Professional Documents
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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:
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
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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
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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
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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
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Prodigy7 User Manual
Table of Contents
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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.
Symboles de sécurité
Ce symbole signale l’existence d’instructions importantes relatives au
produit dans ce manuel.
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.
1-1
Figure 1-1 Prodigy7 schematic
Chapter 1: Introduction
1-2
Prodigy7 User Manual
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.
Chapter 1: Introduction
1-3
Prodigy7 User Manual
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.
Chapter 1: Introduction
1-4
Prodigy7 User Manual
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
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
Chapter 1: Introduction
1-5
Prodigy7 User Manual
1.5.4 Quantitative Full Frame Feature
Chapter 1: Introduction
1-6
Prodigy7 User Manual
1.6 View Configurations
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).
1.6.2 Dual-View
Dual-view systems have a radial mirror mounted to the side of the air knife spacer
(Figure 1-8).
Chapter 1: Introduction
1-7
Prodigy7 User Manual
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.
Chapter 1: Introduction
1-8
Prodigy7 User Manual
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
Chapter 1: Introduction
1-9
Prodigy7 User Manual
Chapter 1: Introduction
1 - 10
Prodigy7 User Manual
Prodigy7 User Manual
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".
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)
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)
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
Pump Platens
Pump Clamps
Rotating Cylinder
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).
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.
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.
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.
NOTE
The Prodigy7’s is designed for demountable “hybrid” torches. Usage of hybrid
torches can significantly reduce argon gas consumption.
Torch Bayonet
Alignment Pin
Vernier Scale
Ball Joint
2. With the torch lock lever loose, rotate the torch bayonet in a counter-clockwise
direction, disengaging the alignment pin (Figure 2-7).
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).
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.
Torch Adjustment
Knob
Torch Bayonet
Ball Joint
2. With the torch lock lever loose, rotate the torch bayonet in a counter-clockwise
direction, disengaging the alignment pin (Figure 2-12).
3. Continue rotating the torch bayonet until the alignment pin is out of the alignment
slot (Figure 2-13).
4. With the alignment pin disengaged from the slot, withdraw the torch bayonet
(Figure 2-14).
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".
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.
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.
Torch
Torch Bayonet
Alignment Pin
Vernier Scale
Ball Joint
2. Use the torch body adjustment knob to change the position of the torch
(Figure 2-18).
NOTE
The torch is typically set to approximately 2 mm from zero measured on the
vernier scale (Figure 2-19).
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.
Torch
RF Load Coil
Dual-View Mirror
Torch Adjustment
Knob
Torch Bayonet
Ball Joint
NOTE
For spray chamber maintenance procedures refer to Section 8.4.8 "Cleaning
the Spray Chamber" in Chapter 8: "Maintenance Procedures".
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.
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.
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.
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.
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.
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.
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.
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.
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
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.
3. The ANALYTICAL PARAMETERS SCREEN should now look similar to the one illustrated
in Figure 2-29.
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".
For information on igniting the plasma manually, refer to Section 5.4.4 "Plasma
Controls".
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.
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.
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).
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.
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.
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.
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.
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".
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.
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.
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.
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.
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).
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.
2.11 Calibration
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.
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.
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".
NOTE
Element concentrations in the Standard Lines Table should reflect the
concentrations present in the standard solution used.
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).
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.
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".
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.
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.
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)
NOTE
Element concentrations in the Standard Lines Table should reflect the
concentrations present in the standard solution used.
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.
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.
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.
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.
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).
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.
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
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
NOTE
Whenever a method is modified, a new copy of the method parameters is
copied to the active analysis chapter.
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.
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)".
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.
2. Click on the RUN STANDARD BUTTON to display the 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.
NOTE
Results for each scan will automatically populate the Navigation Panel when
the Analysis Tab is selected.
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.
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.
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".
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
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".
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.
3.4.1 Integrations
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.
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.
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.
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.
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".
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"
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.
Caution
Running the plasma at higher power levels usually requires that the coolant
flow be increased somewhat to prevent the torch from overheating.
NOTE
Longer residence time can make the plasma appear unstable (flicker),
however, the detection limits will be lower than a more conventional looking
plasma.
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
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.
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.
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.
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:
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.
SEQUENCE provides the ability to create (new), open, save, and print sample
racks as well as import sample sequences (Set Sequence Method).
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.)
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 RUN STAT BUTTON opens the RUN STAT SAMPLE DIALOG. This allows an
automated sequence to be interrupted for an urgent sample.
The DATA AUDIT BUTTON opens the audit trail for review.
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.
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.
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.
Click on the MAINTENANCE BUTTON to display the SCHEDULED MAINTENANCE DIALOG. Items
that require maintenance are indicated by a red “X” (Figure 4-6).
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.
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.
When the SEQUENCE application tab is selected, the NAVIGATION PANEL will display the
anticipated order of:
Standards
Samples
Quality Control Checks
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.
When the system is waiting for the next operation to be entered “Ready” appears on the
STATUS BAR.
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.
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:
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.
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.
Chapter 5: Method
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Prodigy7 User Manual
Figure 5-3 Open method dialog
Information
beneath each
column can be
sorted by clicking
on the heading
Chapter 5: Method
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Prodigy7 User Manual
Figure 5-4 Instrument control screen
NOTE
The supported rack types are defined on the Sequence Tab.
Chapter 5: Method
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Prodigy7 User Manual
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".
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
Chapter 5: Method
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Prodigy7 User Manual
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.
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.
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Prodigy7 User Manual
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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Prodigy7 User Manual
Extinguish
The EXTINGUISH BUTTON shuts down:
RF supply
Torch gases
Gas knife
Pump
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.
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Prodigy7 User Manual
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.
5.4.6 Spectrometer
NOTE
The low purge rate may be adjusted by editing the startup.ini file.
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Prodigy7 User Manual
Figure 5-12 View control
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).
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).
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.
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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Prodigy7 User Manual
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.
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
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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
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.
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.
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Prodigy7 User Manual
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.
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.
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).
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.
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).
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Figure 5-21 The mercury (Hg Ref) lamp 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.
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Figure 5-24 Entering calibration standard concentrations
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
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.
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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).
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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).
Overwriting Replicates
If updates are being run manually, individual replicates can be over-written:
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".
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.
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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.
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.
1. Select the MODIFY QC BUTTON to open the MODIFY QC DIALOG box to make global
modifications.
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.
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
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.
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.
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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.
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Figure 5-39 Example of mismatch shared QC standard error message
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
Last Standard
to be run in the
sequence.
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.
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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).
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
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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.
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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.
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.
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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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
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.
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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).
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6.1.3 Sequence Navigation Panel
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".
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.
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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.
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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.
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).
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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).
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
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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.
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
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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.
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NOTE
The “CP” is necessary because the sample is not the first cup to be run.
Figure 6-17 shows the use of multiple updates assigned as CUP MACROS.
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
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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.
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.
7-1
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.
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
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).
Highlight the
chapter while
viewing the
Results Tab
Select the Rename Button to rename an analysis item (and all replicates)
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Figure 7-5 Sample renaming history - traceable renaming structures
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
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.
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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.
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.
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Figure 7-11 Raw subarray data
Region of
Background Interest (ROI) Background
Correction Correction
Points 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.
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.
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
Probability Report
Detected Peak
Wavelength
Selected
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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"
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
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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".
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.
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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.
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.
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Prodigy7 User Manual
Figure 7-21 Blank subtraction set-up
5) Select
type of
output.
3) Highlight a
sample to be
used as the
blank
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.
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Figure 7-22 Format 1 report example
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Figure 7-24 Format 2 report data
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Prodigy7 User Manual
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.).
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Prodigy7 User Manual
Figure 7-27 Creating a quick report
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.
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Prodigy7 User Manual
2. Select the method to be reported from the 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.
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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Prodigy7 User Manual
Figure 7-31 Report generated using sequence reports
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Prodigy7 User Manual
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.
NOTE
Historical data is never removed.
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Prodigy7 User Manual
7.10 Collecting Echellograms
1. Select the ECHELLE BUTTON to open the RUN FULL FRAME DIALOG (Figure 7-34).
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.
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Prodigy7 User Manual
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:
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.
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.
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.
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
8.3.5 Weekly
1. Daily checks.
2. If more than 500 samples are run in a week, check the pump tubing for wear.
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.
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
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.
The following panels shown in Figure 8-3 are referred to in the maintenance procedures
of this chapter.
LED Nameplate
Power Button
Data Connections
Water Recirculation System
Reservoir
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.
2. Lift approximately 4” to
disengage the panel from the
panel hangers.
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".
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.
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).
Window
Cassette
3. Grasp the cassette grip and pull straight out (Figure 8-8).
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.
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).
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.
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.
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.
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.
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.
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".
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 (80C 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 (80C 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 50C 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.
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).
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).
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.
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.
NOTE
Do not fill the camera water reservoir with anything other than distilled water
or anti-algae solution.
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.
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.
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.
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.
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.
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.
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.
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.
NOTE
Do not run the recirculator without water. Damage may occur to the pump.
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.
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".
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".
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".
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".
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.
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".
Because all labware is a potential source of contamination, thorough cleaning before use
is essential. Refer to Section 8.4.10 "Cleaning Labware".
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".
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.
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.
4. A warning message will appear (Figure 8-17). Click the OK button to reset the
positions.
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:
NOTE
Do not fill the camera water reservoir with anything other than distilled water
or anti-algae solution.
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".
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.
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).
NOTE
Salsa does not recognize changes in the Startup.ini file until it is has been restarted.
8.8.2 Sales
Representatives
Visit our website at www.teledyneleemanlabs.com for a complete list of US and
International Sales Representatives.
NOTE
Refer to the Teledyne Leeman Lab’s website (www.teledyneleemanlabs.com)
for a list of consumables and spare parts for the Prodigy7.
NOTE
Background shifts are by far the most common (and most easily corrected)
spectral interference.
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.
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.
NOTE
Background correction is always applied with the Prodigy7 or Prodigy7
Spectrometer.
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
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.
NOTE
When confronted by a curved background, first attempt selecting a different
emission line.
NOTE
When confronted by a complex background, first attempt selecting a different
emission line.
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
Figure A-7 Spectral scans for pure Zn, mixed Zn and Ni and pure Ni solutions
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:
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.
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.
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).
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.
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.
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).
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).
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.
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.
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.
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.
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.
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:
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).
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.
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).
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.
Note that the standard icon has changed to reflect the Method of Standard Additions (MSA).
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.
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.
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.
1. On the METHOD TAB, select METHOD in the MENU BAR, then IMPORT.
3. Select the method to be imported and click OPEN. The selected method will appear
on the 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.
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.
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.
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.
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.
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.
3. Select the database archive to be opened from the OPEN DATABASE ARCHIVE window.
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).
When the database is open for viewing, Menu Bar selections are inactive (grayed out)
as shown above.
6. Click the OPEN SALSA.MDB BUTTON and the working database will be reloaded.
NOTE
It is recommended that a copy of the archive be made before the archive is
renamed to preserve the original archive.
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.
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:
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.
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.
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.
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:
concentration
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.
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.
IEC corrections to standard and update concentrations are computed via the following
formula:
Where
user input standard/update concentration for element i
or for
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.
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
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:
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 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:
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
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
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 .
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.
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
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.
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".
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.
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.
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.
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
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