show an
increase in intensity. Collecting wavelength scans at a couple of different power levels is
the easiest way to perform this comparison.
A complete table of ionization potentials can be found in the CRC Handbook of
Chemistry and Physics.

Automated Wavelength Scans


A sequence can be created to automate the analysis of samples. Refer to Section 2.14
"Build Sequences".
After the sequence is built, click the RUN SEQUENCE BUTTON . Scans are viewed in
the same manner as when a manual run is performed.

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3.3 Estimating Analyte Concentrations in Samples
Before preparing calibration standards, the analyst must first have some knowledge of
the approximate analyte concentrations in the samples. This estimation is usually made
using spectral scan data. The Salsa software offers a unique feature capable of providing
very good concentration estimates using scan data. The feature is used by first collecting
scans for all samples, a blank and at least one standard. The scans are then added to the
SCANS TAB. To view the scans, make the ANALYSIS TAB active, then select the SCANS TAB, and
perform the following actions:
1. Select the standard peak and enter the concentration of the analyte in the text box
to the right of CONCENTRATION.
2. The calibration is now accepted for the scans. As each sample is selected a
concentration is calculated and displayed next to the SET CONC BUTTON. Refer to
Figure 3-8 and Figure 3-9.
In our example, the wavelength scan for “Std 2” has a known concentration of Calcium
(Ca) at 317.933 nm is 5.0 ppm. The wavelength scan for the unknown “ammonium”
sample has a calculated concentration of 4.532 ppm.

Figure 3-8 Selecting scans for estimating concentrations

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Figure 3-9 Estimating concentrations using the selected wavelength scans

3.4 Selecting Parameters

3.4.1 Integrations

Each determination of an element on the Prodigy7 consists of a series of integrations,


providing short-term statistics on the measurement. In a simultaneous instrument, such
as the Prodigy7 ICP, the integrations for all elements are done at once.
Multiple integrations for a given analysis are available for short-term statistics.

NOTE
A typical value for the number of integrations is three.

The number of integrations is defined on the ANALYTICAL PARAMETERS SCREEN (with the
METHOD TAB active select ANALYTICAL PARAMETERS in the NAVIGATION PANEL). The Salsa
software reports a mean, standard deviation, and relative standard deviation for the
series of integrations on the RESULTS TAB when the STATISTICS BUTTON is selected.

NOTE
Dual-view optics, require two sets of integrations, one axial and the other
radial.

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3.4.2 Rinse Time

When the autosampler is in operation, the sample tip will return to, and remain in, the
rinse station for the amount of time specified by the rinse time. The rinse time is defined
under ANALYTICAL PARAMETERS on the METHOD TAB.
 For samples containing wide concentration ranges or high levels of dissolved
solids, a long rinse time should be used; up to sixty seconds may be necessary.
 For samples of low or similar concentrations, as well as low levels of dissolved
solids, shorter rinse times can be used; thirty seconds or less. If there is
evidence of sample carryover, the rinse time should be increased.

3.4.3 Uptake Time

Uptake time is a delay period for the sample to move from the sample filter tip, through
the pump tubing, through the spray chamber, and into the plasma and equilibrate
before the reading commences.

NOTE
A normal uptake time is approximately 30-45 seconds.

If an autosampler is not in use, the uptake time must also be long enough to ensure
equilibration of the sample introduction system. When manual readings are selected,
the operator can override the uptake time by clicking the uptake time check box in the
RUN FULL FRAME IMAGE DIALOG.

3.4.4 Peaking Line

The peaking line is the element and emission line used to select the best viewing zone in
the plasma for each view.
 In axial viewing, this position usually corresponds to the middle of the
center channel in the plasma.
 In radial viewing, this corresponds to a horizontal position relative to the
middle of the center channel of the plasma and a vertical position located a
few millimeters above the load coil.

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The PEAK SOURCE BUTTON, located on the INSTRUMENT CONTROL SCREEN (with the METHOD
TAB active select INSTRUMENT CONTROL in the NAVIGATION PANEL ) is used to find the
optimum viewing zone for the current view. Refer to Table 3-1 "Recommended Peaking
Lines".

Table 3-1 Recommended Peaking Lines


Type of Analysis Peaking Line Source Positioning Solution
Concentration
Radial Viewing Axial Viewing
General Aqueous Matrices Mn - 257.610 nma 10 ppm Reduce these
concentrations by a
factor of10.
General Aqueous Matrices Ni - 231.604 nm 20 ppm Reduce these
concentrations by a
factor of 10.
Samples in Organic Solvent Fe - 259.940 nm 20 ppm Reduce these
(such as kerosene) concentrations by a
factor of 10.
a. This line will result in an observation height that will give excellent results for all elements.

NOTE
The element line must be added to the method in order to select it as a source
positioning line. To add a wavelength line refer to Section 2.4 "Create an
Analytical Method".

3.4.5 Plasma Parameters

With the Prodigy7 ICP, the operator has the ability to adjust five plasma parameters:
1. RF Power
2. Nebulizer Pressure
3. Coolant Gas Flow
4. Auxiliary Gas Flow
5. Sample Uptake Rate
These plasma parameters, and their effect on emission line intensity, are shown in Table
3-2 "Plasma Parameters"

Table 3-2 Plasma Parameters


Parameter Effect on Emission Line Notes
Intensity
RF Power Significant
Effects are varied depending emission line
Nebulizer Pressure Significant
Coolant Gas Flow Relatively small Usually adjusted to accommodate a particu-
lar sample type, such as samples in organic
Auxiliary Gas Flow Relatively small
solvent or high dissolved solids, rather than
Sample Uptake Rate Relatively small to obtain the best detection limits.

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Specific plasma parameter setting are shown in "Plasma Parameter Settings". Each
plasma parameter is discussed in detail in the following sections of this chapter.

Plasma Parameter Settings


Typical plasma parameter settings for aqueous samples, by instrument configuration,
are shown in Table 3-3 "Recommended Plasma Parameters for Aqueous Samples"
below:

Table 3-3 Recommended Plasma Parameters for Aqueous Samples


Parameter Radial Torch Axial Torch
Power (kW) 1.0 - 1.2 (1.0) 1.1 - 1.3 (1.1)
Coolant Flow (L/min) 12 - 14 (14) 12- 18 (14)
Auxiliary Flow (L/min) 0 - 1.5 (0) 0 - 1.5 (0)
Neb Pressure (psi) 24 - 40 (34) 26 - 40 (34)
Uptake Rate (rpm) 10 - 40 (25) 10 - 40 (25)
(25=1.4 mL/min)

RF Power
The RF power selected for analysis should be the lowest possible while maintaining
plasma stability. This will result in the best signal to background ratios for a given set of
conditions, thus giving the best detection limits. Refer to Table 3-4 "Recommended RF
Power by Sample Type".

NOTE
The Prodigy7 allows plasma powers as high as 2.0 kW.

Table 3-4 Recommended RF Power by Sample Type


Sample Type Axial/Dual Radial
Aqueous 1.1 kW 1 kW
High Dissolved Solids 1.2 kW or 1.3 kW 1.1 or 1.2 kW
Samples in Organic Solvent 1.2 kW or 1.3 kW 1.1 or 1.2 kW
Alkali Metals n/a 0.8-0.9 kWa
Energetic Lines (Nitrogen 174
1.4 kW 1.4kW
nm or Phosphorus 177 nm)
a. RF powers that are too low may result in problems from chemical interferences.

Caution

Running the plasma at higher power levels usually requires that the coolant
flow be increased somewhat to prevent the torch from overheating.

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Nebulizer Pressure
Nebulizer pressure must be high enough to allow the sample to penetrate the plasma,
but not so high that there is insufficient interaction between the sample and the plasma.
Nebulizer pressure is dependant two factors:
 Nebulizer type
 Inside diameter of the injector tube
Lower pressure yields lower velocity of the aerosol and therefore longer residence time
in the plasma. This longer residence time will yield higher sensitivity that translates to
lower detection limits (for difficult lines such as arsenic, selenium, lead, etc.).
Recommended nebulizer pressures are shown in Table 3-5 "Recommended Nebulizer
Pressure by Sample Type".

NOTE
Longer residence time can make the plasma appear unstable (flicker),
however, the detection limits will be lower than a more conventional looking
plasma.

Table 3-5 Recommended Nebulizer Pressure by Sample Type


Nebulizer Uptake Tubing Sample Type
Nebulizer
Pressure
Concentric 35- 45 psi Black/Black Aqueous, Organic
Hildebrand grid 40-55 psi Black/Black Aqueous
V-Groove Nebulizer 35-45 psi Black/Black Organic
(Standard Pressure)
V-Groove Nebulizer 45-60 psi Black/Black Organic
(High Pressure)

Regardless of which viewing feature is being used (axial or radial), the best pressure can
be selected by observing the trends of the signal for Magnesium (Mn) (or Iron [Fe] in the
case of samples in organic solvent) using the OPTIMIZE SAMPLE INTRODUCTION BUTTON on
the INSTRUMENT CONTROL SCREEN. Refer to Section 5.4.3 "Optimize Sample Introduction"
for more information.

NOTE
The type of nebulizer used will affect the sample uptake rate.

Coolant Flow
The argon flow that sustains the plasma is referred to as the coolant flow. Its effect on
emission intensities is very small over the normal operating range. Consequently,
coolant flow is only adjusted for a particular sample type rather than to optimize
emission line intensities. Refer to Table 3-6 "Recommended Coolant Flow by Sample

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Type".

Table 3-6 Recommended Coolant Flow by Sample Type


Sample Type Instrument View Coolant Flow
Aqueous Radial 12-16 (L/min)
Samples in Organic Solvent Radial 15-18 (L/min)
High Dissolved Solids Radial 15-18 (L/min)
Alkali Radial 14-16 (L/min)

NOTE
Prodigy7 ICP dual-view and axial systems will operate in the 14-18 L/min
range. This is important to avoid melting or shortening the life of the torch.

For all sample types and torch orientations, the minimum coolant flow is set by the
Silicon (Si) emission coming from the torch. Too low a setting will cause the torch to
overheat, raising the Si emission level. If an unacceptable level is observed, the coolant
flow should be increased. Operating at too high a flow simply wastes argon without
gaining any analytical benefit.

Auxiliary Flow
The purpose of the auxiliary flow is to raise the plasma away from the injector tube. This
prevents both carbon build-up with samples in organic solvent and clogging of the
injector with samples containing high dissolved solids. The role of the auxiliary gas in
optimizing the plasma from the standpoint of detection limits is extremely limited.

Table 3-7 Recommended Auxiliary Flow by Sample Type


Sample Type Auxiliary Flow
Aqueous 0-0.7 L/min
Samples in Organic Solvent 1.5 L/min
High Dissolved Solids 1.5 L/min

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Sample Uptake Rate
The sample uptake rate is dependent upon the nebulizer used. Refer to Table 3-8
"Recommended Sample Uptake Rates".

Table 3-8 Recommended Sample Uptake Rates


Nebulizer Spray Chamber Uptake Tubing Uptake Rate Sample Type
Concentric Cyclonic Black/Black 1.0 - 1.4 mL/min Aqueous,
Organic
Hildebrand Grid Scott Black/Black 1.4 - 1.9 mL/min Aqueous
V-groove Cyclonic Black/Black 1.0 - 1.5 mL/min Organic

Regardless of which viewing feature is being used (axial vs. radial), the best uptake rate
can be selected by observing the trends of the signal for Magnesium (Mn) (or Iron [Fe] in
the case of samples in organic solvent) using the OPTIMIZE SAMPLE INTRODUCTION BUTTON
on the I NSTRUMENT C ONTROL Screen. Refer to Section 5.4.3 "Optimize Sample
Introduction" for more information.

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Prodigy7 User Manual
Chapter 4: Salsa Software Overview
The Salsa program is organized according to the primary areas of ICP analysis:
 Method for development of the analytical method
 Sequence for building the automated series of analytical events
 Analysis for the resulting data.
This chapter details the basic functions of the salsa user interface. For more specific
information on any of the application areas refer to Chapter 5: "Method", Chapter 6:
"Sequence", and Chapter 7: "Analysis". For information on the computational
mathematics that Salsa employs refer to Section A.8 "Salsa Computation Mathematics".
When the software is started, the main screen is displayed in Figure 4-1.

Figure 4-1 Salsa main screen

The Salsa main screen contains:


1. A MENU BAR with drop-down menus that provide access to all application
functions in Salsa.
2. A TOOL BAR containing buttons that provide access to commonly used functions.
3. An INSTRUMENT CONDITIONS BAR where the current instrument control parameters
(power, coolant flow, neb flow, pump flow, etc.) are displayed.
4. A NAVIGATION PANEL that contains features or selections relating to the application
tab selected (Method, Sequence, or Analysis). Information in the NAVIGATION PANEL
is organized in a tree structure according to the application tab selected (METHOD
TREE, SEQUENCE TREE, ANALYSIS TREE). Make selections in the NAVIGATION PANEL by
highlighting, or placing a check mark in the box to the left of each item (depending
upon the function). Selecting an item in the NAVIGATION PANEL will add it to the
DISPLAY PANEL.

4-1
5. APPLICATION TABS which allow the user to navigate between application areas
(Method, Sequence and Analysis).
6. A DISPLAY PANEL which actively displays the feature or item selected in the
NAVIGATION PANEL.
7. A STATUS BAR which displays text in the lower left of the screen to indicate the
operation currently being performed.

4.1 Startup Login


Figure 4-2 shows the default “Admin” level user login. If desired, additional user
accounts can be added by selecting USER ACCOUNTS from the TOOLS MENU on the MENU
BAR. Each user account can be assigned a numeric privilege level to grant the user access
to various features and functions within the software. Table 4-1 "Privilege Levels" shows
the privilege levels and the user account privileges associated with each level.

Table 4-1 Privilege Levels


Level Name Privileges
1 Administrator Level No Restrictions
2 Manager Level All capabilities excluding modifica-
tions to critical items related to site
restrictions.
3 Lab Supervisor Level Capable of altering some method
parameters and altering results and
recalculations.
4 Lab Operator Level Capable of updating calibration,
running samples, and reporting
results.
5 Technician Level Most Restrictive

The user ID and passwords, as well as specific permission levels, are controlled by the
system administrator inside the Salsa program. Only individuals with administrative
privileges may add new users. Any authorized operator can change their password at
any time.
If user accounts are configured, the following login window will pop up each time Salsa
is launched:

Figure 4-2 Login prompt

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To gain access to the Salsa software, both the user name and password entries must
match the information stored for authorized users. Once the operating software is

opened, a new operator can login by clicking on the CHANGE USER BUTTON .
4.2 MENU BAR
The MENU BAR contains drop-down menus that provide access to all applications in
Salsa.

Figure 4-3 Menu bar (with method tab selected)

 NAVIGATION TAB MENU


The first menu selection item changes according to the navigation tab selected in
the NAVIGATION PANEL:
 METHOD provides the ability to create (new), open, rename, save, clone,
export, import and exit a method.

 SEQUENCE provides the ability to create (new), open, save, and print sample
racks as well as import sample sequences (Set Sequence Method).

 ANALYSIS provides the ability to create (New) analytical chapters, refine


analysis results by data type (Report Control), as well as change the Report
Type, and Precision. The ANALYSIS MENU is also used to enable Sequence
Reporting.

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The remainder of the menu selections are static and do not change with navigation tab
selection.
 VIEW
Allows navigation between different analysis chapters (ANALYSIS CHAPTERS can be
viewed in the ANALYSIS TREE in the NAVIGATION PANEL with the ANALYSIS TAB active.

 RUN
Corresponds to the icons in the TOOL BAR. Refer to 4.3 "Tool Bar" for information on
each available action.

 TOOLS
Access to primary instrument control and functionality including: Extinguish
Plasma, Auto Align, Change/Modify user accounts, Event Log, Data Audit,
Scheduled Maintenance, and Install Code.

 HELP
Provides information and resources to assist in the use of the Prodigy7 instrument
and the Salsa Software.The HELP MENU also displays the Start-up File and Salsa
properties (software and firmware versions, etc.)

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4.3 Tool Bar
The T O O L B A R provides quick access to commonly used software features.
Active/available icons are shown in color, and inactive icons are shown in gray. The
status of the icons may vary based on the instrument configuration and operations

The STANDARD BUTTON opens the RUN STANDARD DIALOG. Any standard solu-
tion defined in the active method can be selected via a pull-down menu.
When run, the values for concentration and signal intensity will be added
to each analytical wavelength's calibration table.
The QC CHECK BUTTON opens the RUN QUALITY CONTROL SAMPLE DIALOG. Any
quality control solution defined in the active method can be selected via a
pull-down menu. Available quality control solutions are quality check
standards, spikes, and duplicates. When run, the values for concentration
will be compared with acceptance limits for each analytical wavelength.
The SAMPLE BUTTON opens the RUN SAMPLE DIALOG. On the dialog screen new
sample name and correction factors may be entered before each sample
analysis.

The SEQUENCE BUTTON runs the currently configured sequence.

This SEQUENCE BUTTON pauses a sequence that is currently running.

The RUN STAT BUTTON opens the RUN STAT SAMPLE DIALOG. This allows an
automated sequence to be interrupted for an urgent sample.

The ECHELLE BUTTON creates an echellogram image of all wavelengths visi-


ble to the detector. This image is useful in precisely locating each analyti-
cal wavelength on the detector.

The EXTINGUISH BUTTON extinguishes the plasma.

The CHANGE USER BUTTON opens the LOGIN DIALOG.

The DATA AUDIT BUTTON opens the audit trail for review.

The STOP (BREAK) BUTTON stops the current action or sequence.

The AUTO ALIGN Button opens the AUTO ALIGN Dialog used to automatically
align the method lines.

The SAMPLE SEARCH BUTTON opens the SAMPLE SEARCH DIALOG used to search
for analysis items within the database.

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4.4 Instrument Control Bar
The INSTRUMENT CONTROL BAR has a set of displays and provides access to several
instrument control features. The left side of the INSTRUMENT CONTROL BAR displays the
current instrument control parameters including: RF power, coolant and auxiliary gas
flows, nebulizer pressure, and peristaltic pump speed for any method. These values
cannot be adjusted from this location but only from the instrument control display in
the method.

Figure 4-4 Instrument control bar (left side)

The right side of the INSTRUMENT CONTROL BAR has a MAINTENANCE BUTTON for accessing
scheduled maintenance operations, an Interlocks button which displays any interlock
failures, the communication status and current temperature of the system camera and a
reset button to reboot the camera’s processor. If the camera reset button is clicked, the
camera reboots and the Salsa software will reconnect and re-establish communication
with the camera.

Figure 4-5 Instrument control bar (right side)

4.4.1 Maintenance Button

Salsa offers an integrated maintenance schedule with instructional videos. Because


routine maintenance tasks are essential for proper instrument performance, and the
longevity of the instrument, monitoring scheduled maintenance will ensure best data
quality, and will minimize down time and repair costs. The maintenance schedule can
be used to view the status of each maintenance item, anticipate upcoming maintenance
events, and review a maintenance procedure.
Click on the MAINTENANCE BUTTON to display the SCHEDULED MAINTENANCE DIALOG. A
green circle indicates maintenance that is up-to-date. A red X indicates required
maintenance. Each maintenance item has a tutorial illustrating the steps of the
maintenance procedure. To view the tutorial, click on the maintenance item and then
select the MAINTENANCE BUTTON.

NOTE
When a sequence is in progress, the Maintenance Button will be inactive.

Scheduled Maintenance
The SCHEDULED MAINTENANCE DIALOG contains information to determine the last service
date, next service date, and uses left, if applicable.

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Required Maintenance
When maintenance is required, the MAINTENANCE BUTTON on the INSTRUMENT CONTROL
BAR will change to red.

Click on the MAINTENANCE BUTTON to display the SCHEDULED MAINTENANCE DIALOG. Items
that require maintenance are indicated by a red “X” (Figure 4-6).

Figure 4-6 Scheduled maintenance dialog

4.4.2 Interlocks Button

1. The INTERLOCK BUTTON shows precautionary criteria that must be met prior to
operating the Prodigy7.

NOTE
Interlocks protect both the user and the instrument.

2. If the INTERLOCK BUTTON at the top of the window is red, click on that button and
address the interlock error (the icon beside the interlock message will be red).

NOTE
With the exception of the “Air knife” interlock, all interlock errors must be
satisfied before the plasma can be lit. The “Air Knife” interlock will
automatically clear when the Plasma Startup Button is clicked.

Refer to Section 8.5.4 "Interlocks" for information on resolving interlocks.

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4.5 Application Tabs
At the bottom of the NAVIGATION PANEL three application tabs:
 METHOD TAB is where new methods are developed and existing methods are
modified.
 SEQUENCE TAB is where sample lists are merged with method components
(such as calibration and check standards) to create a controlled sequence of
operations.
 ANALYSIS TAB is where individual readings may be viewed and reported.

Figure 4-7 Application tabs

Application Tabs

NOTE
The contents of the Navigation Panel, Detail Panel, Menu Bar, and Tool Bar
correspond to the application tab that is currently active. Analytical readings
can be acquired from any of the application tabs.

4.6 Navigation Panel

4.6.1 Method Applications

The NAVIGATION PANEL changes with the active application tab.


When the METHOD TAB is selected, the NAVIGATION PANEL will display:
 INSTRUMENT CONTROL: Parameters for torch, pump, and optics.
 ELEMENT SELECTION: Analytical wavelength selection, set-up, calibration
details, and Interfering Element Corrections (IEC).
 STANDARDS (CALIBRATION): Definition of standard composition.
 INTERNAL STANDARDS: Definition of internal standards and referenced
wavelengths.
 QUALITY CONTROL CHECKS: Definition of composition and allowed tolerance
range of control standards.
 QC AUTOMATION: Definition of sequential quality control operations.
 ANALYTICAL PARAMETERS: Definition of how analytical measurements will be
acquired and reported.
 SUMMARIES: A quick reference of calibration data and analytical wavelength
parameters.
 GENERAL: A record of method creation and modification.

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4.6.2 Sequence Applications

When the SEQUENCE application tab is selected, the NAVIGATION PANEL will display the
anticipated order of:
 Standards
 Samples
 Quality Control Checks

4.6.3 Analysis Applications

When the ANALYSIS TAB is selected, the NAVIGATION PANEL will display:
 Analysis Chapters
 Samples
 Standards
 Quality control checks
 Echellograms acquired in chronological order.
Highlighting an item on the ANALYSIS TREE will populate the RESULTS, CALC. VALIDATION, or
IMAGE TAB with information for that item.
Placing a check mark beside an item on the ANALYSIS TREE populates the SCANS, PROFILES,
CONTROL CHART, REPORTS or RECALCULATE TABS with information for that item. Multiple
selections can be made on the ANALYSIS TREE at one time.

4.7 Display Panel


The DETAIL PANEL shows specific information based on the highlighted application tab:
 When the METHOD TAB is active, the DETAIL PANEL displays specific method
information.
 When the SEQUENCE TAB is active, the DETAIL PANEL displays information
related to the sample list, anticipated sequence of operations, and
autosampler contents.
 When the ANALYSIS TAB is active, the DETAIL PANEL displays information related
to the sample highlighted in the NAVIGATION PANEL.

4.8 Status Panel


The STATUS PANEL appears at the bottom left side of the Salsa software window. Its
display is controlled from the MENU BAR's view option.

Figure 4-8 Status panel

When the system is waiting for the next operation to be entered “Ready” appears on the
STATUS BAR.

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Chapter 5: Method
5.1 Method Overview
Methods ensure the highest degree of accuracy and precision possible for analytical
results. Chapter 3: "Method Development" contains information on the components of
a method. This chapter will explain the procedures for building and employing a
method in the Salsa software:
 Method creation and access
 Instrument control parameters
 Adding elements
 Adding standards
 QC checks
 QC automation
 Setting analytical parameters

NOTE
All Salsa software selections for this chapter are located under the Method Tab
in the Navigation Panel unless otherwise noted. Menu Bar selections referred
to in this section may only be available when the Method Tab is selected.

Figure 5-1 Home screen with method tab selected

5-1
5.2 Creating a Method
With the METHOD TAB active, select METHOD>NEW from the MENU BAR. The following
window in Figure 5-2 will appear:

Figure 5-2 New method dialog

1. Type the appropriate names under the METHOD NAME and ANALYSIS CHAPTER NAME
fields, respectively. Add any useful method notes.

NOTE
Method Notes may be helpful in identifying the method in the Open Method
Dialog. Refer to Figure 5-3.

2. Click the OK BUTTON when finished.

5.3 Opening an Existing Method


1. With the METHOD TAB active select METHOD>OPEN from the MENU BAR. The OPEN
METHOD DIALOG box will appear, showing a selection of all methods available in the
Salsa database (Figure 5-3).

NOTE
To assist in identifying the method, the Open Method Dialog contains a
Periodic Table that displays the elements contained in the highlighted
method. Method comments are displayed beneath the elements.

NOTE
The columns can be sorted by clicking on the column header. Resting the
cursor on a highlighted element will display a tool tip with the wavelength
information.

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Figure 5-3 Open method dialog

Information
beneath each
column can be
sorted by clicking
on the heading

Raised elements are


present in the
Methods displayed highlighted
can be hidden and method.
shown

Methods that are no longer useful can be hidden.


1. Highlight the method to be hidden in the OPEN METHOD DIALOG.
2. Click the HIDE METHOD BUTTON.
To show a method that has been hidden:
1. Place a check mark in the SHOW ALL box and hidden methods will appear with
asterisk beside them. The asterisk denotes that they are normally hidden.
2. Highlight the hidden method and select the SHOW METHOD BUTTON to make them
visible again.

5.4 Instrument Control


With the METHOD TAB active, select INSTRUMENT CONTROL to display the INSTRUMENT
CONTROL S CREEN (Figure 5-4). This display offers a graphical representation of the
various user determined instrument controls on the Prodigy7. Key areas include:
 Plasma Control
 Spectrometer Temperature
 Torch Gas Controls
 Manual Autosampler Control
 Pump Speed
 Instrument Diagnostics
 Sample Introduction Optimization

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Figure 5-4 Instrument control screen

5.4.1 Autosampler Controls

Figure 5-5 Autosampler control

 Clicking MOVE TIP TO offers two pull-down menus:


1. The left pull-down menu contains the sample racks available
2. The right pull-down menu shows available cup locations
 Clicking the CUP BUTTON moves the autosampler probe directly to the entered
cup position.
 Clicking on the RINSE BUTTON moves the autosampler probe to the rinse
station.
 Clicking on the AIR BUTTON lifts the autosampler probe to its top elevation
setting.
 When running a sequence, the RACK AND CUP fields display the current location
of the autosampler probe.

NOTE
The supported rack types are defined on the Sequence Tab.

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5.4.2 Diagnostics

Clicking on the DIAGNOSTICS BUTTON opens the DIAGNOSTICS DIALOG shown in Figure 5-6.

NOTE
It is strongly recommended that operators make NO changes on this display
without first speaking with Teledyne Leeman Lab’s Customer Support.

For more information on making changes to the D IAGNOSTICS D IALOG , refer to the
Appendix A: "Advanced User Reference".

Figure 5-6 Instrument diagnostics dialog

5.4.3 Optimize Sample Introduction

The OPTIMIZE SAMPLE INTRO BUTTON is a tool for adjusting Sample Introduction system
settings. The optimize sample intro function actively analyzes and displays results of the
analysis for evaluation.

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Figure 5-7 Instrument control screen

Figure 5-8 Optimize sample intro dialog

Three fields are active on the OPTIMIZE SAMPLE INTRO DIALOG:


 The LINE FIELD offers a pull-down of method wavelengths. Highlight one of the
lines to select it.
 The INTEGRATION FIELD accepts numerical values for replicate integration time
in seconds (0.01-300)
 The CONCENTRATION FIELD accepts a numerical value for the standard to be
aspirated.

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The optimize sample into function works by:
 While a standard is aspirating, the panel will display peak and background
intensities for the selected line and calculate corrected intensity, estimated
detection limit, signal to background ratio and background equivalent
concentration.
 Simultaneously it will also report mean, standard deviation, and %RSD of the
last five replicates.
 Replicate readings begin when you click the START BUTTON and continue until
you click the STOP BUTTON. While readings are being acquired, all the
parameters shown on the INSTRUMENT CONTROL SCREEN are active. Click the
CLOSE BUTTON to end the OPTIMIZE SAMPLE INTRO DIALOG.

5.4.4 Plasma Controls

The Plasma Controls found on the INSTRUMENT CONTROL SCREEN include:

Auto Start
The AUTO START BUTTON automatically executes a sequence of operations for the safe
ignition of the plasma as long as all the interlock conditions are satisfied. Changes in the
status of the plasma during the start-up sequence are reflected in the appropriate fields.
The auto start sequence consists of:
 Purge Spray Chamber
 Coolant ON
 Depressurize Spray Chamber
 Igniter ON
 RF Power ON
 Initiate 10 Second Timeout period

NOTE
If the plasma does not ignite after the 10 second timeout, RF power will be
turned OFF and the auto start sequence will return to the Purge Spray
Chamber step.

After ignition, the following sequence occurs:


 Turn OFF Igniter
 Kill Filamentary Plasmas
 Auxiliary Gas OFF
 Turn ON Nebulizer Pressure
 Pump ON
 Method Settings Applied

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Figure 5-9 Plasma auto start flowchart

Manual Start
A manual start is accomplished by using:
 RF power ON and OFF BUTTONS
 RF power settings
 IGNITER BUTTON

NOTE
Successful ignition of the plasma in manual operation requires that the gas
knife be active, coolant gas flowing at an appropriate level, and the nebulizer
flow stopped after purging for an adequate time.

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Extinguish
The EXTINGUISH BUTTON shuts down:
 RF supply
 Torch gases
 Gas knife
 Pump

Extinguish After Rinse


The E XTINGUISH A FTER R INSE BUTTON functions in the same way as the E XTINGUISH
BUTTON, but waits for a predefined delay period. The length of the delay is entered in the
pull-down menu beneath the button.

Gas Knife
Radio buttons for the GAS KNIFE allow for the manual starting and stopping of the shear
gas at the end of the plasma.

NOTE
Interlocks prevent the plasma from running when the gas knife is off so
damage to the optics is avoided.

Figure 5-10 Plasma controls

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5.4.5 Peristaltic Pump Controls

The Pump area provides ON and OFF buttons for the peristaltic pump.
When the pump is ON and black/black sample pump tubing installed, the pump rate [in
Revolutions Per Minute (RPM)] should approximate the value displayed in the
pull-down menu. Click on the MENU BUTTON to change the flow rate value.
The STANDBY BUTTON will stop the peristaltic pump, but pulse its operation periodically
to prolong the tubing’s lifetime.

Figure 5-11 Pump controls

5.4.6 Spectrometer

The Spectrometer Area provides:


 A display of the spectrometer temperature (Temp.) in degrees Celsius.
 The PEAK SOURCE BUTTON which automatically optimizes the active view,
directing the beam onto the spectrometer entrance slit. Refer to Section 2.7
"Position the Plasma (Peak Source)" for plasma positioning procedures.
 The VIEW radio buttons select which beam is directed into the spectrometer,
RADIAL (for major constituents), AXIAL (for trace levels), and HG LAMP (for
wavelength calibration).
 The PURGE radio buttons provide set the purge flow rate to the Prodigy7 ICP
optics path.
1. OFF sets the argon purge to a low nominal flow,
2. LOW sets the purge rate at a default of 2 LPM and HIGH sets the purge rate at 20
LPM to quickly purge air from the optical path after system shutdown.

NOTE
The low purge rate may be adjusted by editing the startup.ini file.

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Figure 5-12 View control

5.4.7 Torch Gas Controls

The torch gas area provides controls for the coolant, auxiliary, and nebulizer gases. Each
gas flow can be toggled ON and OFF. The flow can be regulated by using the pull-down
menu next to each flow.
 Coolant and auxiliary gases are controlled by a mass flow controller and
regulated in Liters Per Minute (LPM).
 Nebulizer flow is controlled by pressure and regulated in Pounds Per Square
Inch (psi).

Figure 5-13 Torch gas control

NOTE
The auto start sequence will override the manually entered flow settings and a
plasma interlock prevents turning the coolant gas OFF while the plasma is ON.

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5.5 Element Selection
With the METHOD TAB active, select E LEMENT SELECTION in the NAVIGATION PANEL to
display the PERIODIC TABLE OF ELEMENTS (Figure 5-14).

Figure 5-14 Element selection

 To select an element, click on the chemical symbol shown in the PERIODIC


TABLE display.

NOTE
To display the elements in an Alphabetical Table rather than the Periodic Table
by clicking on the Alphabetic Button. Clicking on the Periodic Button will
return the element display to the Periodic Table.

 Once an element is selected the AVAILABLE LINES TABLE is populated with


wavelength lines for that element (from the Salsa line library). These lines may
be sorted by wavelength, species, signal/background ration, or alignment
status by clicking on the appropriate column header.
 Radio buttons in the lower right section of the display define whether the
available lines offered will be limited to the “Preferred lines” in the line library
or “All lines”.
 Click on a wavelength to populate the INTERFERENTS TABLE with line
information.

5.5.1 Add a Line to the Method

1. With the METHOD TAB active, select ELEMENT SELECTION in the NAVIGATION PANEL.
2. Select an element from the PERIODIC TABLE.
3. Highlight the desired line from the AVAILABLE LINES TABLE.

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NOTE
Double-clicking on the A DD L INE Button, with an element selected, will
automatically add the preferred line for a particular element without the need
to highlight the desired line.

4. Click the ADD LINE BUTTON. The element will appear under ELEMENT SELECTION
on the NAVIGATION PANEL. Elements included in the method will appear “raised”
on the PERIODIC TABLE.
5. Repeat this process for all the analytical wavelengths of interest.

5.5.2 Line Specific Information

After analytical lines have been added to a method, they appear in the NAVIGATION PANEL
under the E LEMENT SELECTION. E LEMENT SELECTION is collapsible and expandable by
clicking on the box to the left of the option. Analytical lines can be arranged on the
METHOD TREE by dragging and dropping.
Each analytical line is displayed in the NAVIGATION PANEL with the element symbol and
the wavelength. If the wavelength has been assigned a view, other than axial, a letter
indicating the view will follow the wavelength:
 Blank indicates axial
 r is radial
 x is XUV axial
 z is XUV radial
 m is Hg Lamp

Figure 5-15 Method tree

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Clicking on an analytical line in the NAVIGATION PANEL will highlight the wavelength and
display wavelength specific information in the DISPLAY PANEL:
 GENERAL TAB
 CALIBRATION TAB
 ALIGN WAVELENGTH TAB
 IEC TAB

5.5.3 General Tab

The G ENERAL TAB displays information for the analytical line highlighted in the
NAVIGATION PANEL. Information derived from the line library, as well as user defined
variables are displayed. Changes made to the editable fields on the GENERAL TAB are not
executed until the APPLY BUTTON is clicked.

Figure 5-16 General tab containing wavelength information

 The Element Name, Symbol, Wavelength, Species, and (Relative) Intensity


under General Information are defined in the line library and cannot be edited
on this display.
 The ACTIVE check box defines whether information on the highlighted line will
be displayed.
 The CHIP X field contains the row on the CMOS detector where the peak for the
analytical line is to be found.
 The CHIP Y field contains the column on the CMOS detector where the peak for
the analytical line is to be found.

NOTE
CHIP X and CHIP Y values are read from the line library when the line is added to
the method. They may be entered manually or updated from the Subarray Tab.

 Text may be entered in the COMMENTS field.

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 The TORCH VIEW may be selected between HG LAMP, AXIAL or RADIAL view for
each line selected.

NOTE
Only the views supported by the instrument configuration will be available.

Figure 5-17 Wavelength view selection

NOTE
When a method contains both axially and radially viewed lines, two exposures
are required.

Clicking on the D ELETE L INE B UTTON will immediately remove the analytical line
highlighted from the NAVIGATION PANEL from the method.

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5.5.4 Calibration Tab

The CALIBRATION TAB displays information for the analytical line highlighted in the
NAVIGATION PANEL.

Figure 5-18 Calibration tab

 The graph displays the fit based on the FIT TYPE selected. The FIT TYPE MENU
offers the user a choice of:
1. Linear
2. Quadratic (2nd order polynomial)
3. Weighted linear - The weight factor for each standard is proportional to the
%RSD value for that standard
4. Wtd 1/C - The weight factor for each standard is based on the reciprocal of the
concentration of that standard, and
 The Calibration Data contains the mathematical fit for the displayed
calibration curve where:
Conc. = AI2 + BI + C (with “I” being the corrected intensity)
 Rho is the correlation coefficient of the fit.
 Both weighted linear curve fits require repeats and is weighed proportional to
%RSD, thus favoring the low end of calibration more than a linear curve fit.
 Individual replicate readings may be excluded by clicking on a standard and
then clicking off the check box of the replicate to be excluded.
 The entire standard can be excluded from the curve fit calculation via
Standards/MSA in the NAVIGATION PANEL.

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5.5.5 Align Wavelength Tab

The ALIGN WAVELENGTH TAB displays information for the analytical line highlighted in the
NAVIGATION PANEL.
The display is used to position the analytical subarray over the observed emission
intensity for the analytical wavelength in the echellogram exposures (where the entire
spectrum is captured).

Figure 5-19 Aligning wavelength tab

In the subarray area, all of the subarray characteristics are displayed. Each of the
subarray fields may be edited. Changes made to any of the fields are not saved to the
method until the Apply button is clicked.
 Height is the number of pixels in the subarray columns. Depending on the
wavelength, Salsa will select a height of either 3 or 5 pixels.
 Width is the number of pixels in each subarray row.
 The AUTO button automatically aligns the subarray to the brightest image on
the currently viewed full frame.
 The RESTORE button resets the physical position of the visible wavelength to its
default location derived from the line library.
Echellograms that have been collected appear in the table below the subarray area. Use
the scroll bar to locate an echelle image which contains emission intensity for the
element highlighted in the NAVIGATION PANEL. When you highlight an echelle image, its
title, integration time, torch view and date/time stamp are displayed in the ECHELLE
IMAGES TABLE (Figure 5-19).
The large area to the right of the display will show the intensity profile for the area of the
detector where the subarray is located. The subarray is depicted by a rectangle whose
border appears brighter where peak and background assignments are defined. Click on
the appropriate arrow keys to move the subarray indicator box over the emission
intensity for the analytical line (the higher the intensity, the brighter the pixel is
displayed).
 The ZOOM OUT BUTTON provides a larger region around the subarray to view.
 The CONTRAST BUTTON applies a logarithmic scale to the pixel intensities so
that less intense signals can be found.

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Below the subarray image is a histogram which shows the relative intensity of each pixel
(red bars). At the bottom of this graph are graphical representations (green markers) of
the peak and background points. You may use the mouse drag and drop feature to
change the peak and background points.

Automatic Alignment of Wavelengths


Auto align peaks method lines using intelligent adjustment of exposure times.
1. Click the AUTO ALIGN BUTTON in the MENU BAR to display the AUTO
WAVELENGTH ALIGNMENT DIALOG and perform the alignment. Figure 5-20 shows the
automatic alignment of the Hg reference wavelength, followed by several
analytical wavelengths in a method.

Figure 5-20 Mercury lamp alignment

2. First align the mercury reference wavelength (253.652 nm) by viewing the HG LAMP
and updating the deltas found in diagnostics.

NOTE
The first panel has only Hg selected (Hg does not need to be in the method).

3. Click the AUTO ALIGN BUTTON to peak Hg.


4. Click ACCEPT to accept the Hg ref alignment. The Hg values change to green to
indicate the alignment has been accepted.
5. Other method lines may now be selected for alignment as shown in Figure 5-21.

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Figure 5-21 The mercury (Hg Ref) lamp aligned and accepted

6. Select a standard solution to aspirate or manually aspirate a solution into the


plasma.
7. Click AUTO ALIGN button to align the selected wavelengths. After exposure, the
cursor can be moved to highlight each line and the area around the wavelength will
appear similar to Figure 5-21. The crosshairs show the original location of the peak
and the red area defines the new location, if accepted. The amount of change for
each wavelength is indicated by dX and dY (Figure 5-22).

Figure 5-22 Newly aligned wavelengths aligned and accepted

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5.5.6 Interfering Element Corrections (IEC) Tab

The IEC TAB displays information for the analytical line highlighted in the NAVIGATION
PANEL.
Interfering Element Corrections (IEC) are designed to compensate for spectral overlap.
Adjustments are made to analyte concentration based on the concentration of the
interfering element(s) present in the sample. Any other analyte element in the method
may include an Interfering Element Correction (IEC). Typically, only major constituents
in the sample should be candidates for IECs.
Refer to Section A.1.6 "Interfering Element Corrections (IEC)" for more information on
using IECs.

5.6 Standards
With the METHOD TAB active, click on the STANDARDS/MSA in the NAVIGATION PANEL to
view the standards display.

5.6.1 Add a Standard

1. Click on the ADD STANDARD BUTTON in the center of the display.

Figure 5-23 Adding a calibration standard

2. Enter a name, concentration and units.


3. Select the Update Type to define the standard. Refer to Section 5.6.4 "Update
Standards" for more information.
4. Click the OK button to accept.
5. The standard name will be added to the STANDARDS TABLE and the standard
concentration applied to all the elements in the method. The STANDARD LINES TABLE
displays the method wavelengths, concentrations and status of each wavelength
(checked lines are active) when a standard in the STANDARDS TABLE is highlighted.

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Figure 5-24 Entering calibration standard concentrations

6. Concentrations and units may be customized wavelength by wavelength. To do


this, highlight the relevant standard in the STANDARD NAME TABLE and the relevant
wavelength in the STANDARD LINES TABLE. Type the correct concentration in the
concentration box and note that the concentrations at all wavelengths for that
element are automatically updated.
7. If any of the standards do not contain the entire suite of elements, highlight the
appropriate standard and uncheck the appropriate wavelengths to remove them
from the standard.

5.6.2 Modify a Standard

1. If an existing standard needs to be modified, click on the MODIFY STANDARD button


to display the MODIFY STANDARD DIALOG (Figure 5-25).

Figure 5-25 Modifying standard dialog

When the Modify Standard


Dialog appears, the
concentration field will appear
blank if wavelength specific
concentration variations are
detected - otherwise the base
concentration will be initialized.

The user can enter a value to globally modify the


standard concentration and/or concentration units

2. Make the necessary changes to the standard and click the OK BUTTON to accept the
changes.

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5.6.3 Delete a Standard

To delete a standard once it has been added to the STANDARDS LIST:


1. Highlight the standard in the STANDARD NAME TABLE.
2. Click the DELETE STANDARD BUTTON in the center of the display.
3. The standard will be removed from the STANDARDS TABLE and the method.

5.6.4 Update Standards

Any standard can be assigned as an Update Intercept (UI) or Update Slope (US). The
assignment of Update Intercept and Update Slope standards allows the user to run
multiple updates and update the calibration curves in multiple places.

Add/Modify an Update
To add an update, or to modify an existing standard to be an update:
1. Add standards using the procedures in Section 5.6 "Standards". Once updates have
been added to the method, the STANDARDS/MSA window will look similar to Figure
5-26.

Figure 5-26 Multiple updates in a method

Note the unique identifier ([US4] for example) given


to each update standard.

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Running Updates Using Assigned Frequencies
Updates can be run periodically over the course of a sample sequence and each update
can be run at a different frequency, if desired. These updates are added to the sample
sequence and assigned frequencies in the QC AUTOMATION section under the METHOD
TAB (Figure 5-27).

Figure 5-27 Specifying update frequencies

Each update and check standard can be


assigned a unique frequency.

Running Updates using Cup Macros


Alternatively, updates can be added to a sample sequence using cup macros in the
SEQUENCE TAB. As illustrated in Figure 5-28, cup macros can be concatenated and
individual updates can be assigned using their unique identifiers ([UI1], [US3], etc.). If a
non-unique identifier is entered ([US]), the first update found from the standard index
of that type will be applied.

Figure 5-28 Using cup macros for updates

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Update Data
When updates are run, the update data for each wavelength can be viewed in the
calibration section of the software. With the METHOD TAB active, highlight one of the
wavelengths in the NAVIGATION PANEL and click on the CALIBRATION TAB. Click the UPDATE
DATA BUTTON to view the numerical and plotted update data (Figure 5-29).

Figure 5-29 Display update data

Overwriting Replicates
If updates are being run manually, individual replicates can be over-written:

1. Select the RUN STANDARD button.


2. Select the appropriate update from the STANDARD ID MENU.
3. Place a check in the box to the right of the drop-down menu to run the standard as
an update. Click on buttons 1, 2 and 3 to highlight which replicate/s to overwrite
and click the OK button.

Figure 5-30 Running a specific replicate for a calibration standard

4. When the update standard has been run, the data will automatically populate the
UPDATE DATA window.

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5.6.5 Internal Standards

Internal standards are selected from entered method lines. For more information on
adding internal standards refer to Section A.3 "Internal Standards".

5.6.6 Method of Standard Additions

The Prodigy7 ICP software supports the method of standard additions (MSA). To use the
METHOD OF STANDARD ADDITIONS (MSA) option, refer to Section A.2.5 "Adding a Method
of Standard Additions" for information on adding a MSA.

5.7 Concentration Ratio


Concentration Ratio (CR) computation techniques are generally useful for alloy analysis
of base metal digests. The goal of concentration ratio is to produce an assay report that
has all components add to 100%. The concentration ratio is a ratio of each element
concentration divided by the concentration of a base element. The calibration curves
are plotted as CR versus Intensity Ratios. Where Intensity ratios are calculated with the
denominator being the intensity of the base element for the given repeat of the given
standard. This differs from the use of Internal Standards for three reasons:
1. The concentration level of the base element typically varies between each standard
and sample;
2. The calibration curve for each line element is a plot of CR versus Intensity Ratio, as
opposed to Concentration versus Intensity Ratio;
3. The use of Concentration Ratio allows for only one base element, this is not true
for Internal Standards. When a Concentration Ratio base element is selected the
use of Internal Standards is locked to only one, the base element.
To select the base element line:
1. With the METHOD TAB active, select CONCENTRATION RATIO from the NAVIGATION
PANEL.
2. Select the base element in the METHOD LINES column of the CONCENTRATION RATIO
SCREEN.

Figure 5-31 Setting the base element for concentration ratio

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The calibration curve for each concentration ratio line will reflect the Intensity Ratio in
the Y axis plotted against the Concentration Ratio in the X axis. The coefficients of the
calibration curve are based on this plot. Remember, the coefficients of the curve are not
in terms of concentration. They are in terms of concentration ratio.

Figure 5-32 Calibration curve using concentration ratio

5.8 Quality Control Checks


Each method may contain several quality control sample standards.
1. Highlight QUALITY CONTROL CHECKS (QC) in the NAVIGATION PANEL to view the
quality control standards already available in the method (Figure 5-33).

Figure 5-33 Viewing quality control standards

2. To view the acceptance limits for any QC definition, click on the QC Check name in
the left table and its details will appear in the right table.

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3. Each method is allowed one duplicate definition. Click on the VIEW DUPLICATE
button to see duplicate limits.

NOTE
Headers for the Check Standard Table change when in the VIEW DUPLICATE
mode.

4. After viewing the duplicate limits, return to QC checks or Spikes by clicking on a


check standard or spike.

5.8.1 Add a QC Check

1. Select the ADD QC BUTTON to open the ADD QC DIALOG box.

5.8.2 Modify QC Check Criteria

1. Select the MODIFY QC BUTTON to open the MODIFY QC DIALOG box to make global
modifications.

5.8.3 Modifying QC Acceptance Criteria

1. The acceptance criteria for each QC Check may be modified on a line-by-line basis
by selecting the QC check and entering the new information.
2. Select UPDATE QC to accept the changes.

5.8.4 Delete QC Check

1. Select the DELETE QC BUTTON to remove the highlighted definition.

NOTE
The Delete QC Button is active when an existing QC check is highlighted in the
QC Check Table.

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5.8.5 Extra Volumes for Check Standards

Autosampler sequences containing a large number of samples, or a high frequency of


QC Checks may require a Check Standard liquid volume that exceeds the capacity of a
single cup (resulting in a QC failure). The EXTRA VOLUME feature allows the user to assign
additional QC cups to be used once the ANALYSES PER CUP limit has been reached.

Figure 5-34 Setting up extra volumes for QC standards

To enable the EXTRA VOLUME feature:


1. Select the EXTRA VOLUME REQUIRED check box.
2. Assign how many extra cups and the number of analyses taken from each single
cup.

NOTE
The Extra Volume option is available for each Check Standard.

5.9 QC Automation
QC AUTOMATION is designed to control the application of quality control checks during
automated sequence runs. With the METHOD TAB active, select QC AUTOMATION. The QC
AUTOMATION TAB will display the method name in the top left corner, and three
sequencing tables (Figure 5-35). Clicking ACCEPT will save any changes made to the QC
sequencing.
The QC AUTOMATION S CREEN is divided into three Quality Control check sequence
options:
 INITIAL - BEFORE SAMPLES ARE RUN - Actions that are performed prior to sample
analysis.
 CONTINUOUS - DURING SAMPLE RUN - Actions that are performed continuously
while the samples are being run.
 FINAL - AFTER SAMPLES ARE RUN - Actions that are performed at the completion
of the sample run.

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5.9.1 Initial - QC Standards Before Samples Run

The INITIAL - BEFORE SAMPLES ARE RUN TABLE contains all calibration and quality control
standards.
1. Place a check mark beside the QC standard in the TASK column.
2. Select a failure action from the ACTION MENU. An example of failure actions is
shown in Figure 5-35.

Figure 5-35 QC Automation screen

Automatic Assignment of QC Standard Locations


1. The CUP column allows the placement of Quality Control standards in default or
custom locations. For default locations click the AUTO ASSIGN BUTTON. QC
standards will be given sequenced locations (including any extra QC standards) as
shown in Figure 5-36.

NOTE
Any extra (duplicate) QC standards are identified by an “*” placed after the
standards name. Refer to Section 5.8.5 "Extra Volumes for Check Standards" for
more information.

Figure 5-36 Automatic assignment of QC standard locations

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Custom Assignment of QC Standard Locations
1. Standards and QC Standards can be placed in custom locations by choosing
locations from the drop-down menu in the CUP field, as seen in Figure 5-37.

Figure 5-37 Custom assignment of QC standard locations

An example of Standards and QC Standards being placed in custom location is


shown Figure 5-38. If the total number of Standards/QCs is greater than 14, Salsa
will permit the operator to place them into the sample rack.

Figure 5-38 Custom QC standard locations

Shared Cup Locations


1. Custom placement will also allow Standards and QCs to share the same physical
location in the autosampler rack. A shared location will display a bold circle in the
rack graphic, as shown in Figure 5-38.
In this example, STD0 and the Update Intercept are sharing the first location in the
autosampler rack. Salsa will check to see if the solutions in a shared location are
correct by comparing elements and concentrations. If Salsa finds the solutions
should not share a common location, an error message will be displayed. An
example of an error caused by a mismatch is shown in Figure 5-39.

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Figure 5-39 Example of mismatch shared QC standard error message

A shared cup is identified by a


black ring around the cup.

5.9.2 Continuous - QC Standards During Sample Run

The CONTINUOUS - QC STANDARDS DURING SAMPLE RUN contains all QC standards. QC


standards selected in the TASK COLUMN will be performed throughout the analysis at the
frequency designated.
1. Place a check mark beside the QC standard in the TASK column.
2. Enter a frequency. The FREQUENCY value defines the number of samples to be
analyzed before (or between) the QC standard.
3. Select a failure action from the ACTION MENU.

5.9.3 Final - QC Standards After Samples are Run

ThE FINAL - QC STANDARDS AFTER SAMPLES ARE RUN TABLE contains all QC standards. QC
standards selected in the TASK COLUMN will be performed after the last sample has been
analyzed.
1. Place a check mark beside the QC standard in the TASK column.
2. Select a failure action from the ACTION MENU.

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5.9.4 Post-Calibration Action

In a post-calibration action, the last checked standard in a sequence is used to control


the action assignment (Figure 5-40). A post-calibration action no longer requires the last
added standard to be run in order to accept the calibration or execute the assigned
action. Post-calibration actions provide more automated flexibility in terms of
standardization and updating.

Figure 5-40 Post calibration action

Last Standard
to be run in the
sequence.

Action assignment and auto acceptance of calibrations

5.10 Analytical Parameters


With the METHOD TAB active, select ANALYTICAL PARAMETERS in the NAVIGATION PANEL.
 Integration: Numeric values may be entered into the AXIAL and RADIAL fields.
These times will be used when analytical readings are taken within the
method.

NOTE
The H G L AMP view will always use the A XIAL TIME on an A XIAL or D UAL -VIEW
system.

 Pump: The pump area contains fields for rinse time between samples (when
running a sequence). Select the EXTRA check box to add an additional rinse for
use only after running a sample whose concentration exceeds the calibration
range. Designate the rinse time.

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Figure 5-41 Analytical parameter screen

 Uptake: Uptake is the time required for the sample to travel to the torch. When
running manually, this delay can be disabled in the run dialog.
1. Selecting the FAST UPTAKE option will speed up the pump during the uptake
time.

NOTE
A short stabilization period will follow the uptake time, before integration
begins.

2. Check boxes for weight, volume, dilution and interfering element corrections
must be selected here if desired.
3. Selecting EARLY WITHDRAWAL will extract the autosampler tip from the sample
prior to completion of the last replicate.
4. To work properly, the uptake time must be set accurately. Utilize the uptake
timer tool to assist in setting the uptake accurately.

Figure 5-42 Sample uptake timer

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 Procedure: Selecting the PROCEDURE option takes a full frame echellogram for
each sample run. Select the integration time for each view.
 Summaries: Selecting SUMMARIES creates a spreadsheet summary of the
Method (Figure 5-43).

Figure 5-43 Method data summary screen

5.11 General
With the METHOD TAB active, select GENERAL in the NAVIGATION PANEL to view details of
the method file. Information includes:
 Date the method was created
 Date of last modification
 Who created the method
 Who last modified the method
 The status of the current calibrations
 Recorded method comments
Only Method Comments may be edited.
1. Enter text into the NOTES field
2. click on the UPDATE NOTES button to save

5.12 Creating a SemiQuant Method


The SemiQuant feature will create a method based upon the best wavelengths for each
of 70 elements and an estimated calibration curve based on Teledyne Leeman Lab’s
semi-quantitative standards. The standards are made in two solutions:
1. Set 1 (34 elements)
2. Set 2 (36 elements)

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Refer to the Teledyne Leeman Lab’s website (www.teledyneleemanlabs.com) for more
information on consumables, spare parts and accessories.

NOTE
When using SemiQuant, updates are predefined.

1. With the METHOD TAB active, select METHOD>NEW from the MENU BAR.
2. Type the appropriate names under the METHOD NAME and ANALYSIS CHAPTER NAME
fields, respectively. Add any useful method notes.

NOTE
Method Notes may be helpful in identifying the method in the Open Method
Dialog. Refer to Figure 5-3.

3. Put a check in the SEMIQUANT box at the bottom of the window (Figure 5-44).
4. Click the OK BUTTON when finished.

Figure 5-44 New method dialog - semiquant

Similar to other methods, the wavelengths in a semiquant method must be aligned


before they can be used (most of the wavelengths will most likely have not been
previously used). Refer to Section 5.5.5 "Align Wavelength Tab" for information on
aligning wavelengths.
Once the wavelengths are aligned the new SemiQuant method can be used for sample
analysis using the predefined calibration curves. The user may also choose to run an
update on the calibration curves using a multi-element standard.

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To update the predefined calibration curves:
1. Click on the RUN STANDARD button.
2. Select the appropriate standard from the STANDARD ID MENU and select the RUN AS
USQ option. The window will look similar to Figure 5-45.

Figure 5-45 Running a semiquant update standard

3. Aspirate the QC soup solution and click the OK button to run the SemiQuant
update.
Running the QC soup will allow the software to calculate updates for the base lines
as marked on the method SemiQuant screen shown in Figure 5-46. Salsa will use
these update values and ratios to determine new values for all wavelengths in the
method.

Figure 5-46 Calculating semiquant ratios

NOTE
If the CALCULATE R ATIOS button is selected, the software will calculate ratios
between the original and updated slopes for each wavelength.

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Prodigy7 User Manual
Chapter 6: Sequence
6.1 Sequence Overview
For information on creating a sequence refer to Section 2.14 "Build Sequences".
The S EQUENCE TAB is used to define automated sequences. The S EQUENCE S CREEN
consists of three primary areas:
 SAMPLE LIST TABLE
 SEQUENCE TREE (in the NAVIGATION PANEL)
 RACK MAP

Figure 6-1 Sequence tab

Sequence Tree
The Sample List Table

Rack Map

NOTE
All Salsa software selections for this chapter are located under the Sequence
Tab in the Navigation Panel unless otherwise noted. Menu Bar selections
referred to in this section may only be available when the Sequence Tab is
selected.

6-1
6.1.1 Editing Tools

The rack file can be edited using right-click tools and icons above the rack entry table.
 Auto Fill: Automatically fills the SAMPLE ID field by copying the sample name
entered in the first selected field into the rest of the selected fields.
 Sequence # Fill: Similar to the Auto Fill function, with the addition of a number
to the end of the sample name. The interval is decided by the user.
 Toggle Individual Samples On/Off: Turns samples On/Off so they can be
omitted from a sequence run.
 Toggle All Samples On/Off: Turns all the samples On/Off
 Insert/Delete - Insert or delete samples by right clicking on a sample row. A
INSERT/DELETE DIALOG will open.
 Print Rack File: Prints the current rack file.
 Toggle Cursor “right” or “down”: Changes whether the cursor moves to the
right or down when the ENTER key is pressed.

Figure 6-2 Rack edit tools

Toggle Cursor to Move Toggle All


“right” or “down”, after Samples
pressing “enter” On/Off
Toggle individual
Samples On/Off Sequence # Fill Autofill Print Rack File

Right Mouse click menu edit tools

6.1.2 Sample List Table

The SAMPLE LIST TABLE contains:


 Sample IDs (simple and extended), weights, volumes, dilutions, as well as
special cup macro commands.
 Locations in the autosampler for each sample are defined in the CUP column.
Values in parentheses in the CUP column represent the sample rack number
and the second value represents cup location within the rack.

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Sample Weights, Volumes, and Dilutions
The rack file allows the user to enter correction factors for weight, volume and dilution.
The weight and volume correction will account for the following dilutions:
 Weight to weight
 Weight to volume
 Volume to volume

Correction Factors
To correct for a dilution:
1. Enter the sample’s weight (or volume) into the Wt. column
2. Enter the final weight (or volume) into the Vol column. The dilution factor will be
applied to the sample’s results.
A second correction factor called “Dilution” is located in the autosampler rack file. The
correction will simply multiply the sample’s result by whatever value is entered in the
column. For example, if the values entered into the Dilution column is 100 and the
sample result is 0.356, the corrected sample result will be 35.6. If there are values entered
in the Wt and Vol columns, they will also be applied to the final result.

NOTE
Before any of the correction factors are applied, it is necessary to check the
appropriate boxes on the Analytical Parameters Screen (make the Method Tab
active, then select Analytical Parameters).

Figure 6-3 Weight and volume corrections

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6.1.3 Sequence Navigation Panel

1. The SEQUENCE NAVIGATION PANEL displays a SEQUENCE TREE containing each


operation planned, in the anticipated order. It combines standards and quality
control checks from the method and samples from the SAMPLE LIST TABLE
(including cup macro actions).

NOTE
When a calibration curve or a quality control check falls outside acceptable
limits, the anticipated order of analysis will change based on the failure action
defined in Method Tab>QC Automation Screen. Refer to 5.9 "QC Automation".

Figure 6-4 Sequence tree

6.1.4 Rack Map

The rack map shows the location of samples and standards graphically. Move the cursor
over a mapped location and a tool tip with the sample or standard name will appear.
 The RACK MAP and the SAMPLE LIST TABLE’s CUP column are defined by the rack
type.

Figure 6-5 Autosampler rack map

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6.1.5 Editing the Rack While Running a Sequence

Additional samples can be added while a sequence is running. Add samples in the same
manner as building the sequence sample list. Refer to Section 2.13.1 "Add Samples".
1. Once new entries are added to the rack, click the Update button to prompt the
autosampler to run the new samples when it reaches the cup positions.

NOTE
Any samples that had been updated into the SEQUENCE TREE using the UPDATE
button cannot be edited. The samples are locked to the sequence run and the
rack editing fields are displayed in gray to avoid editing.

Figure 6-6 Sample sequence “locked in”

Figure 6-7 Additional sample added to sequence

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6.2 Sequence Methods
The SEQUENCE METHOD feature permits the operator to analyze samples using two
different methods during the same autosampler run. Each method is set-up and
configured separately and then linked together in the SEQUENCE TAB.
Before the methods are linked, calibration standards, updates and check standards must
be created and assigned autosampler locations as shown in Figure 6-8.

Figure 6-8 QC Standard locations set in two methods

Linked methods can share locations for standards, updates or check standards provided
there is at least one common element and concentration in any shared solution.
If a location is shared and there are no common elements and concentrations, Salsa will
display a warning highlighting the solution(s) that are mismatched (Figure 6-9).

Figure 6-9 Standard or QC mismatch error message

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6.2.1 Set-Up a Sequence Method Run

1. Open the first method to be used in the sequence by making the METHOD TAB
active, then selecting METHOD>OPEN from the MENU BAR(Figure 6-10).

Figure 6-10 Select the first sequence method

2. Next, select the SEQUENCE TAB.


3. To select the second method, select SEQUENCE from the MENU BAR, then select SET
SEQUENCE METHOD (Figure 6-11).

Figure 6-11 Select set sequence method

4. Select the second method to be used from the SET SEQUENCE METHOD DIALOG
(Figure 6-12).

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Figure 6-12 Select the second method

The standards and check standard for both methods are then displayed in the
autosampler rack graphic.

NOTE
The second method’s standards and QC Standards are easily recognized by the
gray square behind them (Figure 6-13).

Figure 6-13 Second method standards and QCs added to rack map

A gray square denotes


standards and QC
standards associated
with the second
method.

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5. Add the samples for the first method (Figure 6-14). Refer to Section 2.14 "Build
Sequences" for information on adding samples.

Figure 6-14 Samples added for the first method

6. Add the samples for the second method. Refer to Section 2.14 "Build Sequences"
for information on adding samples. Once samples have been added:
 Type the letter “M” into the CUP MACRO field of the first sample.
 Click the UPDATE button (Figure 6-15).

NOTE
The second method’s samples are easily recognized by the gray square behind
them(Figure 6-15).

NOTE
It is not necessary to place the samples for the second method immediately
after the samples of the first method. Having empty positions between the
two method’s samples will allow the operator to add additional samples to the
first method after the run has already begun. If there are available positions,
additional samples for the second method can be added after the run has
started.

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Figure 6-15 Samples added for the second method

A gray square denotes samples associated with the second method.

7. Click the RUN SEQUENCE BUTTON to begin the analysis.


8. The EXTINGUISH PLASMA BUTTON can be set to take effect after the second method’s
samples have been completed (Figure 6-16). With the METHOD TAB active, select
INSTRUMENT CONTROL from the NAVIGATION PANEL.
1. Select the EXTINGUISH AFTER RINSE option under PLASMA CONTROL.
2. Select a delay time from the DELAY MENU.

Figure 6-16 Setting the extinguish plasma option

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6.3 Cup Macros (Flexible QC Automation)
Each sample may be programmed with a variety of special macro operations. Below is a
list of the macro operations available and examples of how they would work.

NOTE
The macro commands are case sensitive, use the upper case only.

6.3.1 Available Cup Macros

Table 6-1 Cup Macro Commands


Macro Command
A Apply% recovery
C1...C7 Run check standard #1 through
CP Run a sample analysis on this cup. This
field is only needed if the sample cup is
NOT the first item in the list. Allows defin-
ing the sequence of operations when the
Runner is to run this cup position. See
Example 2: Use of the "CP" Action below
CxRy Run check standard “x” with “y” replicates
D This cup is a duplicate
P Calculate% recovery
S Spiked
S1...S7 This cup is spikes #1 through 7
U Unspiked
UI1...UI33 Run an Update Intercept #1 through 33
US1…US33 Run an Update Slope #1 through 33

6.3.2 Cup Macro Examples

Example 1: A typical Cup Macro Action Indicator List


 S1 C2 US
This would result in the following sequence of events when the cup was analyzed:
 The sample cup would be run as a “spiked” sample
 A percent recovery calculation would be performed
 Check standard 2 would be run
 An Update Slope would be run

Example 2: Use of the "CP" Action


 C1 CP UI

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NOTE
The “CP” is necessary because the sample is not the first cup to be run.

This list would result in the following sequence of events:


 Check standard 1 would be run
 The sample cup would be run
 An update intercept would be run

6.3.3 Multiple Updates Using Cup Macros

Figure 6-17 shows the use of multiple updates assigned as CUP MACROS.

Figure 6-17 Using cup macros

Cup macros can be concatenated

Individual updates can be assigned by cup macro using its unique identifier
[US3]. If a non-unique identifier is entered [US] the first update found from
standard index 0 of that type will be applied.

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Figure 6-18 Using the “CP” cup marco command

The cup macro command “CP” enables placement of


other cup actions relative to the sample cup.

6.4 Synchronizing External Hardware to Sample Sequence


Salsa allows the control of external hardware via the sequence of sample runs, as if a
pseudo autosampler. An example of this, would be using a laser ablation system as a
sample introduction to the ICP. This feature is optional and, if needed, must be installed.
Contact Teledyne Leeman Labs for more information. Refer to Section A.6
"Synchronizing External Hardware to Sample Sequence" for information on this
procedure.

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Chapter 7: Analysis
7.1 Analysis Overview
When the ANALYSIS TAB is selected, acquired results for the active method are displayed.
The results are displayed in a variety of formats when one of the tabs (Figure 7-1) is
selected.

Figure 7-1 Analysis tab

NOTE
All Salsa software selections for this chapter are located under the Analysis Tab
in the Navigation Panel unless otherwise noted. Menu Bar selections referred
to in this section may only be available when the Analysis Tab is selected.

7.2 Results Tab


The RESULTS TAB can be displayed in DETAILED or STATISTICS view by clicking on the radio
buttons.
 The DETAILED view displays: Sample Name, Element symbol, Wavelength,
Concentration, Corrected Intensity, Left background intensity, Right
background intensity, and Raw peak intensity.
 In STATISTICS view displays: Sample Name, Element symbol, Wavelength,
Mean, SD, RSD, and Units. The table is populated with data when an analytical
reading is taken and appear in chronological order. Analytical readings include
calibration and check standards, samples, and MSA spikes.

7-1
Figure 7-2 Results tab

 Entries in the RESULTS TABLE appear in the NAVIGATION PANEL as sample names
only.
 Selecting a sample in the NAVIGATION PANEL will display results for the
highlighted sample in the RESULTS TABLE.
 When the contents of the RESULTS TABLE (or the NAVIGATION PANEL) exceed the
display limit, scroll bars will appear.
 The RESULTS TABLE can be printed at any time by clicking the PRINT BUTTON.

7.2.1 Show/Hide Items in the Analysis Tree

Hide Items
Samples, Standards and QC Standards can be removed from view in the NAVIGATION
PANEL.
1. Highlight a chapter heading (folder) in the NAVIGATION PANEL
2. Select entries to hide in the RESULTS TABLE (Figure 7-3).
3. The selected items will be removed from the ANALYSIS TREE in the NAVIGATION
PANEL. The items will still appear in the RESULTS TABLE with an asterisk beside each
hidden item.

NOTE
The folder graphic changes appearance when an entry is hidden (Figure 7-3).

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Figure 7-3 Hidden items

Standard Folder

Folder with
hidden items

An asterisk denotes the item is hidden

Show Items
1. Select samples in the RESULTS TABLE.
2. Click the SHOW BUTTON.
3. The selected items will be displayed in the ANALYSIS TREE in the NAVIGATION PANEL.
4. Clicking the SHOW ALL BUTTON will show all analysis items in the ANALYSIS TREE
(without the need to highlight each item in the RESULTS TABLE).

7.2.2 Renaming Samples and Analysis Items

Figure 7-4 Renaming samples

Highlight the
chapter while
viewing the
Results Tab

Select the Rename Button to rename an analysis item (and all replicates)

The history of renaming can be viewed as shown in Figure 7-5.

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Figure 7-5 Sample renaming history - traceable renaming structures

Select “Name History” to view the history of an analysis name.

7.2.3 Display Modes

The RESULTS TAB can display analytical data (selected from the NAVIGATION PANEL) in
SINGLE or ALL formats:
 SINGLE displays results one sample at a time by selecting the item in the
NAVIGATION PANEL.
 ALL displays all results at once. A scroll bar will appear to the right of the
RESULTS TAB. When an item is selected in the NAVIGATION PANEL the RESULTS TAB
will jump forward to that item.

NOTE
The use of Single viewing greatly speeds the Analysis Tab refresh rate when
large numbers of samples and/or chapters exist.

THE SINGLE/ALL display modes for the RESULTS TAB are shown in Figure 7-6 and Figure
7-7.

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Figure 7-6 “Single” display tab results

Figure 7-7 “All” display tab results

7.2.4 Searching for Existing Results

Select the SAMPLE SEARCH BUTTON to search for results in the Salsa database. The
SAMPLE SEARCH DIALOG will be displayed (Figure 7-8).
Type the name of the sample into the SAMPLE ID text box and all results with that string of
characters will appear in the field. Search results will display:
 Full sample name
 Date and time the sample was analyzed
 Method and chapters under which the sample data was collected

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Figure 7-8 Sample search results

NOTE
Search results can be narrowed by putting check marks in the BEGINNING DATE
and ENDING DATE boxes and selecting appropriate dates.

7.3 Scans Tab


The SCAN TAB provides the ability to compare the intensity profile (the intensity on and
off peak) of different samples and standards.
The scans displayed correspond to the samples/standards checked in the NAVIGATION
PANEL and the wavelengths selected using the LINE MENU. The LINE MENU contains all
the wavelengths that have been added to the method. The S CAN ID TABLE displays
samples and standards selected in the NAVIGATION PANEL along with the numerical
background corrected peak height. The LIST OF POTENTIAL INFERENCES below the SCAN ID
TABLE indicates wavelengths of elements that are potential interferences (Figure 7-9). To
review scans:
1. Place a check mark in the box beside the sample/standard to view its intensity
profile.
2. The intensity profile for each sample selected in the NAVIGATION PANEL will be
assigned a unique color ID. This color is shown both in the SCAN ID TABLE and the
scan display for easy identification.

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Figure 7-9 Overlaying wavelength scans

Select samples or
standards to The Line Menu contains all the wavelengths that have been added to the method.
include in the
overlay
wavelength scan
results by placing a
check mark beside
the sample or
standard.

The Scan ID Table


displays the samples
and standards
selected in the
Navigation Panel.
The color of each
sample/standard
corresponds to the
wavelength scan
graphic depiction.

A graph depicts the background corrected peak height


The List of Potential Inferences
indicates wavelengths of elements
that are potential interferences.

3. Click on the LINE MENU to select the wavelength to be displayed. Arrow keys or a
scroll wheel can be used to quickly navigate the LINE MENU.
4. The numerical background corrected peak height is shown in the SCAN ID TABLE
and a graphic depiction is shown beneath the intensity profile. Green regions
depicting peak and background points can be manipulated by placing the cursor
on that region and dragging.

NOTE
Changes made to the scans will be applied to the current method. Points may
be relocated, expanded or contracted.

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5. To compare scan concentrations:
1. Highlight a scan in the Scan ID TABLE.
2. Enter the concentration in the text box to the right of CONCENTRATION.
3. Clicking on any of the other Scan IDs in the table will display their relative
concentration in the text box.
6. Click the CLEAR ALL BUTTON to deselect all samples.
7. Clicking the PRINT BUTTON will print the display.

7.4 Profiles Tab


The P ROFILES TAB will display thumbnail spectral plots at each of the analytical
wavelengths in the method when a sample is selected in the NAVIGATION PANEL. Multiple
samples may be displayed simultaneously. Clicking on any of the profiles will display the
wavelength’s individual scan.

Figure 7-10 Thumbnail wavelength scan profile

7.5 Calc. Validation Tab (Raw Data)


The C ALC .VALIDATION TAB displays raw data in a table with subsequent intensity
calculations. The numbers below correspond to the numbers in the Figure 7-11.
1. The top row displays the emission intensities for each of the pixels in the subarray
appear.
2. The second row re-displays these intensities for selected peak and background
correction points.
3. The next three rows summarizes the intensities for the left background correction
point, the right background correction point, and the peak average in the second
column.
4. The third row displays the calculated background intensity at each pixel.
5. Peak intensities are re-displayed after subtracting the calculated background
intensity.
6. The last row displays the average corrected peak intensity.

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Figure 7-11 Raw subarray data

Region of
Background Interest (ROI) Background
Correction Correction
Points Points

7. The bottom of the display a graph depicts:


1. Red bars indicate total intensity for each pixel with a black line depicting the
calculated background intensities.
2. Green bars the Region of Interest (ROI) where the analytical peak is measured.
3. Blue bars depict selected background correction points.

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7.6 Image Tab
The IMAGE TAB displays the spectrum as it appears on the detector. For echellogram
spectra, the entire detector surface is displayed (The Prodigy7 ICP displays segments
centered at method lines).
For sample analysis, calibration, or quality control readings (non-echellograms), only
the subarray areas specified in the active method are reported. The physical location of
each subarray on the detector appears when the data for these readings is viewed on the
IMAGE TAB.

Figure 7-12 Example of full frame image

Method
Line
Selected

Image
Name

Subarrays identified by
element and wavelength.

In Figure 7-12, each pixel is represented by a color. Darker colors indicate pixels with
lower intensity counts while lighter colors indicate pixels with higher intensity counts.
 Moving the cursor over the image will display X: and Y: pixel locations.
 If the cursor is positioned over a method subarray, the element and
wavelength are displayed. Clicking on the “Method Lines” will display all the
subarrays identified by element and wavelength.
 Clicking on the detector image will automatically center that pixel location in
the display.
 The name of the image is displayed just above the CONTRAST button. This file
name can be used to search through the Salsa directory folder for the source of
the image.

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To use the IMAGE TAB controls:
 The ZOOM MENU allows for viewing the whole detector area or expanding the
view for a smaller portion of the detector.
 The RESET BUTTON will reset the echellogram image to its original position and
zoom level.
 The CONTRAST BUTTON displays the emission logarithmically so that less
intense emissions can be seen.
 The IDENTIFIER BUTTON will show emission lines in the vicinity of the cursor
location.

NOTE
To simplify the evaluation of echellograms, spectral images may be added
together or subtracted.

 The DISPLAY button will show lines by element.


 The METHOD LINES button will display the method subarray locations.

7.6.1 Fingerprint Spectra (QA Mode)

QUALITATIVE A NALYSIS is a post-analysis scanning mode for full echelle images that
compares detected peaks against preferred and aligned library lines to calculate a
probability report of elements present. The report presents all the detected wavelengths
sorted in the order of probability for easy display and review.
This tool has great usefulness following a spectral subtraction of a reference or blank.
Applications include forensics, stat samples, method development.
1. Select the image from the ANALYSIS TREE in the NAVIGATION PANEL.
2. Click the QA BUTTON to display the QUALITATIVE ANALYSIS DIALOG (Figure 7-13).
3. The PROBABILITY REPORT (Figure 7-14) will show a list of all detected elements and
their wavelengths.

NOTE
Wavelengths with an “A” beside them indicate they are aligned.

4. Select the detected peak wavelengths in the PROBABILITY REPORT, for review
(Figure 7-14).

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Figure 7-13 Selecting a full frame for QA

Figure 7-14 QA probability report

Probability Report

Detected Peak
Wavelength
Selected

“A” Indicates the wavelength is aligned

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7.7 Control Chart (Crtl Chrt) Tab
The CONTROL CHART TAB provides tools to plot selected samples or quality control checks
along with desired markers. To use the Control Chart:
1. Place a check mark beside the samples or standards in the NAVIGATION PANEL to
include in the plot.
2. Click on the LINES BUTTON and select the wavelengths to include (11 wavelengths
maximum). At any point in time selected wavelengths can be highlighted and the
display for that wavelength can be toggled off/on, or the wavelength can be
removed from the selected line list.
3. Use the selection of buttons on the CONTROL CHART TAB to adjust the values
displayed. Button functions are listed in Table 7-1 "Control Chart Button
Functions"

Table 7-1 Control Chart Button Functions


Button Function
MARKERS Add specific or calculated values (such as
mean or standard deviation)
HARDWARE Allow the selection and display of moni-
tored hardware items
ARROW LEFT/RIGHT Move the display cursor within selected
entries and provide numerical display for a
given sample
CLEAR ALL Remove all lines and samples from the dis-
play
ZOOM Expand the region highlighted
UNZOOM Return the display to full view
NORMALIZE Sets readings to 100%
TOGGLE PT Remove the point where the cursor
resides from the display

In Figure 7-15, the 5 ppm solution is run as a sample and an update slope standard. Also
appearing on the plot are the calculated mean and 3X the standard deviation for the
highlighted wavelength.

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Figure 7-15 Control chart data

7.8 Report Tab


The REPORT TAB is used to configure and generate reports.
The LINE TABLE contains wavelengths lines included in the report. The ITEMS TABLE lists
reportable data types. Select wavelength lines from the LINE TABLE and data types from
the Item table to include in the report. As each item is selected, they will be added to the
report below.
A fully configured report looks similar to Figure 7-16.

Figure 7-16 Report criteria

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To configure and generate a report:
1. Place a check mark in the box beside the samples and standards in the NAVIGATION
PANEL you want included in the report. Use shift + left click to define first and last
entries to select all entries between the two. Options for controlling and filtering
analysis types included in the report, are explained in Section 7.8.1 "Report
Control and Filtration".
2. Use the radio buttons to choose between DETAILED and STATISTICS views.
 The STATISTICS view will display summary results for multiple replicates.
 The DETAILED view will display data for each replicate
3. In the LINE TABLE, place a check mark in the box beside the analytical wavelength
lines to include in the report.
4. In the ITEMS TABLE, place a check mark in the box beside the data type to be
included in the report.
5. Use the selection of buttons on the REPORT TAB to customize displayed data and
output custom reports. Button functions are listed in Table 7-2 "Report Data
Selection Button". Additional data customizations are explained in and Section
7.8.2 "Report Limits and Averaging" and Section 7.8.3 "Report Precision
Customization".

Table 7-2 Report Data Selection Button


Button Function
ALL - LINE TABLE Include all wavelengths
CLEAR ALL Remove all sample and standard selec-
tions
DEFAULT - ITEMS TABLE Populate the ITEM TABLE with Sample ID,
(When detailed view is Line, Concentration, Intensity and Units in
selected) the detailed view
DEFAULT - ITEMS TABLE Populate the ITEM TABLE with Sample ID,
(When Statistics view is Line, Mean, Deviation, RSD, and Units in
selected) the statistics view
DETAILED Display data for each replicate
LT STATISTICS Calculates statistics across samples with
the same sample ID
NONE- ITEMS TABLE Clear all the selected items in the REPORT
TABLE
NONE - LINE TABLE Exclude all wavelengths
STATISTICS Display summary results for multiple repli-
cates.

6. When the report has been configured choose a report format and a type of output.
Report formats are explained in Section 7.8.4 "Report Formats and Outputs".

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7.8.1 Report Control and Filtration

Use REPORT CONTROL to limit the sample types available for reporting on the REPORT TAB.
Only sample types that are permitted can be selected on the A NALYSIS TREE in the
NAVIGATION PANEL. Restricted sample types will be visible, but cannot be selected to
include in the report.
By configuring sample types through REPORT CONTROL, a report can be generated from
an analysis chapter (rather than making individual sample type selections). Only those
sample types selected in Report Control will be included in the report.

NOTE
Report Control must always be defined. If a sample type cannot be added to a
report, first ensure it is included under Report Control.

1. With the ANALYSIS TAB active, select ANALYSIS >REPORT CONTROL in the MENU BAR.
2. Click on each item to include or exclude it from the ANALYSIS TREE in the
NAVIGATION PANEL.

Figure 7-17 Report control menu

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7.8.2 Report Limits and Averaging

REPORT TYPES limit, average are used to enhance the ability to report results. Once the
REPORT TABLE is populated, REPORT TYPE and REPORT CONTROL options appear beneath
Analysis on the MENU BAR.
REPORT TYPE contains two options:
 Conc. Limits - Numerical results appear with print limits. Print limits are
defined under METHOD TAB>ELEMENT SELECTION>WAVELENGTH LINE>GENERAL
TAB.
 Conc. Average - Numerical results appear as a calculated value.

NOTE
Report types apply to the report generator results, as well as, the Results Tab.

Figure 7-18 Selecting the report type

7.8.3 Report Precision Customization

Report precision modes determine what numerical reporting format is used, and how
many significant values are included in the analysis results and REPORT TAB values.
Select Analysis from the MENU BAR and choose REPORT PRECISION from the drop-down
menu selection. Precision formats are given in two formats:
 “F” formats are fixed precision
 “G” formats automatically switch to scientific notation
The number associated with each format determines the number of decimal points.

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Figure 7-19 Changing the report precision mode

Select a precision
mode to update
Results and Report
Tab values.

Precision format examples are displayed here.

Figure 7-20 Scientific notation mode

The precision format


“G” will switch to
scientific notation to
preserve significant
figures.

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Figure 7-21 Blank subtraction set-up

1) Check samples to 2) Select “Blank 4) Click “Set” Blank


report in the Analysis Subtraction” as a Subtraction button
Tree report item

5) Select
type of
output.

3) Highlight a
sample to be
used as the
blank

7.8.4 Report Formats and Outputs

The report generator has two formats available. Refer to Table 7-3 "Report/Output
Button Functions" for a description of each. Both formats can be printed or saved as a
CSV file.

Table 7-3 Report/Output Button Functions


Button Function
Format 1 This format coordinates well with a
spreadsheet program (such as Excel)
Format 2 This format is typically better for printed
reports.
Printer Send the configured report to the default
printer.
CSV Generates a Comma Separated Values
(CSV) file. CSV files are a useful file
exchange format.

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Figure 7-22 Format 1 report example

Figure 7-23 Printed example of format 1 report data

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Figure 7-24 Format 2 report data

Figure 7-25 Printed example of format 2 report data

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7.8.5 Saving/Loading/Deleting Report Specs

Once a report’s specifications have been determined, they can be saved as a Report Spec
template for future use. Saving a report spec is convenient for frequently generated,
customized reports. The saved report will automatically include preset reporting
selections (wavelength lines, data types, precision, etc.).

Figure 7-26 Report spec options

Save a Report Spec


1. Make all report selections and then click the SAVE BUTTON in the Report Spec
section of the REPORT TAB.
2. The REPORT SPEC DIALOG will appear.
3. Name the report, and click OK.

Load a Saved Report Spec


1. Click the LOAD BUTTON in the Report Spec section of the REPORT TAB.
2. Select the desired Report Spec to load and click OK.
3. The report specifications will be automatically populated.

Delete a Saved Report Spec


1. Click the DELETE BUTTON in the REPORT SPEC section of the REPORT TAB.
2. Select the desired Report Spec to delete and click OK.

7.8.6 Quick Report


The REPORT TAB can be used in a quick report configuration (Figure 7-27).
1. Select the REPORT TAB.
2. Select the samples of interest in the ANALYSIS TREE in the NAVIGATION PANEL.
3. Click the ALL BUTTON to automatically select all wavelengths in the method.
4. Click the DEFAULT BUTTON to select a default set of report items.
5. Click either FORMAT 1 or FORMAT 2 to report the data in columns or tables,
respectively. Refer to Section 7.8.4 "Report Formats and Outputs", for more
information on report formats.
6. Click either the PRINTER or CSV BUTTON to generate a report in a hard copy or
electronic format, respectively.

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Figure 7-27 Creating a quick report

7.8.7 Sequence Reporting

SEQUENCE REPORTING allows the user to review and report results from a method other
than the one that is currently running. This feature is only enabled when Salsa is running
a sequence using another method. To access Sequence Reporting:
1. Select the ANALYSIS from the MENU BAR, then select then SEQUENCE REPORTING.

Figure 7-28 Starting sequence reporting

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2. Select the method to be reported from the OPEN SEQUENCE REPORTING METHOD
DIALOG:

Figure 7-29 Open sequence reporting method dialog

3. Once the method is selected, Salsa enters SEQUENCE REPORTING mode. This is
indicated at the bottom of the NAVIGATION PANEL (Figure 7-30), replacing the
standard METHOD, SEQUENCE AND ANALYSIS TABs.

Figure 7-30 Sequence reporting mode

4. The REPORT TAB can now be used to create reports or generate CSV files (Figure
7-31). While sequence reporting is enabled, other tabs with the ANALYSIS TAB can be
viewed, but the data cannot be changed.

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Figure 7-31 Report generated using sequence reports

5. If SEQUENCE REPORTING mode is used when an analytical sequence is not underway,


an error message will be shown (Figure 7-32).

Figure 7-32 Sequence reporting error message

7.9 Recalculate Tab


Changes may be made to the active method and applied to previously acquired data. For
example, a background correction point may be moved after standards and samples
have been analyzed. The calibration curve will automatically be updated to reflect the
changes and selected results can then be recalculated based on the changes made.
R ECALCULATE TAB button functions are shown in Table 7-4 "Recalculate Button
Functions". An example of the RECALCULATE TAB is shown in Figure 7-33 "Recalculation
tab".

Table 7-4 Recalculate Button Functions


Button Function
ACTIVATE METHOD Brings forward older methods.
CLONE Allows a copy of the method (prior or cur-
rent form) to be generated without associ-
ated sample readings.
PRINT Prints the sample data from the window
above.
REVIEW METHOD Used to look at the method at any point in
its development.

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1. Make a change to the active method and apply (or save) it.
2. Select the RECALCULATE TAB and select samples to be recalculated. The order that
the samples are checked determines the order of the recalculated data.

NOTE
When one of the samples is selected in the Navigation Panel all of its analyses
details are displayed. These details will not appear when a recalculated sample
is highlighted.

3. Once all samples to be recalculated have been selected, click the RECALCULATE
BUTTON. Many changes such as changing standard concentrations, background
correction points, and the fit type on the calibration curve require recalculation.

NOTE
Changes to weight, volume and dilution, do not require recalculating
the calibration curve.

It is important to recalculate calibration standards prior to recalculating samples


in some cases. Recalculated standards and samples populate the NAVIGATION PANEL
as a new set of data. Each recalculated sample appears in the NAVIGATION PANEL
within a red border to indicate the data has been recalculated.

NOTE
Historical data is never removed.

Figure 7-33 Recalculation tab

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7.10 Collecting Echellograms
1. Select the ECHELLE BUTTON to open the RUN FULL FRAME DIALOG (Figure 7-34).

Figure 7-34 Run full frame image dialog

2. Enter the sample name, the length of time the exposure will be collected.
 The uptake time specified on the ANALYTICAL PARAMETERS SCREEN (with the
METHOD TAB active select ANALYTICAL PARAMETERS in the NAVIGATION PANEL)
can be bypassed by deselecting the Uptake check box.
3. Select OK and the instrument will acquire the Echellogram.

7.11 Archiving Analytical Data


The speed of ANALYSIS TAB data may diminish as the database increases in size. The
maximum size of the Salsa database is 2GB. To keep an acceptable performance speed it
is recommended that the database be archived once its size begins to approach 1GB. For
information on archiving a database refer to Section A.5 "Database Manager".

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Chapter 8: Maintenance Procedures
8.1 Routine Maintenance
Certain routine maintenance tasks are essential for proper instrument performance.
Following a predetermined schedule will ensure best data quality, and will minimize
down time and repair costs. Failure to perform these simple routine maintenance tasks
will degrade your analytical performance and possibly damage your instrument.

NOTE
Damage to the instrument caused by inadequate maintenance may not be
covered under the service contract. The camera is the most expensive
component in the instrument, proper operation and maintenance is critical to
avoid damage.

8-1
8.2 Instrument Maintenance Log
Maintaining an instrument log whenever you replace or service the Prodigy7 (pump
tubing, nebulizer, torches, etc.), can be an invaluable tool when problems are
encountered.
A typical maintenance log should contain the following information:

Table 8-1 Maintenance Log


Camera:
1. Purge gas dehydrator
Nebulizer:
1. Adjustment (If applicable)
2. Cleaning
3. Inspection
4. Optimization parameters for the plasma recorded when adjusted
Pump and Pump Tubing:
1. Pump tubing maintenance
2. Adjusting pump tension
3. Pump rollers
4. Optimization for the plasma
Sample Introduction Assembly:
1. Removal and replacement
2. Torch disassembly
3. Spray chamber disassembly
4. Assembly and alignment
5. Cleaning procedures
RF Oscillator Water Recirculation System:
1. Filling the water system
2. Flushing the water system
3. Performing a chemical wash and rinse
4. Recirculator maintenance
5. Filter cleaning and replacement
Camera Water Cooling System:
1. Filling the water system
2. Flushing the water system
Air Cooling System:
1. Cleaning the air filter
2. Ventilation requirements

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8.3 Maintenance Schedule

8.3.1 Attention Items

Camera cooling system should always be ON when the instrument is ON. This is
important because the camera cooling system removes heat from the camera’s
solid-state chilling system located inside of the camera body. Failure to keep the camera
cooling system ON will result in overheating the camera body and potential failure of the
camera.

NOTE
The camera cooling system should never be set to below 20 °C. Low
temperatures can cause condensation on the camera body. Temperatures near
freezing (0 °C) can cause the distilled water to freeze in the chiller. Frozen
chiller water will not pump and the camera will overheat!

The camera cooling system requires removal of heat via a secondary external water
recirculator. The external water recirculator must ON anytime the camera cooling
system is ON.
Always use distilled water in the RF oscillator water recirculator and the camera cooling
system. Never use anti-freeze products. Deionized water can cause premature failure of
the pumps.

NOTE
Special attention is required when changing argon gas supplies or when first
installing the Prodigy7 ICP instrument. Moisture contamination inside the
purged volume of the camera can cause ice crystals to form. Ice crystals on the
camera chip surface may cause damage to the device. Refer to Section 8.4.5
"Purge Gas Cylinders Replacement" for details of changing argon gas supplies.

8.3.2 Prior to Start Up

1. Check pump tubing and replace if worn (typical life span is ~40 hours)
2. Check sample introduction system and ensure uptake and drain flow. For
self-aspirating types, such as concentric nebulizers, verify that NO uptake occurs
when the nebulizer pressure is ON and the pump is OFF.

NOTE
Nebulizers should always be force fed from the pump and not allowed to
self-aspirate. Self-aspiration will result in reduced analytical precision. This is
particularly true with samples of varying viscosity.

3. Turn ON argon gas supply.

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Caution

If the argon gas has been shut off to the instrument for longer than one hour
do not start the Salsa software until the argon gas has been on for four hours.
Argon gas supplied to the instrument purges the camera and prevents
damaging ice crystals from forming.

NOTE
If the instrument has been connected to nitrogen for purge make sure the
purge gas has been turned on.

4. Check water level in Camera Water Cooling System.


The Prodigy7 ICP is equipped with an internal water reservoir to cool the camera.
The reservoir is located on the left side of the instrument. Ensure the reservoir is
full and fill, if necessary. Refer to the "Camera Water Cooling System Fill
Procedure".
5. Turn ON the external water recirculator.
6. Replace rinse solution (acid matrix of samples is acceptable).

8.3.3 At End of Day

1. Clean sample introduction using on line cleaning by aspirating clean solvent


(acidified water or organic solvent) for ten minutes prior to shutdown. Follow the
solvent cleaning with a deionized water rinse.
2. Extinguish plasma.
3. Do not turn OFF the purge gas.

NOTE
The camera is purged at 100cc/min in order to keep it dry and free of moisture.

4. Do not turn OFF the water recirculator unless the camera will be allowed to return
to room temperature.
5. Release pump tension.
6. Shut the main power OFF (optional). If the main power is shut OFF, the camera
external water recirculator can also be turned OFF.

8.3.4 Daily

1. Check water level in Camera Water Cooling System.

8.3.5 Weekly

1. Daily checks.
2. If more than 500 samples are run in a week, check the pump tubing for wear.

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8.3.6 Monthly

1. Daily and weekly checks.


2. Clean the spray chamber. Refer to Section 8.4.8 "Cleaning the Spray Chamber".
3. Clean the nebulizer. Refer to Section 8.4.9 "Cleaning the Nebulizer".
4. Check in-line water filter and clean if necessary. Refer to "Water Recirculation
System Filter Cleaning and Replacement".
5. Drain and refill recirculator with distilled water. Refer to "Water Recirculation
System Water Change".
6. Drain and Refill Camera Water Cooling System with distilled water. Refer to
"Camera Water Cooling System Fill Procedure".
7. Wash or vacuum all air filters on the ICP, spectrometer, power supply and water
recirculator. Refer to Section 8.4.17 "Cleaning Air Filters".
8. Wipe down sample introduction area and autosampler tray.

8.3.7 Every 2 Months

1. Backflush water lines and replace water. Refer to Section 8.4.16 "Water
Recirculation System".
2. Inspect sample introduction o-rings and replace, if necessary.

8.3.8 Every 6 Months

1. Clean the camera water recirculator completely using the chemical wash
procedure. Refer to "Water Recirculation System Chemical Wash".
2. Replace camera purge gas dehydrator (every year, if argon <10 ppm water). Refer to
Section 8.4.4 "Camera Purge Gas Dehydrator Replacement".
3. If the external water recirculator has a filter, replace. Refer to Section 8.4.16 "Water
Recirculation System".

8.3.9 Annually

Schedule a preventative maintenance service call by a Teledyne Leeman Lab’s Field


Service Engineer.

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8.4 Maintenance Procedures

8.4.1 Powering OFF the Instrument Before Servicing

1. Find the main circuit breaker located on the back panel of the Prodigy7 ICP
(right side in rear, behind RF oscillator). Turn OFF the breaker by rotating it down.

Figure 8-1 Shutting off the main power breaker

2. Remove the power cord from wall.

Figure 8-2 Unplug power cord from wall

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8.4.2 Prodigy7 Access Panels

The following panels shown in Figure 8-3 are referred to in the maintenance procedures
of this chapter.

Figure 8-3 Prodigy7 front

LED Nameplate

Torch Access Panel


Front Access Panel

Power Button

Figure 8-4 Prodigy7 left side

Data Connections
Water Recirculation System
Reservoir

Cooling Fans (Air Filter Removed)


Gas Connections

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8.4.3 Front Access Panel Removal

1. Remove the Front Access Panel by pulling out from the bottom to release it from
the magnetic catches.
2. When released, lift the panel upward approximately 4” to disengage it from the
panel hangers (Figure 8-5).
3. Holding the cover away from the instrument, locate the LED nameplate cable.
Unplug the LED nameplate cable before completely moving the panel.

Figure 8-5 Front panel removal sequence

2. Lift approximately 4” to
disengage the panel from the
panel hangers.

1. Pull bottom of the panel out to release


it from the magnetic catches.

3. While holding the panel,


disconnect the LED nameplate
cable.

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8.4.4 Camera Purge Gas Dehydrator Replacement

The purge gas dehydrator should be replaced with a new unit, or a regenerated unit,
every six months when argon contains greater than 10 ppm of water. For argon supplies
that have <10 ppm of water, the dehydrator should be replaced every year. To regenerate
a dehydrator follow the instructions attached to the dehydrator. The dehydrator can be
found by removing the Prodigy7 Front Access Panel. The dehydrator is the silver colored
metallic cylinder that is about 14" long and 2" in diameter. It is mounted to the left of the
gas control system (Figure 8-6).

WARNING
Dangerous voltages are inside instrument. Power off instrument using the
procedures in Section 8.4.1 "Powering OFF the Instrument Before
Servicing".

1. Power OFF the instrument.


2. Remove the Front Access Panel according to Section 8.4.3 "Front Access Panel
Removal".
3. Turn OFF gas pressure at the supply tank.
4. Locate the Dehydrator and remove it from mounting clips.

Figure 8-6 Locating the gas dehydrator

5. Disconnect compression fittings from Dehydrator.


6. Remove the cap fittings from the new Dehydrator and connect to the tubing in
instrument.
7. Finger-tighten fittings, then tighten 1/6 of a turn with a wrench.
8. Replace the Dehydrator in the mounting clips.
9. Turn ON gas at tank. Gas is now flowing through the dehydrator and through the
camera body.
10. Reverse disassembly of instrument and turn instrument power ON.
11. Start Salsa and at the prompt, do NOT start chilling camera.
12. Allow the instrument to purge the camera with purge gas for four hours.
13. Exit Salsa, then restart Salsa. If asked to cool the camera click OK.

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8.4.5 Purge Gas Cylinders Replacement

NOTE
This procedure is also applicable if nitrogen has been used as a purge gas.

The argon gas cylinder replacement requires special attention to avoid condensation
and subsequent icing of the camera. It is best to replace the gas cylinder immediately,
when the “Argon Low” or “Argon Off” interlocks are triggered. Follow one of the two
procedures depending on how long the instrument has been without argon gas supply.

Gas change 1. Replace gas cylinder with as small amount of air becoming entrained, in the gas
less than 1 hr regulator and gas line, as possible.
after low gas 2. Reset the regulator to operating pressure to 80-90 psi (5.5-6.2 bar).
condition
3. Exit Salsa software.
4. Wait 10 minutes.
5. Start Salsa software.
6. A prompt will ask “if camera has been purged long enough to start chilling”. Click
OK.
7. Wait for camera to stabilize five minutes.
8. Instrument is ready for operation.

Gas change 1. Replace gas cylinder with as small amount of air becoming entrained in the gas
more than 1 hr regulator and gas line, as possible.
after low gas 2. Reset the regulator to operating pressure to 80-90 psi (5.5-6.2 bar).
condition
3. Exit Salsa software.
4. Allow the instrument to purge the camera with argon gas for four hours.
5. Start Salsa software.
6. A prompt will ask “if camera has been purged long enough to start chilling.” Click
OK.
7. Wait for camera to stabilize 5 minutes.
8. Instrument is ready for operation.

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8.4.6 Plasma Viewing Windows - Removal, Cleaning and Replacement

The plasma view windows have a very long life (typically greater than one year), and the
purged axial view window is particularly robust because of the argon purged flow
protecting it. Indications that the plasma viewing window may need cleaning or
replacement:
1. Intensities of calibration standards are identified as dropping significantly over
time.
2. Ultraviolet wavelengths will decrease first (wavelengths below 200 nm).
In some cases, cleaning the window may remedy these symptoms.

NOTE
Start first by cleaning the window thoroughly using the procedures below. If
the symptoms persist, the window will need to be replaced.

Follow the procedures below to remove the window for cleaning or replacement.

Window The Prodigy7 is designed with a convenient viewing window cassette that is easily
Removal and removed to permit window cleaning.
Initial Cleaning 1. Leave the purge gas ON when removing the viewing window cassette.
2. Locate the window cassette (Figure 8-7) in the Torch Box behind the Torch Access
Panel (Figure 8-3).

Figure 8-7 Window cassette

Window
Cassette

3. Grasp the cassette grip and pull straight out (Figure 8-8).

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Figure 8-8 Window cassette removal

Figure 8-9 Torch cassette o-rings

4. Clean both faces of the window using 70% isopropyl alcohol. If the window is not
clean after the isopropyl alcohol cleaning procedure, refer to "Secondary Window
Cleaning (if necessary)" below.

NOTE
Do not use spectral grade or higher purity alcohol as it contains entrainers that
contaminate the surface and reduce ultraviolet wavelength performance.

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5. Reinstall the window cassette with the o-rings toward the optical system.

NOTE
The o-rings in the window cassette are located toward the spectrometer and
away from the plasma. Note the o-ring location and reinstall the window
cassette in the same orientation (Figure 8-9).

Secondary Windows that do not come clean with the use of isopropyl alcohol should be cleaned
Window with hydrofluoric acid (HF). Follow the procedure below to clean with hydrofluoric acid.
Cleaning (if
necessary)
NOTE
In the event that your facility does not allow the use of HF acid, a second
option may suffice. Soak the window in aqua-regia for 24 hours, and rinse with
Deionized (DI) water. After the rinse, bake the window dry.

DANGER
Hydrofluoric acid is extremely dangerous. Read all
precautions on MSDS sheet and follow all good laboratory
practices.

1. Remove the window according to the "Window Removal and Initial Cleaning"
procedure.
2. Place 10 drops of 10%-20% HF onto one of the window surfaces.
3. With a rotating action, coat the window with acid and continue the rotating action
for 20 seconds.
4. Pour acid into an acid waste container.
5. Rinse thoroughly with DI water.
6. Repeat Steps 1. through 5. on the other side of the window.
7. Dry the window in an oven at 50 °C for 2 hours.
8. Let the window cool to room temperature before reinstalling.
9. Reinstall the window according to the procedures in "Window Removal and Initial
Cleaning".

NOTE
The o-rings in the window cassette are located toward the spectrometer and
away from the plasma. Note the o-ring location and reinstall the window
cassette in the same orientation (Figure 8-9).

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8.4.7 Lubricating the Peristaltic Pump

Oiling of the peristaltic pump is only necessary when a problem occurs with flow, a roller
is sticking or causing a squeaking sound, or if any liquid comes into contact with the
pump. To oil the pump:
1. Carefully place 1 drop of “tusk oil” at the following locations:
 Both ends of the rollers
 Between the front and back plates on the pump head
 The rollers themselves
2. If any oil gets on the surface of the rollers where the pump tubing contacts, remove
it with a clean cloth.

NOTE
Refer to the Te l e d y n e Leeman L a b’s website
(www.teledyneleemanlabs.com) for information on “tusk oil” and a list
of consumables and spare parts for the Prodigy7.

8.4.8 Cleaning the Spray Chamber

Maintaining a clean Sample Introduction System is critical for optimal operation of the
Prodigy7 ICP. Cleaning the spray chamber correctly will prevent washout problems and
increase the life of these components. It is recommended to clean the spray chamber
occasionally to maintain optimal performance.
For routine cleaning and when a degradation in performance is observed (such as
reduced precision or detection limits), clean the spray chamber with Fluka “RBS-25”
(Part # FLUKA25) according to the following procedure:
1. Aspirate a 2.5% Fluka solution for 15 minutes.

NOTE
A 15 minute aspiration of 2.5% Fluka solution will most likely be sufficient to
recover performance.

2. If there is no improvement in performance, soak the spray chamber in a 25% Fluka


solution overnight.

NOTE
If droplets collecting on the internal surfaces of the spray chamber are
observed, this is an indication that stability is degraded. These “resident”
droplets are the most common visible indication of spray chamber instability,
and should be removed by soaking the spray chamber in 25%-strength
RBS-25.

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8.4.9 Cleaning the Nebulizer

Concentric Nebulizer
It is recommended to clean the nebulizer occasionally to maintain optimal
performance. For routine cleaning, and when a degradation in performance is observed
(such as reduced precision or detection limits), clean the nebulizer with Fluka “RBS-25”
(Part # FLUKA25) according to the following procedure:
1. Aspirate a 2.5% Fluka solution for 15 minutes.

NOTE
A 15 minute aspiration of 2.5% Fluka solution will most likely be sufficient to
recover performance.

2. If there is no improvement in performance, soak the nebulizer in a 25% Fluka


solution overnight.

Caution

Do not use ultrasonic baths. This will damage the nebulizer. A special
concentric nebulizer syringe style cleaning device is available. Contact
Teledyne Leeman Labs using Section 8.8 "Teledyne Leeman Lab’s Contact
Information".

General Use a magnifying lens to inspect the concentricity of the gas and liquid tips. Inspect for
Inspection chips on both.

V-Groove Nebulizer
No cleaning procedure is required for the V-Groove Nebulizer.

Hildebrand Grid Nebulizer


The Hildebrand Grid Nebulizer should be rinsed extensively (on-line) with an
appropriate cleaning solution before shutting the system down. Doing so will ensure the
best possible long-term performance of the nebulizer. Disassembly of the sample
introduction system for cleaning purposes is undesirable, both because the procedure is
time consuming and because of the risk of damage associated with unnecessary
handling. Routine on-line cleaning of the nebulizer should allow for 3, 6, or even 9
months of use before a highly aggressive procedure, such as soaking in acid, is necessary.
Symptoms that may indicate the need for more aggressive treatment are:
 Degraded precision in daily QC procedures and/or routinely measured
concentrations; and
 Inability to obtain a stable aerosol production from the nebulizer regardless of
pump or end cap adjustment.

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1. Follow the procedures in Table 8-2 "Recommended Nebulizer Cleaning
Procedures" for recommended cleaning procedures:

Table 8-2 Recommended Nebulizer Cleaning Procedures


Type of Analysis Cleaning Procedure
Dilute Aqueous Solutions Rinse for 10 - 15 minutes using a clean acid matrix
similar to the acid matrix of samples and standards.
Follow with 1 - 2 minutes with deionized water.
High dissolved Solids Aque- Rinse:
ous Solutions >500 ppm 25% aqua regia for 10 - 20 minutes
total dissolved solids(>1000
ppm for Hildebrand Grid Dilute nitric acid (1 - 5%) for 1 - 2 minutes, then
Deionized water for 1 - 2 minutes
Dilute Organic Solvent Rinse 10 - 15 minutes using clean (blank) solvent
Solutions
High Solids Organic Solvent Rinse 20 - 30 minutes using clean (blank) solvent
Solutions
More aggressive solvent systems may be useful, but the integrity of the pump
tubing may be irreversibly affected.

2. An analysis run to follow rinse out.


3. With the ANALYSIS TAB active select the SCAN TAB. Viewing a spectral scan at the end
of the rinse period may indicate that additional rinsing is advisable but,
particularly with high solutions, deposition in the torch and/or degradation of the
pump tubing may lead to apparent peaks which diminish very slowly.

NOTE
A visual inspection of the nebulizer should be done periodically to ensure that
the nebulizer is not defective, or requires repair (concentric nebulizers cannot
be repaired). Contact Teledyne Leeman Labs using Section 8.8 "Teledyne
Leeman Lab’s Contact Information" if necessary.

General The outer end cap should have a flat screen without any tears. The main body of the
Inspection nebulizer also has a screen that should be checked for buildup or tears. Inspect the gas
line coming into the back of the nebulizer for drying and cracks, and the white sample
fitting for leaks. If you suspect the nebulizer needs repair, it can be sent back to Teledyne
Leeman Labs. Contact Teledyne Leeman Labs using Section 8.8 "Teledyne Leeman Lab’s
Contact Information".

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8.4.10 Cleaning Labware

Because all labware is a potential source of contamination, thorough cleaning before use
is essential. The preferred labware materials are Teflon®, high-density polyethylene
(HDPE or CPE), and low density polyethylene (LDPE or LPE). However, it should be
noted that subtle chemistry in some solutions may require the use of polyvinyl chloride
containers. Moody and Lindstrom (Analytical Chemistry 49, 2264 (1977)) have
recommended the following cleaning procedure:
1. Fill with 1:1 HCl (AR grade™).
2. Allow to stand one week at room temperature (80C for Teflon®™).
3. Empty, then rinse with DI water.
4. Fill with 1:1 HNO (AR grade™).
5. Allow to stand one week at room temperature (80C for Teflon®™).
6. Empty, then rinse with DI water.
7. Fill with purest available deionized water.
8. Allow to stand several weeks or until needed, changing water periodically to ensure
continued cleaning.
9. Rinse with the purest water available and allow to dry in a particle and fume-free
environment. For trace analysis using ICP emission spectrometry, the following
somewhat less aggressive procedure will reduce contaminants to less than
detectable levels:
 Rinse with deionized water.
 Fill with 1:1 HNO3 (AR grade™).
 Allow to stand one week at room temperature.
 Empty, then rinse three to six times with 18 M deionized water.
 Dry in a particle and fume free environment.
 Seal until needed.
The 1:1 HNO 3 acid can be recycled until testing indicates detectable levels of
contaminants. In addition, an acid bath may be used to soak labware which cannot be
easily sealed: e.g., autosampler cups, watch glasses, etc. Finally, an accelerated leaching
can be achieved by maintaining the acid filled vessels at 50C for several hours. All
standard solutions should be checked for accuracy by comparing to another source or
remaking the standards to ensure freshness and analytical reliability.

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8.4.11 Torch

8.4.12 Changing Torch Injectors

Teledyne Leeman Labs offers a selection of Torch Injectors. Refer to the Teledyne
Leeman Lab’s website (www.teledyneleemanlabs.com) for more information on
consumables, spare parts and accessories. Changing the torch injector tubes is a simple,
straightforward process. To change the torch injector:
1. Remove the ball joint end cap (Figure 8-10).

Figure 8-10 Unscrew torch cap

2. Carefully withdraw the injector tube (Figure 8-11).

Figure 8-11 Withdraw torch injector tube

3. Remove the injector tube (Figure 8-12).

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Figure 8-12 Remove the injector tube

4. To install a new injector tube, reverse the procedure.

8.4.13 Cleaning the Torch

Maintaining a clean Sample Introduction System is critical for optimal operation of the
Prodigy7 ICP. Cleaning the torch correctly will prevent washout problems and increase
the life of these components. To remove the torch refer to Section 8.4.11 "Torch".
The best procedure for cleaning the torch is to soak it in an acid bath overnight. For
aqueous torches use a 20-40% nitric acid solution. For organic torches use a warm
soapy water bath or the solvent used for sample dilution (e.g.kerosene).

8.4.14 Autosampler Maintenance

1. Clean the autosampler rails with isopropyl alcohol to remove any residual material
that may have built up.
2. Place 2 or 3 drops of “tusk oil” on the rails and work in with a soft cloth.

NOTE
Refer to the Teledyne Leeman Lab’s website (www.teledyneleemanlabs.com)
for information on “tusk” oil and a list of consumables and spare parts for the
Prodigy7.

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8.4.15 Camera Water Cooling System

Visually check the camera water reservoir daily to ensure there is adequate water. The
water level can be checked by opening the water reservoir door located on the left side of
the Prodigy7 (Figure 8-13). Only fill the reservoir with distilled water or diluted anti-algae
solution as described in the "Camera Water Cooling System Fill Procedure" below.

Figure 8-13 Camera water cooling reservoir

Camera Water Cooling System Fill Procedure


1. Open the camera water reservoir access door.
2. Remove the threaded filler cap.
3. Fill the water reservoir with distilled water and/or anti-algae solution.

NOTE
Do not fill the camera water reservoir with anything other than distilled water
or anti-algae solution.

4. Reinstall the cap.


5. Close the camera water reservoir access door.

Use of
Anti-algae
Solution
NOTE
Use of anti-algae solution in internal camera water cooling system is
acceptable, if prepared according to the procedures below.

1. Prepare a 50 ppm (0.05gr/liter) solution of Chloramine-T (also referred to as


Tosylchloriamide Sodium, or Sodium N-chloro-para-Toluenesulfonamide, or
C7H8ClNO2S*Na) in distilled water.

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NOTE
Do not use deionized water.

2. Change every month.

8.4.16 Water Recirculation System

The water recirculator installed on the Prodigy7 is designed specifically to cool the
internal electronics in the oscillator and to act as a secondary cooling system for the
camera. It should be maintained properly to avoid power fluctuations in the plasma, as
well as potentially damaging the internal electrical components. The water in the
reservoir should be changed at least every month. This will prevent any buildup that
may occur due to normal wear of components in the pump head and instrument.

NOTE
Deionized water (due to its aggressive nature) and tap water (due to it's higher
mineral content)) should not be used in the recirculator. The recirculator
should only be filled with distilled water.

Water Recirculation System Water Change


To change the water in the recirculator, follow the procedure below:
1. Drain the water recirculation system reservoir completely by disconnecting the
external water recirculator’s “water out” line from the Prodigy7’s “Water In”
connection, and placing it into a waste container.
2. Turn the external water recirculator ON and allow it to pump the water out of the
system.

NOTE
It may be necessary to tilt the recirculator forward to completely drain the
tank.

3. Once the recirculator ceases to pump water from the system, immediately turn it
OFF.

NOTE
Do not run the recirculator without water. Damage may occur to the pump.

4. Wipe the reservoir clean.


5. Refill with fresh distilled water.

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6. Reconnect the external water recirculator’s “water out” line to the Prodigy7’s
“Water In” connection.

NOTE
It is advised to consistently perform the Water Recirculator System water
change every two months. If Water Recirculation System maintenance
procedures are neglected (water change and filter replacement), it may be
necessary to perform a more vigorous rinse of the Water Recirculator System.
Refer to "Water Recirculation System Backflush Procedure" and "Water
Recirculation System Chemical Wash" below.

Water Recirculation System Filter Cleaning and Replacement


The screen filter on the water recirculator should be checked and cleaned. If it cannot be
properly cleaned, it should be replaced. To remove the Water Recirculation System filter:
1. Remove the back filter of the recirculator by sliding it up and out.
2. Locate the pump head assembly; there are two large nuts on the head assembly.
The nut on the bottom, facing down, contains the filter screen.
3. Remove the nut and screen and rinse with tap water until all particulates are
removed. Replace and check for leaks.

Additional Some recirculators also have an additional water filter mounted on the outside rear of
Water Filter the unit. This filter should be changed every six months. To replace this filter during a
(Optional) routine changing of the recirculator water:
1. Rotate the bottom portion of the filter holder counterclockwise.
2. Remove the filter and rinse any sediment that has accumulated on the bottom of
the holder.
3. Place the new filter in the holder and reattach, making sure to not cross thread the
components.

Water Recirculation System Backflush Procedure


The Prodigy7’s plasma can be affected by power fluctuations caused by ionic particles
circulated through the load coil. The Water Recirculation System backflush procedure
can often dislodge these particles, cleaning the system, and removing the power
fluctuations.

NOTE
If the water recirculation system is blocked or has low flow, the backflush
procedure may clear the blockage. When using the backflush procedure to
clear a blockage, extreme care must be taken not to overpressure the system.

1. Drain the water recirculation system reservoir completely by disconnecting the


external water recirculator’s “Water Out” line from the Prodigy7’s “Water In”
connection, and placing it into a waste container.

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2. Turn the external water recirculator ON and allow it to pump the water out of the
system.

NOTE
It may be necessary to tilt the recirculator forward to completely drain the
tank.

3. Once the recirculator ceases to pump water from the system, immediately turn it
OFF.

NOTE
Do not run the recirculator without water. Damage may occur to the pump.

4. Wipe the reservoir clean.


5. Refill with fresh distilled water.
6. Reverse the normal connections to the external water recirculator. Connect the
recirculator’s “Water Out” line to the Prodigy7’s “Water Out” connection.
7. Connect the recirculator’s “Water In” line to the Prodigy7’s “Water In” connection.
8. Turn the external water recirculator ON and allow the clean distilled water to flow
backward through the system for 2 - 3 minutes (maximum 5 minutes).

Caution

Do not backflush the system for longer than five minutes. The instrument may
be damaged if exceeded.

NOTE
Because the backflush procedure dislodges particles the water recirculation
system water should once again be changed.

9. Reconnect the external water recirculator’s “Water In” line to the Prodigy7’s “Water
Out” connection.
10. Drain the water recirculation system reservoir completely by placing the external
water recirculator’s “Water Out” line into a waste container.
11. Turn the external water recirculator ON and allow it to pump the water out of the
system.

NOTE
It may be necessary to tilt the recirculator forward to completely drain the
tank.

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12. Once the recirculator ceases to pump water from the system, immediately turn it
OFF.

NOTE
Do not run the recirculator without water. Damage may occur to the pump.

13. Wipe the reservoir clean.


14. Refill with fresh distilled water.
15. Reconnect the external water recirculator’s “Water Out” line to the Prodigy7’s
“Water In” connection.

Water Recirculation System Chemical Wash


The procedure should only be performed at the suggestion of a Teledyne Leeman Lab’s
representative. However, such a cleaning is commonly needed if the distilled water is
contaminated with dissolved solids. For the chemical wash procedure, contact Teledyne
Leeman Lab’s customer support using Section 8.8 "Teledyne Leeman Lab’s Contact
Information".

8.4.17 Cleaning Air Filters

There is one air filter located on the left side of the instrument. The filter may be cleaned
by either vacuuming or washing. Remove the foam filter by pulling directly out.

Figure 8-14 Air filter location

NOTE
If the instrument is operated in an extremely dusty environment, contact a
Teledyne Leeman Lab’s representative for assistance in mitigating adverse
effects. While it may violate the warranty of the product, Teledyne Leeman
Lab’s can advise the user on procedures to extend the life of the product.
Contact Teledyne Leeman Labs using Section 8.8 "Teledyne Leeman Lab’s
Contact Information".

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8.4.18 Ventilation Requirements

The Prodigy7 requires that a vent be placed above the chimney (but not directly
connected) and should draw a minimum of 100 Cubic Feet per Minute (CFM). Refer to
Section 1.1.1 "Site Requirements" or the Prodigy7 Preinstallation Guide for details. If a
preinstallation guide is needed, contact Teledyne Leeman Labs using Section 8.8
"Teledyne Leeman Lab’s Contact Information".

8.5 Troubleshooting
This troubleshooting guide is designed to assist the user in determining the source of an
analytical problem or mechanical failure. The diagnostics associated with these
procedures are intended to assist the user or Teledyne Leeman Lab’s representative in
determining the best and safest approach to resolving mechanical and analytical issues.
When assistance is required, contact Teledyne Leeman Labs using Section 8.8 "Teledyne
Leeman Lab’s Contact Information".

8.5.1 Peristaltic Pump

Proper use and maintenance of the peristaltic pump, an integral part of the Sample
Introduction System, is essential to producing consistent and reliable sample data. The
two most common problems encountered are:
1. Incorrect tension being placed on the tubing. For information on adjusting the
peristaltic pump refer to Section 2.1.2 "Peristaltic Pump".
2. Over or under lubricating the pump. For information on lubricating the peristaltic
pump refer to Section 8.4.7 "Lubricating the Peristaltic Pump".

8.5.2 Plasma Ignition Issues

Plasma Will Not Ignite


The Prodigy7 operates at a power setting typically ranging from 1.0 to 1.2 KW. There are a
number of causes that can lead to difficulty in igniting the plasma ranging from sample
introduction to mechanical or electronic failure.
The system is equipped with interlocks to locate the particular area or type of problem, if
they should occur. The interlocks are displayed on the INSTRUMENT CONDITIONS BAR as a
button that turns red if an interlock is present. Click on the INTERLOCKS BUTTON to display
interlock details. Refer to Section 8.5.4 "Interlocks" for more information.
All interlocks must be cleared in order to ignite the plasma. If a POWER interlock is
present before turning the instrument OFF, check the interlocks display to determine the
exact cause. Record which interlock(s) are showing red, and contact Teledyne Leeman
Labs using Section 8.8 "Teledyne Leeman Lab’s Contact Information". Having this
information prior to calling Teledyne Leeman Labs, will greatly assist the technician in
determining the corrective action to take, as well as expedite the process of scheduling
on-site service, if required.

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Plasma Ignition Troubleshooting Checklist
If no interlocks are showing red, and the plasma still will not ignite, check the possible
causes in Table 8-3 "Plasma Ignition Troubleshooting Checklist".

Table 8-3 Plasma Ignition Troubleshooting Checklist


Worn o-rings in Sample Introduction System Check and replace as necessary
Nebulizer adapter cap is loose Reset the end cap
Air leak in the gas system Check and repair as necessary
Argon tank is bad Was the argon tank changed recently? Try a
new argon source.
Ignitor wire is not connected properly or is Check and replace as necessary
corroded

8.5.3 Check Standard Failures

Good analytical practice dictates that a check standard or standards should be run after
a calibration, and at set intervals throughout the sample run. This is done to verify that a
valid calibration has been performed and that the ICP is maintaining reliable sample
results. A separate source is recommended for the check standard to ensure that
calibration standards are not biased or were incorrectly diluted to concentration. When
check standards fall outside a set tolerance limit, there are necessary actions to take to
verify where the problem lies. The following list gives the user a starting point for
determining check standard failures.
1. A new solution should be prepared (in the same matrix as the standards) to ensure
there is not a problem with the check standard itself.
 Corrective Action: remake solution, check calibration of pipette (if
adjustable).

NOTE
Teledyne Leeman Labs recommends that all standards be made up
gravimetrically (weight to weight).

2. A calibration standard can be run at the closest level available to the check
standard itself to see if there is any bias between the calibration standard stock
solution and the check standard stock solution.
 Corrective Action: use another source, remake solutions.

NOTE
New stock solutions and custom standards can be ordered through Teledyne
Leeman Labs. Contact Teledyne Leeman Labs using Section 8.8 "Teledyne
Leeman Lab’s Contact Information".

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3. Check the LINE CALIBRATION SCREEN (METHOD TAB>ELEMENT) to see if the calculated
value is within tolerance. This is what the instrument is going to read based on the
stored calibration, so if this number is not close to the true value, it will make it
difficult to pass a check standard. This is a very useful check especially if the blank
check standard (CCB) is failing.
 Corrective Action: An update intercept and update slope can be performed
to find the slope of the stored line calibration, or if this is an undesirable
option due to method guidelines, a recalibration may be necessary at
values that produce improved linearity within the check standard range.
4. Ensure that the cups in which the solutions are placed are stored in a clean area
free from contamination. Also, if carry over is suspected, clean the sample
introduction system and/or replace pump tubing.
 Corrective Action: Clean vessels and sample introduction system as
described in Section 8.4.10 "Cleaning Labware", Section 8.4.8 "Cleaning the
Spray Chamber", Section 8.4.9 "Cleaning the Nebulizer", and Section 8.4.13
"Cleaning the Torch". Check that uptake times and rinse times are set
accordingly.

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8.5.4 Interlocks

Table 8-4 Interlock Diagnosis and Corrective Action


Interlock Meaning Controlled By Corrective Action
Door The torch box door is not Two magnetic proximity Ensure the magnets are aligned, making
closed. switches. contact, and are securely mounted to the torch
box door.
Argon If flashing, input pressure has A argon pressure sensor on Check pressure on argon tank, and/or ensure
dropped below 80 psi (5.5 the argon mass flow control the system does not have leaks.
bar). module. The sensor is located
If lit, there is either too much beneath the spectrometer on
incoming pressure (>90 psi the electronics module.
[6.2 bar]) or insufficient input
pressure (<80 psi [5.5 bar]).
Water If flashing, water flow The water flow switch Measure the water flow coming out of the
through the system has located on the right back instrument. If flow is less than 2 LPM, there is a
fallen below required level side of the ICP. restriction in the system or the water supply
(around 1.8 L/min). If lit, there has dropped. Check that the water supply is
is insufficient water flow capable of supplying > 3 LPM, if so, the flow
through the ICP (around 1.5 switch or ICP control board has malfunctioned.
L/min).
Cover The oscillator cover is not in Two magnetic proximity Ensure the magnets are aligned, making
place. switches on the filament contact, and are securely mounted. Check the
cover and on the top bracket cabling to ensure it is not damaged.
of the main cover.
Power A high voltage power supply Contact Teledyne Leeman Labs using Section
problem has occurred. 8.8 "Teledyne Leeman Lab’s Contact Informa-
tion".
Air Knife The air knife is OFF or A pressure sensor located on Verify the air pump tubing is not kinked and
pressure has dropped below top of the main electronics that the air reservoir bottle cap is tight.
6 psi (0.4 bar). circuit board on the electron-
ics module.
Camera Purge The camera is not being A pressure sensor located Check argon gas pressure. Verify all gas
purged with enough argon inside the camera body. connections are made to camera.
flow. Camera solid-state
chiller has been turned OFF
to avoid ice build up.

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8.5.5 Camera Full Echellogram Shows Unusual Shapes in Continuum

If the camera full echellogram images have unusual shapes in bright light regions, there
may be ice crystals on the camera chip (Figure 8-15). This can cause failure of the device.
It is important to avoid shutting OFF the gas which will lead to warming of the camera
and trigger the camera purge interlock. To resolve this issue follow the steps below:

NOTE
When the camera purge interlock is tripped only a boot up of the Salsa
software will reset the camera solid state chiller.

1. Edit the Startup.ini file in the Salsa directory to add the following line:
CamCoolerTemp –10. If the parameter CamCoolerTemp exists, edit the numerical
value to be –10.
2. Save the Startup.ini file
3. Restart Salsa software. This will set the camera temperature to –10 °C.
4. Continue purging the camera with dry argon until ice crystals sublime from
surface. Run test echellograms to determine when the camera is free of ice crystals.
5. Exit the Salsa software.
6. Replace the argon gas supply with a gas supply known to contain less than 10 ppm
of water or replace the gas dehydrator with a new or a regenerated one. For
information on changing the argon gas cylinder refer to Section 8.4.5 "Purge Gas
Cylinders Replacement".
7. Wait 10 minutes for the camera purge to equilibrate.
8. Edit the Startup.ini file in the Salsa directory to add the following line:
CamCoolerTemp –40 or delete the CamCoolerTemp line completely.
9. Save the Startup.ini file
10. Restart Salsa software. This will set the camera temperature to –40 °C.
11. Set the plasma view to axial or radial and take a 10 second full frame echellogram.
Check for ice crystals.
12. Repeat step 11. for at least 10 minutes. If no ice crystals are observed, continue
with operating instrument. If ice crystals are observed, repeat the full procedure
and verify the gas dehydrator and argon gas are in good working condition.

Figure 8-15 Ice crystal on detector chip

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8.5.6 Instability (High RSDs)

Most analytical problems show up as poor precision or instability in results indicated by


update coefficients that are too high, or an occasional large excursion in results. The
most common source of these problems is the sample introduction system: peristaltic
pump, nebulizer, gas flows etc. The following section is a starting point for diagnosing
the issues with instability. Troubleshooting for instability should start with the most
common areas and then proceed to more complex tests. The most common areas that
affect stability are as follows:

Sample Introduction System

NOTE
Pump flow and nebulizer instability is the most common cause of instability in
results.

1. To ensure that the sample flow and drain are smooth and consistent, lift the
sample tip out of the rinse solution, then place it back in. By creating an air pocket,
the bubble can be followed up the length of the tubing. “Hitching”, or hesitation in
the bubble, indicates that the clamp tension requires adjustment.
2. Adjust the pump rate accordingly to correct the problem. For information on
adjusting the Peristaltic Pump refer to Section 2.1.2 "Peristaltic Pump".

Nebulizer
1. Remove the nebulizer from the spray chamber.
2. Disconnect the spray chamber from the torch, by removing the metal clamp and
separating the ball and socket joint.
3. Pull off the end cap.
4. With the METHOD TAB active, select INSTRUMENT CONTROL in the NAVIGATION PANEL.
Turn the nebulizer and pump ON.
5. Place the sample tip in DI water so that when the nebulizer is exposed there is no
acid being aspirated.
6. Optimize the nebulizer as described in Section 2.1.6 "Nebulizer".

Parameters
Check to ensure that uptake times and rinse times are set appropriately, and are not
contributing to instability in results.

Conditions
The sample introduction system should be clean and maintained properly to ensure
consistent results. Carry over can occur if the spray chamber, torch and nebulizer are
deposited with material contributing to the instability problems. Clean these
components as stated in Section Section 8.4.9 "Cleaning the Nebulizer".

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Leaks
Leaking sample at tubing connections and argon leaks in the sample introduction or
argon control system could potentially contribute to unstable results. Refer to Table 8-5
"Leak Points" for possible leak points.

Table 8-5 Leak Points


Location Assessment Procedure
Nebulizer End Cap O-rings Check for drying or Replace the o-rings and clean the sur-
cracking face of the spray chamber that contacts
the end cap to ensure there is not a
“film” built up preventing a good seal.
Nebulizer End Cap The end cap should Replace the o-rings and clean the sur-
have a snug fit and face of the spray chamber that contacts
should not be able to the end cap to ensure there is not a
be pulled off easily. “film” built up preventing a good seal.
Torch Gas Connection Check these connec- Disassemble the torch body and
tions for cracks and/or inspect all o-rings.
leaks at connectors.
Nebulizer Gas Connection Check these connec- Inspect the o-ring in the nebulizer gas
tions for cracks and/or connection for wear or cracking.
leaks at connectors.

8.5.7 Chemistry and Labware

Because all labware is a potential source of contamination, thorough cleaning before use
is essential. Refer to Section 8.4.10 "Cleaning Labware".

8.5.8 Water Recirculation System

The water recirculation system can contribute instability in results if the water is not
properly maintained. Distilled water is recommended in the water recirculator, but
contaminants may make their way into the system, either by improper maintenance or
normal wear of materials in the recirculator and instrument. The plasma can be affected
by power fluctuations caused by ionic particles circulated through the load coil. If this is
suspected, replacing the water and performing the backflush procedure (reversing the
water in and water out connections) should dislodge the particles and clean the system.
For information on the backflush procedure refer to Section 8.4.16 "Water Recirculation
System".

NOTE
If the water recirculation system is blocked or has low flow, the backflush
procedure may clear the blockage. When using the backflush procedure to
clear a blockage, extreme care must be taken not to overpressure the system.

If this does not resolve the problem, a chemical wash can be performed. For the
chemical wash procedure contact Teledyne Leeman Labs using Section 8.8 "Teledyne
Leeman Lab’s Contact Information".

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8.6 Diagnostics
When the areas most commonly affecting unstable results and/or check standard
failures have been addressed and the problem still exists, it may be necessary to perform
more complex diagnostics to troubleshoot the issue. Several tests can be performed to
isolate the exact problem. The most powerful test is described below.

8.6.1 Installation Test Procedure

Contact Teledyne Leeman Labs customer support using Section 8.8 "Teledyne Leeman
Lab’s Contact Information" and request the Installation Test Procedure for the Prodigy7
ICP. Follow the short-term precision test as described for your instrument type. The
results of the precision test can quickly isolate a spectrometer, RF, or sample
introduction problem. Most analytical problems are historically caused by the sample
introduction.

NOTE
Experience on the Prodigy7 ICP has shown that the most common problem
with detection limits and/or precision is due to a dirty nebulizer.

Further information on interpreting the results is available. Contact Teledyne Leeman


Labs using Section 8.8 "Teledyne Leeman Lab’s Contact Information".

8.6.2 Autosampler Calibration

If problems occur with the autosampler, or if the sample tip is not hitting the correct
sample cups, it may be necessary to recalibrate the autosampler’s coordinates. To do so,
contact Teledyne Leeman Labs using Section 8.8 "Teledyne Leeman Lab’s Contact
Information" for the latest method of calibrating the autosampler.

8.6.3 Resetting Source Mirror

If a histogram peak is not shown when performing a plasma positioning, it may be


necessary to reset the source mirror. The source mirror can be reset using the PEAK
SOURCE BUTTON. Perform the following procedure:
1. With the METHOD TAB active select INSTRUMENT CONTROL in the NAVIGATION PANEL.
2. Click on the PEAK SOURCE BUTTON.
3. Click the RESET DEFAULTS BUTTON in the PEAK SOURCE DIALOG (Figure 8-16).

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Figure 8-16 Peak source dialog

4. A warning message will appear (Figure 8-17). Click the OK button to reset the
positions.

Figure 8-17 Reset mirror message

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8.7 Instrument Set-up

8.7.1 Installation Short Procedure

If the Prodigy7 ICP is being reinstalled or moved to a new location the following
abbreviated installation procedure will assist in the process.

NOTE
This procedure is not meant to replace the actual installation and test
procedures as trained and published by Teledyne Leeman Labs.

Begin by inspecting the instrument, its connections, and its supplies. Ensure the criteria
in Table 8-6 "Instrument Inspection" are met:

Table 8-6 Instrument Inspection


General
1. Check that the peristaltic pump tubing is not deformed and is properly seated. Make sure
the pressure platens and lock down levers are in the run position.
2. Check that the torch is properly located within the RF coil and that the spray chamber
and nebulizer are tightly fastened.
3. Check the continuity of the sample line from the sipper probe to the nebulizer, and the
waste line from the spray chamber to the waste receptacle.
Spectrometer Connections
1. Ensure that the USB cable is connected from the computer to the spectrometer.
2. Check connections from the monitor and printer to computer.
3. If an autosampler is installed, check it for communications and power connections.
Accessories and Supplies
1. Check the connection of the Water Recirculator System to the back of the RF oscillator.
2. Check that the recirculator is full of coolant water and turned ON.
3. Check that argon pressure to the instrument is adequate 80-90 psi (5.5-6.2 bar)
4. Check that exhaust ventilation is active.
5. Check that the camera chiller is full of distilled water and turned ON. Set temperature
to 28 °C.

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Internal Camera Chiller Startup Procedure
1. Open the camera water reservoir access door.

Figure 8-18 Camera water cooling reservoir

2. Remove the threaded filler cap.


3. Fill the water reservoir with distilled water.

NOTE
Do not fill the camera water reservoir with anything other than distilled water
or anti-algae solution.

4. Reinstall the cap.


5. Turn the instrument ON. This will also turn ON the camera water chiller. If the
pump is primed correctly there should be a considerable drop in the reservoir tank
water.
6. Turn OFF the instrument for 5 to 10 seconds.
7. Turn the instrument back ON and allow any trapped air to escape from the chiller
pump and tubing.
8. Refill the camera water reservoir to within ½ inch of the top.

Caution

If the pump is not primed correctly it will make a loud “whirring” sound. Turn
OFF the instrument immediately. Contact Teledyne Leeman Labs using
Section 8.8 "Teledyne Leeman Lab’s Contact Information".

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On the Instrument Control Panel

NOTE
If argon has been supplied to instrument for the first time, wait 4 hours before
allowing Salsa software to chill camera. It is important to dry out the camera
with argon to prevent ice buildup. Ice crystals on the camera can lead to
damage of the camera.

1. Check that the purge gas is ON.


2. With the METHOD TAB active, select INSTRUMENT CONTROL in the navigation panel.
Select the desired torch view on the INSTRUMENT CONTROL screen. (Figure 8-19)

Figure 8-19 Instrument control panel

3. Position plasma (PEAK SOURCE button) if necessary.


4. AUTO START to begin the plasma ignition sequence.
5. Check the plasma appearance and sample introduction system after start-up. The
plasma should begin about 1/8” (3 mm) - 1/4”(6 mm) beyond the central channel
and end directly above the air knife (if axial view). The peristaltic pump should be
rotating with no liquid build-up in the spray chamber and the sample mist should
be visible in the spray chamber.

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8.7.2 Reducing Power and Gas Consumption

The Prodigy7 ICP can be operated in modes of low power and gas consumption with
very little compromise of performance.
The optical spectrometer has been optimally designed to perform in the low ultraviolet
with as little as 0.5 Liters Per Minute (LPM) gas consumption. The three levels of
spectrometer purge flow rate are located on the INSTRUMENT CONTROL S CREEN . The
modes are labeled OFF, LOW, and HIGH. The factory default flows are approximately 0.2,
1.0, and 14 LPM respectively. To change the flow rates associated with each of these
settings, the Starup.ini file must be edited. For example, if the required flow rates are 0,
0.5, and 10 for the OFF, LOW, and HIGH, edit the OpticsPurgeFlow line: OpticsPurgeFlow
0, 0.5, 10
Save the new Startup.ini file and restart Salsa to use the new values. Lower gas flows can
also be used, but UV performance may deteriorate for wavelengths below 185 nm.
The optical spectrometer is very stable and generally does not need to have the
temperature changed if long term (>2hours) analytical stability is not required. If the
thermostat portion of the spectrometer were set to a temperature much lower than the
room temperature, the thermostat heater would not come on and a lower power
consumption would be realized. Set the Startup.ini file parameter OpticsThermostat to a
low value such as 10 °C (i.e. OpticsThermostat 10).
Various combinations of putting the instrument into a sleep mode can realize significant
reductions in gas and power reduction. Refer to Table 8-7 "Power Consumption
Settings" and Table 8-8 "Gas Consumption Settings" below for approximate gas and
power consumption amounts.

NOTE
The camera is purged with argon to prevent icing of moisture in the air
migrating into the camera. The camera purge is always ON, at about 0.2 LPM. If
the camera purge is to be turned OFF by shutting off the argon supply, it is
recommended to set the CamCoolerTemp to room temperature
(i.e.- CamCoolerTemp 22).

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Table 8-7 Power Consumption Settings
Power Item Aqueous Organic Aqueous Organic Aqueous Normal Sleep Super
(Watts) Operation Operation Operation Operation Operation Quiescenta Modeb Sleepc
Dual-View Axial Radial Radial DV or Axial
(DV) or (1.4Kw) (1.0Kw) (1.4Kw) unthermo-
Axial stated spec-
(1.0Kw) trometer
(1.0Kw)
Prodigy7 ON ON ON ON ON ON ON ON
Internal ON ON ON ON ON ON ON Set
Camera Chiller to
30 °C
Spectrometer ON ON ON ON Set to 10 °C ON ON Set
Heater to
10 °C
Computer ON ON ON ON ON ON OFF OFF
Monitor ON ON ON ON ON ON OFF OFF
Printer ON ON ON ON ON ON OFF OFF
Recirculator ON ON ON ON ON OFF OFF OFF
Total Power 2500 3300 2500 3300 2420 400 200 80
a. Fastest startup and warm-up of instrument
b. Fast warm-up but requires user interaction to startup
c. Slow startup, slow warm-up (fast warm-up if un-thermostated spectrometer mode used)

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Table 8-8 Gas Consumption Settings
Argon Item Aqueous Organic Aqueous Organic Aqueous Normal Sleep Super
Gas Operation Operation Operation Operation Operation Quiescenta Modeb Sleepc
(LPM) Dual-View Axial Radial Radial DV or Axial
(DV) or (1.4 Kw) (1.0 Kw) (1.4 Kw) unthermo-
Axial stated spec-
(1.0 Kw) trometer
(1.0 Kw)
Coolant 12 14 12 14 12 0 0 0
Nebulizer 0.7 0.7 0.7 0.7 0.7 0 0 0
Auxiliary 0.2 0.5 0.2 0.2 0.2 0 0 0
Camera Purge 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Spectrometer 1 1 1 1 1 1 0.2 0
Purge
Total Gas 14.1 16.4 14.1 16.1 14.1 1.2 0.4 0.2
Total Gas 6768 7872 6912 7728 6768
(Liters per
8 hr day)
Total Gas 1728 576 288
(Liters per
24 hr day)
a. Fastest startup and warm-up of instrument
b. Fast warm-up but requires user interaction to startup
c. Slow startup, slow warm-up (fast warm-up if un-thermostated spectrometer mode used)

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8.7.3 Installation of the Cetac ASX500 Series Autosampler

Table 8-9 Cetac ASX500 Series Autosampler


Component Description
Cable USB Salsa operates the Cetac ASX-500 autosampler via a USB cable con-
nected between the autosampler and the Prodigy7 CPU. The Cetac
ASX500 has been tested with the USB port for the Prodigy7 instrument
running under the Salsa software. Do not attempt using an RS-232 serial
port without contacting Teledyne Leeman Labs. Contact Teledyne Lee-
man Labs using Section 8.8 "Teledyne Leeman Lab’s Contact Informa-
tion".
Cable Length The cable supplied is 16 ft (5M) long. Cables of longer length may not
work.
Drivers As with all USB devices the initial plug-in of the autosampler launches a
“Detected New Hardware” wizard to install device drivers. The Cetac
ASX-500 autosampler comes with a CDROM containing the drivers. If
your computer was supplied through Teledyne Leeman Labs, the neces-
sary drivers will be installed. If you are supplying your own computer you
will have to install these drivers.
COM ID The USB connection to the autosampler creates a “virtual” serial port.
The COM port ID for the autosampler can be found in the Device Man-
ager under “Ports” once the autosampler has been connected, powered
ON and the correct device drivers have been installed.
Calibration The Cetac ASX-500 autosampler requires no calibration.
Autosampler Off If you wish to operate the Prodigy7 with the Cetac ASX-500 powered
OFF, the startup.ini file parameter ASPresent must be set to “no”.
Rinse The Cetac ASX-500 has a flow-through rinse that is fed by a onboard
pump. The pump only turns on when the tip is down in the rinse.

SartUp.INI Parameters for Cetac ASX500


Salsa requires some additional startup.ini file parameters to operate the Cetac ASX500
autosampler. To edit the startup.ini file:
1. Locate the startup.ini file in the Salsa directory
Edit the file using Wordpad or Notepad.
2. Enter the following lines:
 CommAS [COM port ID]
 Astype Cetac
 ASRacktype 4
 ASPresent yes

NOTE
Salsa does not recognize changes in the Startup.ini file until it is has been restarted.

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8.8 Teledyne Leeman Lab’s Contact Information

8.8.1 Teledyne Leeman Labs

Teledyne Leeman Labs


110 Lowell Road
Hudson, NH 03051 U.S.A
www.teledyneleemanlabs.com
Main: 603-886-8400
Fax: 603-886-9141
Email:LeemanLabsInfo@teledyne.com

8.8.2 Sales

US and International: +1 800-634-9942 or +1 603-886-8400


US and International Fax: +1 603-886-9141
salesinfo@teledyne.com

Representatives
Visit our website at www.teledyneleemanlabs.com for a complete list of US and
International Sales Representatives.

8.8.3 Technical Support

US: +1 800-533-6267 (1-800-Leemans)


International: +1 603-886-8400
Email: service@teledyne.com

8.8.4 Replacement Parts and Consumables

US and International: +1 800-533-6267


Email: LeemanLabsInfo@teledyne.com

NOTE
Refer to the Teledyne Leeman Lab’s website (www.teledyneleemanlabs.com)
for a list of consumables and spare parts for the Prodigy7.

8.8.5 Plasma-Pure Laboratories

US and International: +1 603-521-3289


US and International Fax: +1 603-886-9141 (Attn: Plasma Pure Standards)
E-mail: ssacra@teledyne.com

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Prodigy7 User Manual
Appendix A: Advanced User Reference
A.1 Spectral Interferences
The Inductively Coupled Plasma (ICP) is one of the most widely used sources for routine
trace metal analysis due to four attributes:
1. Freedom from chemical interference (when compared with other types of sources,
such as the air-acetylene and nitrous oxide-acetylene flames used in Atomic
Absorption (AA) and Atomic Emission Spectrometry (AES)
2. Speed of analysis
3. Superior dynamic range
4. Multi-element capability
The property of the ICP most responsible for its freedom from chemical interference is
the high temperature of the plasma discharge. Flames used in AE and AA spectrometry
are chemical in nature, hence their upper temperature is limited to about 3000 °C. This
temperature is too low to decompose all the molecules that may be present in the flame.
This in turn reduces the free atom population necessary for emission or absorption
measurement, resulting in interferences. In comparison, the temperature of the ICP in
the axial channel where the sample penetrates is more than 6000 °C. This temperature is
sufficient to decompose virtually any molecule resulting in the elimination of practically
all chemical interferences.
Conversely, the high temperature of the plasma discharge is the cause of spectral
interference, one of the most common types of interference found in ICP spectrometry.
Because nearly every species present in the ICP emits light, spectral interferences are
encountered frequently. Spectral interferences in ICP occur as:
 Background shifts
 Complete or partial spectral overlap
Fortunately, compensating for spectral interferences in ICP is not difficult.

NOTE
Background shifts are by far the most common (and most easily corrected)
spectral interference.

A.1.1 Background Correction

The observed emission intensity at an analyte wavelength consists of two components:


1. Light emitted from the analyte species and
2. Light emitted from another sample component or the plasma itself.
Light at the analyte wavelength that does not originate from the analyte itself can be
classified as background. A spectral scan demonstrating the difference between signal
and background is shown in Figure A-1.

A-1
In constructing a calibration plot, the analyst will want to plot the emission intensity
resulting only from the analyte (the net analyte intensity) as a function of the analyte
solution concentration. To do otherwise can result in either positive or negative
deviations in the determination of the analyte concentration in a sample. Fortunately,
the analyte signal and background add directly and hence if one determines the
background intensity level then this can be subtracted from the total intensity observed
at the analyte wavelength thus yielding the net analyte intensity.

Figure A-1 A) Illustration of the concept of net signals

Review of Figure A-1 shows that the background level is essentially the same for the
standard, sample and the blank. This being the case, background correction is not
needed. A case when background correction must be used is shown in Figure A-2. The
sample has a different background level than the blank and standards. If a calibration
were performed in the usual way and the sample intensity shown in the figure were used
for in the concentration calculation, the result would be too high since the analyte
intensity is higher than it should be. The opposite situation in which the sample
background intensity is lower than the standards’ background intensity can also take
place thus producing a result which is too low.

Figure A-2 B) Illustration of the concepts of matrix-induced background shift

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A.1.2 Background Correction Types

It is generally considered good analytical practice to do background correction, although


there are times when background correction is not necessary. In order to determine
whether background correction is required, wavelength scans of samples to be analyzed
should be collected and compared to scans of standards and blanks. The background
signal in ICP can be classified in one of four ways:
 Simple
 Sloped
 Curved
 Complex
In the next section, an example of each type will be illustrated along with how the
correction should be applied.

NOTE
Background correction is always applied with the Prodigy7 or Prodigy7
Spectrometer.

Simple Background Shift


Figure A-3 illustrates a simple background shift in red. In this case the analyte signal is
offset by a constant amount across the scan. The shift can be caused by a difference in
the matrix composition between the sample and the standard, the presence of other
elements, or recombination continua. It is possible, in some cases, for the background to
be shifted down. In any of these cases, the correction is straightforward. A single
background correction point at the lowest stable position (denoted by the arrow) on
either side of the analyte line will compensate for the shift.

Figure A-3 Simple background shift

Sloping Background
Figure A-4 illustrates a sloping background shift. In this case, the offset is not constant
but varies in a linear fashion across the scan. This may be caused by the presence of a
severely broadened nearby spectral line. Correction of the offset is a bit more involved.
The use of a single background correction point will either over or under-correct the
signal depending on which side it is placed. For this type of background offset, it is

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necessary to use a two-point correction. The two points should be placed at equal
distances on either side of the analyte peak. For the most accurate results, particularly at
the trace level, another line should be chosen if possible.

Figure A-4 Sloping background

Curved Background
The background shift in Figure A-5 is similar to the sloping background in Figure A-4,
with the exception that the offset is not linear over the scan interval. This type of shift is
caused by the analyte peak being located on the wing of a larger peak just outside the
scan window. The use of a two-point background correction in this case does not give
accurate results, since it assumes the background shift is changing linearly. Two-point
background correction will result in an over or under-correction, depending upon where
the points are placed and the intensity of the larger peak. Treating this case using an
interfering element correction (discussed in Section A.1.3 "Spectral Overlap and
Interfering Element Correction (IEC)") will give a more accurate result.

Figure A-5 Curved background

NOTE
When confronted by a curved background, first attempt selecting a different
emission line.

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Complex Background
A complex background shift, shown in Figure A-6, is comprised of intensity shifts that
vary considerably over the scan interval. This is caused by numerous, overlapping
emission lines inside the scan window. Their presence may be due to different elements
in the sample or arise from a single element that is spectrally rich in the particular
wavelength region. In many cases, it will be difficult to perform an accurate background
correction, since the background under the analyte peak may not be same as the
background level at the correction point.

Figure A-6 Complex background

It may be possible to matrix-match standards to samples if the identity and


concentrations of the other emission lines can be determined. If the cause of the
complex background varies in the samples, it may be possible to treat this situation as
an interfering element and correct accordingly.

NOTE
When confronted by a complex background, first attempt selecting a different
emission line.

A.1.3 Spectral Overlap and Interfering Element Correction (IEC)

Virtually all species present in the plasma discharge emit light. Consequently, the
potential exists for thousands of emission lines to appear in any particular sample.
Fortunately, the resolution and dispersion of the Prodigy7 ICP spectrometer minimizes
the occurrence of spectral overlap by interfering elements. Like background shifts,
interfering elements can be categorized. Typically there are two types:
1. Partial
2. Direct overlaps

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Partial And Direct Spectral Overlap
The first step in compensating for an interfering element interference is to recognize its
presence. Spectral interferences resulting from a sample component are easy to detect
by scanning a solution containing the interferent at the analyte wavelengths. An
example of this technique is demonstrated in Figure A-7. In this figure, a line totally free
of interference is shown followed by two partial overlaps and a direct overlap (Figure
A-7(A). The partial overlap can be difficult to detect at low interferent concentrations
(Figure A-7(B) but is more pronounced at high concentrations (Figure A-7 (C). In the
case of the direct overlap (Figure A-7(D), the interfering element and the analyte are so
close that the scan shows only one apparent peak.

Figure A-7 Spectral scans for pure Zn, mixed Zn and Ni and pure Ni solutions

Zn 206.000 nm line demonstrating no Zn 202.548 nm line showing a partial


spectral interference overlap from a nickel emission line

Zn 213.856 nm line with more severe


Zn 202.548 nm line showing a partial
direct spectral overlap from a nickel
overlap from a nickel emission line

To detect a direct spectral overlap during a method development, or to determine if an


overlap has appeared during the analysis of a particular sample, scans at more than one
wavelength are necessary. Comparison of the relative intensities between the standards
and samples at the different wavelengths would confirm the existence of a direct
spectral overlap. For example, if the background corrected intensity ratio of Zn 213.856
nm to Zn 206.000 nm is calculated, the value is found to be 1.5 for a pure Zn solution.
However, if the same ratio is calculated for a Zn solution containing 100 ppm Ni, the
ratio will be 2.5. This indicates that an interferent is present on the Zn 213.856 nm line. If
the ratio for the sample solution were smaller than 1.5, the interference would be on the
Zn 206.000 nm line. Aside from comparing intensities, the other way of detecting a
spectral overlap is to collect spectral scans of solutions containing the major matrix
elements, one at a time. This is similar to the case in Figure A-4(C) where a scan was
collected for a 1000 ppm Ni solution.

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Whenever one is confronted with an interfering element, the first choice is to select
another analytical line. It is the simplest course of action. The WAVELENGTH TABLE in Salsa
can assist in selecting another wavelength. To perform an Interfering Element
Correction refer to Appendix A: "Advanced User Reference", Section A.1.4 "Interfering
Element Correction (IEC) Factors".

A.1.4 Interfering Element Correction (IEC) Factors

In those cases when a suitable alternate wavelength cannot be found, the contribution
to the analyte intensity at the wavelength in question can be accounted for by using an
Interfering Element Correction (IEC) factor. The emission intensity from the interfering
element will cause the measured intensity to be greater than if only the analyte were
present. This will cause the calculated analyte concentration to be higher than if the
interferent were not present. The purpose of the IEC is to calculate the contribution to
the concentration that is resulting from the interferent. This quantity is then subtracted
from the total concentration determined at the analyte wavelength to yield the true
concentration of the analyte. Follow the procedures below to perform an IEC:

Determine the Identity of the Interfering Element


This may require the use of the INTERFERENTS TABLE located on the E LEMENT
SELECTION SCREEN (With the METHOD TAB active select ELEMENT SELECTION in the
NAVIGATION PANEL ), as well as other sources of data for emission lines. Prior
knowledge of the sample may simplify identification of the interfering element. If
the element is one whose presence is unknown or unexpected, using the
SemiQuant program may help. Refer to Section 5.12 "Creating a SemiQuant
Method".

Calculate the Interfering Element Correct Factor (IEC)


This is determined by measuring a standard of known concentration of the
interfering element at the analyte line and calculating the apparent concentration
of the analyte element. Keep in mind that this “apparent” analyte concentration is
resulting from light emitted by the interferent at the analyte wavelength. The ratio
of the “apparent concentration” of the analyte to the concentration of the
interfering element standard is the IEC factor. The instrument will use this factor
to correct the interference during sample analyses. The IEC factor can either be
determined by the instrument automatically, or entered manually by the operator.
The IEC process can be summarized as follows:
1. The instrument is calibrated for the analyte. A standard containing a known
concentration of the interferent (the IEC Standard) is then run. This factor uses
the apparent concentration of the analyte (determined at the analyte
wavelength) and the actual concentration of the IEC standard and is calculated
as shown in the formula below, where FIEC is the IEC factor, Capparent is the
apparent analyte concentration resulting from the interferent and CIEC is the
concentration of the interferent in the IEC standard.

Figure A-8 Formula 1

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2. Samples are then analyzed and the contribution to the analyte concentration
resulting from the interferent is subtracted from the measured concentration at
the analyte wavelength as shown in the formula below, where CA is the true
analyte concentration, CM is the measured concentration (including the
contributions from the analyte and interferent), FIEC is the IEC factor, and CI is
the concentration of the interferent in the analyte solution.

Figure A-9 Formula 2

A.1.5 IEC Practical Example

In this section, the process will be demonstrated step-by-step.


1. In this case, we will use the Ni overlap with Zn 213.856 nm already presented
above. To determine the IEC factor, a line for each of the elements involved must
be in the method. In this case, a Ni line must be present, even if there is no interest
in measuring Ni for analytical purposes. In order to calculate and apply the
correction, the instrument needs to determine the concentration of the interferent
(Ni in this example) in all samples being analyzed. The line chosen to measure Ni
must also be free from other interfering element effects. If not, the Ni wavelength
must also be corrected. The Ni wavelength also cannot be the wavelength that is
causing the interference. For purposes of example, the wavelengths entered into
the method will be Zn 213.856 nm and Ni 231.604 nm.
2. During the course of method development, you would have already selected
wavelengths for all analytes of interest, scanned all solutions (blank, standards,
samples), selected background correction points, and determined that Ni is an
interferent at the Zn 213.856 nm line. For this example, we will assume that all of
this has been done and that the wavelengths for Zn and Ni have been added to the
method under ELEMENT SELECTION in the NAVIGATION PANEL.
3. Ni and Zn must now be identified as the interferent and analyte of interest to allow
the software to calculate and apply correction factors appropriately. To do this,
highlight the Zn 213 nm wavelength in the NAVIGATION PANEL and click on the IEC
TAB. Place a check mark beside the Ni 231.604 nm wavelength to indicate that Zn
has an interference from Ni. A row of zeros should appear next to Ni in the
coefficient cell and the DISPLAY PANEL should look similar to Figure A-10.

Figure A-10 IEC Practical example - setting up an IEC correction

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4. Highlight the Ni 231.604 nm wavelength in the NAVIGATION PANEL and click the IEC
TAB. Prepare a high concentration single-element Ni standard and enter the
concentration of that standard in the text box under IEC STANDARD (Figure A-11).

NOTE
The standard should be prepared at a concentration close to that expected to
be present in the samples to be analyzed to ensure that the IEC factor is
accurately calculated. For example, if Ni is expected to be present at 200 ppm,
do not prepare and run a Ni IEC standard at 25 ppm.

Figure A-11 IEC Practical example - running an IEC standard

5. Aspirate the single-element Ni standard into the instrument and click the RUN
IECSTANDARD button. Once the instrument has analyzed the IEC standard and
calculated the IEC correction factor, the coefficient will automatically be entered
into the IEC TABLE for Zn. To verify this, highlight the Zn 213.856 nm wavelength in
the NAVIGATION PANEL and select the IEC TAB.
6. The final step in setting up IECs is to indicate that correction factors need to be
used during analysis. To do this, make the METHOD TAB active, and then click on
ANALYTICAL PARAMETERS in the NAVIGATION PANEL. Select USE IEC on the ANALYTICAL
PARAMETERS SCREEN (Figure A-12).

NOTE
The calibration concentration range of the interferent standard (Ni, in this
case) must be high enough to ensure an accurate calibration. The accuracy of
the analyte results (Zn in this case) depends on the accuracy of the interferent
determination. The highest concentration used to calibrate the interferent
must be higher than that used as an IEC standard. The concentration of the IEC
standard must also fall within the calibration range for the interferent.

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Figure A-12 IEC Practical example - using IECs in a method

7. Before proceeding, the IEC correction factor should be tested to verify that it is
accurate. This can be done in one of two ways:
 Use a single element Ni solution as a sample and make a concentration
measurement for Zn. The corrected Zn concentration should be close to its
detection limit.
 Analyze a sample containing Ni (at a concentration that falls within the
calibration range for this element) and a known concentration of Zn. If the
Zn concentration is correct, within experimental error, then the IEC is
working. If not, the procedure should be checked for errors. Keep in mind
that if any background correction points are in use on either element, they
must not be removed or changed. If either is done, the IEC factor must be
recalculated. The same is true if a background correction point is added
later.
The IEC factor can also be calculated manually. The procedure is the same as above,
except an IEC standard is not set on the IEC display. The instrument is calibrated
normally. An Ni standard is analyzed as a sample, generating an apparent Zn
concentration. The IEC factor is then calculated using the first equation in "Calculate
the Interfering Element Correct Factor (IEC)". This value would then be entered into the
IEC TABLE for Zn (Figure A-10).

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A.1.6 Interfering Element Corrections (IEC)

Interfering Element Corrections (IEC) are designed to compensate for spectral overlap.
Adjustments are made to analyte concentration based on the concentration of the
interfering element(s) present in the sample. Any other analyte element in the method
may include an Interfering Element Correction (IEC). Typically, only major constituents
in the sample should be candidates for IECs.

How to Apply an IEC


1. Create a method including all wavelengths for the analytes of interest and for
major sample constituents. Remember you may need to select less sensitive
wavelengths for the major constituents.
2. Calibrate all the wavelengths. For the major constituents in your samples and any
other suspected interferent, aspirate a concentrated solution containing only one
of the elements. To obtain an accurate IEC, it is critically important that these
solutions be free of other contaminants.
3. At each analytical wavelength determine the baseline offset (in concentration)
resulting from the interferent and divide that value by the interferent
concentration to obtain the IEC coefficient.
4. Place a check mark beside each interferent and then enter the calculated
coefficient in the COEFFICIENT column.

Figure A-13 Selecting an interfering element

5. When subsequent analyses occur each interfering element concentration will be


determined at its analytical wavelength as specified in the IEC TABLE. Each
interfering element concentration is then multiplied by its coefficient and the
results are subtracted from the analyte signal.

IEC Example Assume samples will contain about 1000 ppm of iron and we suspect it may be
interfering with arsenic determinations at 193.759 nm.
1. Calibrate the method for arsenic at 193.759 nm.
2. Next, calibrate iron a a wavelength where 1000ppm will be in the analytical range.
For this example assume the wavelength 373.713 nm is selected for iron.
3. When a pure standard of 1000 ppm iron is read as a sample, suppose the value
reported for arsenic at 193.759 nm is 0.022 ppm. The calculation for the Interfering
Element Correction (IEC) coefficient becomes 0.022/1000 or 0.000022. The IEC
value is entered into the coefficient cell for iron according to the display to the left.
4. When samples are subsequently run, the iron concentration will be determined (at
373.713 nm) and that concentration multiplied by the IEC coefficient is subtracted
from the arsenic result.

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5. The results are generated using an iterative approach to a solution. This is
necessary when the references of interferences are circular. In example, Fe affects
Pb affects As, which in turn affects Fe. If a solution cannot be found the result is
“divergent” and the results for that line will show as a “D”.
6. Salsa software can calculate the coefficients automatically for you. After the
interferents have been identified for each analyte, highlight the an interferent in
the NAVIGATION PANEL, enter the concentration of the interferent (a single-element
standard) to be aspirated in the IEC STANDARD FIELD and click the SET BUTTON.
7. While the solution is aspirating click the RUN IEC STANDARD BUTTON.
8. When the reading is completed, the coefficient will appear next to the interferent
when the interfered upon wavelength is highlighted.

Figure A-14 Running an IEC standard

NOTE
Setting interferences (Figure A-13) apply only to the highlighted analyte.

NOTE
Running IEC Standards (shown left in Figure A-14) apply only to the
highlighted interferent; however, calculated coefficients for this interferent
will appear only when the analyte is highlighted (Figure A-14).

A.2 Matrix Interferences


The matrix of a sample is considered any solution component other than the analyte(s)
of interest. Take, for example, a solution being analyzed for Copper (Cu) content and
also containing water, nitric acid and sodium chloride. Cu is the analyte, while the
matrix consists of water, nitric acid and sodium chloride. The matrix can produce
spectral interferences and background shifts. Matrix effects can be divided into two
specific types:
1. Spectroscopic matrix effects
2. Non-spectroscopic matrix effects
Spectroscopic matrix effects and have been discussed previously in Section A.1 "Spectral
Interferences".

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Other Non-spectroscopic matrix effects involve the processes occurring when the
sample is nebulized, atom and ion formation, and how atoms and ions are excited
within the plasma. Non-spectroscopic matrix effects become a problem when the
composition of the calibration standards is very different from the samples.
Non-spectroscopic matrix effects can be sub-divided into two categories according to
the location in which they occur:
1. Those occurring in the sample introduction system, and
2. Those occurring in the plasma.
Each is considered separately in the following sections.

A.2.1 Sample Introduction System Matrix Effects

Analyte intensity measurements are made under steady-state conditions. This means
that the amount of sample being introduced to the plasma remains constant with time.
Consequently, the sample transport rate must be the same for standards and samples.
Because solution composition affects viscosity and surface tension, variances in the
sample transport rate can result. As an example, consider a calibration performed using
standards containing 1% nitric acid and samples containing 15% nitric acid. Since the
solution composition is very different, the solution viscosities and surface tensions will
differ resulting in differing sample transport rates for the two solutions. The difference in
sample transport rates will ultimately lead to erroneous results for the sample analysis. A
similar situation would be encountered if a solution contained a high concentration of
dissolved solids (a sample matrix composed of 1% aqueous salt).

A.2.2 Plasma Matrix Effects

When a sample is introduced to the plasma, atoms and ions are formed and then
undergo excitation processes. The solution matrix will affect the relative numbers of
atoms and ions both formed and excited. When we make intensity measurements for
either species, we assume that the formation and excitation processes will be the same
for both standards and samples. Therefore if the composition of either standards or
samples varies considerably, significant errors may result. A general understanding of
matrix effects will ensure that the analyst can compensate for and eliminate potential
errors.
As an example, consider an aqueous solution containing zinc as an analyte at 10 ppm
concentration and a matrix of 10,000 ppm calcium are to be analyzed. In this example,
the instrument was calibrated using Zn standards, which contained no Ca. Then the
samples containing Zn and the 10,000 ppm Ca are run. Because Calcium is an easily
ionized element a significant number of calcium ions are formed in the plasma, in
comparison to the number of atoms formed. A significant error will result in the Zn
determination due to the presence of the Ca because the Ca in the samples will suppress
the emission of light from Zn ions in the plasma. In comparison to the calibration
standards, the Zn emission intensity will be lower than it should be which will result in
an erroneously low value for this element.

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A.2.3 Determining if Matrix Effects are a Problem

Perhaps the easiest way to determine if matrix effects will be a problem is to use a
technique called “spike addition”. The procedure is carried-out by spiking a known
quantity of one or more analytes into an aliquot of the sample solution. Calibration
standards are prepared and the instrument is calibrated according to the procedures
contained in Section 2.11 "Calibration". Both the spiked and unspiked solutions are
analyzed and the percent recovery for each analyte is calculated as follows:

where %R is the percent recovery, CS and CU are the measured analyte concentrations in
the spiked and unspiked solutions (respectively) and C spike is the known analyte
concentration added to the sample. In theory, a 100% recovery should be achieved
(within experimental error) if no matrix effects are occurring. However, if the percent
recovery is significantly higher or lower than 100%, signal enhancement or suppression
resulting from the matrix is the cause. Instead of the matrix corrections to be discussed
in Section A.2.4 "Coping with Matrix Effects", the % recovery can be used as a correction
factor for analyte concentrations. The correction is performed by dividing the analyte
concentration by the fractional recovery. For example, if the analyte concentration and
percent recovery were found to be 1.204 ppm and 94% respectively, then the true analyte
concentration would be 1.204/0.94 or 1.281 ppm.
The Salsa software can perform % recovery calculations automatically.
1. With the METHOD TAB active, select QUALITY CONTROL CHECKS in the NAVIGATION
PANEL.
2. Click the ADD QC BUTTON.
3. In the ADD QC DIALOG, enter an appropriate name for the spike standard and select
SPIKE from the QC TYPE MENU.
4. Enter the default concentration of the addition and desired acceptance limits and
click OK to accept. In Figure A-15, a spike of 10 ppm was entered with acceptance
limits of 100 +/-10%. The concentration and acceptance limits for each element in
the spike may be edited individually by highlighting the Spike QC name and
entering new information in the SPIKE TABLE.
5. To accept changes click the UPDATE LINES BUTTON.

Figure A-15 Adding a spiked QC for spike recovery analysis

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For use with the autosampler, a sequence must be created. Refer to Chapter 6:
"Sequence" for information on creating a sequence. After entering the sample IDs in the
sequence, additional information must be entered in the last column of the SAMPLE LIST
TABLE in the form of a letter code. The codes tell the software how to treat the data
collected for each sample. Table A-1 "Cup Macro Codes" shows a list of pertinent codes:

Table A-1 Cup Macro Codes


Code Action
A Apply% recovery
D Duplicate
P Calculate% recovery
S Spiked
U Unspiked

A sequence using these codes will look similar to Figure A-16. In the last column, more
than one code can be used in any given row, however they must be separated by a space.
In this example, the first three rows, having the IDs unspiked 1, 2 and 3, are for unspiked
samples. The “U” designation tells the software that the sample is unspiked while the “d”
designates a duplicate. These three sample IDs are followed by three spiked samples
having the designation “S” and “S D”. The software will pool the data from the three
unspiked samples and the three spiked samples to perform the percent recovery
calculation. The third spiked sample in the set also carries the code “P”. This tells the
software to perform the percent calculation using all of the data collected up to and
including the third spiked sample. The sample ID “Unapplied” has no codes in the last
column and thus is treated as if it were an ordinary sample. The last sample ID “Applied”
has an “A” code associated with it, telling the software that the percent recovery
correction is to be applied to this sample. It is important to realize that the sample IDs
used in this example are not unique. Any ID could have been used. Only the codes used
are unique.

Figure A-16 Sequence recovery commands

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Numerous sample matrices can be analyzed by ICP. This requires that the analyst always
be diligent in ensuring that matrix interferences do not cause erroneous results.
Fortunately there are ways to minimize or correct for matrix effects that result from
sample introduction or that occur within the plasma. Refer to Section A.2.4 "Coping with
Matrix Effects".

A.2.4 Coping with Matrix Effects

Matrix Matching
The best way to correct for matrix effects is through a process called matrix matching. In
this correction procedure, the matrix of the calibration standards is matched in
composition as closely as possible to the matrix of the samples. Therefore any changes
in sample introduction or within the plasma due to sample matrix will also occur for the
standards. To be effective, the match between sample and standard matrix should be as
close as possible, but need not be perfect. This procedure can be time consuming and
requires the use of high purity chemical compounds to form the matrix. The software
set-up is the same as if matrix matching were not being used.

Method of Standard Addition (MSA)


In this correction method, two or more accurately measured aliquot of the sample are
used in the determination. One of the aliquots is left in its original state and is referred to
as standard MSA1. The second sample aliquot is treated by spiking in a known volume of
a standard solution containing the elements of interest. This sample aliquot is referred
to as MSA2. The procedure is repeated for each additional aliquot (if any) removed from
the original bulk sample with each successive spike aliquot designated MSA3, MSA4, etc.
The alphanumeric standard designation is used because each successive addition must
result in a higher concentration of added elements in the respective spiked aliquot. If the
element intensities in each aliquot were measured and plotted as a function of the
element concentration resulting due to the spike addition, a calibration plot similar to
that in Figure A-17 would result.

Figure A-17 Method of standard addition calibration plot

To determine the analyte concentrations in the original sample, the data points are fit to
a straight line and the slope and intercept are calculated. The absolute value of the
intercept is the analyte concentration in the sample.

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Alternatively, the procedure can be treated mathematically by considering the
relationship between intensity and concentration. For the analyte in the sample, the
intensity is related to concentration as follows:

where IA is the analyte intensity, k is a constant and CA is the analyte concentration. In


the analysis, a known volume of the sample is spiked with a standard resulting in an
added standard concentration in this volume of CS. The total intensity measured for this
solution can be expressed as:

where I T is the total measured intensity resulting from the sum of the analyte
concentration, CA, and the concentration of the added standard, CS.
If the volume of the added standard is sufficiently large, then a volume correction factor
must be used for both CA and CS:

where C A,F is the final analyte concentration resulting from the initial analyte
concentration in the aliquot, CA,I, having an initial volume, VA,I, and diluted to the final
volume, V F, after being spiked. A similar expression can be written for the added
standard:

where CS,F is the final added standard concentration resulting from the initial standard
concentration in the spike, CS,I, having an initial volume, VS,I, and diluted to the final
volume, VF, after being added.
Substituting the following equations:

into the equation below:

results in the following equation:

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If VS,I is very small in comparison to the aliquot volume, VA,I, then VA,I = VS,I = VF and the
equation above simplifies to the equation below. If IT is plotted as a function of CS, from
equation 3.4.4.2B, a straight line will result having an intercept equal to kC A . The
solution to the equation is obtained when IT equals zero:

In this case CA will equal –CS.

NOTE
The calculation of the intercept is based on the intensity being the
independent variable (i.e.-X) and the concentration being the dependent
variable (i.e.-Y).

A.2.5 Adding a Method of Standard Additions

To use the Method of Standard Additions:


1. With the METHOD TAB active, select STANDARDS MSA in the NAVIGATION PANEL.
2. Click the METHOD OF STANDARD ADDITIONS BUTTON and fill in the MSA TABLE with
addition concentrations.
3. The MSA samples are arranged in a horizontal pattern in the autosampler. For
example, for a 44cup (15mL) rack cup position 1 would be MSA1 (unspiked), cup
position 12 would be MSA2, cup position 23 would be MSA3, and cup position 34
would be MSA4. The next sample would start with cup position 2 as MSA1 and the
pattern repeats.

Figure A-18 Sample placement for method of standard additions

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A.2.6 Running MSA Additions

The Prodigy7 ICP software supports the Method of Standard Additions (MSA). To use the
MSA feature:
1. With the METHOD TAB active, select HIGHLIGHT STANDARDS/MSA in the NAVIGATION
PANEL.

Figure A-19 Selecting the MSA mode

2. In the DISPLAY PANEL select the METHOD OF STANDARD ADDITIONS (MSA) BUTTON and
enter the concentration for the desired additions. You may use 1, 2 or 3 additions.
 MSA2 should be filled for one addition,
 MSA2 and MSA3 should be filled for two additions.
 All three (MSA2, MSA3, & MSA4) must be filled if three additions are employed.
The number of integrations may be changed for MSA replicates using the
pull-down menu in the center of the STANDARDS/MSA SCREEN (with the METHOD
TAB active select STANDARDS/MSA in the NAVIGATION PANEL).

NOTE
Any changes made to the MSA Standards Table are not accepted until the
Update MSA Button is clicked.

3. Once the MSA additions have been defined, click on the RUN MSA BUTTON
to start an MSA analysis. When this button is clicked the RUN MSA
DIALOG below will appear (Figure A-20).

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Figure A-20 Running an MSA sample manually

4. The sample name for this sample should be entered before clicking on the OK
BUTTON. Once OK is clicked the sample will be integrated (just like a sample or
standard in normal mode).
5. After the sample has been run, click on the RUN MSA SAMPLE BUTTON again.

NOTE
Radio buttons for the defined additions will be active. Once a radio button is
selected the sample title field will be populated with the entered sample
name.

6. Click OK to integrate each of the defined additions.


7. When all the defined additions have been integrated the sample concentration will
be calculated and displayed on the RESULTS TAB and the MSA curve displayed on
the CALC VALIDATION TAB.

Figure A-21 MAS results

Note that the standard icon has changed to reflect the Method of Standard Additions (MSA).

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Figure A-22 Displaying an MSA calibration curve

A.2.7 Internal Standard


The theory behind the use of an internal standard is that any change occurring for the
analyte (whether it be related to processes in the plasma or sample introduction) will
also occur for the internal standard. If the analyte signal is enhanced (or depressed) then
the internal standard signal will also be enhanced (or depressed).
For the correction to be effective, the internal standard must be enhanced or depressed
by the same factor as the analyte. If this is the case, using the ratio of the intensity of the
analyte to the intensity of the standard will cancel-out the enhancement or depression
factors. The internal standard must also meet the following additional requirements:
 It cannot be found in the samples, standards or blanks
 It must respond to matrix conditions in a manner similar to that of the analyte
 It must be free of spectral interferences and should not cause spectral
interferences
 It must be chemically inert in the sample matrix
In practice, a known quantity of the internal standard is added to all blanks, standards
and samples such that the concentration in each will be the same. Any element meeting
the previously mentioned requirements can be used as an internal standard. Two
common choices are Yttrium (Y) or Scandium ( Sc). To use this feature in the Salsa
software:
1. Add one or more element wavelengths to be used as the internal standard, to the
protocol.
2. With the METHOD TAB active, select INTERNAL STANDARDS in the NAVIGATION PANEL
(Figure A-23).
3. Place a check mark beside each wavelength(s) to be used as an internal
standard(s). The wavelength(s) will then appear at the top of the table as separate
columns. In the example shown, Yttrium (Y) is selected as internal standard.

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Figure A-23 Assigning internal standards

4. Pair the analytes with the internal standard(s) by selecting the check-box in one of
the internal standard columns for each analyte (click again to deselect). In our
example, Y 410.238 serves as an internal standard for Ca and Ti and Y377.433
serves as the internal standard for Fe, Zn, and Cd.

NOTE
Add the internal standard to the blank, standards and samples in equal
concentrations for this type of analysis.

5. Select STANDARDS/MSA in the NAVIGATION PANEL. Add the concentration of the


internal standard to all standards.
In this example, if Y is the internal standard and the concentration of Y in all
standards is 5 ppm, then this concentration must be entered for all standards in
the method. After calibration, the calibration plot for internal standards displays
an “I.S.” (indicating internal standard) instead of a calibration curve. The average
intensity for all the standards in the calibration table becomes the normalized
intensity for that internal standard.
When samples are analyzed with an internal standard applied, the intensities for each
analyte referenced to an internal standard is multiplied by the normalized internal
standard intensity then divided by the internal standard intensity observed during the
sample analysis.

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A.3 Internal Standards
Internal standards are selected from entered method lines. In the example offered below
Yttrium (Y) is employed as an internal standard.
1. With the METHOD TAB active, select INTERNAL STANDARDS in the NAVIGATION PANEL to
show a list of method lines.
2. To select an internal standard, click on the check box to the left of the wavelength
to be used as an internal standard (Figure A-24).

Figure A-24 Assigning internal standards

3. Once a wavelength is selected, a new column appears with the check boxes for the
internal standard disabled. Click check boxes for wavelengths referenced to the
internal standard.
4. Multiple internal standards can be selected and a new column will be created for
each internal standard added.

NOTE
Users with dual-view instruments must use a separate internal standard for
each view (axial and radial). The same wavelength may be used for both views;
however, it must be entered into the method twice and the view for one of the
wavelengths must be set to radial view.

During calibration, the internal standard wavelengths should be calibrated with all
standard(s) defined as containing the same concentration. Calibration curves
report data in terms of intensity ratios.

NOTE
If changing an existing method to an internal standard method, clear the
existing calibration.

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NOTE
An equal concentration of the internal standard(s) must be added to all
standards, samples and quality control checks. This can be accomplished by
individually spiking all standards and samples, or by on-line merging of an
internal standard solution using the peristaltic pump.

A.4 Import/Export of Methods


Salsa is capable of importing and exporting methods between databases.The exported
methods will have the file name form of METHODNAME.METHOD.

A.4.1 Export a Method

1. Open the method that is to be exported.


2. With the METHOD TAB active, select METHOD in the MENU BAR then EXPORT.

Figure A-25 Export method

3. A SAVE AS DIALOG box opens to allow the database to be saved to a location of


choice.

NOTE
Because of Salsa’s database memory structure, the software permanently
retains the original Method name. When the method is imported into another
Salsa database, it will appear with its original name. If a method is renamed,
the change is superficial.

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Figure A-26 Method export “save as”

4. Click SAVE to export the Method.

A.4.2 Importing a Method

1. On the METHOD TAB, select METHOD in the MENU BAR, then IMPORT.

Figure A-27 Import method

2. The OPEN FILE DIALOG will be displayed (Figure A-28).

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Figure A-28 Import method dialog

3. Select the method to be imported and click OPEN. The selected method will appear
on the OPEN METHOD DIALOG.

Figure A-29 Open method dialog

4. Salsa will display an error message if the method is already in the Salsa database.

NOTE
Because of Salsa’s database memory structure, the software permanently
retains the original Method name, regardless if the method has been renamed.
The message shown in Figure A-30 will also be displayed if the method has
had its name changed and the user is attempting to import it back into the
database.

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Figure A-30 Import method error display

NOTE
If the intent is to create a copy of the method, make the Method Tab active,
select Method in the Menu Bar, then Clone.

A.5 Database Manager


Salsa software stores methods and analytical data in a relational database named
SALSA.MDB. This database must reside in the directory that Salsa is installed in (e.g.,
C:\Salsa\Salsa.mdb).

A.5.1 Archiving Databases

As a database increases in size, the user may notice a decrease in speed, especially when
working on the ANALYSIS TAB. The maximum size of the Salsa database is 2GB. To keep an
acceptable performance speed it is recommended that the database be archived once its
size begins to approach 1GB.
When a database is archived, all analytical data will be archived. The remaining database
will contain only methods data (elements, wavelengths, standards concentration,
calibration data, etc.). As part of the archival process, Salsa will ask to delete any full
frame images.

NOTE
Once a database has been archived, new data cannot be added to the
database, nor can it be made active again. Archived database's are intended as
reference tools only.

Follow the steps below to archive the database are:


1. With the METHOD TAB active, select TOOLS from the MENU BAR and then select
DATABASE MANAGER (Figure A-31).

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Figure A-31 Open database manager

2. Click the CREATE ARCHIVE button.

Figure A-32 Database manager

3. Prior to archiving Salsa will ask to delete all the Full Frame Images (if any are
present) associated with the database.
 If YES is selected, the images are permanently deleted.
 If NO is selected, the images will remain in the Salsa\FF folder.

Figure A-33 Delete full frame images prompt

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4. Once the process is complete, the archived database will be found in the Salsa
directory. The archive name will show the date the database was archived to
simplify finding and loading the archived data at a later time.

Figure A-34 Open database archive dialog

5. Salsa will then connect to a new database that will have all of the method
information, but no analytical data. A comparison of the ANALYSIS TREE for an
original and archived database is shown in the Figure A-35. The new database is
now ready for use.

Figure A-35 Comparison of analysis tree before and after archiving

Database After Archival

Database Prior to Archival

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A.5.2 Viewing Archived Databases

Salsa permits the user to view data contained in archived databases. The archived
database view will allow examination of wavelength scans and analytical data, reporting
and recalculation of the sample result.

NOTE
Once a database has been archived, new data cannot be added to the
database, nor can it be made active. Archived databases are intended as
reference tools only.

1. With the METHOD TAB active, select TOOLS from the MENU BAR and then select
DATABASE MANAGER.

Figure A-36 Open database manager

2. Click the OPEN ARCHIVE button.

Figure A-37 Database manager

3. Select the database archive to be opened from the OPEN DATABASE ARCHIVE window.

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Figure A-38 Open archive dialog

4. Once the archive is loaded, the user will have access the Sample ID, Symbol,
Wavelength, Concentration, Intensity, Background Correction Points, and Raw
Intercept (Figure A-39).

NOTE
When an archived database is opened, icons for instrument operations, such
as RUN STANDARDS or COLLECT FULL FRAME IMAGES are disabled (Figure
A-39).

Figure A-39 Database in archive view

When the database is open for viewing, Menu Bar selections are inactive (grayed out)
as shown above.

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5. To return to the active Salsa database, make the METHOD TAB active. Select TOOLS
from the MENU BAR, then select DATABASE MANAGER.

Figure A-40 Open database manager

6. Click the OPEN SALSA.MDB BUTTON and the working database will be reloaded.

Figure A-41 Database manager

A.5.3 Reusing a Database Archive

Though not recommended, it is possible to reuse a database archive.

NOTE
It is recommended that a copy of the archive be made before the archive is
renamed to preserve the original archive.

To reuse a database archive:


1. Exit the Salsa software
2. Navigate to the Salsa directory (C:\Salsa\Salsa.mdb)
3. Rename the active Salsa database
4. Rename the archive file to be loaded to Salsa.mdb
5. Restart the Salsa program

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A.6 Synchronizing External Hardware to Sample Sequence
Advanced users can control external hardware via the sequence of sample runs as if a
pseudo autosampler. An example of this, would be using a laser ablation system as a
sample introduction to the ICP. This feature is optional and, if needed, must be installed.
Contact Teledyne Leeman Labs for more information.
To use the feature (known as ‘SampSync’) the user needs to add the string SampSync
followed by other instructions into the Startup.ini file found in the Salsa directory. The
structure of the command text is shown below:
SampSync Port, Baudrate, Databits, Parity, Stopbits, “Before Sequence”, “Before Uptake”,
“After Uptake”, “After Sample”, “After Sequence”
The ASCII code necessary for the actions on the external device are entered in the
appropriate spot in the line inside quotations.
The graphic below demonstrates the event driven flow of the ASCII code transmission.

Figure A-42 Using sampsync

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A.6.1 SampSync Special Characters or String Commands

NOTE
\: is used in conjunction with letters to indicate various special characters

Example:
 \r is a carriage return
 \n is new line (line feed)
 %{}: is used in conjunction with special variables to output text based data
from SALSA
Example:
 %{c0} is to output a string of currently running cup number (where cup 1 is
output as 0)
 %{c1} is to output a string of currently running cup number (where cup 1 is
output as 1)
 %{dx} is to Wait x seconds before proceeding to next event.
Two examples for startup file:
1. SampSync 3,9600,8,E,1,””,“X=1\r”,“34”,”X=3\r”,”
In this example the port is COM3:, baudrate=9600, 8 databits used, Even parity, 1
stopbit, before sequence send no command, Before uptake send ‘X=1’ followed by
carriage return, After uptake send ‘34’, After sample data collection send ‘X=3’
followed by carriage return, At end of sequence send no command.
2. SampSync 4,9600,8,N,1,
””,”%d{3}StartScan%{c0}\r”,””,”StopScan\r”,”%{d3}SetValves 0\r”
In this example the port is COM4:, baudrate=9600, 8 databits used, No parity, 1
stopbit, before sequence send no command, Before uptake wait 3 seconds and
send ‘StartScan’ followed by cup number to run followed by carriage return, After
uptake send no command, After sample data collection send ‘StopScan’ followed
by carriage return, At end of sequence wait 3 seconds and then send ‘SetValves0’
followed by carriage return. If no action is to be taken for a given event, use the two
double quotations to symbolize a null string.

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A.7 Creating a Custom Line Library

WARNING
This procedure should only be followed by experienced users and/or
Teledyne Leeman Labs trained personnel. If the following procedure is
used it can be reversed by reinstalling a backed up copy of the LINES.TXT
file in the Salsa directory.

NOTE
Before proceeding, backup the file LINES.TXT in the Salsa directory. This may
be performed by making a copy in the Salsa directory or copying the file into
another directory or to another media (CD, flash drive, external hard drive,
etc.).

1. In Windows copy the LINES.TXT file from the C:\Library directory to the C:\Salsa
directory. Copy over the existing LINES.TXT library in the C:\Salsa directory.
2. From Salsa create a Method named “Lib Fit”.
3. Prepare a solution of 10 ppm Tl, As, Sb, P, Pb, and Cs.
4. Add the following lines and views:

Table A-2 Wavelength for Library Fit


Line Viewa
Hg 253.625 Hg
Hg 435.833 Hg
Hg 404.656 Hg
Hg 365.015 Hg
Hg 576.960 Hg
Hg 546.074 Hg
TI 190.864 Axial
As 193.759 Axial
Sb 206.833 Axial
P 213.618 Axial
Pb 220.353 Axial
Cs 894.347 Axial
a. If radial system select radial view instead of axial
view

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5. Switch to the INSTRUMENT CONTROL PANEL and click the DIAGNOSTICS BUTTON. Verify
that the Hg Lamp Deltas located in the upper right corner of the DIAGNOSTICS
DIALOG are zero for both X and Y. If they are not, type in zeros and click APPLY.
6. Switch view to HG LAMP and run a 0.01 sec and a 1 sec FF. Label FFs as “Hg lamp
0.01s” and “Hg lamp 1s”.
7. Switch view to Axial. (Radial, if radial only instrument)
8. Run a 1 sec, 10 sec, and 60sec FF of a BLANK solution. Title FFs as “Blank 1s”,
“Blank 10s”, and “Blank 60s”.
9. Identify the blaze of the grating by the following procedure:
a. View the “Blank 1s” FF.
b. Move the cursor over to the peak intensity visible spectrum (Y position
140+/-40). Record the X,Y position of the cursor. These values are named X1,
Y1.
c. View the “Blank 60s” FF.
d. Move the cursor over to the peak intensity ultraviolet spectrum (Y position 630
+/- 30). Record the X,Y position of the cursor. These values are named X2, Y2.
e. Calculate blaze equation:
[m=(y2-y1)/(x2-x1) b=y2-(m*x2)]
10. Run a 1 sec and a 10 sec FF of a 10 ppm UV soup solution (including Cs). Title FFs
as “UV 1s” and “UV 10s”.
11. Switch to ALIGN WAVELENGTH TAB and align the Hg 253.652 line using the “Hg lamp
0.01 sec” FF.

NOTE
Salsa.exe will not allow alignment of the Hg peaking line producing a dialog
reporting the desired X and Y Hg deltas. Record the deltas.

12. Select INSTRUMENT CONTROL and click the DIAGNOSTICS BUTTON.


13. Type in the Hg X and Y deltas in the fields located at the upper right corner of the
DIAGNOSTICS DIALOG. Click APPLY.
14. Once the Hg Lamp deltas apply has completed close the DIAGNOSTICS DIALOG and
return to the ALIGN WAVELENGTH TAB and verify that the Hg 253.652 line’s subarray
is now aligned using the “Hg lamp 0.01s” FF.

NOTE
If alignment is not correct repeat procedure starting with zeroing out the Hg
Lamp Deltas.

15. Align and accept the remaining method Hg lines (not including 253.652) using the
“Hg lamp 0.01s” and “Hg lamp 1s” FFs.

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16. Align and accept the remaining method lines using the “UV 1s” and “UV 10s” FFs.
When necessary toggle between the “UV” FF and its’ corresponding “Blank” FF to
verify the peak of interest for alignment.

NOTE
If uncertainty remains for aligning a method line generate a single element
solution FF and align.

17. After all lines have been aligned run a single replicate, 30 second sample of the UV
soup solution. Check all results on SCANS TAB for peak alignment within subarray.

NOTE
This action also saves the current version of the library and method.

18. Determine the alternate order orientation for Hg 253.652 by switching to the ALIGN
WAVELENGTH TAB and clicking on the 2nd ORDER BUTTON, align on the peak, and
press accept.

NOTE
Salsa.exe will not allow alignment of the 2nd order Hg peaking line producing
a dialog reporting the X and Y Hg deltas. Record the 2nd order deltas.

19. Switch to the INSTRUMENT CONTROL PANEL and click the DIAGNOSTICS BUTTON. On
the DIAGNOSTICS DIALOG click the LIBRARY FIT BUTTON.
20. On the LIBRARY FIT DIALOG type the 2nd order Hg delta X and Y values recorded in
step 20 into the Hg 254 boxes located on the upper left corner and click APPLY ROT.
21. After the 2 nd order Hg delta X and Y deltas have been applied check the “Err X” and
“Err Y” values in the table for excessive values (>40). If any are present deselect the
check box for that line to remove it from the alignment process.
22. Enter the m and b blaze equation values recorded previously.
23. Click the FIT LIBRARY BUTTON and wait for the results to update (~1 to 2 min).
24. Check fit results and click the ACCEPT FIT check box at the bottom of the LIBRARY FIT
DIALOG if desired to write updated library. If check box is not checked and dialog is
closed the original library will be reinstalled.

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A.8 Salsa Computation Mathematics
The primary purpose of any analyzer is to yield results that are a reflection of the
physical world. In the case of an analytical chemical analyzer, such as a ICP-OES the
results are in terms of concentration. Various computation algorithms are used by the
Analyst to achieve accurate results. The purpose of this section is to explain the
algorithms used within the Salsa software to produce those results. This allows the
analyst to ‘validate’ the software, as to the proper selection of an algorithm, for a given
method.

NOTE
Updates are represented in concentration terms in the Salsa software. This is to
make intuitive decisions based on the values. The UI is in terms of
concentration or concentration ratio based on the calibration. The US is in
terms of sensitivity change of intensity or intensity ratio versus concentration
or concentration ratio. The UI and US terms used in the computations in the
formulae in this document are in different terms. The mathematical definition
of the displayed UI and US are derived from the internal versions of UI and US
as follows:

Is the US in sensitivity correction displayed and reported.

Is the UI in concentration displayed and reported.

Is the US used in the internal computations as described in this section.

Is the UI used in the internal computations as described in this section.

A.8.1 Concentration of Unknown Sample Calculations

Sample calculations are straightforward. For all elements:

concentration

Where the following represents:


A – Quadratic coefficient
B – Linear coefficient
C – Intercept coefficient
I’-Background corrected intensity

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A.8.2 Update Intercept and Update Slope Calculations

For Concentration Ratios and Updates see Section A.8.9 "Concentration Ratios and
Updates".
This document describes the math behind calculating updates for the Prodigy7. If any
line in the method is calibrated using concentration ratio, then all lines follow the
Concentration Ratio Update calculations, as described in other section. The default
values for UI and US are 0 and 1 respectively.
An unknown sample is calculated based on the following formula:
Concentration = US x [A x (i - UI)2 + B x (i - UI) + C]
A, B, and C are our calibration coefficients.
Input “i” is the raw intensity for the data just taken.
Csolution is the actual concentration in the solution as mixed.
The Update Intercept (UI) is calculated based on the following formulae:
UI = I i- Ibc
Where Ii is the background-corrected intensity of the update intercept sample that
was run.
Ibc = -B + [B2 – 4 x A x (C – Csolution)]
2xA
For a quadratic fit; or
Ibc = Csolution - C
B
For a linear fit
The Update Slope (US) is calculated based on the following formula:
US = Csolution _________.
A x (Is – UI)2 + B x (Is – UI) + C
Where Is is the background-corrected intensity of the update slope sample that
was run.

A.8.3 Internal Standard Calculations

The calibration equation for an analyte is derived from the ratio of the measured
intensity for the analyte to the measured intensity of the internal standard for the
analyte. Keep in mind that multiple internal standards are allowed in a given method;
however, only one internal standard is allowed per analyte. For standards, repeat
integrations, a ratio is calculated for each repeat, and the average of the ratios is used to
calculate the calibration curve. When a sample is analyzed, the ratio of the measured
intensity for the analyte (I) to measured intensity of the internal standard (Iis) is used to
compute the concentration, as in
Concentration = A * (I/Iis)2 + B * I/Iis + C
For calculating coefficients A, B, and C use the average ratios for a given concentration
and perform the inverse calculation as would be done for a normal intensity.

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For unknown samples the internal standards report a concentration. A “pseudo”
concentration is computed:
Concentration = I is /I isc I isc = Average of all internal standard intensities during
calibration
This ratio can be qualitatively used to determine how much the system sensitivity has
drifted or is noisy. For example, if no drift of the intensity of the internal standard exists
the “pseudo” concentration will be computed as 1. If the internal standard drifts down to
50% of the original signal a result of 0.5 will be reported.

A.8.4 IEC Calculations

IEC corrections to standard and update concentrations are computed via the following
formula:

Where
user input standard/update concentration for element i

IEC corrected standard/update concentration

IEC coefficient of element j on element i

m - number of lines in the protocol


IECs are then applied iteratively to an element’s sample concentration or to MSA
computed concentrations. The calculations for each element are performed for each
iteration:

or for

At the end of each iteration, is tested for convergence

(i.e. ). If the sample concentrations have not converged, another iteration is


performed, up to a maximum of ten iterations. If the sample concentrations do not
converge after ten iterations, an error message is displayed, and an error exception is
written to the log file.

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A.8.5 Duplicate Sample Calculations

To calculate the Relative Percent Difference (RPD) for duplicate samples and generate
duplicate reports. RPDs are computed via the formula:
RPD = (C2 - C1)/((C2 + C1 ) / 2) * 100
where
C1 - Concentration of original
C2 - Concentration of duplicate
Salsa generates a duplicate report while processing a D cup macro action command.

A.8.6 Spike Recovery and Percent Recovery Calculations

Percent recovery of spikes is calculated inclusive of corrections for weight and dilution.
Percent recovery is computed with spike and unspike concentrations that have been
corrected via weight and dilution factors, i.e.

where
Cdws- Average spiked concentration (or

Cdwu- Average unspiked concentration (or

C- User input spike concentration


Csi- Concentration found for spiked sample
Cui- Concentration found for unspiked sample
Dili- Volume of sample (default = 1)
Wgti- Weight of sample (default = 1)

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A.8.7 Concentration, Calibration, and Ratio Calculations

The terminology used for concentration, calibrations, and ratio calculations of any
element are:

and

to represent the standards concentrations and the average intensities resulting from
running a standard for a particular line. You can specify up to 33 different standards for
the protocol. If a line is corrected by an internal standard, we use:

to compute the correction. IIi is intensity of the internal standard for this element and i
is the standard number. If a line is not IS corrected, we use the actual intensity, i.e.:

These ’s are used to compute the calibration curve coefficients. There are two
methods for computing coefficients. The basic formula for calculating the calibration
coefficients is the least squares equation below:

where ‘n’ is the number of standards run.

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A.8.8 Concentration Ratio Calculations

Concentration Ratio (CR) computation techniques are generally useful for alloy analysis
of base metal digests. The goal of concentration ratio is to produce an assay report that
has all components add to 100%. The concentration ratio is a ratio of each element
concentration divided by the concentration of a base element. The calibration curves
are plotted as CR versus Intensity Ratios. Where Intensity ratios are calculated with the
denominator being the intensity of the base element for the given repeat of the given
standard. This differs from the use of Internal Standards for three reasons:
 The concentration level of the base element typically varies between each
standard and sample.
 The calibration curve for each line element is a plot of CR versus Intensity
Ratio, as opposed to Concentration versus Intensity Ratio.
 The use of Concentration Ratio allows for only one base element, this is not
true for Internal Standards. When a Concentration Ratio base element is
selected the use of Internal Standards is locked to only one, the base element.
Along with the examples above, there is a second way for Concentration Ratio (CR)
corrected elements is to compute the CR via:

where is the standards concentration for the CR base


element. These concentration ratios are used to compute the least squares fit.
No calibration curve is computed for the CR base element, since when we run samples
we compute the base element’s concentration ratio from the concentration ratios and
concentrations of the other elements analyzed in the sample.

A.8.9 Concentration Ratios and Updates

Updates coefficients are the UI and US factors in the equations:

where is the intensity or intensity ratio of the line when an update is run, and I' and
are the “true” intensities or “true” intensity ratios (from a run of a calibration standard or
backed-out of a calibration curve). To compute the update coefficients, solve for UI and
US via:

UI and US are always calculated together.

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Due to the interdependence of UI and US, it is important that users run both before
proceeding to run samples, although not necessary. The following scenarios of running
updates are handled as described:
Precondition 1: UI & US exist in the method
Scenario 1a: UI is run but the US has not been run.
Exception: If multiple US for line, then use the highest concentration
US for line. Calculate and assume
Scenario 1b: US is run but the UI has not been run.
Exception: If multiple UI for line, then use the lowest

concentration UI for line. Calculate and assume


Scenario 1c: UI & US have been run at some time in the ANALYSIS TREE. Also, one of them
has just been run. This is the normal case.
Procedure: Calculate and based on the most recent

available runs. Use the and from the most recent US std and UI std runs.
Precondition 2: UI only exists in the method
Scenario 2a: UI is run.
Exception: If UI = single std then US = same std else set

from the high standard and assume


Precondition 3: US only exists in the method
Scenario 3a: US is run.
Exception: If US = single std then UI = 0 conc. else set from

the low standard and assume .

The following text explains how to calculate the and .

and must be computed before computing UIand US. If the

update standard is also a calibration standard, then and are the actual intensities
or intensity ratios read at calibration time. If the update standard is not a calibration
standard, or the calibration standard has been “deselected” on the LINE CALIBRATION

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SCREEN, and are computed from the calibration equation by finding the roots of:

where and are the concentrations or concentration

ratios of the update intercept and slope. , , and are the

calibration coefficients. Note that and are computed

after IS correction; also note that and are not computed for the CR base
element since the base element’s CR is computed from the (updated) data of the other
elements.

The calculations of and must be performed first to calculate


the and . There are three cases to calculate the and

the .
Case 1: The update standard is the same as a standard.

If the update standard is not a calibration standard or the calibration standard has been
“deselected” on the LINE CALIBRATION SCREEN (i.e.- all repeats unchecked), then case 2 or
3 must be used.
Case 2: The calibration line of interest is a linear fit.

Case 3: The calibration line of interest is a quadratic fit.

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A.8.10 Concentration Ratios and Sample Calculations

Sample calculations are straightforward. For all elements except the CR base element,
we internal standard correct the intensities of the appropriate elements, update the
element’s intensity via:

and then compute the concentration or concentration ratio for the element (not the CR
base element) by concentration or CR

To compute the concentration for the CR base element, we use:

where
Sum of the computed concentrations of all elements which are not CR
corrected, excluding the CR base element.
Sum of the CRs of all elements which are CR corrected, excluding the CR base
element.
To compute the concentration for a CR element, use:

where
element’s concentration ratio
concentration of base element

NOTE
Conc. Ratio requires that all calibrations units are in weight%.The software will
warn a user before running a standard or sample if the element concentrations
of any standard add to more than 110.

A.8.11 Calculation Sequence and Protocol

Sample calculations are performed as a repeatable process. The process is a sequential


and/or iterative set of mathematical calculations as performed by the software. The goal
of this text is to describe the process of calculation based on the users setup in the
Method. The process sequence of sample calculation is outlined below:
 Internal Standard computation
 Blank Subtraction executed (only available post run in report generation)
 Concentration Ratio computation
 IEC computation (An iterative solution)
 Weight, Volume and Dilution computation
 Duplicate Relative Percent Difference (based on historical data)
 Spike Percent Recovery (based on historical data)
 MSA result computation (based on historical data)

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A.9 Diagnostics
Clicking on the DIAGNOSTICS button opens the display shown in Figure A-43.

NOTE
It is strongly recommended that operators make NO changes on this display
without first speaking with Teledyne Leeman Lab’s Customer Support.

For more information on the DIAGNOSTICS DIALOG refer to the Appendix A: "Advanced
User Reference".

Figure A-43 Instrument diagnostics screen

A.9.1 Motors Area

In the top left are all the system motor controls:


 Mirror X, Y are for the source mirror
 Slit X,Y are for the optional adjustable slits
 Autosamp X,Y,Z are for the autosampler probe.
The current location of each motor appears in the left box. The motor can be moved to a
new position by entering a number in the appropriate window (or use the up/down roll
buttons). When the new position is entered, click the < button to apply the new location.
Each motor is installed with a sensor that tells it its home position. The right-most
buttons in this area define the motor status as “Home” when the sensor is engaged by
changing its display to HOMED. The STATUS BAR will indicate “Homing Motor X”. Each
motor can be reset (sent to home) by clicking on the HOME button. Home is defined as a
location of 100 steps.

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A.9.2 A/D Channels Area

Below the motor controls are outputs that the system controller monitors. These outputs
are reported in either counts or physical units based on the status of the check box. The
A/D channels are recorded for each sample analysis and can be played back by making
the ANALYSIS TAB active and selecting the CONTROL CHART TAB.

A.9.3 Optics Area

In the Optics area are two editable fields for minor corrections to the detector image
mapping. These adjustments (deltas) will help to position the analytical wavelength
subarrays over the emission peaks. Use the Hg 253.652 nm line and view the Hg lamp to
align optics (see Operator's Manual).
Below the delta fields are displayed the current locations for each view (uneditable) and
MANUAL SET BUTTONS.

Caution

Clicking on the Axial, Radial, or Hg Lamp Button will take the Mirror X, Y values
currently displayed in the Motor Area and set the chosen view to that location.

A.9.4 Set Points

The current values programmed for spectrometer heater temperature, peltier cooler
temperature (camera), optics purge flow rate, and camera coolant water temperature
appear in the Set Points area but are not editable here. Changes may be made in the
startup.ini file only. The CLOSE Button will exit the DIAGNOSTICS DIALOG.

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Compliance Statements

DECLARATION OF CONFORMITY
Equipment: Prodigy 7
Name and address of
Teledyne Leeman Labs
applicant: 110 Lowell Rd
Hudson, NH 03051
Name and address of
manufacturer: Same as Applicant

Name and address of


the factory: Same as Applicant

Rating and principal


characteristics: 208-250AC, 30A, 50/60 Hz

Trade mark: (If any)

Model / Type ref.: Prodigy 7

A sample of the product has Low Voltage Directive 2006/95/EEC &


been tested and found to be
EMC Directive 2004/108/EEC
compliant with the:

Standard(s) used: EN 61010-1 / IEC 1010-1 Safety Requirements for Electrical


Equipment for Measurement, Control and Laboratory Use EN
61326-1: 2006, Electrical Equipment for Measurement, Control and
Laboratory use EMC requirements EN55011,2009 European
Industrial scientific and medical (ISM) radio-frequency equipment-
Electromagnetic disturbance characteristics-Limits and methods of
measurement, Group 2 Class A
EN 61000-3-2, 2006, Section 2, with A2 (2005) Limits for Harmonic
Current Emissions (Equipment Input Current<16 Amps per phase)
EN 61000-3-3, 2008, Section 3, with A2 (2005), Limitations of Voltage
Fluctuations and Flicker in Low Voltage Supply Systems for
Equipment with Rated Current <16 Amps.
EN 61000-4-2 – Electrostatic Discharge
EN 61000-4-3 – Radiated Electromagnetic Fields
EN 61000-4-4 – Electrical Fast Transient/Burst
EN 61000-4-5 – Surge Immunity Requirements
EN 61000-4-6 – Conducted Disturbances Induced By Radio-
Frequency Fields
EN 61000-4-11– Voltage Dips, Short Interruptions and Voltage
Variations Immunity Test

As shown in the 2013-161_Leeman_Labs_Report EMI_EMC ALR.PDF, All documents


Test Reports: in Q:\Documentation\152-
CONFORMITY_TESTING_&_REPORTS_&_CERTIFICATES\152-
00013 CE Reports Prodigy7\Test Results Safety
Date: July 1, 2014 Signature:

Name: Arthur Reed


Title: Dir. R&D/Engineering
PN 152-00013
Company: Teledyne Leeman Labs
Warranty

LIMITED WARRANTY
(a) For Goods: Seller warrants that all Goods delivered under Buyer’s Order shall be free from defects in
material and workmanship, and conform to Seller’s specifications for a period equal to (a) twelve (12)
months from the date of original shipment for instruments, and (b) ninety (90) days from the date of original
shipment for consumables, spare parts, and accessories. This warranty does not apply to any Goods that,
upon examination by Seller, are found to have been (a) mishandled, misused, abused, or damaged by
Buyer or Buyer’s customer, (b) altered from their original state, (c) repaired without Seller’s prior written
approval, or (d) improperly stored, installed, operated, or maintained in a manner inconsistent with Seller’s
instructions. This warranty does not apply to defects attributed to normal wear and tear. Seller, at its sole
option, shall either repair or replace defective Goods, or issue Buyer a credit for the original price of the
defective Goods. Such repair, replacement, or credit by Seller shall be Buyer’s sole remedy for defective
Goods. Under no circumstances is Seller liable for recall, retrieval, removal, dismantling, re-installation,
redeployment, or re-commissioning of any defective Goods or any costs associated therewith.
Consumables obtained from third parties shall bear the warranty of their manufacturer. The warranty period
for repaired or replaced Goods or re-performed Services shall be the unexpired portion of the original
warranty period.

(b) For Services: Seller agrees to perform repair Services and standard preventative maintenance of the
equipment specified on the face of Buyer’s Order. Seller shall perform the Services (a) in a professional
and workmanlike manner, (b) in accordance with applicable professional and industry standards, and (c) in
compliance with all applicable laws. Unless agreed otherwise by Seller and specified on the face of Buyer’s
Order, parts, on-site Service, freight, and travel expenses are not included in the Service fee. Parts
supplied under Buyer’s Order shall be new or reconditioned and shall meet Seller’s specifications for the
equipment. Parts that are replaced by Seller become the property of Seller. The determination as to
whether to repair or replace equipment or related parts shall be at the sole discretion of Seller. Seller
warrants all Services for ninety (90) days after completion unless otherwise mutually agreed by the Parties
under a separate Service contract. In the case of defective Services, Seller shall re-perform such Services
and such re-performance by Seller shall be Buyer’s sole remedy for defective Services.

(c) THESE EXPRESS WARRANTIES, INCLUDING THE REMEDIES SET FORTH HEREIN, ARE
EXCLUSIVE AND ARE IN LIEU OF ANY AND ALL OTHER WARRANTIES, EXPRESS OR IMPLIED. NO
WARRANTY OF MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE IS INTENDED OR
GIVEN. IN THE CASE OF GOODS OTHER THAN THOSE OF SELLER’S OWN MANUFACTURE,
SELLER MAKES NO WARRANTIES, EXPRESS, STATUTORY, OR IMPLIED.
Prodigy7 User Manual
Index

A D
access panels database manager, 7-27
front removal, 8-8 reusing archived databases, A-32
overview, 8-7 viewing archived databases, A-30
adding element wavelengths, 3-2 diagnostics, 8-32
air filters Installation Test Procedure, 8-32
cleaning, 8-24 resetting source mirror, 8-32
locations, 8-24 screen, 5-5, A-47
analytical parameters dual-view mirror
setting, 2-26 adjustment, 2-14
autosampler, 5-4
controls, 5-4 E
maintenance, 8-19 echellogram
troubleshooting, 8-32 unusual shapes in, 8-29
auxiliary flow, 3-16 emission line, 3-9
atomic, 3-9
B freedom from interferences, 3-9
background correction, A-1 hard, 3-9
complex background, A-5 ionic, 3-9
correction position, A-4 linear dynamic range, 3-8
curved background, A-4 soft, 3-9
simple background shift, A-3
sloping background, A-4 H
buttons hazard severity levels, 1-2
maintenance button, 4-6 histogram peak
overview, 4-5 not showing, 8-32

C I
calibration, 2-41 Inductively Coupled Plasma (ICP), A-1
accepting, 2-47 temperature, A-1
examining, 2-47 instability
calibration standards troubleshooting, 8-30
adding, 2-41 Installation Test Procedure, 8-32
deleting, 2-44 instrument control bar, 4-6
modifying, 2-43 Interfering Element Correction
recalculating, 2-57 automatic, A-7
reviewing data, 2-46 calculate, A-7
running, 2-44 calculation example, A-7
camera entering data, A-9
icing, 8-29 interfering element correction factors, A-7
camera water cooling system manual, A-10
fill procedure, 8-20 testing for accuracy, A-10
use of anti-algae solution, 8-20 interlocks
check standards, 2-48 diagnosing and corrective action, 8-28
adding, 2-48
deleting, 2-49
failures, 8-26 L
modifying, 2-49 labware
running, 2-50 cleaning, 8-17
coolant flow, 3-15 LDR

I-1
emission line, 3-3 plasma parameters
auxiliary flow, 3-16
M coolant flow, 3-15
maintenance effects on emission intensity, 3-13
access panels, 8-7 nebulizer pressure, 3-15
button, 4-6 RF power, 3-14
front access panel removal, 8-8 sample uptake rate, 3-17
powering off the instrument, 8-6 samples in organic solvent, 3-14
procedures, 8-1 Si emission, 3-16
required, 4-7 powering off the instrument, 8-6
routine, 8-1 privilege levels, 4-2
scheduled, 4-6 purge gas
matrix effects cylinder replacement, 8-10
determining presence, A-14 dehydrator replacement, 8-9
plasma, A-14
sample introduction, A-13 Q
matrix interference quality control
correcting, A-16 automation, 5-28
internal standard, A-21 checks, 2-48
matrix matching, A-16 creating standard, 5-27
method of standard addition, A-16 standard locations, 5-30
menu bar, 4-3 standards, 5-28
method standards - extra volume, 5-28
creating a method, 5-2
creating a semiquant method, 5-34 R
development, 3-1 recalculation of data, 2-57
opening existing methods, 5-2 reporting data, 2-59
selecting wavelengths, 3-2 CSV file output, 2-61
method of standard addition, A-16 exporting data to LIMS, 2-61
saving report parameters, 2-60
N required maintenance, 4-7
navigation panel, 4-8 results
analysis, 4-9 reviewing, 2-56
method, 4-8 RF power, 3-14
sequence, 4-9 rinse
nebulizer time using autosampler, 3-12
cleaning, 8-15 routine maintenance, 8-1
installation and adjustment, 2-18 log, 8-2
pressure, 3-15 routine maintenance procedures, 8-6
sample uptake rate, 3-17 autosampler, 8-19
notation, 1-2 camera water cooling system, 8-20
labware cleaning, 8-17
P nebulizer cleaning, 8-15
peak source, 2-29 plasma viewing window, 8-11
peristaltic pump pumps and tubing, 8-14
controls, 5-10 sample introduction assembly, 8-19
set-up and adjustment, 2-3 schedule, 8-3
troubleshooting, 8-25 spray chamber cleaning, 8-14
plasma torch, 8-18
auto start, 2-27, 5-7
auto start flowchart, 5-8 S
controls, 5-7 Salsa
igniting, 2-27 buttons, 4-5
manual start, 5-8 software overview, 4-1
position, 2-29 Salsa calculations, A-38
troubleshooting, 8-25 calculation sequence, A-46
troubleshooting checklist, 8-26 concentration and calibration, A-38
viewing window cleaning, 8-11 concentration ratio, A-43

Index
I-2
Prodigy7 User Manual
concentration ratio and updates, A-43 interlocks, 8-28
duplicates, A-41 labware, 8-31
interfering element (IEC), A-40 overview, 8-25
internal standard, A-39 peristaltic pump, 8-25
recovery, A-41 plasma, 8-25
unknown sample concentration, A-39 plasma will not ignite, 8-26
update intercept and slope, A-39 resetting source mirror, 8-32
sample sample introduction, 8-30
analysis, 2-52 unusual shapes in full echellogram, 8-29
analyzing, 2-52 water recirculation system, 8-31
running, 2-52 twist-n-lock sample introduction system, 2-5
uptake rate, 3-15, 3-17 axial and dual-view systems, 2-6
uptake time, 3-12 radial view systems, 2-8
sample introduction system
optimization by sample type, 2-19 U
scheduled maintenance, 4-6 uptake time, 3-12
sequence user privilege levels, 4-2
building, 2-54
edit rack while running, 6-5
methods, 6-6 V
reporting, 7-23 view configurations, 1-7
sample correction factor, 6-3
sample list table, 6-2 W
using external hardware, 6-13, A-33 water recirculation system
source mirror backflush procedure, 8-22
resetting, 8-32 chemical wash procedure, 8-24
spectral interferences filter replacement, 8-22
cause, A-1 overview, 8-21
spectral overlap, A-5 system water change, 8-21
detecting, A-6 troubleshooting, 8-31
direct, A-6 wavelength
partial, A-6 alignment overview, 2-34
spectrometer automatic alignment, 2-38
auto alignment, 2-33 manual alignment, 2-34
manual alignment, 2-31 scans, 2-41
spike recovery, A-14 selection, 3-2
code in autosampler rack file, A-15 wavelength scans, 3-3
spray chamber calibration standards, 3-4
cleaning, 8-14 collecting, 3-4
installation and adjustment, 2-16 without autosampler, 3-4
weight and volume
T recalculating, 2-58
tool bar, 4-5
torch
adjustment, 2-12
axial, 1-7
changing injectors, 8-18
cleaning, 8-19
dual-view, 1-7
position, 2-11
radial, 1-8
troubleshooting
autosampler, 8-32
camera icing, 8-29
check standard failures, 8-26, 8-32
chemistry and labware, 8-31
diagnostics, 8-32
high RSDs, 8-30
installation test procedure, 8-32

Index
I-3
Prodigy7 User Manual
Index
I-4
Prodigy7 User Manual

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